Purification of Food-Grade Magnesium Chloride: 2 Experimental
Purification of Food-Grade Magnesium Chloride: 2 Experimental
Purification of Food-Grade Magnesium Chloride: 2 Experimental
1051/ matecconf/20166202004
ICCFE 2016
Abstract: The application of the varying weights of bischofite dissolved in the distilled water was investigated. The
effects of the temperature on the rate of evaporation and the thermal precipitation time on the purity of the crystal
products were fully investigated. Two validation tests including magnifying tests and recycling residue were also
studied. Our results demonstrate that the contents of NaClǃKCl and CaSO4 in the filtrate reached a minimum value
after the pretreatment of 350 g bischofite dissolved in 100 ml distilled water. In the crystal products from the second
evaporating stage of the validation tests, the contents of MgCl2·6H2O, SO4 and NaCl+KCl are 99%, ≤0.1±0.01% and
≤0.8±0.04%, respectively. The content of magnesium chloride in the solution was increased to a greater extent, and
the impurities reduced correspondingly through the dissolution pretreatments of bischofite. This could decrease
energy consumption for the impurity removing stage, evaporation and crystallization process, and thus reduce costs
for the industrial production of food-grade magnesium chloride
1 Introduction
The positive correlation between diet and health has led 2 Experimental
health agencies around the world to control the intake of
certain food components that are thought to promote 2.1 Reagents and instrumentation
some disorders [1].According to the national standards
for food safety (GB2760ˉ1996ˉ2005), the additives The raw ore used in this study included bischofite
used in food production must be food grade additives. (Golmud zhenghai magnesium science and technology
Edible magnesium chloride (MgCl2·6H2O) as additive has development Co., Ltd.)
more widely application in food, salt, mineral water, The instruments used for the analyses included stirrer
medicine and other industries [1-4]. (IKA EUROSTAR 60; Shanghai Chuangyi Science and
The Qinghai salt lakes in the qaidam basin are well education equipment Co., Ltd.), oil bath pan (DF-101S;
known for their huge reserves of potassium chloride (KCl) Gongyi Yuhua Instrument Co., Ltd.), an inductively
and magnesium chloride (MgCl2) in China [5]. In recent coupled plasma–atomic emission spectrometer
years, about 4.5 Mt·a-1 potassium fertilizer has been (ICAP6500 DUO; America Thermo Scientific, USA).
produced with 24-30 Mt·a-1 magnesium chloride as
by-product, and a large amount of magnesium chloride 2.2 Experiments
has been left as the by-product or even waste in salt lakes
of Qinghai [6,7]. This has caused not only the waste of
magnesium resources, but also the environmental 2.2.1 Solution analysis
pollution [8]. The production of food grade magnesium
The solution with a certain amount of bischofite dissolved
chloride used bischofite as raw material is another
in the distilled water was mechanically stirred at a
effective utilization way of magnesium resources of salt
frequency of 300 rpm for 30 min at room temperature (20
lake, in which it is playing an active role.
± 2 °C). Subsequently, the residue and filtrate were
This study investigated the performance of the
separated and weighed. The filtrate was analyzed using
varying weights of bischofite dissolved in the distilled
EDTA volumetric analysis to determine the Mg2+, Cl-
water, determined the optimal ratio relationship between
concentrations, and inductively coupled plasma–atomic
bischofite and distilled water under the condition of the
emission spectrometry (ICP) to determine the Na+, K+,
least amount of impurity in the filtrate, and confirmed the
Ca2+, As, Pb, SO42- and B2O3.
reliability and repeatability of the optimal dissolution
ratio.
2.2.2 Evaporative crystallization
a
Corresponding author: [email protected]
© The Authors, published by EDP Sciences. This is an open access article distributed under the terms of the Creative Commons Attribution
License 4.0 (http://creativecommons.org/licenses/by/4.0/).
MATEC Web of Conferences 62, 02004 (2016) DOI: 10.1051/ matecconf/20166202004
ICCFE 2016
(1) First evaporating stage refrigerated to 40 °C for filtration. Finally, the product of
The filtrate was heated up to110±5 °C for some water crystals MgCl2·6H2O was obtained and analyzed using
loss, and then thermally precipitated for 1h, finally, EDTA volumetric analysis to determine the Mg2+
conducted with thermal filtration. concentrations, and ICP to determine the Na+, K+, Ca2+
(2) Second evaporating stage and SO42-concentrations.
In order to obtain crystals MgCl2·6H2O, this filtrate The process flowsheet for purification of food-grade
from the first evaporating stage was heated up to140 °C magnesium chloride was shown in Figure 1.
again for some water loss, and then the thermal
Bischofite
Residue
2
MATEC Web of Conferences 62, 02004 (2016) DOI: 10.1051/ matecconf/20166202004
ICCFE 2016
Test 1 stages g
Evaporation loss for the first stage 17.32
Crystal for the first stage 12.68
Evaporation loss for the second stage 45.65
Crystal for the second stage 194.79
Test 2 stages g
Evaporation loss for the first stage 16.25
Crystal for the first stage 3.63
Evaporation loss for the second stage 45.34
Crystal for the second stage 203.84
3
MATEC Web of Conferences 62, 02004 (2016) DOI: 10.1051/ matecconf/20166202004
ICCFE 2016
Table 4. Contents of crystal products for the second stage Table 6. Contents of crystal products for the second stage