CN104291367B - A kind of production method of magnesium sulfate monohydrate - Google Patents
A kind of production method of magnesium sulfate monohydrate Download PDFInfo
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- CN104291367B CN104291367B CN201410505117.5A CN201410505117A CN104291367B CN 104291367 B CN104291367 B CN 104291367B CN 201410505117 A CN201410505117 A CN 201410505117A CN 104291367 B CN104291367 B CN 104291367B
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- magnesium sulfate
- filter cake
- sulfate monohydrate
- aqueous solution
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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
- C01F5/40—Magnesium sulfates
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Abstract
The invention discloses a kind of production method of magnesium sulfate monohydrate, it is characterized in that: be the mass percent concentration adding 1200 ~ 3500 mass parts in the magnesium sulfate saturated aqueous solution of 50 ~ 90 DEG C to the temperature of 1500 ~ 2500 mass parts magnesium sulfate heptahydrates or 1800 ~ 3000 mass parts under stirring be the vitriol oil of 90% ~ 98%, stirring reaction 1 ~ 2 hour, obtains the suspension of magnesium sulfate monohydrate; By suspension filtered, filter cake magnesium sulfate saturated aqueous solution washs once, then washes 1 ~ 2 time with water; By the filter cake after washing at the temperature of 120 ~ 150 DEG C dry 0.5 ~ 1 hour, i.e. obtained magnesium sulfate monohydrate.Production technique of the present invention is short, equipment simple, less energy consumption, cost are low, is suitable for industrialized production, and commercial effect is good, practical.
Description
Technical field
The invention belongs to the preparation of the compound of MAGNESIUM METAL, relate to a kind of production method of magnesium sulfate monohydrate.Magnesium sulfate monohydrate prepared by the present invention has purposes such as making dual element fertilizer, foodstuff additive, stablizer, printing and dyeing weighting agent, weighting agent, can be widely used in the industries such as agricultural, food, process hides, papermaking, medicine, plating.
Background technology
Magnesium sulfate is as a kind of important inorganic chemical product, and purposes is very extensive.Common magnesium sulfate is mainly magnesium sulfate heptahydrate and magnesium sulfate monohydrate two series products, magnesium sulfate heptahydrate have compared with magnesium sulfate monohydrate sulfur-bearing magnesium component compared with low, product easy caking stored for a long time, to mix the shortcomings such as difficulty is large, price is not high, market is limited with unclassified stores, magnesium sulfate heptahydrate being processed into magnesium sulfate monohydrate can increase magnesium sulfate value-added content of product further.Therefore, the magnesium sulfate monohydrate how utilizing existing magnesium sulfate heptahydrate to produce high added value has great importance.
In prior art, the production method of magnesium sulfate monohydrate mainly contains: (1) obtains magnesium sulfate monohydrate by magnesia and direct reaction of sulfuric acid; (2) high temperature crystallization method: this method utilizes the changes in solubility of magnesium sulfate, is heated to certain temperature by Adlerika and makes it crystallize out, continue to heat, pressurize after obtain magnesium sulfate monohydrate through subsequent disposal; (3) dryness shrinkage creek: this method method mainly utilizes various high-end devices through persistently overheating heating magnesium sulfate heptahydrate solid, by controlling the heating condition of magnesium sulfate heptahydrate, make its different temperature ranges progressively drying and dehydrating obtain sulfuric acid monohydrate magnesium products.
Existing magnesium sulfate monohydrate production method, ubiquity operational path is long, high to equipment requirements, energy consumption large, the more high defect of production cost, can produce a large amount of waste gas, waste liquid simultaneously, bring harm to environment in the process of producing.
Summary of the invention
Object of the present invention is intended to overcome deficiency of the prior art, solve existing dryness shrinkage creek and prepare the shortcomings such as magnesium sulfate monohydrate complex process, equipment requirements is high, energy consumption is large, the employing vitriol oil dewaters the mode directly prepared from magnesium sulfate heptahydrate, provides a kind of production method of easy, energy-conservation magnesium sulfate monohydrate.
Content of the present invention is: a kind of production method of magnesium sulfate monohydrate, it is characterized in that step is:
Under a, stirring, (slowly) is to 1500 ~ 2500 mass parts (such as Kg, the mass percent concentration adding afterwards together) 1200 ~ 3500 mass parts in magnesium sulfate heptahydrate is the vitriol oil of 90% ~ 98%, (continuation) stirring reaction 1 ~ 2 hour, obtains the suspension of magnesium sulfate monohydrate;
B, (while hot) are by suspension filtered, and filter cake (solids obtained after namely filtering) washs once with magnesium sulfate saturated aqueous solution, then washes 1 ~ 2 time with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing at the temperature of 120 ~ 150 DEG C dry 0.5 ~ 1 hour, i.e. obtained magnesium sulfate monohydrate.
In content of the present invention: 0.05 ~ 0.2 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 70 ~ 90 DEG C, consumption is filter cake quality.
In content of the present invention: the quality of the water of washing leaching cake described in step b is 0.2 ~ 0.5 times of filter cake quality at every turn.
Content of the present invention can also be: a kind of production method of magnesium sulfate monohydrate, it is characterized in that step is:
Under a, stirring, (slowly) is to 1800 ~ 3000 mass parts (such as Kg, afterwards with) temperature be the mass percent concentration adding 1200 ~ 3500 mass parts in the magnesium sulfate saturated aqueous solution of 50 ~ 90 DEG C be the vitriol oil of 90% ~ 98%, continue stirring reaction 1 ~ 2 hour, obtain the suspension of magnesium sulfate monohydrate;
B, (while hot) are by suspension filtered, and filter cake (solids obtained after namely filtering) washs once with magnesium sulfate saturated aqueous solution, then washes 1 ~ 2 time with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing at the temperature of 120 ~ 150 DEG C dry 0.5 ~ 1 hour, i.e. obtained magnesium sulfate monohydrate.
In content of the present invention: 0.05 ~ 0.2 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 70 ~ 90 DEG C, consumption is filter cake quality.
In content of the present invention: the quality of the water of washing leaching cake described in step b is 0.2 ~ 0.5 times of filter cake quality at every turn.
Compared with prior art, the present invention has features and beneficial effect:
(1) adopt the present invention, the Adlerika of magnesium sulfate heptahydrate or certain temperature is through finite concentration vitriol oil dehydration reaction i.e. obtained magnesium sulfate monohydrate, and method is easy, and chemical equation is as follows:
MgSO
4·7H
2O+H
2SO
4=MgSO
4·H
2O+6H
2O+H
2SO
4;
(2) compared with the method for existing production magnesium sulfate monohydrate, the present invention have use production unit simple, operational path is short, energy consumption is low, the feature of less investment, filter and wash the filtrate that produces and directly can return and realize closed circulation for the production of magnesium sulfate heptahydrate or Adlerika and utilize, waste gas is not had to produce the discharge not having waste gas to produce, do not have waste liquid, environmentally safe;
(3) compared with the method for existing production magnesium sulfate monohydrate, adopt energy consumption of the present invention to reduce by 10% ~ 25%, invest minimizing 20% ~ 40%, cost reduces by 25% ~ 50%, commercial effect is good;
(4) adopt the present invention, production technique is short, equipment is simple, less energy consumption, cost are low, is suitable for industrialized production, easily operates, practical.
Embodiment
The invention will be further described for embodiment plan given below; but can not be interpreted as it is limiting the scope of the invention; some nonessential improvement and adjustment that person skilled in art makes the present invention according to the content of the invention described above, still belong to protection scope of the present invention.
Embodiment 1:
In glass lined reaction vessel, pump into the saturated solution of magnesium sulfate 2000Kg of 60 DEG C, start and stir, slowly add mass concentration be 90% sulfuric acid 760Kg or mass concentration be 98% sulfuric acid 650Kg, continue stirring reaction 1 hour after reinforced.Then pump into plate-and-frame filter press while hot to filter, filter the backward plate-and-frame filter press of end and pump into the saturated solution of magnesium sulfate washing leaching cake of 70 DEG C once, then use tap water 1-2 time, merging filtrate and washing lotion, return for the production of magnesium sulfate heptahydrate or Adlerika.Take out filter cake and send into vibrating bed moisture eliminator dry 0.5 hour obtained magnesium sulfate monohydrate at 120-150 DEG C.
Embodiment 2:
In glass lined reaction vessel, add the magnesium sulfate heptahydrate of 2000Kg, slowly add mass concentration be 90% sulfuric acid 680Kg or mass concentration be 98% sulfuric acid 600Kg, slowly start stirring reaction 80 minutes after reinforced.Then pump into plate-and-frame filter press while hot to filter, filter the backward plate-and-frame filter press of end and pump into the saturated solution of magnesium sulfate washing leaching cake of 70 DEG C once, then spend tap water 1-2 time, merging filtrate and washing lotion, return for the production of magnesium sulfate heptahydrate or Adlerika.Take out filter cake and send into vibrating bed moisture eliminator dry 0.5 hour obtained magnesium sulfate monohydrate at 120-150 DEG C.
Embodiment 3:
In glass lined reaction vessel, pump into the saturated solution of magnesium sulfate 2000Kg of 80 DEG C, start and stir, slowly add mass concentration be 90% sulfuric acid 720Kg or mass concentration be 98% sulfuric acid 620Kg, continue stirring reaction 80 minutes after reinforced.Then pump into plate-and-frame filter press while hot to filter, filter the backward plate-and-frame filter press of end and pump into the saturated solution of magnesium sulfate washing leaching cake of 70 DEG C once, then use tap water 1-2 time, merging filtrate and washing lotion, return for the production of magnesium sulfate heptahydrate or Adlerika.Take out filter cake and send into vibrating bed moisture eliminator dry 0.5 hour obtained magnesium sulfate monohydrate at 120-150 DEG C.
Embodiment 4:
A production method for magnesium sulfate monohydrate, step is:
A, in glass lined reaction vessel, stir lower slow in 1500 mass parts (such as Kg, the mass percent concentration adding afterwards together) 1200 mass parts in magnesium sulfate heptahydrate is the vitriol oil of 90%, continues stirring reaction 2 hours, obtains the suspension of magnesium sulfate monohydrate;
B, while hot by suspension filtered (can plate-and-frame filter press be adopted), filter cake (after namely filtering the solids that obtains) with the washing of magnesium sulfate saturated aqueous solution once, then wash 1 time with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing dry (vibrating bed moisture eliminator can be adopted) 0.5 hour at the temperature of 120 DEG C, i.e. obtained magnesium sulfate monohydrate.
0.05 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 70 DEG C, consumption is filter cake quality; The quality of described washing leaching cake water is 0.2 times of filter cake quality at every turn.
Embodiment 5:
A production method for magnesium sulfate monohydrate, step is:
A, in glass lined reaction vessel, stir lower slow in 2500 mass parts (such as Kg, the mass percent concentration adding afterwards together) 3500 mass parts in magnesium sulfate heptahydrate is the vitriol oil of 98%, continues stirring reaction 1 hour, obtains the suspension of magnesium sulfate monohydrate;
B, while hot by suspension filtered (can plate-and-frame filter press be adopted), filter cake (after namely filtering the solids that obtains) with the washing of magnesium sulfate saturated aqueous solution once, then wash 2 times with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing dry (vibrating bed moisture eliminator can be adopted) 1 hour at the temperature of 150 DEG C, i.e. obtained magnesium sulfate monohydrate.
0.2 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 90 DEG C, consumption is filter cake quality; The quality of described washing leaching cake water is 0.5 times of filter cake quality at every turn.
Embodiment 6:
A production method for magnesium sulfate monohydrate, step is:
A, in glass lined reaction vessel, stir lower slow in 2000 mass parts (such as Kg, the mass percent concentration adding afterwards together) 2350 mass parts in magnesium sulfate heptahydrate is the vitriol oil of 94%, continues stirring reaction 1.5 hours, obtains the suspension of magnesium sulfate monohydrate;
B, while hot by suspension filtered (can plate-and-frame filter press be adopted), filter cake (after namely filtering the solids that obtains) with the washing of magnesium sulfate saturated aqueous solution once, then wash 2 times with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing dry (vibrating bed moisture eliminator can be adopted) 0.8 hour at the temperature of 130 DEG C, i.e. obtained magnesium sulfate monohydrate.
0.1 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 80 DEG C, consumption is filter cake quality; The quality of described washing leaching cake water is 0.4 times of filter cake quality at every turn.
Embodiment 7 ~ 13:
A production method for magnesium sulfate monohydrate, step is:
A, in glass lined reaction vessel, stir lower slow in 1500 ~ 2500 mass parts (such as K
g, rear with) mass percent concentration that adds 1200 ~ 3500 mass parts in magnesium sulfate heptahydrate is the vitriol oil of 90%, continue stirring reaction 1 ~ 2 hour, obtain the suspension of magnesium sulfate monohydrate;
In each embodiment, the concrete mass parts consumption of each raw material sees the following form:
B, while hot by suspension filtered (can plate-and-frame filter press be adopted), filter cake (after namely filtering the solids that obtains) with the washing of magnesium sulfate saturated aqueous solution once, then wash 1 ~ 2 time with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing dry (vibrating bed moisture eliminator can be adopted) 0.5 ~ 1 hour at the temperature of 120 ~ 150 DEG C, i.e. obtained magnesium sulfate monohydrate.
0.05 ~ 0.2 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 70 ~ 90 DEG C, consumption is filter cake quality; The quality of described washing leaching cake water is 0.2 ~ 0.5 times of filter cake quality at every turn.
Embodiment 14:
A production method for magnesium sulfate monohydrate, step is:
A, in glass lined reaction vessel, stir lower slow in 1800 mass parts (such as Kg, afterwards with) temperature be the mass percent concentration adding 1200 mass parts in the magnesium sulfate saturated aqueous solution of 50 DEG C be the vitriol oil of 90%, continue stirring reaction 2 hours, obtain the suspension of magnesium sulfate monohydrate;
B, to take advantage of) by suspension filtered (can plate-and-frame filter press be adopted), filter cake (solids obtained after namely filtering) with the washing of magnesium sulfate saturated aqueous solution once, then wash 1 time with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing dry (vibrating bed moisture eliminator can be adopted) 1 hour at the temperature of 120 DEG C, i.e. obtained magnesium sulfate monohydrate;
0.05 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 70 DEG C, consumption is filter cake quality; The quality of described washing leaching cake water is 0.2 times of filter cake quality at every turn.
Embodiment 15:
A production method for magnesium sulfate monohydrate, step is:
A, in glass lined reaction vessel, stir lower slow in 3000 mass parts (such as Kg, afterwards with) temperature be the mass percent concentration adding 3500 mass parts in the magnesium sulfate saturated aqueous solution of 90 DEG C be the vitriol oil of 98%, continue stirring reaction 1 hour, obtain the suspension of magnesium sulfate monohydrate;
B, to take advantage of) by suspension filtered (can plate-and-frame filter press be adopted), filter cake (solids obtained after namely filtering) with the washing of magnesium sulfate saturated aqueous solution once, then wash 2 times with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing dry (vibrating bed moisture eliminator can be adopted) 0.5 hour at the temperature of 150 DEG C, i.e. obtained magnesium sulfate monohydrate;
0.2 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 90 DEG C, consumption is filter cake quality; The quality of described washing leaching cake water is 0.5 times of filter cake quality at every turn.
Embodiment 16:
A production method for magnesium sulfate monohydrate, step is:
A, in glass lined reaction vessel, stir lower slow in 2400 mass parts (such as Kg, afterwards with) temperature be the mass percent concentration adding 2350 mass parts in the magnesium sulfate saturated aqueous solution of 70 DEG C be the vitriol oil of 95%, continue stirring reaction 1.5 hours, obtain the suspension of magnesium sulfate monohydrate;
B, to take advantage of) by suspension filtered (can plate-and-frame filter press be adopted), filter cake (solids obtained after namely filtering) with the washing of magnesium sulfate saturated aqueous solution once, then wash 2 times with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing dry (vibrating bed moisture eliminator can be adopted) 0.8 hour at the temperature of 130 DEG C, i.e. obtained magnesium sulfate monohydrate;
0.1 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 70 ~ 90 DEG C, consumption is filter cake quality; The quality of described washing leaching cake water is 0.4 times of filter cake quality at every turn.
Embodiment 17 ~ 23:
A production method for magnesium sulfate monohydrate, step is:
A, in glass lined reaction vessel, stir lower slow in 1800 ~ 3000 mass parts (such as Kg, afterwards with) temperature be the mass percent concentration adding 1200 ~ 3500 mass parts in the magnesium sulfate saturated aqueous solution of 50 ~ 90 DEG C be the vitriol oil of 98%, continue stirring reaction 1 ~ 2 hour, obtain the suspension of magnesium sulfate monohydrate;
In each embodiment, the concrete mass parts consumption of each raw material sees the following form:
B, to take advantage of) by suspension filtered (can plate-and-frame filter press be adopted), filter cake (solids obtained after namely filtering) with the washing of magnesium sulfate saturated aqueous solution once, then wash 1 ~ 2 time with water; Merging filtrate and washings, the aqueous solution of step a for the production of magnesium sulfate heptahydrate or magnesium sulfate can be returned;
C, by the filter cake after washing dry (vibrating bed moisture eliminator can be adopted) 0.5 ~ 1 hour at the temperature of 120 ~ 150 DEG C, i.e. obtained magnesium sulfate monohydrate;
0.05 ~ 0.2 times that the temperature of the magnesium sulfate of washing leaching cake described in step b saturated aqueous solution is 70 ~ 90 DEG C, consumption is filter cake quality; The quality of described washing leaching cake water is 0.2 ~ 0.5 times of filter cake quality at every turn.
In above-described embodiment: each raw material adopted is commercially available prod.
In above-described embodiment: in the percentage adopted, do not indicate especially, be quality (weight) percentage or well known to a person skilled in the art percentage; Described quality (weight) part can be all gram or kilogram.
In above-described embodiment: the processing parameter (temperature, time, concentration etc.) in each step and each component raw material numerical quantity etc. are scope, and any point is all applicable.
The concrete same prior art of technology contents described in content of the present invention and above-described embodiment.
The invention is not restricted to above-described embodiment, all can implement described in content of the present invention and there is described good result.
Claims (4)
1. a production method for magnesium sulfate monohydrate, is characterized in that step is:
The mass percent concentration adding 1200 ~ 3500 mass parts under a, stirring in 1500 ~ 2500 mass parts magnesium sulfate heptahydrates is the vitriol oil of 90% ~ 98%, and stirring reaction 1 ~ 2 hour, obtains the suspension of magnesium sulfate monohydrate;
B, by suspension filtered, filter cake with magnesium sulfate saturated aqueous solution washing once, then wash 1 ~ 2 time with water;
C, by the filter cake after washing at the temperature of 120 ~ 150 DEG C dry 0.5 ~ 1 hour, i.e. obtained magnesium sulfate monohydrate.
2. by the production method of magnesium sulfate monohydrate described in claim 1, it is characterized in that: in step b, the temperature of washing leaching cake magnesium sulfate saturated aqueous solution is 70 ~ 90 DEG C, consumption is 0.05 ~ 0.2 times of filter cake quality.
3. by the production method of magnesium sulfate monohydrate described in claim 1 or 2, it is characterized in that: in step b, the quality of washing leaching cake water is 0.2 ~ 0.5 times of filter cake quality at every turn.
4. a production method for magnesium sulfate monohydrate, is characterized in that step is:
A, stir under be the mass percent concentration adding 1200 ~ 3500 mass parts in the magnesium sulfate saturated aqueous solution of 50 ~ 90 DEG C to the temperature of 1800 ~ 3000 mass parts be the vitriol oil of 90% ~ 98%, continue stirring reaction 1 ~ 2 hour, obtain the suspension of magnesium sulfate monohydrate;
B, by suspension filtered, filter cake with magnesium sulfate saturated aqueous solution washing once, then wash 1 ~ 2 time with water;
0.05 ~ 0.2 times that the temperature of washing leaching cake magnesium sulfate saturated aqueous solution is 70 ~ 90 DEG C, consumption is filter cake quality;
The quality of washing leaching cake water is 0.2 ~ 0.5 times of filter cake quality at every turn;
C, by the filter cake after washing at the temperature of 120 ~ 150 DEG C dry 0.5 ~ 1 hour, i.e. obtained magnesium sulfate monohydrate.
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CN115353131B (en) * | 2022-09-14 | 2023-09-12 | 丹东金辽化工有限公司 | Production method of magnesium sulfate monohydrate |
Citations (4)
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---|---|---|---|---|
CN1109845A (en) * | 1994-11-09 | 1995-10-11 | 郑州工学院 | Process for directly producing magnesium sulfate monohydrate |
RU2104936C1 (en) * | 1996-11-13 | 1998-02-20 | Акционерное общество "БХЗ" | Method for production of magnesium sulfate |
CN103232048A (en) * | 2013-05-07 | 2013-08-07 | 中国科学院青海盐湖研究所 | Process for recovering magnesium sulfate monohydrate from boron extraction mother liquor |
CN103803612A (en) * | 2012-11-15 | 2014-05-21 | 朱振明 | Preparation method of basic magnesium sulfate |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
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KR100388035B1 (en) * | 1998-12-23 | 2003-09-19 | 주식회사 포스코 | Method for preparing magnesium sulfate aqueous solution from magnesia chromium waste refractory |
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2014
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1109845A (en) * | 1994-11-09 | 1995-10-11 | 郑州工学院 | Process for directly producing magnesium sulfate monohydrate |
RU2104936C1 (en) * | 1996-11-13 | 1998-02-20 | Акционерное общество "БХЗ" | Method for production of magnesium sulfate |
CN103803612A (en) * | 2012-11-15 | 2014-05-21 | 朱振明 | Preparation method of basic magnesium sulfate |
CN103232048A (en) * | 2013-05-07 | 2013-08-07 | 中国科学院青海盐湖研究所 | Process for recovering magnesium sulfate monohydrate from boron extraction mother liquor |
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