CN1608995A - Halogen-blended process of preparing low-sodium carnallite - Google Patents

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

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CN1608995A
CN1608995A CN 200410065204 CN200410065204A CN1608995A CN 1608995 A CN1608995 A CN 1608995A CN 200410065204 CN200410065204 CN 200410065204 CN 200410065204 A CN200410065204 A CN 200410065204A CN 1608995 A CN1608995 A CN 1608995A
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halogen
bittern
salt
sodium
ion
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CN 200410065204
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CN1248966C (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 preparation process of low-sodium carnallite features that the subtype magnesium sulfate bittern as material is prepared into low-sodium carnallite through natural evaporation in saltern to separate out solid salt and to obtain bittern with Mg ion content not less than 7.0 %, subsequent blending with mixed potassium salt in the weight ratio of 1-3 to produce crystallization reaction, and filtering. The present invention has simple process and convenient operation, and the low-sodium carnallite product produced directly from bittern has sodium chloride content of 1.35 %, purity up to 98 % and no floatation chemical contained. The blending process has single time potassium ion recovering rate up to 66.50 %. The said technological process has no environmental pollution.

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 4.7H 2O, schoenite K 2SO 4.MgSO 4.6H 2O, kainite KCl.MgSO 4.3H 2O, carnallitite KCl.MgCl 2.6H 2O etc.) after, make the magnesium ion Mg in the bittern ++Percentage composition is not less than 7.0%, gets old halogen; Then old halogen and potassium mixed salt are selected bittern (1-3) by weight: 1 converts the halogen crystallization reaction, filters promptly to get low-sodium carnalite.Described potassium mixed salt is selected the common saturation point bittern that bittern is meant sodium-chlor, Repone K, epsom salt and schoenite.
Technical problem to be solved by this invention can also further realize by following technical scheme.Above-described method is characterized in, potassium ion K in the described potassium mixed salt point bittern +Percentage composition be not less than 0.5%, magnesium ion Mg ++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 ++Percentage composition is 7.0%, gets old halogen; Then old halogen and potassium mixed salt are selected bittern and converted the halogen crystallization reaction by weight 2: 1, filter and promptly get 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 4.7H 2O, schoenite K 2SO 4.MgSO 4.6H 2O, kainite KCl.MgSO 4.3H 2O, carnallitite KCl.MgCl 2.6H 2Behind the O etc., make the magnesium ion Mg in the bittern ++Percentage composition is 8.0%, gets old halogen; Then old halogen and potassium mixed salt are selected bittern and joined by weight 1: 1 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 ++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 4.7H 2O, schoenite K 2SO 4.MgSO 4.6H 2O, kainite KCl.MgSO 4.3H 2O, carnallitite KCl.MgCl 2.6H 2Behind the O etc., make the magnesium ion Mg in the bittern ++Percentage composition is 9.0%, gets old halogen; Then old halogen and potassium mixed salt are selected bittern and joined by weight 3: 1 and convert in the halogen container, under the temperature of 40C, 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 ++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 4.7H 2O, schoenite K 2SO 4.MgSO 4.6H 2O, kainite KCl.MgSO 4.3H 2O, carnallitite KCl.MgCl 2.6H 2Behind the O etc., make the magnesium ion Mg in the bittern ++Percentage composition is 9.5%, gets old halogen; Then old halogen and potassium mixed salt are selected bittern and joined by weight 2.5: 1 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 ++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 ++) 8.31%, chlorion (Cl -) 22.19%, sulfate ion (SO 4 =) 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 ++) 5.73%, chlorion (Cl -) 16.94%, sulfate ion (SO 4 =) 2.02%, water (H 2O) 73.95%, in converting the halogen container be 3: 1 mixed according to the weight ratio of old halogen and potassium mixed salt point bittern, electronic at ambient temperature stirring 1.5 hours is filtered then and can be obtained 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 ++) 8.79%, chlorion (Cl -) 23.28%, sulfate ion (SO 4 =) 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 ++) 7.11%, chlorion (Cl -) 18.94%, sulfate ion (SO 4 =) 4.87%, water (H 2O) 66.46%, in converting the halogen container be 1.5: 1 mixed according to the weight ratio of old halogen and potassium mixed salt point bittern, electronic at ambient temperature stirring 1 hour is filtered then and can be obtained 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 ++) 9.24%, chlorion (Cl -) 24.95%, sulfate ion (SO 4 =) 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 ++) 6.65%, chlorion (Cl -) 17.59%, sulfate ion (SO 4 =) 6.18%, water (H 2O) 66.0%, in converting the halogen container be 1.5: 1 mixed according to the weight ratio of old halogen and potassium mixed salt point bittern, electronic at ambient temperature stirring 0.5 hour is filtered then and can be obtained 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 (6)

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 ++Percentage composition is not less than 7.0%, gets old halogen; Then old halogen and potassium mixed salt are selected bittern (1-3) by weight: 1 converts the halogen crystallization reaction, filters promptly to get low-sodium carnalite.
2, method according to claim 1 is characterized in that, potassium ion K in the described potassium mixed salt point bittern +Percentage composition be not less than 0.5%, magnesium ion Mg ++Percentage composition be 5.0-7.7%.
3, 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.
4, method according to claim 3 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.
5, method according to claim 1 is characterized in that, the described halogen crystallization reaction of converting carries out under 10-40 ℃ temperature.
6, 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 Expired - Lifetime CN1248966C (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
CN104477941A (en) * 2014-12-16 2015-04-01 中国科学院青海盐湖研究所 Method for preparing carnallite from potassium mixed salts by low-temperature refrigeration
CN104743580A (en) * 2015-03-13 2015-07-01 陈杰 Method for extracting and recycling residual potassium chloride from salt-lake tail salt and waste 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
CN111533138A (en) * 2020-05-06 2020-08-14 中国科学院青海盐湖研究所 Method for preparing potassium chloride by utilizing carnallite

Cited By (10)

* 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
CN104477941A (en) * 2014-12-16 2015-04-01 中国科学院青海盐湖研究所 Method for preparing carnallite from potassium mixed salts by low-temperature refrigeration
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
CN104743580A (en) * 2015-03-13 2015-07-01 陈杰 Method for extracting and recycling residual potassium chloride from salt-lake tail salt and waste 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
CN111533138A (en) * 2020-05-06 2020-08-14 中国科学院青海盐湖研究所 Method for preparing potassium chloride by utilizing carnallite
CN111533138B (en) * 2020-05-06 2022-08-26 中国科学院青海盐湖研究所 Method for preparing potassium chloride by utilizing carnallite
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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