United States Patent [19]

Jung
[54] METHOD FOR THE CONVERSION OF CRYSTALLINE SILICA RAW MATERIALS INTO AMORPHOUS SILICA
2,931,708 3,853,520 4/1960 12/1974

[11]
[45]

4,040,795
Aug. 9, 1977

Aamot ............................... .. 13/21 X Rau .................................. .. 65/302 X

[76] Inventor:

Lothar Jung, 31 Lurline Drive, Millington, NJ. 07946

Primary Examiner-James H. Tayman, Jr. Attorney, Agent, or FirmLane, Aitken, Dunner &
Ziems

[21] Appl.No.: 568,431 [22] Filed: Apr. 16,1975

Related US. Application Data
[62]
[51]

[5 7]

ABSTRACT

. The apparatus is a rotatable resistance heating furnace

including a rotatable cylindrical body portion having an

interior space in the form of a truncated cone. The base of the truncated cone forms a discharge opening for

Division of Ser. No. 476,220, June 4, 1974, Pat. No.

3,895,174.
Int. 01.2 ........................ .. c031; 5/26; c0312 5/02;

rapid discharge of the amorphous silica. The furnace is

provided with a resistance heating element which ex

C01B 33/12; BOlJ 6/00

[52] U5. c1. ............................. .. 23/293 R; 23/277 R;

23/279; 23/286; 423/335; 423/340; 65/134;

65/347; 65/DIG. 8; 13/21; 13/25
[58] Field of Search ............... .. 23/293 R, 277 R, 279,

23/286; 423/335, 340; 65/134, 347, DIG. 8;

13/21

[56]
2,007,755 7/1935

References Cited
U.S. PATENT DOCUMENTS
Ferguson ............................. .. 65/134

tends into the furnace interior through a top opening. In one embodiment a slidable ?lling tube is provided for charging the furnace during rotation thereof. The pro cess utilizes the above-described apparatus and involves heating the crystalline silica to a temperature suf?cient to convert it to the amorphous state, evacuating the furnace during the conversion to draw off by-product gases, and rotating 'the furnace to a speed suf?cient to bring about a separation between the silica charge and the resistance heating element.

4 Claims, 9 Drawing Figures

U.S. Patent

Aug. 9, 1977

Sheet 1 of4

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FIG. 20.

Fl6.3a.

gil/I'!

 U.S. Patent

Aug. 9, 1977

I Sheet 2 of4

4,040,795

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US. Patent

Aug. 9, 1977

Sheet 3 of4

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VACUUM PUMP
p

U.s. Patent Aug.9,1977

>Sheet4of4
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I 4,040,795

2
.

METHOD FOR THE CONVERSION OF CRYSTALLINE SILICA RAW MATERIALS INTO

AMORPHOUS SILICA

for many end use applications, a physical separation of the contaminated products from the uncontaminated is
necessary.

~ CROSS REFERENCE TO RELATED

APPLICATION '

This is a division of US. application Ser. No. 476,220 ?led June 4, 1974 for METHOD AND APPARA TUS FOR CONVERSION OF CRYSTALLINE SIL
ICA RAW MATERIALS INTO AMORPHOUS SIL
ICA, now issued as US. Pat. No. 3,895,174.

The prior art apparatus and process employing silica sand as a refractory material, surrounding the melt, encounter further dif?culties. The prior art technique for insulating the melt results in the adherence of un fused silica sand and layers of cristobalite to the con verted product. The skin must be removed prior to any
further processing since it represents an unwanted con

taminating material. Furthermore, the thermal conduc tivity, particularly the radiation conductivity of fused
- silica and crystalline silica, is comparatively high at

BACKGROUND OF THE INVENTION

The present invention relates to a method and appara tus for the conversion of crystalline silica into amor

temperatures near the melting point of cristobalite, lead ing to signi?cant losses of thermal energy.
In devices wherein the resistance elements run

phous silica.
Amorphous silica is widely used to form, usually by slip-casting methods, various refractory bodies and articles for hightemperature applications in the chemi
cal and metalurgical industries. Because the coefficient of linear expansion of cristobalite differs signi?cantly from that of amorphous silica, the presence of signi?

through the furnace, with terminal ends located at each end of the furance housing, considerable thermal losses
were found to occur because of the inevitable ?ow of
20 heat from the resistance heating element or electrode

into the connectors. In addition to such thermal losses,

losses of electrical power were encountered as a result

of the increase of the reactance of the furnace circuit with the introduction of an appreciable self-inductance cant amounts of, cristobalite in the ?nished- refractory products will render those products unsuitable for use 25 as a result of looping the power feed lines. in high temperature applications. Signi?cant amounts of Rotatable resistance furnaces, such as that disclosed cristobalite within the articles will cause them to crack in US. Pat. No. 2,936,505 issued to Witucki et al, have

apart when subjected to high temperatures.

It is well known in the art that any and all crystalline forms of silica are converted into the amorphous state when heated above 1728 C, the melting point of cristo

been employed in-other applications. However, such apparatus is unsuitable for the production of amorphous silica because it does not provide for rapid discharge and quenching of the hot product, which rapid dis
charging is necessary to minimize cristobalite formation

balite. The prior art has commonly employed electrical arc furnaces to produce the thermal energy required for

during cooling of the product.

SUMMARY OF THE INVENTION
In accordance with the present invention, a novel

the fusion and conversion of the crystalline silica. How

ever, the electrical arc furnace is known to produce

temperatures much higher than those required for fu

sion of silica and therefore consumes more energy than

required for conversion. In addition to the thermal

losses associated with the electric arc processes, super

technique for the production of amorphous silica is provided which avoids all the above-noted problems and which produces amorphous silica of a high degree
toxic by-products produced and further provision for collecting such gaseous by-products.
The apparatus of the present invention includes a

heating of the silica charge results in a high rate of 40 of purity with a minimum amount of power consump tion and with provision for controlling the amount of consumption of the carbon or graphite electrodes and a

loss of signi?cant amounts of silica through vaporiza

tion. Another drawback of the prior art are melting process resides in the production of gaseous by-pro

ducts which are formed within the furnace as a function 45 generally cylindrical furnace housing mounted for rota tion about a central axis. The furnace housing de?nes an of the temperature and degree of super-heat of the car

bon electrodes and silica charge. The unwanted by-pro duct reactions include those resulting in the formation
of silicon carbide and the very toxic gas carbon monox

interior cavity having the shape of a truncated cone

with a bottom opening at the base of the cone for dis

charging the contents of the furnace. Means is provided

ide. The prior art apparatus and process allow varying

amounts of carbon monoxide to escape from the fur nace, thus presenting a safety hazard and an environ

for introducing particulate crystalline silica into the

interior of the furnace and for insertion of a resistance

mental problem. Silicon carbide also forms in a gaseous phase reaction but tends to crystallize on the carbon or graphite electrodes, if the electrodes are freely sus pended above the melt. Still another drawback of the prior art technology results from direct contact between the hot fused silica and the heated carbon or graphite electrodes. Such direct contact results in the formation of silicon carbide which tends to disassociate at the surface of the elec trodes resulting in the formation of silicon vapor and carbon monoxide gas. The direct contact between the hot'fused silica and the electrodes also results in con

heating element. A cover plate is provided for closing and sealing the discharge opening and is designed to allow rapid discharge of the furnace contents.
In one embodiment the furnace is provided with a silica charging means in the form of a slidably mounted tube which may be inserted to the bottom of the furnace

and gradually withdrawn during the ?lling operation so

that a layer of crystalline silica may be evenly distrib uted over the vertical wall of the rotating furnace. In a preferred embodiment, the apparatus of the pre sent invention is additionally provided with means for

evacuating the furnace interior.

In another embodiment a portion of the furnace hous

tamination of the fused silica product by carbon, silicon

carbide, or even silicon. The contamination of the fused silica tends to turn its color from white into gray, brown or black. Since the contaminated silica is not acceptable

ing is provided with a jacket adapted for circulation of

a heat exchange medium which may be utilized to re cover a portion of the heat generated within the fur
nace. ~

4,040,795

The process of the present invention utilizes the

above-described apparatus and involves charging the furnace with the particulate crystalline silica and heat
ing the silica charge to a temperature suf?cient to melt and convert the silica to the amorphous state. The fur nace interior is evacuated during the conversion process

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a perspective view of one type of electrode, in the form of a split tube, suitable for use in the present

invention;
FIG. la is a partial elevation, in cross-section, of the
lower end of the electrode or return resistance element shown in FIG. 1; FIG. 2 is a perspective view of another type of return resistance element suitable for use in the present inven
tion;

to draw-off gaseous by-products and thereby prevent

contamination of the silica product. During the conver
sion process the furnace is rotated at a speed suf?cient

to cause the silica to be forced against the furnace wall,

spaced from the carbon electrode. After conversion, the

silica product is discharged through the bottom opening

provided in the furnace.
In a preferred embodiment, the converted silica is cooled sufficiently within the furnace so that it will retain its shape upon discharge but is not allowed to cool to temperatures within the range where the rate of formation of cristobalite is the greatest. Start-up of the furnace may be conveniently accom

plished by following either of two procedures. In a ?rst method the silica charge is heated to its melting point to
induce volumetric contraction which results in the silica

FIG. 2a is a partial elevation of the lower end of the electrode as shown in FIG. 2; FIG. 3 is a perspective view of yet another form of electrode suitable for use in the present invention; FIG. 3a is a partial elevation, in cross-section, of the electrode shown in FIG. 3; FIG. 4 is an elevational view, in cross-section, of the apparatus of the present invention showing a silica melt contained therein and crystalline silica feed stored in a

feed hopper;
FIG. 6 is an elevational view, in cross-section, of

another embodiment of the apparatus of the present this first method rotation of the furnace body is started invention having a slidable ?lling tube and depicts the only after such separation has been affected. In a second 25 procedure for filling the furnace using such means; and method, rotation of the furnace body is commenced FIG. 5 is an elevational view of the apparatus of the prior to the ?lling operation and filling is accomplished present invention including means for collecting and through an axially movable ?lling tube which is initially quenching the amorphous silica after discharge from inserted to a point near the bottom of the furnace and the furnace. 30
gradually withdrawn during ?lling so as to deposit a
the furnace. -

charge separating from the central carbon electrode. In

layer of silica along the rotating vertical interior wall of

Accordingly, it is an object of the present invention to

DESCRIPTION OF THE PREFERRED

produce an amorphous silica product containing re vention is illustrated in FIG. 4. In FIG. 4 is shown a 35 duced amounts of cristobalite. vertically-mounted rotatable cylindrical furnace hous It is a further purpose of the present invention to ing 15 supported by a stationary frame which includes a
provide an apparatus for the production of amorphous silica containing minimal amounts of cristobalite.

EMBODIMENTS One embodiment of the apparatus of the present in

plurality of vertical support legs 14. Rotatable support

of the furnace housing 15 is provided by means of a minimize and remove gaseous by-products resulting 40 roller thrust bearing 16 which is mounted between cir cumferential mounting collars 17 and 18. Mounting from the conversion of crystalline silica to amorphous collar 17 is integral with the support frame and remains silica in a furnace containing a carbon electrode. stationary. Mounting collar 18 is rigidly affixed around It is yet another object of the present invention to the circumference of the rotatable cylindrical furnace provide a technique and apparatus for the conversion of crystalline silica to amorphous silica with a minimum 45 housing 15. The bottom of furnace 15 is closed by cover means or amount of energy consumption. hinge plate 19 which is held in the closed position by It is still another object of the present invention to locking means 20. Mounting means or hinge member 21 improve the working environment by removal and provides for movement of the cover means 19 between containment of the toxic gaseous by-products asso 50 open and closed positions. ciated with such a conversion process. . The top of the cylindrical housing 15 is closed by an Yet another object of the present invention is to pro
It is a further objective of the present invention to
vide for conversion of the silica charge in such a manner as to avoid a large temperature gradient across the

upper cover means or stationary plate 26. Stationary

plate 26 is supported by roller bearing 27 which is in

turn rigidly af?xed to ?ange 28 which represents the
55 upper terminal surface of the furnace housing 15. The

thickness of the charge and thereby minimize wasteful

superheat.
Another object is to prolong the life of the carbon or graphite electrodes used in such a process and appara
tus.

Still another object of the present invention is to pro vide means whereby the silica charge can be maintained

top plate 26 is a hollow construction to allow for circu lation of a heat exchange medium which enters at port 29 and exits at a second port 30. Circulation of a heat exchange medium through plate 26 allows at least a portion of the heat from the furnace to be conserved for
reuse.

physically separated from the carbon or graphite elec

trodes during conversion to the amorphous state and

thereby avoid electrode wear and contamination of the

silica product. '

The top plate 26 is provided with means for charging particulate crystalline silica into the furnace interior.
The charging means includes an openings 31 in the top closure .26, a feed hopper 32 for storing the raw material and a shut-off valve 33 which may be operated to pre vent further ?lling after fusion of the initial charge. Fusion of the initial charge results in a shrinkage of that

Other objects and further scope of applicability of the 65 present invention will become apparent from a reading of the detailed description to follow, taken in conjunc tion with the accompanying drawings.

5
diminishes with melting.

4,040,795
' i

mass as the void space between the particulate material

The resistance heating element should be suf?ciently

large to provide enough of a radiating surface area to

In an alternate embodiment, depicted in FIG. 6, means for ?lling during rotation of the furnacehousing is provided. Filling means of the embodiment shown in FIG. 6 includes a water-jacketed ?lling tube 66 inte grally connected to a feed hopper 92. The ?lling tube 66 is slideably mounted within the top plate member 54. Cooling water enters through port 62 and exits through port 63 to cool and protect the ?lling tube during opera tion of the furnace. The ?lling tube 66 is pro?led or cut
away at its lower end 64 to guide the discharge of the
silica raw material in a preferred direction. A cover

avoid large temperature gradients within the silica charge. Likewise, thinner layers of silica, forced against the furnace linear 41 by centrifugal force, will result in
lower temperature gradients within the silica mass. Large temperature gradients are to be avoided for rea

sons previously mentioned, e.g. generation of gaseous

by-products and losses of electrode material and silica. A tube 41 is mounted within the furnace housing 15 and is provided with a tappered inner surface which
de?nes an interior space 34 having a con?guration ap
' proximating a truncated cone. The conical con?gura~

member 61 is rotatably mounted on the top of the sta

tionary plate 64 to seal off the port provided for the ?lling tube after removal of the ?lling tube upon com

tion of the space de?ned by the inner surface of the tube or inner wall member 41 is such that the diameter of the

pletion of the ?lling operation. A suitable insulating

body 67 is provided on the interior surface of cover member 61 to protect cover 61 from the furnace heat

interior increases gradually toward the bottom opening of the furnace and thus provides for easy and quick
separation of the melt from the furnace lining of tube 41

by gravity discharge. The slope of the inner surface

20 should be at least 1 to allow gravity discharge. The when in the closed position. only requirement for the material forming tube 41 is that Returning to FIG. 4, a central opening in the top plate it be capable of withstanding the temperature required 26 is provided for insertion of the electrode or return for completion of the fusion of silica and of suf?cient resistance element 36. The return element 36 is secured chemical inertness to preclude contamination or reac within the central opening of the top plate 26 by means tion with the melt. Tube 41 is vertically supported be of a threaded connector 94, a threaded retainer or bolt tween annular ring composite bodies 42 and 43. 96 and bushing members 35, 37, and 98. Bushing mem The outer surface of tube 41, in conjunction with ber 35 is an electrical connector which surrounds the outer furnace wall 15a, de?ne an annular space ?lled by upper end portion of the electrode 36 and is insulated

from the metallic plate member 26 by means of the bushing or annular insulating spacer 37. Electrical con nector 35 is likewise insulated from the threaded con nector 94 by means of a second bushing or insulating
member 98. The electrical connector 35 is also a hollow

an insulating material 44. The annular members 42 and

43, and the composite 44, which ?lls the space between
the interior-exterior walls of the furnace housing are

fabricated from the materials having high insulating

values. Suitable insulating materials include carbon loose grains or felt, graphite loose grains or felt and zirconium loose grains or felt. Such insulating materials are superior to the unfused silica employed in the prior art devices. The interior of the furnace is provided with

construction to permit circulation of cooling water which enters and exits through ports 100 and 102. Ter
minals 39 and 40, mounted on the electrical connector '35 and threaded connector 94, respectively, are con nected to a power source (not shown) which provides

further insulation in the form of disc members 45 and 46 fabricated of carbon, graphite or zirconium felt. Insulat the electrical energy necessary to effect heating and ing disc 45 serves to insulate and product bottom plate fusion of the silica raw material. or cover 19. Likewise, insulating disc 46 serves to insu The return resistance element 36 shown in FIG. 4 late and protect the top plate or cover 26. corresponds to the design of the element shown in FIG. With the furnace insulated in this manner, a nearly 2 and FIG. 2a. However, the element shown in FIG. 1 complete fusion of the entire silica charge can be ac and FIG. 1a or that shown in FIG. 3 and FIG. 3a could also be employed in the apparatus depicted in FIG. 4. 45 complished leaving only minute qualities or unfused silica 47 and cristobalite 48. Such small quantities do not The return resistance element of FIG. 1 is in the form of require any special treatment for removal prior to fur a tube split in two down the length of a major portion of ther processing of the product. its vertical axis. The electrical power is connected to To prevent direct contact between the resistor and terminal points 8 and 9. The design of FIG. 1 may be the melt, the furnace is rotated about its vertical axis at modi?ed for use in certain applications by varying the

electrically conducting cross-section of the element in

order to achieve a desirable temperature pro?le, such as

a speed suf?ciently fast to generate enough centrifugal force to hold the melt in place, against the lining or tube
41 and away from the resistor. The drive means in cludes gear means 49, reduction gears 50 and an electric motor 51.

by means of providing a tappered end portion 10. Sur face 11 shown in FIG. 1a, is declined outwardly from the interior of the electrode in order to prevent the deposition of furnace charge material when installed in
a vertical position. With reference to FIG. 2 and FIG.

The apparatus of the present invention further in

cludes means to reduce and control emission of the

2a, the wall portion 8 may be electrically connected to terminal 39 of the furnace and post 9 electrically con nected to terminal 40. The element shown in FIG. 3 is in the form of a solid

toxic by-product gases and thereby reduce pollution

associated with the process. To this end, sealing means

have been provided to render the entire furnace housing

vacuum tight. Stationary vacuum seals 52 and 54 and a

body being centrally split along a major portion of its

vertical axis. Terminal end portion 8b may be electri cally connected to either of terminals 39 and '40 of the furnace with terminal 9b being connected to the other terminal. Surface 11b, shown in FIG. 3a, is also pro vided with an outwardly declining slope to avoid accu
mulation of the material being treated. '

rotary vacuum seal 55 between the stationary top plate 26 and the rotatable furnace housing 15 have been pro

65

vided. Additionally, the furnace is connected to a suit able vacuum pump 100 (see FIG. 5) which communi cates with the interior of the furnace via port 58. In this
manner all gases escaping from the furnace can be con

trolled at the exhaust port of the vacuum pump and

4,040,795

routed to treatment means, such as gas scrubber and/or condenser means, rather than being released into the environment in which the furnace is located.

,The temperature within the furnace during the con

version process is maintained within a range from about

1728 C to about 2000 C for a period of time suf?cient

to effect conversion of the crystalline raw material to the amorphous state. For reasons of economics and ef?cient power utilization, a range of from about 1728

Referring now to FIG. 5, the furnace is shown

mounted above the ?oorlevel 72 on a plateform sup

ported by vertically standing legs 71 and ?oor 70 above

which the furnace arrangement as described in FIG. 4 is

located. The furnace housing 15 penetrates the ?oor 70 as to permit gravity discharge of the melt. During oper
ation the bottom plate or closure means 19 is in the

to about 1900" C is preferred. A vacuum, preferably established before start of the conversion process, is maintained throughout conver
sion in order to increase the insulation capacity of the

closed position and locked in place by locking means 20.

A rotating union 22 is attached to the center of the

bottom plate 19, with the stationary portion of the union

23 linked to a hydraulic operating means 73 by rod member 24. The hydraulic means 73, which is linked to the bottom closure by rod 24, operates to open the bottom closure means or plate 19 to discharge the silica product at the appropriate time. The opposite end of the ?uid operated cylinder 73, is attached to the vertical part of the platform 71 by way of a clevis 76. The cylin~ der 73 is equipped with ?uid ports 74 and 75 to provide
for a two way stroke, which will open and close the

furnace and to draw off the gaseous by-products. Any degree of vacuum suf?cient to accomplish these objec tives is satisfactory. These objectives may be conve
niently obtained with a vacuum within the range of

from about 1 torr to about 300 torrs. Higher degrees of

vacuum, i.e. less than 1 torr, tend to produce an unac

ceptable degree of volatilization of the carbon electrode and silica charge. Evacuation of the furnace during
conversion results in a product essentially free from gaseous inclusions.

The speed of rotation of the furnace during the con

version process will vary in accordance with the inner

diameter of the furnace used. The only criteron for the speed of rotation is that it-must be suf?cient to maintain Directly underneath the furnace 15 is provided a 25 the silica contents of the furnace removed from contact cooler or heat exchanger tank 77 for receiving and with the electrode. The speed of rotation of the furnace cooling the melt upon discharge from the furnace. Tank may be decreased during the conversion process be 77 rests on two side arms located in two trunnions 79. A super structure 90 is mounted in a trolley through inter cause, as the silica charge melts, the diameter of the connected shock absorbers 81. The trolley is equipped 30 void space increases and the centrifugal force at the inner surface of the melt correspondingly increases. The with suitable wheels 82 and with break shoes 83. On the rotation of the furnace forces the silica into a cylindri top of tank 77 is a plate 78 mounted to pivot about pin cally shaped body, which stays clear of the stationary 85 between open and closed positions. The purpose of the tank 77 is to cool the hot fused silica melt to mini resistance element, thus avoiding friction and abrasion mize the time of transition through the temperature 35 of the element. range wherein the growth rate of cristobalite is greatest, In one embodiment, rotation of the furnace is started
i.e 1,200 -1300 C. '

bottom plate as required.

In order to recover a major fraction of the thermal energy contained in the melt, the tank 77 and cover plate 78 are made of a double wall construction to allow

for the introduction of a heat exchange ?uid which enters the tank 77 through port 86 and exits the tank via port 87. From port 87 the ?uid passes into top plate 78 by way of a ?exible hose connection 88 and ?nally, the heated ?uid is removed from the entire apparatus 45 to a point near the bottom of the furnace. The ?lling through port 89 for further utilization. tube is then gradually withdrawn from the rotating In operation, the bottom plate 19 is closed and locked furnace, the speed of withdrawal being regulated to in the manner previously described. The electrical deposit a uniform layer of raw silica along the interior power is switched on and the furnace is preheated. The vertical surface of the furnace. Since the ?lling of the

only after the silica charge has been heated suf?ciently to effect melting and subsequent separation from the centrally located electrode. In another embodiment, charging of the furnace is accomplished by means of the apparatus depicted in FIG. 6, which employs the water cooled ?lling tube or pipe 66. In this second ?lling procedure, rotation of the furnace is started prior to ?lling and the ?lling tube or pipe 66 is initially inserted

furnace is then charged with particulate crystalline silica from the pre-charged hopper 32. With grate or
valve 33 open, the raw silica falls freely into the interior

50

furnace proceeds with considerable speed, it is feasible

to start up the resistor or electrode while the ?lling

of the furnace, ?lling it to the top. When ?lled, the ?ow

of silica raw materials ceases automatically and the gate is automatically shut. In this manner, only a minute quantity of raw silica within the ?lling pipe 31 will enter the furnace upon fusion and shrinkage of the initial charge. Optionally, the furnace may be vibrated or

operation is in progress. For furnaces of larger inner diameters, i.e. 4 vfeetvand larger, the volume of the
charge of silica raw material cannot be increased in

proportion to the large interior space provided by the furnace without creation of intolerably large tempera
ture gradients across the wall of the fused silica melt. In

such large furnaces, the ?rst mentioned procedure for

tapped in order to achieve the maximum ?lling density.

charging the furnace is inappropriate. The second men It is now believed, contrary to previous reports and 60 tioned ?lling procedure employing the movable ?lling ?ndings, that the nascent melt does not separate from tube serves to limit the vertical layer or charge of raw the resistance element due to the in?uence of gaseous material to a thickness smaller than the distance be: pressure, but rather as a result of forces produced by the tween the furnace liner 41 and the electrode 36. ~ increase of volume in the annular section of the melt in ' The time required for conversion to the amorphous which the silica changes into cristobalite. This effect 65 state will vary in accordance with the nature of the causes the melt to continuously increase its inner diame~ heating element and the volume of the furnace. Accord ter while the thickness of the layer of the fused silica ingly, a suitabletime must be determined experimen-. increases vaccordingly. 1 tally in conjunction with the use of a given apparatus.

4,040,795
After heating at a temperature and for a time suffi
cient to convert the entire silica mass to amorphous
ply. _ ~

10.
;

200 volts and 2,500 ampheres is used as the power sup

state, power to the electrode or heating element 36 is discontinued to allow the furnace to gradually cool.

During this initial cooling period rotation of the~ furnace

is continued to prevent the silica melt from collapsing and coming into contact with the carbon electrode. The charge is retained in the rotating furnace until cooled to a temperature within the range of l,3001,400 C. vAfter cooling to a temperature within therange of 10

Because the thermal inertia of the above-described electrode is small, fused temperatures are reached in less than ten minutes after turning on the power. Thirty minutes after turning on the power supply, themelt is

sufficiently separated fromlthe resistance element and

rotation of the furnace is started. The time required to

complete fusion of the silica charge is approximately 3

hours (being dependent on the size of the charge, the

l,300-l,400 C, the melt is ready to be discharged for

more rapid cooling. At a temperature within the range of 1,3001,400 C the silica mass becomes suf?ciently rigid to retain its shape so that it will not collapse and come in contact with the carbon electrode but still has
not cooled to a temperature range wherein the maxi

nature'of the insulation, and the heat input). The furnace employed in this experiment is a nominal
- three foot diameter furnace having anginterior I30

inches in length and gradually sloped from a 27 inch ID. at the top to a 30 inch I.D. bottom opening.
At the outset of the run the pressure in the interior of

mum

growth

rate

of cristobalite

occurs,

i.e.

the furnace is reduced to approximately 1 torr. During

the course of the three hour conversion process, the

1,200-1,300 C. At this point in time, the rotation of the

furnace may be stopped and the vacuum pump may also be turned off. The discharge of the hot silica mass must be as rapid as possible to minimize the formation of cristobalite. Gravity is a preferred means for discharge.

pressure gradually increases to approximately 300 torrs

due to the increased vapor pressure of the contents of thefurnace. The speed of rotation of the furnace is initially 220 rpm and is gradually reduced over the span
of the three hour run to 150 rpm. Given the mass of the

Gravity discharge is easily effected using the apparatus

and vertical arrangement depicted in FIG. 5. The coni cal shape of the interior of the furnace, previously de scribed, aids in obtaining a rapid release of the silica
mass from the furnace.

silica, furnace dimensions, and power input employed

here, the temperature at the interior surface of the melt is approximately 1,880" C and the temperature at the outer surface of the melt, adjacent to the interior wall of the furnace liner, is approximately l,730 C. At the end of the three hour period the motor rotating

After the rotation of the furnace has ceased, the fur nace is oriented in a position which permits the opening of the bottom plate 19 by means of actuation of the 30 the furnace is shut down and the vacuum pump turned off. The silica charge is then allowed to cool in the hydraulic means 73, following the release of the lock 20. closed furnace to a temperature of approximately 1350 The melt will leave the furnace under the influence of C. The silica charge is then instantly dropped into the its own weight in a fraction of a second and drop into empty cooler. Water at room temperature is circulated tank 77. FIG. 5 shows the solidified silica 84 within tank 77. Immediately thereafter, a reverse stroke of the cylin 35 through the jacket of the cooler. der closes the bottom plate 19 again, thus retaining an Upon examination of the fused material, it will be found that there is virtually no contamination with appreciable amount of thermal energy within the fur regard to residual alpha-quartz cristobalite, graphite or nace. Likewise, the top plate 78 of the tank 77 is closed. The batch type operation described above has been silica. Furthermore, it will be found that the density of found to be more ef?cient with regard to conserving 40 the fused silica will be approximately 2.2 grams/cc (lower quality raw materials will result in a correspond energy than prior art continuous processes. Continuous ing decrease in the density of the product). As a result processes are rather limited in this respect because of of the use of vacuum, a good portion of the silica prod the inevitable flow of heat through the mass of fused uct is completely transparent and therefore comparable silica which is continuously extruded from the furnace. to high purity fused silicas which are usually prepared It will be appreciated from the foregoing that the in much smaller batches and at much smaller rates per furnace heat recovery means of the present invention includes both hollow top plate 26 and hollow bushing hour. The results outlined in the foregoing example corre or connector 35. The heat recovery means associated spond to a production rate of approximately 1200 with quench tank includes both the hollow wall con 50 pounds per hour, including the time required for load struction of the tank proper and the lid 78.

ing and discharging of the furnace. This production rate It should be obvious from the foregoing description is higher than those reported for continuous melters that the loading and unloading of the furnace is accom of corresponding size. It is feasible to obtain even higher plished in a simple and inexpensive manner, exclusive of production rates since much larger elements and larger sophisticated mechanical means. The following example is provided to further de 55 furnaces than that described above are technically feasi ble. The consumption of electrical energy in the exam scribe a preferred embodiment of the present invention.
EXAMPLE with the power consumption rates for prior art batch and continuous melters, i.e. approximately 0.4 kilowatt Two tons of silica sand having a grain size of minus 30 mesh is introduced into a furnace of a design corre 60 hours per pound of fused silica. As can be appreciated from the foregoing, the opera sponding to that of FIG. 4 and FIG. 5. The time re tion described above may be considered quasi-continu quired to load the furnace by gravity feed is less than 15 ous since the time for loading and discharging the minutes. The furnace is equipped with a resistance ele furnace is short as compared to the fusion time. The ment having an outer diameter of 5.25 inches, a length output obtained in the above described manner when of 108 inches, and manufactured from standard graphite projected into a cycle time for complete runs indicates stock in accordance with the design of FIG. 2. The a higher hourly rate than for a so-called continuous resistance of this heating element is approximately 0.08 process. In this connection it should be noted that the ohms. A single phase transformer providing 500 kVA at

ple described above is favorably low in comparison

11

4,040,795

12

so-called continuous melter is actually quasi-continuous

since such melters do not allow for the continuous re moval of the melt.

?ning an interior of a con?guration approximating a truncated cone, the base of the cone de?ning a bottom

discharge opening, the improvement comprising:

cooling the amorphous silica mass within the furnace to a temperature within the range of 1,300-1,400 C to rigidify the mass and then rapidly discharging said cooled rigid mass through the furnace bottom

The invention may be embodied in other speci?c forms without departing from the spirit or essential characteristics thereof. The present embodiments are
therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being

by gravity to permit more rapid cooling.

indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the

2. The process of claim 1 wherein the furnace is ?lled with particulate silica and then heated to a temperature within the range of from about 1,728 to about 1,900" C for a period of time suf?cient to bring about a separation claims are therefore intended to be embraced therein. of the silica mass from the resistance heating element What is claimed: and wherein rotation is started at the end of said period 1. In a process for the conversion of particulate crys talline silica into an amorphous silica mass by charging 5 of time. 3. The process of claim 1 utilizing a furnace addition a furnace with the particulate crystalline silica and heat ally provided with an axially movable ?lling tube and ing the charge to a temperature within the range of wherein rotation of the furnace is started prior to charg from about 1,728 to about 1,900 C for a period of time
.

suf?cient to melt and convert the silica to the amor

phous state while evacuating the furnace to draw off gaseous by-products and rotating the furnace at a speed

20

ing the particulate silica through said ?lling tube, said process further comprising withdrawing the ?lling tube
from the furnace during charging so as to deposit the

suf?cient to cause the silica charge to be forced against furnace. the furnace wall, wherein the furnace is a vertically 4. The process of claim 1 wherein the amorphous mounted rotatable electric furnace provided with a a cooling tank. central internal resistance heating element and with a 25 silica is discharged into i i i i

particulate silica along the length of the interior of the

cylindrical body portion having an interior surface de

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50

55

65