CN1171794C - Preparation method of potassium sulfate with sulfate-type salt lake bittern containing potassium salt - Google Patents

Preparation method of potassium sulfate with sulfate-type salt lake bittern containing potassium salt Download PDF

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CN1171794C
CN1171794C CNB011136421A CN01113642A CN1171794C CN 1171794 C CN1171794 C CN 1171794C CN B011136421 A CNB011136421 A CN B011136421A CN 01113642 A CN01113642 A CN 01113642A CN 1171794 C CN1171794 C CN 1171794C
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potassium
flotation
solid
sulfate
sodium chloride
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CN1318515A (en
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宋文义
刘毓
赵士骧
戴芳发
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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 relates to a method for preparing potassium sulfate from sulfate type salt lake bittern containing potassium. Bittern is sunned to prepare the solid of coarse potassium and magnesium mixed salts; the solid is pulverized, conversion liquid is added into milled solid to carry out primary conversion rection, and primary conversion completed material liquid is obtained; flotation is carried out to the primary conversion completed material liquid by a flotation agent for the flotation of picromerite; obtained picromerite is dehydrated into a solid to carry out secondary conversion reaction with potassium chloride and water in a reactor, and a potassium sulfate solid is obtained. The technology removes sodium, and additionally, the technology also remove the undissolved substances of sand, stones, etc. The purity and the chrominance of a product are good. Energy sources are saved at normal temperature. The problems of the salt formation of equipment, the blockage of a pipeline, etc. in a cooling process are avoided.

Description

A kind of sulfate type potassium-containing salt lake brine is produced the method for vitriolate of tartar
The present invention relates to a kind of preparation method of vitriolate of tartar, particularly the sulfate type potassium-containing salt lake brine is produced the method for vitriolate of tartar.
In the prior art, Chinese patent CN-1131639A discloses a kind of method of preparing potassium sulfate with sulfate type bittern.Its technology contents is as follows: (1) technical process is: system potassium magnesium mixed salt, decomposition and inversion one, filtration, decomposition and inversion two, filtration washing, dry packing, product are shone in the salt pan; (2) processing condition are: the salt pan is shone system potassium magnesium mixed salt and is divided into three solarization systems step such as sodium pond, bittern-mixing pool and potassium magnesium mixed salt pond, the halogen of converting of bittern-mixing pool compares=1: 0.1 ~ 0.8, the invert point of decomposition and inversion one is 10 ~ 25 ℃, and the invert point of decomposition and inversion two is 45 ~ 60 ℃.The key problem in technology of this method is to take off sodium technology and realizes in the salt pan part.Shine in the system potassium magnesium mixed salt solid process on the bittern beach, bittern at first removes most of sodium-chlor in the sodium salt pond, utilize magnesium chloride that sodium-chlor is had this characteristic of remarkable salting out then, in the bittern-mixing pool in salt pan, be blended into the magnesium chloride solution of high density, can obtain the low high-grade potassium magnesium of sodium mixed salt solid through spontaneous evaporation again.The high-grade potassium magnesium of this low sodium mixed salt can directly change into the high-quality schoenite, and then transforms the production vitriolate of tartar.The weak point of this method is that the quality that potassium magnesium mixed salt is obtained in the salt pan is influenced greatly by natural climatic factor, and temperature, dust storm etc. all have considerable influence to the colourity of insolubles content index, product in the rate of recovery of potassium ion and the product vitriolate of tartar etc.In addition, this method requires relatively stricter to salt field process control condition, because the salt pan production cycle is long, aborning, in case the condition of a certain link does not guarantee, then whole production is in the cycle, and subsequent process will be influenced by it all will, even whether the quality that has influence on the finished product-potassium magnesium mixed salt in salt pan can reach the requirement that directly transforms.
The objective of the invention is at the prior art deficiency, proposed the method that a kind of sulfate type potassium-containing salt lake brine that adopts direct floatation process to remove sodium-chlor and unnecessary sulfate impurities is produced vitriolate of tartar.
The objective of the invention is to be reached by following technical scheme, the present invention is the method that a kind of sulfate type potassium-containing salt lake brine is produced vitriolate of tartar, be characterized in that this method may further comprise the steps:
(a) the sulfate type potassium-containing salt lake brine is shone through the beach, separate the solid sodium chloride of separating out earlier, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing (NaCl) 10-45% through continuing the beach;
(b) the thick potassium magnesium mixed salt with sodium chloride-containing (NaCl) 10-45% is crushed to particle diameter less than 20 millimeters, adds by 6.5-9.5 part potassium ion (K +), 0.6-2.5 part sodium ion (Na +), 1.0-3.0 part magnesium ion (Mg 2+), 13.5-17.5 part chlorion (CL -), 3.5-5.8 part sulfate radical (SO 4 2-), the conversion fluid that constitutes of 71.2-74.1 part water mixes, and is levigate again, making particle diameter is that 0.15 millimeter particle surpasses 70%, carries out under 10-60 ℃ temperature one section conversion reaction 0.5-3 hour, obtains containing schoenite (K 2SO 4MgSO 46H 2O), feed liquid is finished in one section conversion of Repone K (KCl), sodium-chlor (NaCl) and sulfate impurities;
(c) with flotation schoenite (K 2SO 4MgSO 46H 2O) flotation reagent is finished feed liquid to one section conversion and is adopted floatation process to carry out flotation, discharges the flotation mother liquor of sodium chloride-containing (NaCl) and sulfate impurities, again with the schoenite (K that obtains 2SO 4MgSO 46H 2O) dehydration makes sodium chloride content less than 9% schoenite (K 2SO 4MgSO 46H 2O) solid;
(d) will make sodium chloride content less than 9% schoenite (K 2SO 4MgSO 46H 2O) solid and purity are not less than 85% Repone K and water, by 1: 0-0.8: the effective ingredient weight ratio of 0.45-2.0 is mixed in reactor, under 10-70 ℃ temperature, carried out two sections conversion reaction 0.25-3 hours, and separated two sections again and transform mother liquor, the vitriolate of tartar solid that obtains separating out.
Wherein, the main component of the potassium magnesium mixed salt in above-mentioned (a) step comprises: vitriolate of tartar K 2SO 4, sal epsom MgSO 4, potassium chloride (KCl), sodium chloride nacl, magnesium chloride Mg Cl 2Combination cocrystallization body and mixture.In above-mentioned (b) step, the principle of one section conversion reaction is according to its phase region at five yuan of mutual system phase diagrams, and adding that conversion fluid sizes mixing is in order to make it put the crystallization phase region that is transferred to schoenite under this temperature mutually, to make potassium-bearing mineral all be converted into schoenite K 2SO 4MgSO 46H 2O and potassium chloride (KCl) are separated out the blended solid of schoenite solid or schoenite and Repone K.And in above-mentioned (d) step, two sections conversion reactions are schoenite (K 2SO 4MgSO 46H 2O) principle of potassium sulfate making is according to its phase region at the mutual system of quadruplex phasor, adds Repone K (KCl) and water, is mixed in proportion, and is in order to make it put the crystallization phase region that is transferred to vitriolate of tartar under this temperature mutually, directly to separate out the vitriolate of tartar solid.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar, be characterized in in two sections conversion reactions isolating two sections transform mother liquors and return and make conversion fluid in one section conversion reaction and use.This is that its composition is identical with the conversion fluid composition of one section conversion, it is recycled both save cost, also can further improve product yield because of isolating two sections saturated solutions that transform mother liquors for the low high potassium of magnesium in two sections conversion reactions.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar, be characterized in shining in the thick potassium magnesium mixed salt solid process of system with sulfate type potassium-containing salt lake brine beach, the sulfate type potassium-containing salt lake brine shone through the beach to potassium ion reach when saturated, separate the solid sodium chloride of separating out again, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing (NaCl) 10-45% through continuing the beach.Make bittern in beach solarization process, the few as far as possible loss of potassium ion, sulfate ion, the best moment of as often as possible sloughing sodium-chlor again.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar is characterized in that in one section conversion reaction process, temperature of reaction is 20-45 ℃, and the reaction times is 0.6-1 hour.This is the optimal reaction temperature and the optimum reacting time of this reaction process.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar is characterized in placing the beach, salt pan to shine in the flotation mother liquor that floatation process is discharged, and shines system potassium magnesium mixed salt.Continue to participate in reaction, can improve the rate of recovery of potassium ion.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of producing vitriolate of tartar is characterized in flotation schoenite (K 2SO 4MgSO 46H 2O) flotation reagent is finished after the flotation of feed liquid employing floatation process to one section conversion, before the flotation mother liquor of discharging sodium chloride-containing (NaCl) and sulfate impurities, the flotation reagent flotation one time that adds flotation Repone K (KCl) again, with Repone K (KCl) dehydration that obtains, be placed on down the step operation and use.
The present invention compared with prior art, the technology of its source mill is to the ore deposit, salt pan, promptly the salt pan adaptive faculty of shining the potassium magnesium mixed salt of system obviously improves; Because the direct floatation process that adopts can not only be taken off sodium, removes the effect of insolubless such as sandstone simultaneously in addition, and is therefore, all guaranteed to the purity and the colourity of product vitriolate of tartar.In addition, because direct floatation process operates at normal temperatures, therefore take off sodium technology and compare and to save a large amount of energy with high temperature; Simultaneously normal-temperature operation has also been avoided the engineering problems such as equipment salt crust, line clogging in the process for cooling process, more is suitable for suitability for industrialized production.The present invention has made full use of potassium ion in the bittern and useful sulfate ion, has reduced production cost.
Accompanying drawing is technological process of production figure of the present invention.
Embodiment one.The following examples have further described summary of the invention of the present invention.In the present embodiment, the sulfate type potassium-containing salt lake brine is selected East Platform Ji salt lake brine like this for use, its beach shone to potassium ion reach when saturated, separate the solid sodium chloride of separating out earlier, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing 10% through continuing the beach, thick potassium magnesium mixed salt is crushed to particle diameter less than 20 millimeters, adds by 6.5 parts of potassium ion K +, 0.6 part of sodium ion Na +, 1.0 parts of magnesium ion Mg 2+, 13.5 parts of chlorion CL -, 3.5 parts of sulfate radical SO 4 2-, the conversion fluid that constitutes of 71.2 parts of water mixes, and is levigate again, making particle diameter is that 0.15 millimeter particle surpasses 70%, carries out one section conversion reaction 0.5 hour under 60 ℃ temperature, obtains containing schoenite K 2SO 4MgSO 46H 2Feed liquid is finished in one section conversion of O, potassium chloride (KCl), sodium chloride nacl and sulfate impurities; To be flotation reagent finish feed liquid to one section conversion adopts floatation process to carry out flotation with the sulfovinate collecting agent, discharges the flotation mother liquor of sodium chloride-containing NaCl and sulfate impurities, again with the schoenite K that obtains 2SO 4MgSO 46H 2O dehydration makes sodium chloride content less than 9% schoenite K 2SO 4MgSO 46H 2The O solid; The schoenite K of sodium chloride content less than 9% will be made 2SO 4MgSO 46H 2O solid and purity are 90% Repone K and water, mix in reactor by 1: 0.8: 2.0 effective ingredient weight ratio, carry out two sections conversion reactions 0.25 hour under 70 ℃ temperature, separate two sections again and transform mother liquor, the vitriolate of tartar solid that obtains separating out.Product purity reaches 98%, and the potassium ion rate of recovery is 40.37% in the whole technological process.
Embodiment two.The following examples continue to have described summary of the invention of the present invention.In the present embodiment, the sulfate type potassium-containing salt lake brine is selected East Platform Ji salt lake brine like this for use, its beach is shone, separate the solid sodium chloride of separating out earlier, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing 25% through continuing the beach, thick potassium magnesium mixed salt is crushed to particle diameter less than 20 millimeters, adds by 7.6 parts of potassium ion K +, 1.3 parts of sodium ion Na +, 2.1 parts of magnesium ion Mg 2+, 16.5 parts of chlorion CL -, 4.5 parts of sulfate radical SO 4 2-, the conversion fluid that constitutes of 72.6 parts of water mixes, and is levigate again, making particle diameter is that 0.15 millimeter particle surpasses 80%, carries out one section conversion reaction 0.7 hour under 25 ℃ temperature, obtains containing schoenite K 2SO 4MgSO 46H 2Feed liquid is finished in one section conversion of O, potassium chloride (KCl), sodium chloride nacl and sulfate impurities; To be flotation reagent finish feed liquid to one section conversion adopts floatation process to carry out flotation with lipid acid and aliphatic amide collecting agent respectively, discharges the flotation mother liquor of sodium chloride-containing NaCl and sulfate impurities, again with the schoenite K that obtains 2SO 4MgSO 46H 2The dehydration of O and potassium chloride (KCl) mixes, and makes sodium chloride content less than 9% schoenite K 2SO 4MgSO 46H 2The blended solid of O and Repone K; It is made sodium chloride content less than 9% schoenite K 2SO 4MgSO 46H 2O solid and purity are 85% Repone K and water, mix in reactor by 1: 0.52: 1.31 effective ingredient weight ratio, carry out two sections conversion reactions 1 hour under 55 ℃ temperature, separate two sections again and transform mother liquor, the vitriolate of tartar solid that obtains separating out.With in two sections conversion reactions isolating two sections transform mother liquors and return and make conversion fluid in one section conversion reaction and use.Its product purity reaches 98%, and the potassium ion rate of recovery is 55% in the whole technological process.
Embodiment three.The following examples continue to have described summary of the invention of the present invention.In the present embodiment, the sulfate type potassium-containing salt lake brine is selected East Platform Ji salt lake brine like this for use, its beach is shone, separate the solid sodium chloride of separating out earlier, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing 45% through continuing the beach, thick potassium magnesium mixed salt is crushed to particle diameter less than 20 millimeters, adds by 9.5 parts of potassium ion K+, 2.5 parts of sodium ion Na +, 3.0 parts of magnesium ion Mg 2+, 17.5 parts of chlorion CL -, 5.8 parts of sulfate radical SO 4 2-, the conversion fluid that constitutes of 74.1 parts of water mixes, and is levigate again, making particle diameter is that 0.15 millimeter particle surpasses 75%, carries out one section conversion reaction 3 hours under 10 ℃ temperature, obtains containing schoenite K 2SO 4MgSO 46H 2Feed liquid is finished in one section conversion of O, potassium chloride (KCl), sodium chloride nacl and sulfate impurities; To be flotation reagent finish feed liquid to one section conversion adopts floatation process to carry out flotation with hydrocarbyl sulfonate and aliphatic amide collecting agent respectively, the flotation mother liquor of discharging sodium chloride-containing NaCl and sulfate impurities places the beach, salt pan to shine, shine system potassium magnesium mixed salt, again with the schoenite K that obtains 2SO 4MgSO 46H 2The dehydration of O and potassium chloride (KCl) mixes, and makes sodium chloride content less than 9% schoenite K 2SO 4MgSO 46H 2The blended solid of O and Repone K; It is made sodium chloride content less than 9% schoenite K 2SO 4MgSO 46H 2O solid and purity are 90% Repone K and water, mix in reactor by 1: 0.18: 0.45 effective ingredient weight ratio, carry out two sections conversion reactions 3 hours under 10 ℃ temperature, separate two sections again and transform mother liquor, the vitriolate of tartar solid that obtains separating out.With in two sections conversion reactions isolating two sections transform mother liquors and return and make conversion fluid in one section conversion reaction and use.Its product purity reaches 98%, and the potassium ion rate of recovery is 70% in the whole technological process.

Claims (6)

1, a kind of sulfate type potassium-containing salt lake brine is produced the method for vitriolate of tartar, it is characterized in that this method may further comprise the steps:
(a) the sulfate type potassium-containing salt lake brine is shone through the beach, separate the solid sodium chloride of separating out earlier, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing NaCl10-45% through continuing the beach;
(b) the thick potassium magnesium mixed salt with sodium chloride-containing NaCl10-45% is crushed to particle diameter less than 20 millimeters, adds by 6.5-9.5 part potassium ion K +, 0.6-2.5 part sodium ion Na +, 1.0-3.0 part magnesium ion Mg 2+, 13.5-17.5 part chlorion CL -, 3.5-5.8 part sulfate radical SO 4 2-, the conversion fluid that constitutes of 71.2-74.1 part water mixes, and is levigate again, making particle diameter is that 0.15 millimeter particle surpasses 70%, carries out under 10-60 ℃ temperature one section conversion reaction 0.5-3 hour, obtains containing schoenite K 2SO 4MgSO 46H 2Feed liquid is finished in one section conversion of O, potassium chloride (KCl), sodium chloride nacl and sulfate impurities;
(c) with flotation schoenite K 2SO 4MgSO 46H 2The flotation reagent of O is finished feed liquid to one section conversion and is adopted floatation process to carry out flotation, discharges the flotation mother liquor of sodium chloride-containing NaCl and sulfate impurities, again with the schoenite K that obtains 2SO 4MgSO 46H 2O dehydration makes sodium chloride content less than 9% schoenite K 2SO 4MgSO 46H 2The O solid;
(d) will make sodium chloride content less than 9% schoenite K 2SO 4MgSO 46H 2O solid and purity are not less than 85% Repone K and water, by 1: 0-0.8: the effective ingredient weight ratio of 0.45-2.0 is mixed in reactor, under 10-70 ℃ temperature, carried out two sections conversion reaction 0.25-3 hours, and separated two sections again and transform mother liquor, the vitriolate of tartar solid that obtains separating out.
2, the method for producing vitriolate of tartar according to claim 1, it is characterized in that with in two sections conversion reactions isolating two sections transform mother liquors and return and make conversion fluid in one section conversion reaction and use.
3, the method for producing vitriolate of tartar according to claim 1, it is characterized in that shining in the thick potassium magnesium mixed salt solid process of system with sulfate type potassium-containing salt lake brine beach, the sulfate type potassium-containing salt lake brine shone through the beach to potassium ion reach when saturated, separate the solid sodium chloride of separating out again, shine the thick potassium magnesium mixed salt solid that makes sodium chloride-containing NaCl10-45% through continuing the beach.
4, the method for producing vitriolate of tartar according to claim 1 is characterized in that in one section conversion reaction process, temperature of reaction is 20-45 ℃, and the reaction times is 0.6-1 hour.
5, the method for producing vitriolate of tartar according to claim 1 is characterized in that placing the beach, salt pan to shine in the flotation mother liquor that floatation process is discharged, and shines system potassium magnesium mixed salt.
6, the method for producing vitriolate of tartar according to claim 1 is characterized in that with flotation schoenite K 2SO 4MgSO 46H 2The flotation reagent of O is finished after the flotation of feed liquid employing floatation process to one section conversion, before the flotation mother liquor of discharging sodium chloride-containing NaCl and sulfate impurities, the flotation reagent flotation one time that adds the flotation potassium chloride (KCl) again with the potassium chloride (KCl) dehydration that obtains, is placed on down step operation use.
CNB011136421A 2001-05-24 2001-05-24 Preparation method of potassium sulfate with sulfate-type salt lake bittern containing potassium salt Expired - Lifetime CN1171794C (en)

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Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1321893C (en) * 2002-09-25 2007-06-20 国投新疆罗布泊钾盐有限责任公司 Method for preparing potassium sulfate from bittern containing potassium and magnesium sulfate
GB2427190B8 (en) * 2003-12-31 2009-07-22 Council Scient Ind Res Process for recovery of sulphate of potash
DE602005022506D1 (en) * 2005-11-10 2010-09-02 Council Scient Ind Res IMPROVED METHOD OF OBTAINING CALIUM SULPHATE (SOP, SULPHATE OF POTASH) FROM SULPHATE-MADE NUTSOLE
CN1810644B (en) * 2006-02-11 2010-06-16 国投新疆罗布泊钾盐有限责任公司 Improved process of preparing potassium sulfate with bittern containing potassium and magnesium sulfite
CN102674405B (en) * 2012-05-30 2014-03-19 河北工业大学 Method for preparing potassium sulfate by using picromerite
CN107188208B (en) * 2017-07-06 2019-11-22 化工部长沙设计研究院 A method of Shoenite is extracted with the carnallite of containing magnesium sulfate
WO2019071349A1 (en) * 2017-10-13 2019-04-18 Novopro Projects Inc. Systems and methods of producing potassium sulfate
CN107935637B (en) * 2017-11-10 2021-10-08 国投新疆罗布泊钾盐有限责任公司 Method for preparing top-grade potassium-magnesium fertilizer
CN115571899A (en) * 2022-11-12 2023-01-06 中蓝连海设计研究院有限公司 Method for extracting potassium sulfate from solar salt bittern

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