CN100595152C - Method for preparing magnesium sulfuric acid monohydrate with mixture salt of sodium chloride and epsomite - Google Patents
Method for preparing magnesium sulfuric acid monohydrate with mixture salt of sodium chloride and epsomite Download PDFInfo
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- CN100595152C CN100595152C CN200810031775A CN200810031775A CN100595152C CN 100595152 C CN100595152 C CN 100595152C CN 200810031775 A CN200810031775 A CN 200810031775A CN 200810031775 A CN200810031775 A CN 200810031775A CN 100595152 C CN100595152 C CN 100595152C
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- salt
- magnesium sulfate
- sulfate monohydrate
- chlor
- sodium
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Abstract
The invention relates to a method for preparing magnesium sulfate monohydrate by utilization of salt-mixture of sodium chloride and epsomite, comprising the following steps: firstly, the salt-mixtureof raw materials sodium chloride and epsomite is uniformly mixed; secondly, mixture is prepared by the following raw materials by weight portion: 545 to 555 portions of the salt-mixture, 246 to 256 portions of water and 535 to 545 portions of brine; thirdly, the prepared mixture material is heated up to between 74 and 76 DEG C so as to promote dissolution of the salt-mixture; fourthly, undissolvedNaCl is filtered; fifthly, mother liquor after the undissolved NaCl is filtered is heated up to between 74 and 76 DEG C and then evaporated and concentrated until fine grains, namely the magnesium sulfate monohydrate, and rough grains, namely the sodium chloride are crystallized; sixthly, after filtration, mixture of the fine grains, namely the magnesium sulfate monohydrate, and the rough grains,namely the sodium chloride is obtained; and seventhly, a standard sieve with 325 meshes is adopted for sieving at a temperature of between 74 and 76, with the sodium chloride as oversize materials, and undersize materials are dried at a temperature of between 74 and 76 so as to obtain the magnesium sulfate monohydrate product. The method has mild operating conditions, low energy consumption, lowproduction cost, no liquid waste emission, and no environmental pollution.
Description
Technical field
The present invention relates to a kind of mixing salt that utilizes sodium-chlor and epsom salt and produce the method for magnesium sulfate monohydrate.
Background technology
Sal epsom is widely used in a series of production fields such as medicine, leather and feed, is one of basic chemical raw materials of industrial and agricultural production.
At present, the production of magnesium sulfate monohydrate normally prepares epsom salt earlier, then, crystal water is taken off in the epsom salt heating, obtains magnesium sulfate monohydrate.
Being heated to 75 ℃ of evaporating, concentrating and crystallizings by bittern, obtaining magnesium sulfate monohydrate, is the novel process of present domestic production magnesium sulfate monohydrate.The raw brine of this process using must be low sodium high-magnesium brine, and promptly the content to sodium-chlor and epsom salt has certain requirement, and this material is at 75 ℃ of following Na usually
+, Mg
2+//Cl
-, SO
4 2----H
2Na in loca position and the phasor in the O quaternary system phasor
2Cl
2The line extended line on summit can not drop on bloedite district or process bloedite district, otherwise crystallization goes out bloedite, and can not get magnesium sulfate monohydrate or magnesium sulfate heptahydrate.At the above-mentioned mixing salt that contains bittern water or sodium-chlor and epsom salt that is unsuitable for direct evaporation, concentrates the generation magnesium sulfate monohydrate, the effective ways of taking at present are to adopt method for floating that sodium-chlor is separated with epsom salt, obtain the purified epsom salt, then the epsom salt concentrate that obtains is made with extra care by the chemical industry method again, thereby made magnesium sulfate monohydrate or magnesium sulfate heptahydrate.This method energy consumption is higher, and production cost is also higher, and the waste liquid environmental pollution of discharging is heavier.
Summary of the invention
The objective of the invention is to overcome the defective that prior art exists, a kind of operational condition gentleness is provided, energy consumption is low, and production cost is low, and the mixing salt that utilizes sodium-chlor and epsom salt of no discharging of waste liquid is produced the method for magnesium sulfate monohydrate.
The objective of the invention is to be achieved through the following technical solutions, it may further comprise the steps 2 (1) the mixing salt mixings with raw material sodium-chlor and epsom salt; (2) batching is pressed mixing salt 545-555 weight part (preferred 551.32 weight parts), fresh water 246-256 weight part (preferred 255.34 weight parts) weight part, bittern 535-545 weight part (preferred 540.46 weight parts) preparation; (3) mixture with the preparation of (2) step is heated to 74 ℃-76 ℃ (preferred 75 ℃), promotes the mixing salt dissolving; (4) undissolved NaCl is filtered out; (5) mother liquor that elimination is not dissolved behind the NaCl is heated to 74 ℃-76 ℃ (preferred 75 ℃), and evaporation concentration (should select vacuum-evaporation for use, to accelerate evaporation concentration speed) goes out particulate magnesium sulfate monohydrate and coarse grain sodium-chlor until crystallization; (6) filter, get particulate magnesium sulfate monohydrate and coarse grain sodium chloride mixture; (7) adopt 325 purpose standard sieves to sieve under 74 ℃-76 ℃ (preferred 75 ℃), screen overflow is a sodium-chlor, and screen underflow is dried through 74-76 ℃ (preferred 75 ℃), promptly gets magnesium sulfate monohydrate.
Described bittern can be the discharging mother liquor (be commonly called as old halogen, main component is a magnesium chloride) behind salt pan processing evaporative crystallization Repone K, the schoenite; Also can be the saturated mother liquor of magnesium chloride (for example, add fresh water and be made into saturated solution) with the bischofite solid salt with artificial preparation.
Mother liquor after (6) step filtered can return and be used for batching, like this, has both helped being lowered into production cost, avoids contaminate environment again.
The present invention is chosen in 75 ℃ of following Na
+, Mg
2+//Cl
-, SO
4 2----H
2O quaternary system phasor (as shown in Figure 1) is as theoretical direction.Raw material is formed J value S point in phasor, and this point is positioned at the NaCl crystallizing field, according to the phase diagram theory analysis, adding old halogen point M is that circulating mother liquor makes system point be positioned at the P point, by adding an amount of water raw material is partly dissolved, the NaCl major part remains in the solid phase, and filtrate N separates out NaCl and MgSO by evaporation
4H
2O, mother liquor M is for recycle next time.
The present invention is to the raw material wide accommodation, and it is also suitable that the sodium-chlor and the mixing salt of epsom salt that utilize low sodium are produced magnesium sulfate monohydrate.
Operational condition gentleness of the present invention, energy consumption is low, and production cost is low, no discharging of waste liquid, environmentally safe.
Description of drawings
Fig. 1 is 75 ℃ of following Na
+, Mg
2+//Cl
-, SO
4 2--H
2O quaternary system phasor;
Fig. 2 is embodiment 1 material balance figure.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
(1) with the abundant mixing of mixing salt (for the mine tailing behind the extraction potassic-magnesian fertilizer) of raw material sodium-chlor and epsom salt, the concrete chemical constitution of raw material sees Table 1; (2) batching takes by weighing mixing salt 551.32g, adds fresh water 255.34g, and bittern (be the discharging mother liquor behind salt pan processing evaporative crystallization Repone K, the schoenite, be commonly called as old halogen, main component is a magnesium chloride) 540.46g stirs; (3) be heated to 75 ℃, thermosol half an hour, promote the mixing salt dissolving; (4) undissolved NaCl is filtered out; (5) mother liquor that elimination is not dissolved behind the NaCl is heated to 75 ℃, and the vacuum multiple-effect evaporation concentrates, until evaporate about 338.2g water (temperature remain on 75 ℃ constant, about 30 minutes of evaporation time), crystallization goes out particulate magnesium sulfate monohydrate and coarse grain sodium-chlor from mother liquor; (7) filter, get particulate magnesium sulfate monohydrate and coarse grain sodium chloride mixture; (8) adopt 325 purpose standard sieves to carry out the heat screening under 75 ℃, screen overflow is a coarse grain sodium-chlor, and screen underflow is the particulate magnesium sulfate monohydrate, through 75 ℃ of oven dry, promptly gets the sulfuric acid monohydrate magnesium products.Mother liquor enters circulation next time, and its material balance is seen Fig. 2.
Table 1 embodiment 1 raw material chemical constitution
| Title | 2Na + | SO 4 2- | 2Cl - | Mg 2+ | H 2O |
| w(％) | 28.82 | 6.55 | 45.92 | 2.17 | 16.54 |
| The J value | 87.53 | 9.53 | 90.47 | 12.47 | 64.18 |
Above-mentioned material balance chemical analysis data sees Table 2.
Table 2 embodiment 1 material chemical analysis data
Embodiment 2
(1) with the abundant mixing of mixing salt (mine tailing behind the extraction potassic-magnesian fertilizer) of raw material sodium-chlor and epsom salt, the concrete chemical constitution of raw material sees Table 3; (2) batching takes by weighing mixing salt 546.12g, adds fresh water 247.05g, and bittern (be the discharging mother liquor behind salt pan processing evaporative crystallization Repone K, the schoenite, be commonly called as old halogen, main component is a magnesium chloride) 536.01g stirs; (3) be heated to 75 ℃, thermosol half an hour, promote the mixing salt dissolving; (4) undissolved NaCl is filtered out; (5) mother liquor that elimination is not dissolved behind the NaCl is heated to 75 ℃, and the vacuum multiple-effect evaporation concentrates, until evaporate about 334.1g water (temperature remain on 75 ℃ constant, evaporation time 30 minutes), crystallization goes out particulate magnesium sulfate monohydrate and coarse grain sodium-chlor from mother liquor; (7) filter, get particulate magnesium sulfate monohydrate and coarse grain sodium chloride mixture; (8) adopt 325 purpose standard sieves to carry out the heat screening under 75 ℃, screen overflow is a coarse grain sodium-chlor, and screen underflow is the particulate magnesium sulfate monohydrate, through 75 ℃ of oven dry, promptly gets the sulfuric acid monohydrate magnesium products.Mother liquor enters circulation next time.
Table 3 embodiment 2 raw material chemical constitutions
| Title | 2Na + | SO 4 2- | 2Cl - | Mg 2+ | H 2O |
| w(％) | 27.92 | 6.85 | 46.82 | 2.07 | 16.52 |
| The J value | 87.69 | 13.08 | 86.92 | 12.31 | 64.18 |
Above-mentioned material balance chemical analysis data sees Table 4.
Table 4 embodiment 2 material chemical analysis datas
Embodiment 3
(1) with the abundant mixing of mixing salt (mine tailing behind the extraction potassic-magnesian fertilizer) of raw material sodium-chlor and epsom salt, the concrete chemical constitution of raw material sees Table 5; (2) batching takes by weighing mixing salt 554g, adds fresh water 256g, and bittern (be the discharging mother liquor behind salt pan processing evaporative crystallization Repone K, the schoenite, be commonly called as old halogen, main component is a magnesium chloride) 544.5g stirs; (3) be heated to 75 ℃, thermosol half an hour, promote the mixing salt dissolving; (4) undissolved NaCl is filtered out; (5) mother liquor that elimination is not dissolved behind the NaCl is heated to 75 ℃, and the vacuum multiple-effect evaporation concentrates, until evaporate about 335.2g water (temperature remain on 75 ℃ constant, about 30 minutes of evaporation time), crystallization goes out particulate magnesium sulfate monohydrate and coarse grain sodium-chlor from mother liquor; (7) filter, get particulate magnesium sulfate monohydrate and coarse grain sodium chloride mixture; (8) adopt 325 purpose standard sieves to carry out the heat screening under 75 ℃, screen overflow is a coarse grain sodium-chlor, and screen underflow is the particulate magnesium sulfate monohydrate, through 75 ℃ of oven dry, promptly gets the sulfuric acid monohydrate magnesium products.Mother liquor enters circulation next time.
Table 5 embodiment 3 raw material chemical constitutions
| Title | 2Na + | SO 4 2- | 2Cl - | Mg 2+ | H 2O |
| w(％) | 29.18 | 5.75 | 47.05 | 2.55 | 15.45 |
| The J value | 82.10 | 8.29 | 91.71 | 17.90 | 62.15 |
Above-mentioned material balance chemical analysis data sees Table 6.
Table 6 embodiment 3 material chemical analysis datas
Claims (5)
1. a mixing salt that utilizes sodium-chlor and epsom salt is produced the method for magnesium sulfate monohydrate, and it is characterized in that it may further comprise the steps: (1) is with the mixing salt mixing of raw material sodium-chlor and epsom salt; (2) batching is pressed mixing salt 545-555 weight part, water 246-256 weight part, the preparation of bittern 535-545 weight part; (3) the mixture material with preparation is heated to 74 ℃-76 ℃, promotes the mixing salt dissolving; (4) undissolved NaCl is filtered out; (5) mother liquor that elimination is not dissolved behind the NaCl is heated to 74 ℃-76 ℃, and evaporation concentration goes out particulate magnesium sulfate monohydrate and coarse grain sodium-chlor until crystallization; (6) filter, get particulate magnesium sulfate monohydrate and coarse grain sodium chloride mixture; (7) adopt 325 purpose standard sieves to sieve under 74 ℃-76 ℃, screen overflow is a sodium-chlor, and screen underflow promptly gets the sulfuric acid monohydrate magnesium products through 74 ℃ of-76 ℃ of oven dry.
2. the mixing salt that utilizes sodium-chlor and epsom salt according to claim 1 is produced the method for magnesium sulfate monohydrate, it is characterized in that, in described (2) step, material proportion is: mixing salt 551.32 weight parts, fresh water 255.34 weight parts, bittern 540.46 weight parts.
3. the mixing salt that utilizes sodium-chlor and epsom salt according to claim 1 and 2 is produced the method for magnesium sulfate monohydrate, it is characterized in that, in described (3) step, is heated to 75 ℃; In (5) step, the mother liquor that elimination is not dissolved behind the NaCl is heated to 75 ℃, and vacuum-evaporation concentrates; In (7) step, heat screening temperature is 75 ℃, and screen underflow particulate magnesium sulfate monohydrate bake out temperature also is 75 ℃.
4, the mixing salt that utilizes sodium-chlor and epsom salt according to claim 1 and 2 is produced the method for magnesium sulfate monohydrate, it is characterized in that, described bittern be behind salt pan processing evaporative crystallization Repone K, the schoenite the discharging mother liquor or with the saturated mother liquor of manually preparing of magnesium chloride.
5. the mixing salt that utilizes sodium-chlor and epsom salt according to claim 3 is produced the method for magnesium sulfate monohydrate, it is characterized in that, described bittern be behind salt pan processing evaporative crystallization Repone K, the schoenite the discharging mother liquor or with the saturated mother liquor of manually preparing of magnesium chloride.
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| CN200810031775A CN100595152C (en) | 2008-07-16 | 2008-07-16 | Method for preparing magnesium sulfuric acid monohydrate with mixture salt of sodium chloride and epsomite |
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| CN100595152C true CN100595152C (en) | 2010-03-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2435367B1 (en) * | 2009-05-29 | 2020-12-16 | Cargill, Incorporated | Method of producing naturally purified salt products |
| CN101602617B (en) * | 2009-06-30 | 2011-11-30 | 雅泰实业集团有限公司 | Method for producing potash magnesium sulphate fertilizer |
| CN102757072B (en) * | 2012-08-02 | 2014-02-26 | 化工部长沙设计研究院 | Process for preparing magnesium sulfate heptahydrate |
| CN108455636B (en) * | 2018-01-29 | 2020-05-19 | 天津科技大学 | Method for producing sodium chloride and magnesium sulfate monohydrate by using high-salt high-sulfur brine |
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