CN101607720A - With the bittern that contains magnesium chloride is the feedstock production method of magnesium oxide - Google Patents
With the bittern that contains magnesium chloride is the feedstock production method of magnesium oxide Download PDFInfo
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- CN101607720A CN101607720A CNA2008101149874A CN200810114987A CN101607720A CN 101607720 A CN101607720 A CN 101607720A CN A2008101149874 A CNA2008101149874 A CN A2008101149874A CN 200810114987 A CN200810114987 A CN 200810114987A CN 101607720 A CN101607720 A CN 101607720A
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Abstract
The invention belongs to the salt chemical engineering field, is the feedstock production method of magnesium oxide with the bittern that contains magnesium chloride particularly.The present invention is to be raw material with the bittern that contains magnesium chloride, and employing yellow soda ash is precipitation agent, and by control reaction temperature, mixing speed, reaction conditionss such as the feed rate of yellow soda ash obtain having the magnesium carbonate trihydrate intermediate (purity reaches 99.0%) of good needle-like crystalline form; Then the needle-like magnesium carbonate trihydrate crystal intermediate high-temperature calcination that obtains is made high-purity magnesium oxide (purity reaches 99.4%).The sodium chloride-containing crystalline mother solution that filtration magnesium carbonate trihydrate crude product obtained when reaction finished separates out the sodium-chlor crystallization through evaporation, concentrated, crystallization, filters and obtains sodium chloride crystal.The present invention is intended to utilize abundant seawater or salt lake brine production needle-like magnesium carbonate trihydrate intermediate, thereby the preparation high-purity magnesium oxide is good in economic efficiency, non-environmental-pollution; The method strong operability that provides, be easy to realize industrialization.
Description
Technical field
The invention belongs to the salt chemical engineering field, particularly a kind of employing yellow soda ash is precipitation agent, and the needle-like magnesium carbonate trihydrate crystal that generates with reaction in the bittern that contains magnesium chloride is an intermediate, thereby produces the method for high-purity magnesium oxide and sodium-chlor.
Technical background
The magnesium compound product reaches the hundreds of kind, requirement maximum wherein, and what kind was maximum is the magnesium oxide series product.Magnesium oxide can be widely used in fields such as papermaking, chemical industry, rubber, medicine, livestock industry, refractory materials, MAGNESIUM METAL refinement, building, military project.2006 annual world magnesium oxide year production statistical result showed, the magnesian throughput of China ranks first in the world, and annual production is approximately 3,230,000 tons.What at present the domestic production high-purity magnesium oxide adopted is the method for calcined magnesite, but this kind method can only the magnesium oxide of production purity about 95%, seldom can reach more than 99%, and energy consumption and environmental protection are not up to standard.External main MgCl with extra large bittern
2Produce high-purity magnesium oxide, but, produce hydrochloric acid in the production process, pollute the ambient atmosphere environment because selected technical process is improper.Also have some offshore companies to adopt the MAGNESIUM METAL direct oxidation to produce highly-purity magnesite, this content of magnesia can reach 99.99%, but this method production cost is too high, is unfavorable for promoting.
There are abundant seawater and salt lake brine MgCl in China
2Resource, China bittern MgCl
2The preparation high-purity magnesium oxide has advantageous condition.As salt lake, Qinghai group is the potash fertilizer production base of China's maximum, discharges a large amount of old halogen to the salt pan when producing potash fertilizer, and old halogen is after spontaneous evaporation, and generation in every year number is with ten million ton bischofite (MgCl
26H
2O), be the high quality raw material of producing high-purity magnesium oxide, because technology does not have scale operation so far, the high-quality magnesium chloride not only is not utilized, and has a strong impact on the ecotope in salt lake, Qinghai on the contrary, promptly so-called " magnesium evil ".Therefore, how fully rationally utilizing salt lake brine for the high-grade magnesium series product of raw material production, be not only the strategic demand of national economic development, also is the needs of protection environment sustainable development.
At present, utilize bittern magnesium chloride or bischofite (MgCl
26H
2O) resource is produced magnesian main method has:
(1) bischofite direct breakdown method: present method adopts bischofite (MgCl
26H
2O) directly calcining generates magnesia, and its principal reaction is:
MgCl
2·6H
2O＝MgO+2HCl↑+5H
2O↑
This method is very high for the purity requirement of bischofite, and simultaneously because the calcination process temperature is very high, the mobile property of gas-liquid-solid three-phase is poor, and byproduct hydrogen chloride gas has serious corrosion for production unit.
(2) the milk of lime precipitator method: milk of lime is joined in the certain density magnesium chloride bittern, following reaction takes place:
MgCl
2+Ca(OH)
2＝Mg(OH)
2↓+CaCl
2
Or MgCl
2+ Ca (OH)
2Mg (OH)
2=2Mg (OH)
2↓+CaCl
2
The magnesium hydroxide that reaction generates obtains magnesium oxide through calcining:
Mg(OH)
2＝MgO+H
2O↑
This method requires high for the activity of calcium hydroxide, generation be precipitated as magnesium hydroxide, the less easy absorption impurity of particle is so product purity is lower; Magnesium hydrate precipitate is a jelly simultaneously, filtration difficulty, and the cake moisture height, drying process energy consumption height, and the calcium chloride added value that generates is low, has formed " white sea " in some areas, and environmental pollution is serious.
(3) ammonia precipitation process method: bittern and ammoniacal liquor reaction are generated magnesium hydrate precipitate, and its reaction formula is as follows:
MgCl
2+2NH
3·H
2O＝Mg(OH)
2↓+2NH
4Cl
The magnesium hydroxide that reaction generates obtains magnesium oxide through calcining:
Mg(OH)
2＝MgO+H
2O↑
This method is reacted the magnesium hydroxide that can obtain larger particles under lower reactant concn, but low concentration can cause yield lower, and free ammonium concentration height in the reaction system causes problems such as operating environment is poor, environmental pollution simultaneously.
(4) carbon ammonium precipitation method: with bicarbonate of ammonia is that precipitation agent reacts, and its reaction formula is as follows:
MgCl
2+2NH
4HCO
3＝MgCO
3↓+CO
2↑+2NH
4Cl+H
2O
2MgCl
2+4NH
4HCO
3+3H
2O＝MgCO
3·Mg(OH)
2·4H
2O↓+3CO
2↑+4NH
4Cl
What reaction generated is magnesiumcarbonate or magnesium basic carbonate, obtains magnesium oxide through calcining:
MgCO
3＝MgO+CO
2↑
MgCO
3·Mg(OH)
2·4H
2O＝2MgO+CO
2↑+5H
2O↑
Carbonic acid gas utilization ratio in this method bicarbonate of ammonia has only 50%, and production consumption bicarbonate of ammonia amount is big, the cost height.
(5) carbonic acid gas, the ammonia precipitator method: the carbonic acid gas and the ammonia of certain flow are fed in the bittern in proportion,, form following reaction with magnesium chloride:
MgCl
2+2NH
3+CO
2+H
2O＝MgCO
3↓+2NH
4Cl
The magnesiumcarbonate that reaction generates obtains magnesium oxide through calcining:
MgCO
3＝MgO+CO
2↑
Carbonic acid gas, ammonia as raw material are comparatively cheap, remarkable in economical benefits, but this reaction relates to gas-liquid-solid phase reaction, and reaction process is wayward, unstable product quality.
Summary of the invention
The purpose of this invention is to provide with the bittern that contains high dense magnesium chloride is raw material production needle-like magnesium carbonate trihydrate crystal intermediate, and then prepares the method for high-purity magnesium oxide.
It is raw material production needle-like magnesium carbonate trihydrate crystal intermediate that another object of the present invention provides with the bittern that contains high dense magnesium chloride, and then prepares the method for sodium-chlor.
Technical scheme of the present invention is to be raw material with the bittern that contains high dense magnesium chloride, and employing yellow soda ash is precipitation agent, and the needle-like magnesium carbonate trihydrate crystal that reaction generates is an intermediate, thereby produces high-purity magnesium oxide.Precipitating with yellow soda ash in the process of magnesium in the bittern, by regulating and controlling processing condition can obtain the having good filtering property needle-like magnesium carbonate trihydrate crystal intermediate of (can reduce filter energy consumption), can reduce absorption like this to impurity, make product have higher purity, guarantee further that simultaneously the magnesium oxide that obtains is high-purity.
The mechanism of magnesium chloride is in yellow soda ash and the bittern:
Na
2CO
3+MgCl
2+3H
2O＝MgCO
3·3H
2O↓+2NaCl
This reaction generates magnesium carbonate trihydrate precipitation crude product, and by product is a sodium-chlor.Magnesium carbonate trihydrate precipitation crude product filters and obtains needle-like magnesium carbonate trihydrate crystal intermediate through washing; Mother liquor obtains solid sodium chloride through concentrated, crystallization.Produce a large amount of yellow soda ash by products in Cellmic C 121 (ADC) the whipping agent production process, precipitation agent yellow soda ash can therefrom obtain, and has so both effectively reclaimed yellow soda ash, has good economic benefit again.
Needle-like magnesium carbonate trihydrate crystal intermediate obtains high-purity magnesium oxide through calcining:
MgCO
3·3H
2O＝MgO+CO
2↑+3H
2O↑
It also can further generate magnesium such as MAGNESIUM METAL is product.So just provide technical support, and had good economic benefit realizing that salt lake resources fully utilizes.
Use yellow soda ash of the present invention generates needle-like magnesium carbonate trihydrate crystal intermediate as precipitation agent, thereby produces method of magnesium oxide, comprises the evaporation of bittern, concentrated, Crystallization Procedure; The precipitation of magnesium carbonate trihydrate crude product, filtration, washing, drying process; The evaporation of sodium chloride-containing crystalline mother solution, concentrated, Crystallization Procedure; The calcination process of needle-like magnesium carbonate trihydrate crystal intermediate.
Of the present invention is that the feedstock production method of magnesium oxide may further comprise the steps with the bittern that contains magnesium chloride:
1) former bittern is carried out spontaneous evaporation, concentrates salt Tanaka, go out sodium-chlor, Repone K, vitriolate of tartar, sal epsom, magnesium potassium double salt etc., obtain containing the crystalline mother solution I of magnesium chloride simultaneously in existing technical crystallization respectively;
2) the crystalline mother solution I that contains magnesium chloride that step 1) is obtained removes by filter impurity, crystallisate through precipitation, obtains containing the refining bittern of magnesium chloride;
3) with step 2) the refining bittern water that contains magnesium chloride that obtains regulates, and making the magnesium chloride starting point concentration is 0.5～3mol/L, and the pH value that will make with extra care bittern with dilute hydrochloric acid is adjusted to 1～3;
4) the pH value that step 3) is obtained is adjusted in the retort that 1～3 refining bittern joins the strap clamp cover, in the chuck of the retort that strap clamp overlaps, feed recirculated water, to make with extra care brine temperature and be adjusted to 10～50 ℃, under the mixing speed of 200rpm～400rpm, the yellow soda ash precipitation agent is joined in the retort, the mol ratio of control yellow soda ash and magnesium chloride is between 1: 1.1～1.2, the control reaction temperature scope is 10～50 ℃, the feed rate of control yellow soda ash precipitation agent is 3～4ml/min or 1～2g/min, behind reinforced the finishing, solution produces main magnesium carbonate trihydrate precipitation crude product through certain induced reaction after date, continues to stir ageing, filters then;
5) the magnesium carbonate trihydrate crude product that obtains after the step 4) ageing is finished is with 10～50 ℃ deionized water wash, and drying obtains exsiccant needle-like magnesium carbonate trihydrate crystal intermediate, obtains sodium chloride-containing crystalline mother solution II simultaneously; Needle-like magnesium carbonate trihydrate crystal intermediate 800～1000 ℃ of calcinings down, is obtained high-purity magnesium oxide.Mg among the sodium chloride-containing crystalline mother solution II
2+Content can be controlled at below the 1g/L, and heavy magnesium efficient is greater than 98.0%, and needle-like magnesium carbonate trihydrate crystal intermediate purity can reach 99.0%, and high-purity magnesium oxide purity can reach 99.4%.
The sodium chloride-containing crystalline mother solution II that the present invention obtains step 5) through pervaporation, concentrate, crystallization, the sodium-chlor crystallization is separated out, filter and obtain sodium chloride crystal, obtain mother liquor III simultaneously; Mother liquid obtained III returns the starting point concentration that is used for adjusting magnesium chloride in the step 3).
Step 2 of the present invention) content of magnesium chloride in the refining bittern that contains magnesium chloride that obtains is 3～4.5mol/L.
Described yellow soda ash is that concentration is sodium carbonate solution or the anhydrous sodium carbonate solid of 0.1～3mol/L.
Described digestion time is 2～6 hours.
The calcination time of described needle-like magnesium carbonate trihydrate crystal intermediate under 800～1000 ℃ is 2～4 hours.
The major diameter of described needle-like magnesium carbonate trihydrate crystal intermediate is about 20～500 μ m, and minor axis is 4～8 μ m; Because crystal habit is better, particle is bigger, so strainability is fine, greatly reduces the filtration energy consumption.
Described bittern is seawater or salt lake brine.
The retort of described strap clamp cover is to have recirculated water to import and export in the outer wall upper and lower of tank body, one end of stir shaft is connected with the tank body external motors, the other end stretches in the tank body, on the stir shaft in tank body agitating vane is installed, on inner tank wall, be installed with four baffle plates, have the tear drop mouth of pipe on tank body top, thermometer socket, pH meter socket.
The present invention utilizes needle-like magnesium carbonate trihydrate crystal intermediate to have good filtering property and dehydrating property, is selected as the final throw out of precipitation magnesium from bittern.The present invention is intended to utilize abundant seawater or salt lake brine production needle-like magnesium carbonate trihydrate crystal intermediate, thereby the preparation high-purity magnesium oxide is good in economic efficiency, non-environmental-pollution; The method strong operability that provides, be easy to realize industrialization.
Advantage of the present invention and active effect are:
(1) use yellow soda ash magnesium chloride in the bittern to be precipitated as precipitation agent, solved the problem that magnesium resource utilizes in present seawater or the salt lake, improve the environment of potash fertilizer producing area, effectively utilized to produce a large amount of yellow soda ash by products in the ADC whipping agent production process, had very high economic benefit.
(2) the adjusting starting point concentration by magnesium chloride, precipitation agent are to reaction conditionss such as feed rate, temperature of reaction, mixing speed and pH values, the growth pattern of control magnesium carbonate trihydrate, make the magnesium carbonate trihydrate crude product that obtains by washing, the oven dry back is for having the needle-like magnesium carbonate trihydrate crystal intermediate of good crystalline form and filtering property; By optimizing the precipitated crystal process,, impurity drops to minimum thereby being carried secretly.This technology can be with Mg in the bittern
2+The concentration primary first-order equation is reduced to below the 1g/L.
(3) gained needle-like magnesium carbonate trihydrate crystal intermediate purity can reach 99.0%, and particle is big, and good crystalline has significantly reduced the absorption of impurity.
(4) gained needle-like magnesium carbonate trihydrate crystal midbody particle is big, has splendid strainability, has solved with magnesium hydroxide to be the heavy existing filtration difficulty of magnesium products, the high problem of filtration energy consumption.
(5) the magnesium oxide purity that is made by the calcining of needle-like magnesium carbonate trihydrate crystal intermediate reaches 99.4%, and also can make high-grade magnesium such as Magnesium Chloride Anhydrous, MAGNESIUM METAL by needle-like magnesium carbonate trihydrate crystal intermediate is product, and has reduced energy consumption.
(7) by product sodium-chlor is the added value high product, can recycle by the salt pan evaporation, and energy consumption is low.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
The retort structural representation that the strap clamp that Fig. 2 uses for crystallisation process of the present invention overlaps.
Reference numeral
A. the tank body b. recirculated water of the retort of strap clamp cover is imported and exported the c. stir shaft
D. the agitating vane e. baffle plate f. tear drop mouth of pipe
G. thermometer socket h.pH counts socket
Embodiment
Embodiment 1
See also Fig. 2.The retort of employed strap clamp cover is to have recirculated water to import and export b in the outer wall upper and lower of tank body a, the end of stir shaft c is connected with the tank body external motors, the other end stretches in the tank body, on the stir shaft c in tank body agitating vane d is installed, on inner tank wall, be installed with four baffle plate e, have tear drop mouth of pipe f on tank body top, thermometer socket g, pH meter socket h.
Technical process of the present invention sees also Fig. 1.
1) former bittern is carried out spontaneous evaporation, concentrates salt Tanaka, crystallization goes out sodium-chlor, Repone K, vitriolate of tartar, sal epsom, magnesium potassium double salt etc. respectively, obtains containing the crystalline mother solution I of magnesium chloride simultaneously;
2) the crystalline mother solution I that contains magnesium chloride that step 1) is obtained is through precipitating, removing by filter impurity, crystallisate, and obtaining content of magnesium chloride is the refining bittern of 3mol/L;
3) with step 2) content of magnesium chloride that obtains is that the refining bittern of 3mol/L is regulated with deionized water, and being mixed with the 2000ml starting point concentration is the refining bittern of 0.5mol/L, and the pH value that will make with extra care bittern with dilute hydrochloric acid is adjusted to 1;
4) the pH value that step 3) is obtained is adjusted in the retort that 1 refining bittern joins the strap clamp cover, in the chuck of the retort that strap clamp overlaps, feed recirculated water, to make with extra care brine temperature and be adjusted to 30 ℃, under the mixing speed of 400rpm, with 2000ml concentration is that the sodium carbonate solution of 0.6mol/L is heated to after 30 ℃ and slowly joins the retort from the top of the retort of strap clamp cover, the adding speed of control sodium carbonate solution is 3ml/min, and control reaction temperature is 30 ℃.Behind reinforced the finishing, solution continues to stir ageing 2 hours through reaction back generation inductive phase magnesium carbonate trihydrate crude product precipitation, filters then;
5) the magnesium carbonate trihydrate crude product that obtains after the step 4) ageing is finished is with 30 ℃ deionized water wash, dry, obtain needle-like magnesium carbonate trihydrate crystal intermediate, the major diameter of needle-like magnesium carbonate trihydrate crystal intermediate is about 20～400 μ m, minor axis is 4～6 μ m, purity is 98.5%, obtains sodium chloride-containing crystalline mother solution II simultaneously; Needle-like magnesium carbonate trihydrate crystal intermediate was calcined 4 hours down at 800 ℃, obtained magnesia crystal whisker, purity is 99.1%.Mg among the sodium chloride-containing crystalline mother solution II
2+Content is 0.36g/L, and sodium chloride-containing crystalline mother solution II through pervaporation, concentrated, crystallization, is filtered and obtains solid sodium chloride and filtrate, and filtrate is returned step 3) and recycled.
Embodiment 2
Utilize the retort of embodiment 1 employed strap clamp cover.
1) former bittern is carried out spontaneous evaporation, concentrates salt Tanaka, crystallization goes out sodium-chlor, Repone K, vitriolate of tartar, sal epsom, magnesium potassium double salt etc. respectively, obtains containing the crystalline mother solution of magnesium chloride simultaneously;
2) crystalline mother solution that contains magnesium chloride that step 1) is obtained removes by filter impurity, crystallisate through precipitation, and obtaining content of magnesium chloride is the refining bittern of 4.5mol/L;
3) with step 2) the refining bittern that contains magnesium chloride that obtains regulates with deionized water, is mixed with liquid at the bottom of the magnesium chloride that the 2000ml starting point concentration is 2mol/L, with dilute hydrochloric acid with magnesium chloride at the bottom of the pH value of liquid be adjusted to 3;
4) liquid joined in the retort of strap clamp cover at the bottom of the pH value that step 3) is obtained was adjusted to 3 magnesium chloride, in the chuck of the retort that strap clamp overlaps, feed recirculated water, liquid temp at the bottom of the magnesium chloride is adjusted to 45 ℃, under the mixing speed of 400rpm, slowly join the retort with the speed of 2g/min from the top of the retort of strap clamp cover 500g yellow soda ash pressed powder, control reaction temperature is 45 ℃, feeding in raw material finishes and react the end back produces magnesium carbonate trihydrate precipitation crude product, continue to stir ageing in 6 hours, filter then;
5) the magnesium carbonate trihydrate crude product that obtains after the step 4) ageing is finished is with 45 ℃ deionized water wash, dry, obtain exsiccant needle-like magnesium carbonate trihydrate crystal intermediate, the major diameter of needle-like magnesium carbonate trihydrate crystal intermediate is about 40～500 μ m, minor axis is 5～8 μ m, product purity is 99.0%, obtains the sodium chloride-containing crystalline mother solution simultaneously; The calcining under 1000 ℃ of needle-like magnesium carbonate trihydrate crystal intermediate was obtained magnesia crystal whisker in 3 hours, and purity is 99.4%.Mg in the sodium chloride-containing crystalline mother solution
2+Content is 0.51g/L, and the sodium chloride-containing crystalline mother solution through pervaporation, concentrated, crystallization, is filtered and obtains solid sodium chloride and filtrate, and filtrate is returned step 3) and recycled.
Embodiment 3
Utilize the retort of embodiment 1 employed strap clamp cover.
1) former bittern is carried out spontaneous evaporation, concentrates salt Tanaka, crystallization goes out sodium-chlor, Repone K, vitriolate of tartar, sal epsom, magnesium potassium double salt etc. respectively, obtains containing the crystalline mother solution of magnesium chloride simultaneously;
2) crystalline mother solution that contains magnesium chloride that step 1) is obtained removes by filter impurity, crystallisate through precipitation, and obtaining content of magnesium chloride is the refining bittern of 4mol/L;
3) with step 2) the refining bittern that contains magnesium chloride that obtains regulates with deionized water, is mixed with liquid at the bottom of the magnesium chloride that the 2000ml starting point concentration is 3mol/L, with dilute hydrochloric acid with magnesium chloride at the bottom of the pH value of liquid be adjusted to 2;
4) liquid joined in the retort of strap clamp cover at the bottom of the pH value that step 3) is obtained was adjusted to 2 magnesium chloride, in the chuck of the retort that strap clamp overlaps, feed recirculated water, liquid temp at the bottom of the magnesium chloride is adjusted to 50 ℃, under the mixing speed of 300rpm, with 3300ml concentration is that the sodium carbonate solution of 2mol/L is heated to that the speed with 4ml/min joins in the retort after 50 ℃, control reaction temperature is 50 ℃, feeding in raw material finishes and react the end back produces magnesium carbonate trihydrate precipitation crude product, continue to stir ageing in 6 hours, filter then;
5) the magnesium carbonate trihydrate crude product that obtains after the step 4) ageing is finished is with 50 ℃ deionized water wash, dry, obtain exsiccant needle-like magnesium carbonate trihydrate crystal intermediate, the major diameter of needle-like magnesium carbonate trihydrate crystal intermediate is about 30～450 μ m, minor axis is 5～7 μ m, product purity is 98.8%, obtains the sodium chloride-containing crystalline mother solution simultaneously; The calcining under 1000 ℃ of needle-like magnesium carbonate trihydrate crystal intermediate was obtained magnesia crystal whisker in 2 hours, and purity is 99.3%.Mg in the sodium chloride-containing crystalline mother solution
2+Content is 0.42g/L, and the sodium chloride-containing crystalline mother solution through pervaporation, concentrated, crystallization, is filtered and obtains solid sodium chloride and filtrate, and filtrate is returned step 3) and recycled.
Claims (9)
1. one kind is the feedstock production method of magnesium oxide with the bittern that contains magnesium chloride, and it is to be raw material with the bittern that contains magnesium chloride, and employing yellow soda ash is precipitation agent, and the needle-like magnesium carbonate trihydrate crystal that reaction generates is an intermediate, it is characterized in that this method may further comprise the steps:
1) bittern is carried out spontaneous evaporation, concentrated, crystallization salt Tanaka, obtain containing the crystalline mother solution I of magnesium chloride;
2) the crystalline mother solution I that contains magnesium chloride that step 1) is obtained removes by filter impurity, crystallisate through precipitation, obtains containing the refining bittern of magnesium chloride;
3) with step 2) the refining bittern water that contains magnesium chloride that obtains regulates, and making the magnesium chloride starting point concentration is 0.5～3mol/L, and the pH value that will make with extra care bittern with dilute hydrochloric acid is adjusted to 1～3;
4) the pH value that step 3) is obtained is adjusted in the retort that 1～3 refining bittern joins the strap clamp cover, in the chuck of the retort that strap clamp overlaps, feed recirculated water, to make with extra care brine temperature and be adjusted to 10～50 ℃, under the mixing speed of 200rpm～400rpm, the yellow soda ash precipitation agent is joined in the retort, the mol ratio of control yellow soda ash and magnesium chloride is between 1: 1.1～1.2, the control reaction temperature scope is 10～50 ℃, the feed rate of control yellow soda ash precipitation agent is 3～4ml/min or 1～2g/min, behind reinforced the finishing, solution produces magnesium carbonate trihydrate crude product precipitation through the induced reaction after date, continue to stir ageing, filter then, obtain sodium chloride-containing crystalline mother solution II simultaneously;
5) the magnesium carbonate trihydrate crude product that obtains after the step 4) ageing is finished is with 10～50 ℃ deionized water wash, dry, obtain exsiccant needle-like magnesium carbonate trihydrate crystal intermediate, needle-like magnesium carbonate trihydrate crystal intermediate 800～1000 ℃ of calcinings down, is obtained magnesium oxide.
2. method according to claim 1 is characterized in that: the sodium chloride-containing crystalline mother solution II that step 4) is obtained through pervaporation, concentrate, crystallization, the sodium-chlor crystallization is separated out, filter and obtain sodium chloride crystal, obtain mother liquor III simultaneously.
3. method according to claim 2 is characterized in that: mother liquid obtained III returns the starting point concentration that is used for adjusting magnesium chloride in the step 3).
4. method according to claim 1 is characterized in that: step 2) content of magnesium chloride in the refining bittern that contains magnesium chloride that obtains is 3～4.5mol/L.
5. according to claim 1 or 4 described methods, it is characterized in that: described bittern is seawater or salt lake brine.
6. method according to claim 1 is characterized in that: described yellow soda ash is that concentration is sodium carbonate solution or the anhydrous sodium carbonate solid of 0.1～3mol/L.
7. method according to claim 1 is characterized in that: described digestion time is 2～6 hours.
8. method according to claim 1 is characterized in that: the calcination time of described needle-like magnesium carbonate trihydrate crystal intermediate under 800～1000 ℃ is 2～4 hours.
9. according to claim 1 or 8 described methods, it is characterized in that: the major diameter of described needle-like magnesium carbonate trihydrate crystal intermediate is about 20～500 μ m, and minor axis is 4～8 μ m.
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| CN114195173B (en) * | 2022-01-12 | 2023-11-28 | 太原理工大学 | Preparation method of needle-shaped sodium chloride crystal |
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