CN1248966C - Halogen-blended process of preparing low-sodium carnallite - Google Patents

Halogen-blended process of preparing low-sodium carnallite Download PDF

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CN1248966C
CN1248966C CN 200410065204 CN200410065204A CN1248966C CN 1248966 C CN1248966 C CN 1248966C CN 200410065204 CN200410065204 CN 200410065204 CN 200410065204 A CN200410065204 A CN 200410065204A CN 1248966 C CN1248966 C CN 1248966C
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bittern
halogen
salt
sodium
converting
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CN1608995A (en
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宋文义
郑世波
张红茹
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Lianyungang Design And Research Institute Of Ministry Of Chemical Industry
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Lianyungang Design And Research Institute Of Ministry Of Chemical Industry
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Abstract

The present invention discloses a method for preparing low-sodium carnallite by mixing bittern. The present invention is characterized in that after solid salt is separated out of collected nagnesium sulfate subtype bittern by solarization on a salt field and natural evaporation, the percentage composition of the magnesium ion Mg<++> in the bittern is not less than 7.0 percent, and aged bittern is obtained; then, a bittern mixing crystallization reaction between the aged bittern and the bittern with the crystallizing point of potassium mixed salt is carried out according the weight proportion of (1 to 3): 1, and the low-sodium carnallite is obtained by filtering. The present invention has the advantages of simple process and convenient operation; the product of the low-sodium carnallite can be produced from the bittern directly, and the product purity of the low-sodium carnallite of which the content of the sodium chloride is 1.35 percent can reach 98 percent in maximum; the product does not comprise a flotation agent, and the added value of the product is high; the maximum recovery rate of potassium ion (K<+>) in the process of bittern mixing in a single time can reach 66.50 percent; the technique does not have environment pollution, and the present invention is favorable for building a green processing plant.

Description

A kind of method of preparing low sodium carnallite by blending halogen
Technical field
The present invention relates to a kind of preparation method of carnallitite, particularly a kind of method that adopts adding halogen method to produce low-sodium carnalite.
Background technology
In the prior art, publication number is 1275531, application number is that 00112360.2 Chinese patent application discloses a kind of name and is called " can directly produce low sodium; the method for high-quality carnallitite ", it is a kind ofly can the solid bischofite be joined among the carnallitite crystallisation stage bittern at normal temperatures and pressures, after stirring, adjust the variation of charging capacity with the degree Beaume measurement, can discharging carry out liquid-solid separation after meeting the requirements of degree Beaume, the solid phase of its gained is the finished product low-sodium carnalite, the high-quality carnallitite, liquid phase of discharging and overflowing liquid merge and old halogen, and old halogen can be made the solid water chloromagnesite again and recycle.This method requires bischofite purer, be that the content of NaCl and insolubles is less in the bischofite, otherwise bischofite need be dissolved to required degree Beaume separately, then insolubles is removed, convert halogen with the bittern that carnallitite is selected again with its clear liquid, could obtain low-sodium carnalite, make technical process become comparatively complicated like this.And when bischofite is dissolved to required degree Beaume, want to remove the insolubles part, certainly will cause clear liquid loss (because of filter do not do absorption mother liquor content higher due to), cause the consumption of bischofite to increase thus, the cost of low-sodium carnalite raises.
Summary of the invention
Technical problem to be solved by this invention is at the deficiencies in the prior art, and the method for a kind of preparing low sodium carnallite by blending halogen that a kind of technology is simple, product purity is high, the rate of recovery is high is provided.
Technical problem to be solved by this invention is to realize by following technical scheme.The present invention is a kind of method of preparing low sodium carnallite by blending halogen, is characterized in, the magnesium sulfate bittern of gathering is separated out solid salt (sodium chloride nacl, epsom salt MgSO by the solarization of beach, salt pan, spontaneous evaporation 47H 2O, schoenite K 2SO 4MgSO 46H 2O, kainite KClMgSO 43H 2O, carnallitite KClMgCl 26H 2O etc.) after, make the magnesium ion Mg in the bittern 2+Percentage composition is not less than 7.0%, gets old halogen; Then that old halogen and sodium-chlor, Repone K, epsom salt and schoenite is saturated altogether potassium mixed salt select bittern by weight (1-3): 1 converts the halogen crystallization reaction, and filtration promptly gets low-sodium carnalite; Potassium ion K in the described potassium mixed salt point bittern +Percentage composition be not less than 0.5%, magnesium ion Mg 2+Percentage composition be 5.0-7.7%.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described method is characterized in, the described halogen crystallization reaction of converting is to carry out in converting the halogen container.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described method is characterized in, old halogen and potassium mixed salt is selected bittern add and carry out the complete mixing flow continuously stirring after converting the halogen container, and the time of stirring is 0.5-2 hour.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described method is characterized in, the described halogen crystallization reaction of converting carries out under 10-40 ℃ temperature.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described method is characterized in, the halogen of converting that filters the back gained is finished liquid and returned the beach, salt pan and shine.
Compared with prior art, technology of the present invention is simple, and is easy to operate, can directly produce the low-sodium carnalite product from bittern, and its sodium chloride content is 1.35%, and product purity reaches as high as 98%, does not contain flotation reagent, value-added content of product height in the product; Convert the potassium ion (K in the halogen process +) the high-recovery of single can reach 66.50%; This technology does not have environmental pollution, helps building up green processing factory.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
The following examples have further described summary of the invention of the present invention according to accompanying drawing.
Embodiment 1.A kind of method of preparing low sodium carnallite by blending halogen is shone the magnesium sulfate bittern gathered, after spontaneous evaporation separates out solid salt, make the magnesium ion Mg in the bittern by the beach, salt pan 2+Percentage composition is 7.0%, gets old halogen; Then that old halogen and sodium-chlor, Repone K, epsom salt and schoenite is saturated altogether potassium mixed salt select bittern and was converted the halogen crystallization reaction by weight 2: 1, and filtration promptly gets low-sodium carnalite.
Embodiment 2.A kind of method of preparing low sodium carnallite by blending halogen is separated out solid salt sodium chloride nacl, epsom salt MgSO with the magnesium sulfate bittern of gathering by the solarization of beach, salt pan, spontaneous evaporation 47H 2O, schoenite K 2SO 4MgSO 46H 2O, kainite KClMgSO 43H 2O, carnallitite KClMgCl 26H 2Behind the O etc., make the magnesium ion Mg in the bittern 2+Percentage composition is 8.0%, gets old halogen; Then that old halogen and sodium-chlor, Repone K, epsom salt and schoenite is saturated altogether potassium mixed salt select bittern and is joined at 1: 1 by weight and convert in the halogen container, under 10 ℃ temperature, carried out the complete mixing flow continuously stirring 0.5 hour, filter and promptly get low-sodium carnalite, the saltwater brine of converting that filters the back gained is returned the solarization of beach, salt pan.Potassium ion K in the described potassium mixed salt point of the present embodiment bittern +Percentage composition be 0.5%, magnesium ion Mg 2+Percentage composition be 5.0%.
Embodiment 3.A kind of method of preparing low sodium carnallite by blending halogen is separated out solid salt sodium chloride nacl, epsom salt MgSO with the magnesium sulfate bittern of gathering by the solarization of beach, salt pan, spontaneous evaporation 47H 2O, schoenite K 2SO 4MgSO 46H 2O, kainite KClMgSO 43H 2O carnallitite KClMgCl 26H 2Behind the O etc., make the magnesium ion Mg in the bittern 2+Percentage composition is 9.0%, gets old halogen; Then that old halogen and sodium-chlor, Repone K, epsom salt and schoenite is saturated altogether potassium mixed salt select bittern and is joined at 3: 1 by weight and convert in the halogen container, under 40 ℃ temperature, carried out the complete mixing flow continuously stirring 2 hours, filter and promptly get low-sodium carnalite, the saltwater brine of converting that filters the back gained is returned the solarization of beach, salt pan.Potassium ion K in the described potassium mixed salt point of the present embodiment bittern +Percentage composition be 0.6%, magnesium ion Mg 2+Percentage composition be 7.7%.
Embodiment 4.A kind of method of preparing low sodium carnallite by blending halogen is separated out solid salt sodium chloride nacl, epsom salt MgSO with the magnesium sulfate bittern of gathering by the solarization of beach, salt pan, spontaneous evaporation 47H 2O, schoenite K 2SO 4MgSO 46H 2O, kainite KClMgSO 43H 2O, carnallitite KClMgCl 26H 2Behind the O etc., make the magnesium ion Mg in the bittern 2+Percentage composition is 9.5%, gets old halogen; Then that old halogen and sodium-chlor, Repone K, epsom salt and schoenite is saturated altogether potassium mixed salt select bittern and is joined at 2.5: 1 by weight and convert in the halogen container, under 25 ℃ temperature, carried out the complete mixing flow continuously stirring 1 hour, filter and promptly get low-sodium carnalite, the saltwater brine of converting that filters the back gained is returned the solarization of beach, salt pan.Potassium ion K in the described potassium mixed salt point of the present embodiment bittern +Percentage composition be 0.7%, magnesium ion Mg 2+Percentage composition be 6.5%.
Embodiment 5.The magnesium sulfate bittern of present embodiment is selected Lop Nur, Xinjiang salt lake brine for use, and its beach solarization, spontaneous evaporation are separated out to solid salt and finished, and it consists of the bittern (being called for short old halogen) of this moment: potassium ion (K +) 0.29%, sodium ion (Na +) 0.32%, magnesium ion (Mg 2+) 8.31%, chlorion (Cl -) 22.19%, sulfate ion (SO 4 2-) 3.77%, water (H 2O) 65.12%; Potassium mixed salt point bittern consists of: potassium ion (K +) 0.65%, sodium ion (Na +) 0.71%, magnesium ion (Mg 2+) 5.73%, chlorion (Cl -) 16.94%, sulfate ion (SO 4 2-) 2.02%, water (H 2O) 73.95%, in converting the halogen container according to old halogen and sodium-chlor, Repone K, epsom salt and schoenite altogether the weight ratio of saturated potassium mixed salt point bittern be 3: 1 mixed, electronic at ambient temperature stirring 1.5 hours, filter then and can obtain low-sodium carnalite, product purity reaches 97%, converts the potassium ion (K in the halogen process +) the single rate of recovery is 11.15%.
Embodiment 6.The magnesium sulfate bittern of present embodiment is selected Lop Nur, Xinjiang salt lake brine for use, its beach solarization, spontaneous evaporation is separated out to carnallitite and is finished, and then continue one section of evaporation, and the bittern of this moment consists of: potassium ion (K +) 0.13%, sodium ion (Na +) 0.18%, magnesium ion (Mg 2+) 8.79%, chlorion (Cl -) 23.28%, sulfate ion (SO 4 2-) 3.39%, water (H 2O) 64.23%; Potassium mixed salt point bittern consists of: potassium ion (K +) 1.91%, sodium ion (Na +) 0.71%, magnesium ion (Mg 2+) 7.11%, chlorion (Cl -) 18.94%, sulfate ion (SO 4 2-) 4.87%, water (H 2O) 66.46%, in converting the halogen container according to old halogen and sodium-chlor, Repone K, epsom salt and schoenite altogether the weight ratio of saturated potassium mixed salt point bittern be 1.5: 1 mixed, electronic at ambient temperature stirring 1 hour, filter then and can obtain low-sodium carnalite, product purity reaches 97.37%, converts the potassium ion (K in the halogen process +) the single rate of recovery is 32.16%.
Embodiment 7.In the present embodiment, magnesium sulfate bittern is selected Lop Nur, Xinjiang salt lake brine for use, its beach solarization, spontaneous evaporation is separated out to carnallitite and is finished, and then continue one section of evaporation.The bittern of this moment consists of: potassium ion (K +) 0.06%, sodium ion (Na +) 0.10%, magnesium ion (Mg 2+) 9.24%, chlorion (Cl -) 24.95%, sulfate ion (SO 1 2-) 2.59%, water (H 2O) 63.06%; Potassium mixed salt point bittern consists of: potassium ion (K +) 2.44%, sodium ion (Na +) 1.14%, magnesium ion (Mg 2+) 6.65%, chlorion (Cl -) 17.59%, sulfate ion (SO 1 2-) 6.18%, water (H 2O) 66.0%, in converting the halogen container according to old halogen and sodium-chlor, Repone K, epsom salt and schoenite altogether the weight ratio of saturated potassium mixed salt point bittern be 1.5: 1 mixed, electronic at ambient temperature stirring 0.5 hour, filter then and can obtain low-sodium carnalite, product purity reaches 94.06%, converts the potassium ion (K in the halogen process +) the single rate of recovery is 50.99%.

Claims (5)

1, a kind of method of preparing low sodium carnallite by blending halogen is characterized in that, the magnesium sulfate bittern gathered is shone, after spontaneous evaporation separates out solid salt, makes the magnesium ion Mg in the bittern by the beach, salt pan 2+Percentage composition is not less than 7.0%, gets old halogen; Then that old halogen and sodium-chlor, Repone K, epsom salt and schoenite is saturated altogether potassium mixed salt select bittern by weight (1-3): 1 converts the halogen crystallization reaction, and filtration promptly gets low-sodium carnalite; The percentage composition of potassium ion K+ is not less than 0.5%, magnesium ion Mg in the described potassium mixed salt point bittern 2+Percentage composition be 5.0-7.7%.
2, method according to claim 1 is characterized in that, the described halogen crystallization reaction of converting is to carry out in converting the halogen container.
3, method according to claim 2 is characterized in that, old halogen and potassium mixed salt is selected bittern add and carry out the complete mixing flow continuously stirring after converting the halogen container, and the time of stirring is 0.5-2 hour.
4, method according to claim 1 is characterized in that, the described halogen crystallization reaction of converting carries out under 10-40 ℃ temperature.
5, method according to claim 1 is characterized in that, the halogen of converting that filters the back gained is finished liquid and returned the beach, salt pan and shine.
CN 200410065204 2004-10-28 2004-10-28 Halogen-blended process of preparing low-sodium carnallite Active CN1248966C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11851340B2 (en) 2020-05-06 2023-12-26 Qinghai Institute Of Salt Lakes, Chinese Academy Of Sciences Method for preparing potassium chloride from carnallite

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100383044C (en) * 2005-07-25 2008-04-23 魏新俊 Method for producing carnallite in low sodium or potassium chloride by using brine of containing potassium
CN100335411C (en) * 2005-07-30 2007-09-05 中蓝连海设计研究院 Method of preparing low sodium carnallite by blending halogen
CN104477941B (en) * 2014-12-16 2016-02-03 中国科学院青海盐湖研究所 A kind of method utilizing potassium mixed salt cryogenic freezing to produce carnallite
CN104743580B (en) * 2015-03-13 2016-11-09 陈杰 A kind of extract the method reclaiming salt lake tail salt, leaving over potassium chloride in useless carnallite
CN104891532A (en) * 2015-05-29 2015-09-09 中国科学院青海盐湖研究所 Method for preparing carnallite by converting picromerite mineral and high-magnesium solution
CN111229144A (en) * 2020-01-20 2020-06-05 西安建筑科技大学 Device and method for producing carnallite by blending brine

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11851340B2 (en) 2020-05-06 2023-12-26 Qinghai Institute Of Salt Lakes, Chinese Academy Of Sciences Method for preparing potassium chloride from carnallite

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