CN102976336A - Method for preparing ammonium fluosilicate solids from fluorosilicone compounds - Google Patents
Method for preparing ammonium fluosilicate solids from fluorosilicone compounds Download PDFInfo
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- CN102976336A CN102976336A CN2012105650168A CN201210565016A CN102976336A CN 102976336 A CN102976336 A CN 102976336A CN 2012105650168 A CN2012105650168 A CN 2012105650168A CN 201210565016 A CN201210565016 A CN 201210565016A CN 102976336 A CN102976336 A CN 102976336A
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Abstract
The invention relates to a method for preparing ammonium fluosilicate solids from fluorosilicone compounds. The method comprises the following steps of: mixing a fluorosilicone compound solution with the fluosilicic acid radical content of 3-40% and ammonia water or liquid ammonia or ammonium carbonate for reaction in a reaction tank, wherein the end point of reaction control is that the pH value of the reaction liquid ranges from 0.5 to 3; feeding the reaction liquid into an evaporation and concentration system, simultaneously adding hydrofluoric acid or an ammonium fluoride solution or ammonium fluoride solids into the reaction liquid, and concentrating the reaction liquid at a vacuum degree of 50-79 kPa and at the temperature of 50-65 DEG C; processing condensed vapor in a sewage treatment workshop; naturally settling ammonium fluosilicate crystals generated by concentration into a liquid seal slot, and feeding ammonium fluosilicate slurry to be dehydrated by a centrifugal machine through a slurry pump, thus obtaining the ammonium fluosilicate crystals and filtrate which can be recycled; and drying the ammonium fluosilicate crystals to obtain the ammonium fluosilicate solids. The method can be used for producing the ammonium fluosilicate solids economically and effectively, solving the problem of fluorine pollution of phosphate fertilizer enterprises, and simultaneously laying a foundation for development of fluorine chemical industry of the phosphate fertilizer enterprises.
Description
Technical field
The present invention relates to the technology of preparing of fluorine chemical industry inorganic fluoride salt in the chemical field, relate in particular to a kind of technological method that utilizes silicofluoric acid or silicofluoric acid and ammonium silicon fluoride mixture to prepare the solid ammonium silicofluoride.
Background technology:In the traditional industries ammonium silicofluoride mainly contain fluorite and quartzy mix acidolysis after, more further ammonification and getting after water absorbs; Ammonium silicofluoride is mainly as the sterilizing agent in the Brewing industry, the glass etching agent, and the fabric mothproofing agent, wood preservative, the metal solder fusing assistant also is used for electroplating industry and for the preparation of cryolith etc.Along with further going deep into of phosphorus ore association fluorine silicon resource comprehensive utilization technique, utilize phosphatic fertilizer company by-product fluosilicic acid production Neutral ammonium fluoride, anhydrous hydrogen fluoride technology to be mature on the whole, therefore utilize the silicofluoric acid of phosphatic fertilizer company to produce ammonium silicofluoride, ammonium silicofluoride is further produced the fluorine chemical series product such as solid Neutral ammonium fluoride, solid ammonium hydrogen fluoride, anhydrous hydrogen fluoride again; Ammonium silicofluoride has become important intermediates of phosphorus ore association fluorine silicon resource comprehensive utilization.When in the fluorine absorption system of phosphatic fertilizer company Phosphoric Acid Concentration for after preventing that the silica gel blocking system from adding ammonium fluoride solution dissolving silica gel, the phosphatic fertilizer company by-product will be the mixture of silicofluoric acid and ammonium silicofluoride.Therefore, in comprehensive utilization phosphatic fertilizer company by-product fluosilicic acid, also should consider the utilization of the mixture of silicofluoric acid and ammonium silicofluoride.
From fluorosilicone compound solution to fluorine chemical series product such as solid Neutral ammonium fluoride, solid ammonium hydrogen fluoride, anhydrous hydrogen fluorides, common characteristics all are the water of deviating from the silicofluoric acid.Therefore, which operation deviating from water in, is the key of phosphatic fertilizer company by-product fluorosilicone compound comprehensive utilization technique.After fluorine analysis ammonium silicate, Neutral ammonium fluoride, ammonium bifluoride and hydrofluoric physico-chemical property, think on technique, to be easy to most realize in the dehydration of preparation ammonium silicofluoride stage.The preparation of solid ammonium silicofluoride is for comprehensive utilization phosphatic fertilizer company fluorosilicone compound development fluorine chemical industry, silication worker industry lay the foundation.
The patent CN102701214A " a kind of method for preparing the high-purity fluorine ammonium silicate " that the patent CN101850978A that utilizes at present the fluorosilicone compound of phosphatic fertilizer company by-product to produce patented technology that ammonium silicofluoride applied for to only have comrade's Cheng Jianfang application " utilizes fluorinated tail gas in the production of phosphate fertilizer to prepare the method for ammonium silicofluoride " and Guizhou Kailin Group Co., Ltd. applies for." utilizing fluorinated tail gas in the production of phosphate fertilizer to prepare the method for ammonium silicofluoride " is to be used for absorbing the phosphate fertilizer fluorinated tail gas with the ammonium silicofluoride crystalline mother solution as washings, obtain the fluorine-containing rich solution of high density, with ammonia neutralization, filter again, with the filtrate cooling and separate out the ammonium silicofluoride crystallization; There are the following problems for this technique: relating in the technique can lot of energy with the high-temperature material crystallisation by cooling, and low temperature filtrate returns that use need heat up also will lot of energy; A large amount of silica gel be can produce in the Phosphoric Acid Concentration system, the impure even difficult filtration of the ammonium silicofluoride that obtains and drying made." a kind of method for preparing the high-purity fluorine ammonium silicate " should be mentioned that to adopt and is not less than 10% silicofluoric acid and ammonia purity and reacts greater than 99.9% liquefied ammonia, pH value of reaction system reaches at 3～5 o'clock, with the concentrated ammonium silicofluoride that obtains under the condition of reaction solution vacuum tightness 80kPa and temperature 70 C in the low-flash concentration systems; There are the following problems for this technique: higher to the liquefied ammonia quality requirements in the technique; Reacting liquid pH value 3 above silicofluoric acid begin to decompose, particularly the pH value produces a large amount of silicon-dioxide more than 4, affect the main content of concentration process, ammonium silicofluoride solid filtering and the reduction product of ammonium silicofluoride.
Summary of the invention:
The purpose of this invention is to provide the method that a kind of phosphatic fertilizer company by-product fluorosilicone compound prepares the solid ammonium silicofluoride, produce the fluorine chemical series product such as solid Neutral ammonium fluoride, solid ammonium hydrogen fluoride, anhydrous hydrogen fluoride for comprehensive utilization phosphatic fertilizer company fluorosilicone compound, development fluorine chemical industry, silication worker industry lay the foundation.
A kind of fluorosilicone compound of the present invention prepares the method for solid ammonium silicofluoride, and the solid silicofluoric acid amine of output can be me, and the patent applied for CN18840773B of unit number " a kind of ammonia solution of fluorosilicone compound and the separation method of fluorine element silicon " supplied raw materials or directly put on market.The method of the invention is characterized in that following these steps to successively carry out:
(1) with the silicofluoric acid root
Content is that fluorosilicone compound solution and the ammoniacal liquor of 3%～40%w/w or liquefied ammonia or volatile salt fully mix in reactive tank and react, and reacting liquid pH value 0.5～3 is reaction control terminal point;
(2) reaction solution that above-mentioned steps (1) is obtained is sent into evaporation concentration system, add simultaneously concentration and be 20%～50%w/w hydrofluoric acid or concentration and be 15%～45%w/w ammonium fluoride solution also or the solid Neutral ammonium fluoride, the consumption of hydrofluoric acid or Neutral ammonium fluoride with fluorine count the fluorosilicone compound raw material fluorine-containing 0.1%～10%; Be that 50kPa～79kPa, temperature are concentrated under 50 ℃～65 ℃ the condition in vacuum tightness; The water vapour that concentration systems is discharged is behind circulating water condensing, and water of condensation is delivered to sewage treatment plant and processed;
(3) the ammonium silicofluoride natural crystal sedimentation of above-mentioned steps (2) generation enters liquid seal trough, by slush pump the ammonium silicofluoride magma of liquid seal trough bottom is sent into centrifuge dewatering, obtain ammonium silicofluoride crystal and filtrate, filtrate is returned step (2) and is continued repetitive operation;
(4) above-mentioned steps (3) obtains the ammonium silicofluoride crystal and can obtain after drying solid ammonium silicofluoride product, and ammonium silicofluoride content is greater than 98%.
The fluorosilicone compound that above-mentioned steps (1) refers to can be silicofluoric acid, also can be the mixture of silicofluoric acid and ammonium silicofluoride.
Above-mentioned steps (1) if in the massfraction of phosphoric acid greater than 0.5% the time, fluorosilicone compound solution enter step (1) front first with solution except phosphoric acid, in fluorosilicone compound solution, add the ironic hydroxide solid, add-on is the theoretical consumption of phosphoric acid in the precipitation solution, filters rear filtrate and is undertaken by step (1) operation.
The optimal conditions of above-mentioned steps (2) is 40%～50%w/w for adding hydrofluoric acid concentration, and ammonium fluoride solution concentration is 35%～45%w/w or solid Neutral ammonium fluoride, and the consumption of hydrofluoric acid or Neutral ammonium fluoride is counted 0.5% fluorine-containing～5%w/w of fluorosilicone compound raw material with fluorine.
The liquid seal trough of above-mentioned steps (3) and the mode of connection of vacuum concentration system are that the extended straight tube in evaporator room bottom inserts below the liquid level of liquid seal trough, utilize pressure reduction between normal atmosphere and the system vacuum degree to set up liquid level in the concentrating unit.
The ammonium silicofluoride crystal behind centrifuge dewatering of above-mentioned steps (3) can be without drying directly as the raw material of producing Neutral ammonium fluoride, ammonium bifluoride, hydrofluoric acid, anhydrous hydrogen fluoride.
Above-mentioned optimum condition is that step (1) reacting liquid pH value 1.5～2.5 is reaction control terminal point.
Compared with prior art, the present invention has following advantage: 1, reacting liquid pH value 1.5～2.5 is reaction control terminal point, and reaction process is not separated out silica gel; 2, concentration process adds hydrofluoric acid or ammonium fluoride solution, and the silica gel that brings in the dissolving raw material also suppresses to be hydrolyzed in the silicofluoric acid radical ion concentration process simultaneously, and the production of high purity solid ammonium silicofluoride of making a living provides safeguard; 3, adopt normal pressure equipment liquid seal trough to be connected with the evaporator room of vacuum concentration system, can guarantee that concentration process carries out under vacuum condition, the ammonium silicofluoride crystal that produces in time can be deposited to liquid seal trough again, be implemented in the vacuum concentration production process ammonium silicofluoride crystal is taken out in normal pressure equipment, liquid seal trough has very large solid ammonium silicofluoride storage capacity simultaneously, can not affect because the solid ammonium silicofluoride does not in time take out the normal operation of concentration systems; Directly send into whizzer if the solid ammonium silicofluoride that produces in the concentration systems evaporator room does not enter liquid seal trough, when the whizzer fault stops or stopping without plan, the solid of failing in time to take out will stop up concentration systems.
Industrial test proof of the present invention can be produced the solid ammonium silicofluoride cost-effectively; The solid ammonium silicofluoride also can come into the market to sell as end product as the raw material of producing Neutral ammonium fluoride, ammonium bifluoride, hydrofluoric acid, anhydrous hydrogen fluoride after drying; For comprehensive utilization phosphatic fertilizer company fluorosilicone compound development fluorine chemical industry, silication worker industry lay the foundation.
Description of drawings
Fig. 1 is the schematic flow sheet of the inventive method.Among the figure: I is reactive tank, and II is evaporator room, and III is steam condenser, and IV is liquid seal trough, and V is whizzer, and VI is the filtrate cycle groove, and VII is graphite heat exchanger, and VIII is propeller pump, and IX is the magma pump, and X is the filtrate cycle pump.Wherein the extended straight tube in evaporator room II bottom inserts below the liquid level of liquid seal trough IV, utilizes pressure reduction between normal atmosphere and the system vacuum degree to set up liquid level in the concentrating unit; All materials when liquid seal trough normal pressure, volume are large enough to hold the operation of concentration systems; The concentrated ammonium silicofluoride crystal that produces of evaporator room in time is deposited to liquid seal trough, and the ammonium silicofluoride crystal takes out under condition of normal pressure.
Embodiment
Embodiment 1
1600 ton/years of ammonium silicofluoride pilot plants that my unit builds adopt the inventive method to produce the solid ammonium silicofluoride.
From Phosphoric Acid Concentration fluorine absorption system silicofluoric acid root
Content is that the fluorosilicone compound solution of 8%w/w fully mixes in reactive tank with liquefied ammonia and reacts, and reacting liquid pH value 2 is reaction control terminal point; Reaction solution is sent into evaporation concentration system, add simultaneously concentration and be about 30% ammonium fluoride solution, adopt 110～120 ℃, the water vapour of 0.05～0.2Mpa heats, and heat-exchange equipment is the tubulation graphite heat exchanger; Be about under the condition that 75kPa, temperature be about 60 ℃ concentrated in vacuum tightness; The water vapour that concentration systems is discharged is behind circulating water condensing, and water of condensation enters the muddy water station, delivers to sewage treatment plant again and processes.
The ammonium silicofluoride natural crystal sedimentation that concentration process produces enters liquid seal trough, and the ammonium silicofluoride magma is sent into centrifuge dewatering by slush pump, obtains ammonium silicofluoride crystal and filtrate, and filtrate is returned evaporation concentration system.
Image data be chosen under the condition that the production charging is stable, control is stable to material in the 1h record, statistics and analysis.Enter the silicofluoric acid root of system
Content is 8%, and flow is 2.3m
3/ h, the ammonium silicofluoride magma of system produce is after the tripod pendulum type batch centrifugal dehydration, and undried solid ammonium silicofluoride is about 261kg.Undried solid ammonium silicofluoride by analysis, ammonium silicofluoride content is greater than 94%.After solid ammonium silicofluoride drying, ammonium silicofluoride content is greater than 98.5%.
After this ammonium silicofluoride pilot plant builds up, move the nearly trimestral time, stable, obtained the required experimental data of project.
Embodiment 2
In the middle control analysis process, find that the massfraction of phosphoric acid in the filtrate cycle groove is 0.75%, the solution in the filtrate cycle groove is delivered to the phosphoric acid precipitates groove, sending into speed is 2.5m
3/ h adds the ironic hydroxide solid at the phosphoric acid precipitates groove, adds speed 27.5kg/h.Filter after stirring lower fully reaction, filtrate is undertaken by the operation of embodiment 1 again.
Claims (7)
1. a fluorosilicone compound prepares the method for solid ammonium silicofluoride, it is characterized in that following these steps to successively carry out:
(1) with the silicofluoric acid root
Content is that fluorosilicone compound solution and the ammoniacal liquor of 3%～40%w/w or liquefied ammonia or volatile salt fully mix in reactive tank and react, and reacting liquid pH value 0.5～3 is reaction control terminal point;
(2) reaction solution that above-mentioned steps (1) is obtained is sent into evaporation concentration system, add simultaneously concentration and be 20%～50%w/w hydrofluoric acid or concentration and be 15%～45%w/w ammonium fluoride solution also or the solid Neutral ammonium fluoride, the consumption of hydrofluoric acid or Neutral ammonium fluoride with fluorine count the fluorosilicone compound raw material fluorine-containing 0.1%～10%; Be that 50kPa～79kPa, temperature are concentrated under 50 ℃～65 ℃ the condition in vacuum tightness; The water vapour that concentration systems is discharged is behind circulating water condensing, and water of condensation is delivered to sewage treatment plant and processed;
(3) the ammonium silicofluoride natural crystal sedimentation of above-mentioned steps (2) generation enters liquid seal trough, by slush pump the ammonium silicofluoride magma of liquid seal trough bottom is sent into centrifuge dewatering, obtain ammonium silicofluoride crystal and filtrate, filtrate is returned step (2) and is continued repetitive operation;
(4) above-mentioned steps (3) obtains the ammonium silicofluoride crystal and can obtain after drying solid ammonium silicofluoride product, and ammonium silicofluoride content is greater than 98%.
2. a kind of fluorosilicone compound as claimed in claim 1 prepares the method for solid ammonium silicofluoride, it is characterized in that the fluorosilicone compound that step (1) refers to can be silicofluoric acid, also can be the mixture of silicofluoric acid and ammonium silicofluoride.
3. a kind of fluorosilicone compound as claimed in claim 1 prepares the method for solid ammonium silicofluoride, it is characterized in that step (1) if in the massfraction of phosphoric acid greater than 0.5% the time, fluorosilicone compound solution enter step (1) front first with solution except phosphoric acid, in fluorosilicone compound solution, add the ironic hydroxide solid, add-on is the theoretical consumption of phosphoric acid in the precipitation solution, filters rear filtrate and is undertaken by step (1) operation.
4. a kind of fluorosilicone compound as claimed in claim 1 prepares the method for solid ammonium silicofluoride, the optimal conditions that it is characterized in that step (2) is 40%～50%w/w for adding hydrofluoric acid concentration, ammonium fluoride solution concentration is 35%～45%w/w or solid Neutral ammonium fluoride, and the consumption of hydrofluoric acid or Neutral ammonium fluoride is counted 0.5% fluorine-containing～5%w/w of fluorosilicone compound raw material with fluorine.
5. a kind of fluorosilicone compound as claimed in claim 1 prepares the method for solid ammonium silicofluoride, the mode of connection that it is characterized in that the liquid seal trough of step (3) and vacuum concentration system is that the extended straight tube in evaporator room bottom inserts below the liquid level of liquid seal trough, utilizes pressure reduction between normal atmosphere and the system vacuum degree to set up liquid level in the concentrating unit.
6. a kind of fluorosilicone compound as claimed in claim 1 prepares the method for solid ammonium silicofluoride, the ammonium silicofluoride crystal behind centrifuge dewatering that it is characterized in that step (3) can be without drying directly as the raw material of producing Neutral ammonium fluoride, ammonium bifluoride, hydrofluoric acid, anhydrous hydrogen fluoride.
7. a kind of fluorosilicone compound as claimed in claim 1 prepares the method for solid ammonium silicofluoride, it is characterized in that step (1) optimum condition is that reacting liquid pH value 1.5～2.5 is reaction control terminal point.
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| CN201210565016.8A CN102976336B (en) | 2012-12-24 | 2012-12-24 | Method for preparing ammonium fluosilicate solids from fluorosilicone compounds |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107522519A (en) * | 2017-07-27 | 2017-12-29 | 宜昌鄂中化工有限公司 | A kind of recycling technique of wet process phosphoric acid by-product fluosilicic acid |
| CN108101069A (en) * | 2017-12-28 | 2018-06-01 | 天津普恒康泰科技有限公司 | A kind of exhaust gas produces ammonium fluosilicate co-producing white carbon black raw material process after recycling |
| CN113860258A (en) * | 2021-11-04 | 2021-12-31 | 多氟多新材料股份有限公司 | Preparation method of hydrogen fluoride |
| CN115072666A (en) * | 2022-06-23 | 2022-09-20 | 中石化南京工程有限公司 | System and method for preparing anhydrous hydrogen fluoride from fluosilicic acid |
| CN115259118A (en) * | 2021-04-30 | 2022-11-01 | 中国科学院过程工程研究所 | Method for separating phosphorus from phosphorus-containing fluorine-containing substance |
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| CN1554570A (en) * | 2003-12-22 | 2004-12-15 | 云南三环化工有限公司 | A method for comprehensive utilization of phosphate fertilizer by-products |
| CN101850978A (en) * | 2010-06-06 | 2010-10-06 | 程建方 | Method for preparing ammonium fluosilicate by utilizing tail gas containing fluorine in phosphatic fertilizer production |
| CN102674367A (en) * | 2012-06-07 | 2012-09-19 | 瓮福（集团）有限责任公司 | Method for preparing ammonium fluorosilicate by utilizing fluorine-containing white slime in anhydrous hydrogen fluoride production |
| CN102701214A (en) * | 2012-06-28 | 2012-10-03 | 贵州开磷（集团）有限责任公司 | Method for preparing high-purity ammonium fluosilicate |
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2012
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1554570A (en) * | 2003-12-22 | 2004-12-15 | 云南三环化工有限公司 | A method for comprehensive utilization of phosphate fertilizer by-products |
| CN101850978A (en) * | 2010-06-06 | 2010-10-06 | 程建方 | Method for preparing ammonium fluosilicate by utilizing tail gas containing fluorine in phosphatic fertilizer production |
| CN102674367A (en) * | 2012-06-07 | 2012-09-19 | 瓮福（集团）有限责任公司 | Method for preparing ammonium fluorosilicate by utilizing fluorine-containing white slime in anhydrous hydrogen fluoride production |
| CN102701214A (en) * | 2012-06-28 | 2012-10-03 | 贵州开磷（集团）有限责任公司 | Method for preparing high-purity ammonium fluosilicate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107522519A (en) * | 2017-07-27 | 2017-12-29 | 宜昌鄂中化工有限公司 | A kind of recycling technique of wet process phosphoric acid by-product fluosilicic acid |
| CN108101069A (en) * | 2017-12-28 | 2018-06-01 | 天津普恒康泰科技有限公司 | A kind of exhaust gas produces ammonium fluosilicate co-producing white carbon black raw material process after recycling |
| CN115259118A (en) * | 2021-04-30 | 2022-11-01 | 中国科学院过程工程研究所 | Method for separating phosphorus from phosphorus-containing fluorine-containing substance |
| CN113860258A (en) * | 2021-11-04 | 2021-12-31 | 多氟多新材料股份有限公司 | Preparation method of hydrogen fluoride |
| CN115072666A (en) * | 2022-06-23 | 2022-09-20 | 中石化南京工程有限公司 | System and method for preparing anhydrous hydrogen fluoride from fluosilicic acid |
| CN115072666B (en) * | 2022-06-23 | 2023-08-18 | 中石化南京工程有限公司 | System and method for preparing anhydrous hydrogen fluoride from fluosilicic acid |
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Effective date of registration: 20170706 Address after: Xifeng County in Guizhou Province, Guiyang city town 551109 Patentee after: Guiyang Kailin Chemical Co. Ltd. Address before: 550002 Guizhou city of Guiyang Province sun Tian Ba Lu No. 1 Patentee before: Guizhou Provincial Inst. of Chemical Technology |
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