CN113800525A - Method for co-producing fluosilicate and hydrochloric acid by using boron salt tail gas - Google Patents
Method for co-producing fluosilicate and hydrochloric acid by using boron salt tail gas Download PDFInfo
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- CN113800525A CN113800525A CN202111293077.9A CN202111293077A CN113800525A CN 113800525 A CN113800525 A CN 113800525A CN 202111293077 A CN202111293077 A CN 202111293077A CN 113800525 A CN113800525 A CN 113800525A
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- tail gas
- hydrochloric acid
- fluosilicate
- boron salt
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a method for co-producing fluosilicate and hydrochloric acid by using boron salt tail gas, which comprises the following steps: introducing mixed gas of silicon tetrafluoride and hydrogen chloride in the tail gas from boron salt production into a solvent dissolved with fluoride salt for primary absorption reaction to prepare fluorosilicate mixed liquid, and absorbing the residual tail gas by secondary water to prepare hydrochloric acid solution. The obtained fluosilicate mixed solution is filtered, washed and dried to obtain a fluosilicate product, and the obtained product has high purity and good quality. The method adopts a two-stage absorption mode to separate the mixed gas of silicon tetrafluoride and hydrogen chloride, utilizes the reaction of the silicon tetrafluoride and potassium fluoride to prepare fluosilicate, and utilizes the hydrogen chloride to dissolve in water to prepare hydrochloric acid solution. The raw materials adopted by the invention are cheap and easily available, the preparation cost is low, the reaction is easy to control, the operation is simple, and the reaction efficiency is high; meanwhile, the method eliminates the pollution of the tail gas silicon tetrafluoride generated by preparing boron salt to the environment.
Description
Technical Field
The invention relates to a method for coproducing fluosilicate and hydrochloric acid from boron salt tail gas, belongs to the technical field of chemical product preparation, and particularly relates to a method for preparing fluosilicate from boron salt byproduct tail gas silicon tetrafluoride.
Background
The statements in this section merely provide background information related to the present disclosure and may not constitute prior art.
Fluorosilicates are commonly used as pesticides in wood preservation, ceramic manufacture, aluminum and magnesium smelting, agriculture, optical glass manufacture, synthetic mica, enamel manufacture, and the like. The prior fluosilicate is mainly produced by fluoride production enterprises and phosphorus chemical enterprises, and most of the production of the fluosilicate adopts the reaction of the fluosilicic acid which is a byproduct of the phosphorus chemical industry or hydrofluoric acid production enterprises and the waste halogen salt produced in the organic fluorination process to generate fluosilicate precipitate, and the fluosilicate product is obtained after treatment. There are several problems: firstly, the preparation cost is high; secondly, the reaction efficiency is not high, the reaction is not easy to control, and the yield of the production method of the fluosilicate is low.
It should be noted that the above background description is only for the sake of clarity and complete description of the technical solutions of the present invention and for the understanding of those skilled in the art. Such solutions are not considered to be known to the person skilled in the art merely because they have been set forth in the background section of the invention.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for co-producing fluosilicate and hydrochloric acid by using boron salt tail gas.
In order to solve the technical problem, the invention provides a method for co-producing fluosilicate and hydrochloric acid from boron salt tail gas, which comprises the following steps: introducing tail gas generated in boron salt production into a solvent dissolved with fluoride salt to perform primary absorption reaction to prepare a fluorosilicate mixed solution, absorbing the residual tail gas by secondary water to prepare a hydrochloric acid solution, and filtering, washing and drying the obtained fluorosilicate mixed solution to prepare a fluorosilicate product.
Preferably, the tail gas for producing the boron salt is a mixed gas with the main component of silicon tetrafluoride and hydrogen chloride.
Preferably, the boron salt is one or a mixture of several of lithium tetrafluoroborate, lithium fluoroborate, lithium difluorooxalate borate and lithium dioxalate borate.
Preferably, the fluoride salt comprises one or more of potassium fluoride, sodium fluoride, magnesium fluoride and lithium fluoride.
Preferably, the solvent is one or more of dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, diethyl ether, ethylene glycol dimethyl ether, ethanol, acetonitrile, dichloromethane and 1, 2-dichloromethane.
Preferably, the fluorosilicate product is dried in a reduced pressure drying mode, and the specific method comprises the following steps: drying for 1 hour under vacuum condition, heating to 60 deg.C, and drying for 3-6 hours under vacuum condition. The obtained product has good quality and high purity.
By means of the technical scheme, the invention has the following beneficial effects:
the invention relates to a method for coproducing fluosilicate and hydrochloric acid by utilizing boron salt tail gas, which adopts a two-stage absorption mode to separate mixed gas of silicon tetrafluoride and hydrogen chloride, utilizes the reaction of the silicon tetrafluoride and fluoride salt to prepare fluosilicate, and utilizes the hydrogen chloride to dissolve in water to prepare hydrochloric acid solution. The raw materials adopted by the invention are cheap and easily available, the preparation cost is low, the reaction is easy to control, the operation is simple, and the reaction efficiency is high; meanwhile, the method eliminates the pollution of the tail gas silicon tetrafluoride generated by preparing boron salt to the environment.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A method for coproducing fluosilicate and hydrochloric acid by using boron salt tail gas comprises the following steps: introducing mixed gas of silicon tetrafluoride and hydrogen chloride in the tail gas from boron salt production into a solvent dissolved with fluoride salt for primary absorption reaction to prepare fluorosilicate mixed liquid, and absorbing the residual tail gas by secondary water to prepare hydrochloric acid solution. And filtering, washing and drying the obtained fluosilicate mixed solution to obtain a fluosilicate product.
The main component of the tail gas produced by the boron salt contains the mixed gas of silicon tetrafluoride and hydrogen chloride.
The boron salt production mainly comprises the production of one or a mixture of more of lithium tetrafluoroborate, lithium fluoroborate, lithium difluorooxalate borate, lithium dioxalate borate and the like.
The fluoride salt comprises one or more of potassium fluoride, sodium fluoride, magnesium fluoride, lithium fluoride and the like.
The solvent is one or more of dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, diethyl ether, ethylene glycol dimethyl ether, ethanol, acetonitrile, dichloromethane and 1, 2-dichloromethane.
The reactions to which the present application relates include:
2MF+SiF4→M2SiF6
the fluosilicate product is dried in a reduced pressure drying mode, and the specific method comprises the following steps: drying for 1 hour under vacuum condition, heating to 60 deg.C, and drying for 3-6 hours under vacuum condition.
The present application is further illustrated with reference to specific examples below:
example 1
1.0mol of lithium difluoro (oxalato) borate is synthesized according to reaction feeding, the generated tail gas is introduced into 1L of dimethyl carbonate mixed solution mixed with 100g of potassium fluoride, and the tail gas is introduced into 1L of water through secondary absorption. Starting stirring to start reaction, after the reaction is finished, filtering the mixed solution in a potassium fluoride bottle, washing with water, weighing to obtain 106.5g of potassium fluosilicate product, wherein the yield is 96.7%, the purity of the obtained product is 98.87%, and the concentration of hydrochloric acid in secondary water absorption is 7.2%.
Example 2
Synthesizing 1.0mol of lithium bis (oxalato) borate according to the reaction feeding, introducing the generated tail gas into 2L of acetonitrile mixed solution mixed with 200g of sodium fluoride, and introducing into 2L of water through secondary absorption. Starting stirring to start reaction, after the reaction is finished, filtering the mixed solution in a sodium fluoride bottle, washing with water, and weighing to obtain 173.7g of sodium fluosilicate product, wherein the yield is 92.4%, the purity of the obtained product is 98.45%, and the concentration of hydrochloric acid in secondary water absorption is 7.1%.
Example 3
Synthesizing 1.5mol of lithium difluoro-oxalato-borate according to the reaction feeding, introducing the generated tail gas into 2L of ethyl acetate mixed solution mixed with 200g of magnesium fluoride, and introducing into 2L of water through secondary absorption. Starting stirring to start reaction, after the reaction is finished, filtering the mixed solution in the magnesium fluoride bottle, washing with water, weighing to obtain 190.8g of magnesium fluosilicate product, wherein the yield is 92.7%, the purity of the obtained product is 99.05%, and the concentration of hydrochloric acid in secondary water absorption is 5.3%.
Example 4
Synthesizing 2.0mol of lithium difluoro (oxalato) borate according to the reaction feeding, introducing the generated tail gas into 2L of dichloromethane mixed liquid mixed with 200g of lithium fluoride, and introducing 2L of water through secondary absorption. Starting stirring to start reaction, after the reaction is finished, filtering the mixed solution in a lithium fluoride bottle, washing with water, weighing to obtain 179.3g of lithium fluosilicate product, wherein the yield is 93.4%, the purity of the obtained product is 98.76%, and the concentration of hydrochloric acid in secondary water absorption is 7.0%.
The invention adopts a two-stage absorption mode to separate the mixed gas of silicon tetrafluoride and hydrogen chloride, utilizes the reaction of silicon tetrafluoride and fluoride salt to prepare potassium fluosilicate, and utilizes the hydrogen chloride to dissolve in water to prepare hydrochloric acid solution. The raw materials adopted by the invention are cheap and easily available, the preparation cost is low, the reaction is easy to control, the operation is simple, and the reaction efficiency is high; meanwhile, the method eliminates the pollution of the tail gas silicon tetrafluoride generated by preparing boron salt to the environment.
Although the invention has been described and illustrated in some detail, it should be understood that various modifications may be made to the described embodiments or equivalents may be substituted, as will be apparent to those skilled in the art, without departing from the spirit of the invention.
Claims (6)
1. A method for coproducing fluosilicate and hydrochloric acid from boron salt tail gas is characterized by comprising the following steps: introducing tail gas generated in boron salt production into a solvent dissolved with fluoride salt to perform primary absorption reaction to prepare a fluorosilicate mixed solution, absorbing the residual tail gas by secondary water to prepare a hydrochloric acid solution, and filtering, washing and drying the obtained fluorosilicate mixed solution to prepare a fluorosilicate product.
2. The method for coproducing fluorosilicate and hydrochloric acid from boron salt tail gas as defined in claim 1, wherein the tail gas from boron salt production mainly comprises silicon tetrafluoride and hydrogen chloride.
3. The method for coproducing fluorosilicate and hydrochloric acid from boron salt tail gas according to claim 1, wherein the boron salt is one or a mixture of lithium tetrafluoroborate, lithium fluoroborate, lithium difluorooxalate borate and lithium dioxalate borate.
4. The method for co-producing fluosilicate and hydrochloric acid from boron salt tail gas as claimed in claim 1, wherein the fluoride salt comprises one or more of potassium fluoride, sodium fluoride, magnesium fluoride and lithium fluoride.
5. The method for co-producing fluosilicate and hydrochloric acid from boron salt tail gas as claimed in claim 1, wherein the solvent is one or more of dimethyl carbonate, diethyl carbonate, methyl ethyl carbonate, diethyl ether, ethylene glycol dimethyl ether, ethanol, acetonitrile, dichloromethane and 1, 2-dichloromethane.
6. A method of co-producing fluorosilicate and hydrochloric acid from a boron salt tail gas as set forth in claim 1, wherein the fluorosilicate product is dried by reduced pressure drying, the reduced pressure drying method comprising: drying for 1 hour under vacuum condition, heating to 60 deg.C, and drying for 3-6 hours under vacuum condition.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111293077.9A CN113800525A (en) | 2021-11-03 | 2021-11-03 | Method for co-producing fluosilicate and hydrochloric acid by using boron salt tail gas |
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| CN202111293077.9A CN113800525A (en) | 2021-11-03 | 2021-11-03 | Method for co-producing fluosilicate and hydrochloric acid by using boron salt tail gas |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114345106A (en) * | 2021-12-30 | 2022-04-15 | 湖北瓮福蓝天化工有限公司 | Method and system for removing chlorine element in anhydrous hydrogen fluoride production process |
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2021
- 2021-11-03 CN CN202111293077.9A patent/CN113800525A/en active Pending
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| JP2003137890A (en) * | 2001-11-05 | 2003-05-14 | Central Glass Co Ltd | Synthesis of ionic metal complex |
| CN102016123A (en) * | 2008-04-22 | 2011-04-13 | 凯米涛弗特公司 | Method of making high purity lithium hydroxide and hydrochloric acid |
| CN104185636A (en) * | 2011-11-14 | 2014-12-03 | 罗克伍德锂有限责任公司 | Process for preparing metal difluorochelatoborates and use as battery electrolytes or additives in electrochemical cells |
| WO2014097772A1 (en) * | 2012-12-21 | 2014-06-26 | セントラル硝子株式会社 | Production method for ionic metal complex salt using organic compound as ligand |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114345106A (en) * | 2021-12-30 | 2022-04-15 | 湖北瓮福蓝天化工有限公司 | Method and system for removing chlorine element in anhydrous hydrogen fluoride production process |
| CN114345106B (en) * | 2021-12-30 | 2023-12-12 | 湖北瓮福蓝天化工有限公司 | Method and system for removing chlorine element in anhydrous hydrogen fluoride production process |
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