CN106044807B - The preparation method of edible magnesium chloride - Google Patents
The preparation method of edible magnesium chloride Download PDFInfo
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- CN106044807B CN106044807B CN201610261843.6A CN201610261843A CN106044807B CN 106044807 B CN106044807 B CN 106044807B CN 201610261843 A CN201610261843 A CN 201610261843A CN 106044807 B CN106044807 B CN 106044807B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- Engineering & Computer Science (AREA)
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- Coloring Foods And Improving Nutritive Qualities (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of preparation method of edible magnesium chloride, including step：A, the first mother liquor is obtained；First mother liquor includes Na+、K+、Mg2+、Cl‑、SO4 2‑、H2O, wherein, Na+Mass percent be 0.1%~0.2%, K+Mass percent be 0.05%~0.1%, Mg2+Mass percent be 8.4%~9.5%, Cl‑Mass percent be 24.5%~28%, SO4 2‑Mass percent be 0.05%~0.1%, remaining is the H2O；B, the first mother liquor is subjected to flush distillation at 100 DEG C~110 DEG C and carries out heat filtering, using gained filtrate as the second mother liquor；In flush distillation, the water reduction rate in the first mother liquor is 4.1%~16.3%；C, the second mother liquor is subjected to double evaporation-cooling, is cooled to less than 90 DEG C and carries out separation of solid and liquid, gained solid phase is edible magnesium chloride.It is simple according to the preparation method of the edible magnesium chloride of the present invention；It it also avoid simultaneously using the problem of mother liquor entrainment is exceeded caused by single evaporation.
Description
Technical field
The invention belongs to Food Chemistry technical field, specifically, is related to a kind of preparation method of edible magnesium chloride.
Background technology
As a kind of additive, edible magnesium chloride (MgCl2·6H2O) have in industries such as food, salt, mineral water, medicine
There is relatively broad application.Due to China's edible magnesium chloride produce it is later, for many years, the application of product food service industry at home
It is less, and its related specifications is constantly in space state.On December 11st, 2003, China is starting《Edible magnesium chloride》
(QB2604-2003) professional standard, and edible magnesium chloride is defined as food stabilizer and coagulator, and in 2 months 2011 21
Day implements food additives magnesium chloride national standard-" national food safety standard, food additives magnesium chloride GB25584-
2010”.Simultaneously《National food safety standard food additives use sanitary standard》(GB2760-1996-2005) also clearly advise
It is fixed：Additive used in food production must be food-grade.China provides, calcium ion content in edible magnesium chloride
(being calculated in mass percent) need to be no more than 0.10%, and sulphates content is (with SO4 2-Mass percentage) need to be no more than
0.40%.
Bittern of the seawater through acquisition of evaporating brine is generally currently used as the raw material for preparing food-grade magnesium chloride, however, salt lake halogen
Equally contain abundant magnesium resource in water, also can be as another important preparing raw material of food-grade magnesium chloride.Qinghai is China
Most important salt lake Distribution Area, the wherein Cha Er Han Salt Lake in the Caidamu Basin are the potash fertilizer bases that China is developing, with
The continuous expansion of KCl production scale, the bischofite of its by-product is continuously increased.Current annual by-product bischofite is about
24000000 tons~30,000,000 tons, in these by-product bischofites, as magnesium chloride primary product often be only sale 300,000 tons~
500000 tons, substantial amounts of bischofite is not utilized, and this not only causes the waste of magnesium resource, and to salt lake ecological environment
Damage, so that forming " magnesium evil ".At the same time, in the preparation technology of current edible magnesium chloride, in evaporation stage
When evaporation final temperature need to strictly be controlled, otherwise impurity will a large amount of separate out and cause last obtained edible magnesium chloride production
Contaminant overstandard in product.Therefore, on the one hand, need to utilize above-mentioned substantial amounts of magnesium resource；On the other hand, existing preparation technology
Control condition is harsh, not easy to operate, and impurity content is easily exceeded in product.For these reasons, it is necessary to which exploitation one kind is with salt
Lake by-product bischofite is the method for raw material and easily prepared edible magnesium chloride.
The content of the invention
, should the invention provides a kind of preparation method of edible magnesium chloride to solve the above-mentioned problems of the prior art
Preparation method can obtain edible magnesium chloride using twice evaporation technique, and in evaporation process, evaporation terminal point control condition is wide
Pine, it is easily prepared.
In order to reach foregoing invention purpose, present invention employs following technical scheme：
A kind of preparation method of edible magnesium chloride, including step：A, the first mother liquor is obtained；Wherein, the first mother liquor bag
Include Na+、K+、Mg2+、Cl-、SO4 2-、H2O, in first mother liquor, the Na+Mass percent be 0.1%~0.2%,
The K+Mass percent be 0.05%~0.1%, the Mg2+Mass percent be 8.4%~9.5%, the Cl-'s
Mass percent is 24.5%~28%, the SO4 2-Mass percent be 0.05%~0.1%, remaining is the H2O；B、
First mother liquor is subjected to flush distillation at 100 DEG C~110 DEG C and carries out heat filtering, gained filtrate is the second mother liquor；Its
In, in the flush distillation, the water reduction rate in first mother liquor is 4.1%~16.3%；C, it is female by described second
Liquid carries out double evaporation-cooling, is cooled to less than 90 DEG C and carries out separation of solid and liquid, gained solid phase is edible magnesium chloride.
Further, in the step A, the preparation method of first mother liquor specifically includes：Gu Kuang is placed in dissolving
In water and it is stirred, carries out separation of solid and liquid again after reaching crystallization of the dissolution and precipitation balance, gained liquid phase is first mother liquor；It is described
Gu Kuang and dissolving water ratio are not less than 3g:1mL；Wherein, the Gu Kuang includes magnesium chloride, potassium chloride, sodium chloride, calcium sulfate,
The potassium chloride, sodium chloride, the mass percent sum of calcium sulfate are no more than 4.6%, and remaining is the magnesium chloride.
Further, the Gu Kuang and dissolving water ratio are 3g~5g:1mL.
Further, the Gu Kuang also includes impurity；Wherein, the mass percent of the impurity is no more than 0.6%.
Further, the Gu Kuang is salt lake by-product bischofite.
Further, in the step C, second mother liquor is subjected to double evaporation-cooling, is in chlorine to second mother liquor
Change magnesium saturation state.
Further, in the step B, the filtration temperature of the heat filtering is 100 DEG C~110 DEG C.
Further, in the step C, second mother liquor is subjected to double evaporation-cooling at 140 DEG C~150 DEG C, then
It is cooled to 35 DEG C~40 DEG C.
Method of the invention by using twice evaporation, you can obtain edible magnesium chloride；And compared with prior art in system
Standby technique, it evaporates the temperature of terminal or the control condition of evaporated water (i.e. water reduction rate) is more loose, easily operated
With preparation；The method of twice evaporation also avoid in product because of entrainment mother liquor and caused by product the problem of contaminant overstandard；Together
When, impurity (referring to calcium ion and sulfate) content in the edible magnesium chloride obtained is well below national standard.
Embodiment
Hereinafter, embodiments of the invention are described in detail in the future.However, it is possible to implement this hair in many different forms
It is bright, and the specific embodiment of the invention that should not be construed as limited to illustrate here.Conversely, there is provided these embodiments be for
The principle and its practical application of the present invention is explained, so that others skilled in the art are it will be appreciated that the present invention's is various
Embodiment and the various modifications for being suitable for specific intended application.
It will be appreciated that although can be used term " first ", " second " etc. to describe various materials herein, but these
Material should not be limited by these terms.These terms are only used for making a distinction a material with another material.
Embodiment 1
Present embodiment discloses a kind of preparation method of edible magnesium chloride, referring in particular to following steps：
In step 1, take 100mL secondary waters that 300g Gu Kuang are placed in one and stirred as water is dissolved, it is molten when reaching
Filtered after solution-precipitation balance, obtain the first filter residue and the first filtrate, using the first filtrate as the first mother liquor, to carry out one
Secondary evaporation.
In the present embodiment, the Gu Kuang is salt lake by-product bischofite, and it derives from Cha Er Han Salt Lake；That is,
The Gu Kuang is during the making from brine in using Cha Er Han Salt Lake is for potassium chloride while obtained.
Specifically, component analysis has been carried out to the Gu Kuang, in the present embodiment, has carried out parallel laboratory test three times to test,
G-1~G-3 is denoted as respectively；Analysis result is as shown in table 1.
The solid ore deposit component complete analysis result (being calculated in mass percent) of table 1
Note：In table 1, " --- " represents to be practically free of impurity.
It will be appreciated by those skilled in the art that in table 1, MgCl2·6H2O、KCl、NaCl、CaSO4Content analysis is equal
Matched somebody with somebody by determining its corresponding ion concentration after being dissolved in water, therefore occurred such as MgCl in G-32·6H2O、
KCl、NaCl、CaSO4Situation of the total content more than 100%, the above situation belongs within error range.
From table 1 it follows that the Gu Kuang includes magnesium chloride (occurrence form MgCl2·6H2O), potassium chloride, chlorination
Sodium, calcium sulfate, may also include impurity；Wherein, potassium chloride, sodium chloride, the mass percent sum of calcium sulfate are no more than 4.6%,
The mass percent of impurity is no more than 0.6%, and remaining is the magnesium chloride.
In the present embodiment, the quality of the first mother liquor of acquisition is 357.79g；First mother liquor of acquisition has been carried out mainly
The content analysis of ion, as a result as shown in table 2.
The mother liquor leading ion content analysis result (being calculated in mass percent) of table 2 first
In the first mother liquor, in addition to above-mentioned each ion, remaining is H2O。
What deserves to be explained is having carried out XRD analysis to the first filter residue, the solid-phase component for finding the first filter residue is CaSO4·
2H2O, NaCl and KClMgCl2·6H2O, so as to show, in the step 1, Gu Kuang is not dissolved completely in dissolving water
In, and when reaching crystallization of the dissolution and precipitation balance, Gu the MgCl in ore deposit2·6H2O, after KCl is dissolved in dissolving water, and with KCl
MgCl2·6H2O form separates out, and CaSO4After being dissolved in dissolving water, and with CaSO4·2H2O form separates out, so that the
Each ion in one mother liquor is substantially at saturation state.
It will be appreciated by those skilled in the art that when plurality of inorganic salt is simultaneously soluble in water, when reaching dissolving-balance
When, the mixed inorganic increasingly complex, various compared with the plurality of inorganic salt before dissolving can be presented in its solid separated out, together
When, the content of the plurality of inorganic salt before dissolving can also influence the species of the mixed inorganic after separating out；That is,
The crystallization of the dissolution and precipitation process of above-mentioned steps one is not the simple procedure for the dissolving for being similar single inorganic salts.And in the present embodiment, root
According to the species and content of each inorganic salts in the solid ore deposit, it is determined that its proper ratio with dissolving water, so that less Ca2 +、SO4 2-、K+、Na+Deng the purity and the ion of index for influenceing final products, and more Mg2+、Cl-Immerse in the first mother liquor,
It is achieved thereby that preliminary removal of impurities.
In step 2, the first mother liquor is subjected to flush distillation at 100 DEG C~110 DEG C and carries out heat filtering, obtain the
Two filter residues and the second filtrate, second filtrate are the second mother liquor.
Specifically, in flush distillation, the quality of the water fallen from the first mother liquor by evaporation loss is 58.32g；Also
It is to say, the water reduction rate in first mother liquor is 16.3%.
In step 3, the second mother liquor is continued to be heated to 140 DEG C~150 DEG C progress double evaporation-coolings, is cooled to 35 DEG C
~40 DEG C and centrifuge, gained solid phase is the edible magnesium chloride.
What deserves to be explained is when carrying out double evaporation-cooling, maximum evaporation limit is that second mother liquor is satisfied in magnesium chloride
During with state；That is, when carrying out double evaporation-cooling, preferably make not separate out solid phase in the second mother liquor；One is it can avoid separating out
Solid phase and the loss for causing magnesium ion, so as to reduce the yield of target product edible magnesium chloride, the second is can prevent what is separated out
Edible magnesium chloride dehydration at high temperature, so as to reduce the purity of target product edible magnesium chloride, the third is preventing double evaporation-cooling institute
Very little, target product edible magnesium chloride amount of precipitation reduces and causes yield to reduce the water of loss after caused cooling.
The edible magnesium chloride obtained to the present embodiment has carried out component analysis, as a result as shown in table 3.
The edible magnesium chloride analysis result (being calculated in mass percent) of table 3
From table 3 it can be seen that impurity (refers to calcium ion in the edible magnesium chloride obtained by the preparation method of the present embodiment
And sulfate) content is well below national standard.
According to the preparation method of the edible magnesium chloride of the present embodiment, during flush distillation, the temperature of terminal is evaporated
And the control of evaporated water (i.e. water reduction rate) is more loose, avoiding evaporation in the prior art, terminal point control is harsh asks
Topic so that whole preparation method is more simple；Meanwhile by using the technique of twice evaporation, it also avoid evaporating using single
Caused by mother liquor entrainment it is exceeded the problem of.
Embodiment 2
It in the description of embodiment 2, will not be repeated here, only described with embodiment 1 not with the something in common of embodiment 1
Same part.The difference of embodiment 2 and embodiment 1 is, in step 1, takes 100mL secondary waters as dissolving water, will
350g Gu Kuang are placed in one and stirred, and are filtered after crystallization of the dissolution and precipitation balance is reached, obtain the first filter residue and the first filtrate,
The first filtrate is taken as the first mother liquor；The quality of the first mother liquor obtained is 388.56g；First mother liquor of the present embodiment it is main
The content analysis result of ion is as shown in table 4.
The mother liquor leading ion content analysis result (being calculated in mass percent) of table 4 first
In the first mother liquor, in addition to above-mentioned each ion, remaining is H2O。
In step 2, the quality of the water fallen from the first mother liquor by evaporation loss is 17.32g；It is that is, described
Water reduction rate in first mother liquor is 4.46%.
Edible magnesium chloride is prepared with reference to described in embodiment 1 in remaining；The edible chlorination that the present embodiment is prepared
Magnesium has carried out component analysis, as a result as shown in table 5.
The edible magnesium chloride analysis result (being calculated in mass percent) of table 5
As can be seen from Table 5, impurity (refers to calcium ion in the edible magnesium chloride obtained by the preparation method of the present embodiment
And sulfate) content is well below national standard.
According to the preparation method of the edible magnesium chloride of the present embodiment, during flush distillation, the temperature of terminal is evaporated
And the control of evaporated water (i.e. water reduction rate) is more loose, avoiding evaporation in the prior art, terminal point control is harsh asks
Topic so that whole preparation method is more simple；Meanwhile by using the technique of twice evaporation, it also avoid evaporating using single
Caused by mother liquor entrainment it is exceeded the problem of.
Embodiment 3
It in the description of embodiment 3, will not be repeated here, only described with embodiment 1 not with the something in common of embodiment 1
Same part.The difference of embodiment 3 and embodiment 1 is, in step 1, takes 100mL secondary waters as dissolving water, will
500g Gu Kuang are placed in one and stirred, and are filtered after crystallization of the dissolution and precipitation balance is reached, obtain the first filter residue and the first filtrate,
The first filtrate is taken as the first mother liquor；The quality of the first mother liquor obtained is 390.03g；First mother liquor of the present embodiment it is main
The content analysis result of ion is as shown in table 6.
The mother liquor leading ion content analysis result (being calculated in mass percent) of table 6 first
In the first mother liquor, in addition to above-mentioned each ion, remaining is H2O。
In step 2, the quality of the water fallen from the first mother liquor by evaporation loss is 16g；That is, described
Water reduction rate in one mother liquor is 4.1%.
Edible magnesium chloride is prepared with reference to described in embodiment 1 in remaining；The edible chlorination that the present embodiment is prepared
Magnesium has carried out component analysis, as a result as shown in table 7.
The edible magnesium chloride analysis result (being calculated in mass percent) of table 7
As can be seen from Table 7, impurity (refers to calcium ion in the edible magnesium chloride obtained by the preparation method of the present embodiment
And sulfate) content is well below national standard.
According to the preparation method of the edible magnesium chloride of the present embodiment, during flush distillation, the temperature of terminal is evaporated
And the control of evaporated water (i.e. water reduction rate) is more loose, avoiding evaporation in the prior art, terminal point control is harsh asks
Topic so that whole preparation method is more simple；Meanwhile by using the technique of twice evaporation, it also avoid evaporating using single
Caused by mother liquor entrainment it is exceeded the problem of.
In above-described embodiment 1-3, Gu Kuang and dissolving water ratio are respectively 3g:1mL、3.5g:1mL and 5g:1mL, but
The present invention is not restricted to this, if continuing to tune up the ratio, because each material has basically reached saturation in the first mother liquor, therefore
The concentration of each ion is not in obvious change in first mother liquor, so as to be equally applicable to follow-up evaporating temperature and steaming
Send out the control condition of terminal.
It will be appreciated by those skilled in the art that for different compositions and the liquid phase mixture of content, the phase representated by it
Point is different, if wanting to prepare identical product, then its process conditions can be incomplete same, or even can use entirely different side
Method；If conversely, the liquid phase mixture for representing different phase points, using identical technique, then the product obtained is then complete
It is different.That is, each method and its in each technological parameter selection, be only applicable to corresponding raw material.
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where not departing from the spirit and scope of the present invention limited by claim and its equivalent, can carry out herein form and
Various change in details.
Claims (2)
1. a kind of preparation method of edible magnesium chloride, it is characterised in that including step：
A, the first mother liquor is obtained；Wherein, first mother liquor includes Na+、K+、Mg2+、Cl-、SO4 2-、H2O, in first mother liquor
In, the Na+Mass percent be 0.1% ~ 0.2%, the K+Mass percent be 0.05% ~ 0.1%, the Mg2+Matter
It is 8.4% ~ 9.5% to measure percentage, the Cl-Mass percent be 24.5% ~ 28%, the SO4 2-Mass percent be
0.05% ~ 0.1%, remaining is the H2O；
The preparation method of first mother liquor specifically includes：
Salt lake by-product bischofite is placed in dissolving water and is stirred, solid-liquid point is carried out again after reaching crystallization of the dissolution and precipitation balance
From gained liquid phase is first mother liquor；The ratio of the salt lake by-product bischofite and dissolving water is the g of 3 g ~ 5:1 mL；Its
In, the salt lake by-product bischofite includes magnesium chloride, potassium chloride, sodium chloride, calcium sulfate and impurity, the potassium chloride, chlorination
Sodium, the mass percent sum of calcium sulfate are no more than 4.6%, and the mass percent of the impurity is no more than 0.6%, and remaining is described
Magnesium chloride；
B, first mother liquor is subjected to flush distillation at 100 DEG C ~ 110 DEG C and carries out heat filtering, using gained filtrate as
Two mother liquors；Wherein, in the flush distillation, the water reduction rate in first mother liquor is 4.1% ~ 16.3%；
C, second mother liquor is subjected to double evaporation-cooling at 140 DEG C ~ 150 DEG C, is in magnesium chloride saturation shape to second mother liquor
State, it is cooled to 35 DEG C ~ 40 DEG C and carries out separation of solid and liquid, gained solid phase is edible magnesium chloride.
2. preparation method according to claim 1, it is characterised in that in the step B, the filtering temperature of the heat filtering
Spend for 100 DEG C ~ 110 DEG C.
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| CN108083303A (en) * | 2017-12-19 | 2018-05-29 | 青海盐湖工业股份有限公司 | A kind of method that potash fertilizer production tail washings produces anhydrous magnesium chloride electrolysis raw material |
| CN109292801B (en) * | 2018-12-05 | 2021-03-23 | 中国科学院青海盐湖研究所 | Preparation method of food-grade magnesium chloride |
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| CN1032742C (en) * | 1993-08-19 | 1996-09-11 | 天津长芦塘沽盐场 | Prodn. technique for prepn. of white magnesium chloride using bitter |
| CN1281499C (en) * | 2004-06-04 | 2006-10-25 | 天津科技大学 | Process for producing high purity magnesia |
| CN100594245C (en) * | 2008-08-12 | 2010-03-17 | 中国科学院青海盐湖研究所 | Process for preparing calcined dolomite from magnesium chloride of chloride type by-product of potassium-extracting from salt lake |
| DE102010049176A1 (en) * | 2010-10-21 | 2012-04-26 | K-Utec Ag Salt Technologies | Obtaining and processing of carnallite, comprises dissolving, processing extracted carnallite brine by evaporation and cooling, isolating carnallite crystals, decomposing crystals and separating mixture and discharging magnesium chloride |
| CN104030327B (en) * | 2014-02-27 | 2016-01-13 | 青海西部镁业有限公司 | A kind of Bischofite in Salt lake continuous-dissolution produces the method for high density magnesium chloride solution |
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