CN101898769B - Method for producing high-purity ammonium bifluoride - Google Patents
Method for producing high-purity ammonium bifluoride Download PDFInfo
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- CN101898769B CN101898769B CN2010101090628A CN201010109062A CN101898769B CN 101898769 B CN101898769 B CN 101898769B CN 2010101090628 A CN2010101090628 A CN 2010101090628A CN 201010109062 A CN201010109062 A CN 201010109062A CN 101898769 B CN101898769 B CN 101898769B
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- ammonium bifluoride
- fluoride
- ammonium
- anhydrous hydrogen
- hydrogen fluoride
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- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000012047 saturated solution Substances 0.000 claims abstract description 16
- 239000000047 product Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000002686 phosphate fertilizer Substances 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000012065 filter cake Substances 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000006227 byproduct Substances 0.000 claims abstract description 5
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 22
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
- 206010013786 Dry skin Diseases 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000009423 ventilation Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 9
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract 1
- 238000005054 agglomeration Methods 0.000 abstract 1
- 230000002776 aggregation Effects 0.000 abstract 1
- 238000005915 ammonolysis reaction Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000010808 liquid waste Substances 0.000 abstract 1
- 230000007774 longterm Effects 0.000 abstract 1
- 239000010413 mother solution Substances 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 239000012808 vapor phase Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- FRWYFWZENXDZMU-UHFFFAOYSA-N 2-iodoquinoline Chemical compound C1=CC=CC2=NC(I)=CC=C21 FRWYFWZENXDZMU-UHFFFAOYSA-N 0.000 description 1
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 229940070337 ammonium silicofluoride Drugs 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- LTPBRCUWZOMYOC-UHFFFAOYSA-N beryllium oxide Inorganic materials O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003206 sterilizing agent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
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- Fertilizers (AREA)
Abstract
The invention discloses a method for producing high-purity ammonium bifluoride, which comprises the following steps of: (1) under the stirring condition, introducing anhydrous hydrogen fluoride into saturated solution of ammonium fluoride until the pH value of the reaction liquid ranges from 1 to 4, and stopping introducing the anhydrous hydrogen fluoride, wherein the temperature is controlled between 25 and 50 DEG C in the reaction process; (2) cooling the reaction liquid to the temperature of between 5 and 20 DEG C, and keeping the temperature for 2 to 4 hours until crystals separate out; and (3) filtering, drying a filter cake to obtain the product of high-purity ammonium bifluoride, and recycling the filter liquor. The method for producing the high-purity ammonium bifluoride has the advantages of small equipment investment, simple process, easy operation, and low moisture content, high purity, high dissolving speed, convenient use, hard agglomeration, and long-term storage of the product ammonium bifluoride. The mother solution is circulated in a closed loop, and the whole technical process has no liquid waste discharge. The raw material ammonium fluoride is prepared by ammonolysis of a byproduct fluosilicic acid in the phosphate fertilizer industry, and the method has the advantages of easily obtained raw materials, low cost, and low production cost. The method provides a new fluoride source, and solves the problem of environmental pollution in the phosphate fertilizer industry.
Description
Technical field
The present invention relates to the production method of ammonium bifluoride, be specifically related to a kind of production method of ammonium bifluoride with high purity.
Background technology
Ammonium bifluoride can be used as chemical reagent, glass etching agent, fermentation industry sterilizing agent and sanitas, by the solvent of beryllium oxide system metallic beryllium and the surface treatment agent of silicon steel sheet, also be used for making pottery, magnesium alloy, the cleaning detergency of boiler feed water system and steam generation systems, and the acid treatment of oil field sandstone, also as alkylation, isomerization catalyst component etc.
The traditional production method of ammonium bifluoride mainly contains two kinds of liquid phase method and vapor phase processs, is raw material with hydrofluoric acid and ammonia all.Liquid phase method is with after the liquefied ammonia gasification, feeds reaction in the hydrofluoric acid of external application frozen water refrigerative 30%～40% and gets, and vapor phase process is pure ammonia and hydrogen fluoride gas direct reaction and get.Also have ammonium fluoride solution is directly concentrated the method that decomposition prepares ammonium bifluoride.Among the above preparation method, the liquid phase method less investment, technology is simple, but the ammonium bifluoride water content height of producing, purity is low, and the product dissolution rate is slow, uses inconvenience, easily lumps, can not standing storage.Vapor phase process exists facility investment bigger, shortcomings such as cost height.Ammonium fluoride solution directly concentrates decomposition preparation ammonium bifluoride and also has the energy consumption height, shortcomings such as cost height.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of ammonium bifluoride with high purity.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind of production method of ammonium bifluoride with high purity may further comprise the steps:
(1) under agitation condition, logical anhydrous hydrogen fluoride in the Neutral ammonium fluoride saturated solution, to reacting liquid pH value be 1～4, stop logical anhydrous hydrogen fluoride, temperature is controlled to be 25～50 ℃ in the reaction process;
(2) reaction solution is cooled to 5～20 ℃, kept 2～4 hours, have crystal to separate out;
(3) filter, the filter cake drying gets product of high-purity ammonium bifluoride, and filtrate is recycled.
Wherein, the Neutral ammonium fluoride in the Neutral ammonium fluoride saturated solution described in the step (1) is separated through ammonia by the silicofluoric acid of phosphate fertilizer industry by-product and is made; The Ventilation Rate of anhydrous hydrogen fluoride is 7～14mol/h in the step (1); Drying described in the step (3) is 40～80 ℃ of air stream dryings; Filtrate described in the step (3) is used for the described Neutral ammonium fluoride saturated solution of preparation steps (1) after reclaiming.
Chemical equation of the present invention is:
NH
4F＋HF＝NH
4HF
2
Facility investment of the present invention is few, and technology is simple, easy handling; The product ammonium bifluoride water content of producing is low, the purity height, and dissolution rate is fast, and is easy to use, prevented from caking, but standing storage; Mother liquor closed cycle among the present invention, whole technological process does not have discharging of waste liquid; The raw material Neutral ammonium fluoride that the present invention uses is separated through ammonia by the silicofluoric acid of phosphate fertilizer industry by-product and is made, and raw material is easy to get, and is cheap, and production cost is low; The present invention has opened up new fluorine source, has alleviated the environmental issue of phosphate fertilizer industry greatly.In sum, the present invention has remarkable economic efficiency, social benefit and environmental benefit, suitable promoting the use of.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further.
Embodiment 1
The production method of ammonium bifluoride with high purity may further comprise the steps:
(1) the 500g Neutral ammonium fluoride is mixed with the Neutral ammonium fluoride saturated solution, join in the reactor, start stirring, logical anhydrous hydrogen fluoride in the Neutral ammonium fluoride saturated solution, the Ventilation Rate of anhydrous hydrogen fluoride is 14mol/h, with congo-red test paper monitoring reaction liquid, has just presented when brown to congo-red test paper in the logical anhydrous hydrogen fluoride process, stop logical anhydrous hydrogen fluoride, the reaction process temperature is controlled to be about 30 ℃;
(2) be cooled to 5 ℃, kept 3 hours, have crystal to separate out;
(3) filter, filtrate is returned step (1) preparation Neutral ammonium fluoride saturated solution, and filter cake gets product of high-purity ammonium bifluoride at 40 ℃ of air stream dryings.
Embodiment 2
The production method of ammonium bifluoride with high purity may further comprise the steps:
(1) the 500g Neutral ammonium fluoride is mixed with the Neutral ammonium fluoride saturated solution, join in the reactor, start stirring, logical anhydrous hydrogen fluoride in the Neutral ammonium fluoride saturated solution, the Ventilation Rate of anhydrous hydrogen fluoride is 7mol/h, with congo-red test paper monitoring reaction liquid, has just presented when brown to congo-red test paper in the logical anhydrous hydrogen fluoride process, stop logical anhydrous hydrogen fluoride, the reaction process temperature is controlled to be about 40 ℃;
(2) be cooled to 10 ℃, kept 4 hours, have crystal to separate out;
(3) filter, filtrate is returned step (1) preparation Neutral ammonium fluoride saturated solution, and filter cake gets product of high-purity ammonium bifluoride at 80 ℃ of air stream dryings.
Embodiment 3
The production method of ammonium bifluoride with high purity may further comprise the steps:
(1) the 500g Neutral ammonium fluoride is mixed with the Neutral ammonium fluoride saturated solution, join in the reactor, start stirring, logical anhydrous hydrogen fluoride in the Neutral ammonium fluoride saturated solution, the Ventilation Rate of anhydrous hydrogen fluoride is 10mol/h, with congo-red test paper monitoring reaction liquid, has just presented when brown to congo-red test paper in the logical anhydrous hydrogen fluoride process, stop logical anhydrous hydrogen fluoride, the reaction process temperature is controlled to be about 50 ℃;
(2) be cooled to 20 ℃, kept 2 hours, have crystal to separate out;
(3) filter, filtrate is returned step (1) preparation Neutral ammonium fluoride saturated solution, and filter cake gets product of high-purity ammonium bifluoride at 60 ℃ of air stream dryings.
The Neutral ammonium fluoride that uses among embodiment 1, embodiment 2, the embodiment 3 is separated through ammonia by the silicofluoric acid of phosphate fertilizer industry by-product and is made.
The mass analysis of the product of high-purity ammonium bifluoride that embodiment 1, embodiment 2, embodiment 3 make the results are shown in Table shown in 1.
The mass analysis result of each embodiment ammonium bifluoride with high purity product of table 1
| Index name | Export commodity | Premium grads | Acceptable end product | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Ammonium bifluoride (butt meter) (%) | ≥98.0 | ≥97.0 | ≥95.0 | 98.5 | 98.8 | 98.7 |
| Weight loss on drying (%) | ≤1.5 | ≤3.0 | ≤5.0 | 0.3 | 0.15 | 0.2 |
| Ignition residue (%) | ≤0.2 | ≤0.2 | ≤0.2 | 0.05 | 0.03 | 0.04 |
| Vitriol (%) | ≤0.1 | ≤0.1 | ≤0.1 | 0.05 | 0.03 | 0.03 |
| Ammonium silicofluoride (%) | ≤0.6 | ≤0.7 | ≤0.65 | 0.4 | 0.35 | 0.35 |
Claims (4)
1. the production method of an ammonium bifluoride with high purity is characterized in that, this method may further comprise the steps:
(1) under agitation condition, logical anhydrous hydrogen fluoride in the Neutral ammonium fluoride saturated solution, the Ventilation Rate of anhydrous hydrogen fluoride is 7～14mol/h, to reacting liquid pH value be 1～4 o'clock, stop logical anhydrous hydrogen fluoride, temperature is controlled to be 25～50 ℃ in the reaction process;
(2) reaction solution is cooled to 5～20 ℃, kept 2～4 hours, have crystal to separate out;
(3) filter, the filter cake drying gets product of high-purity ammonium bifluoride, and filtrate is recycled.
2. the production method of ammonium bifluoride with high purity according to claim 1 is characterized in that, the Neutral ammonium fluoride described in the step (1) in the Neutral ammonium fluoride saturated solution is separated through ammonia by the silicofluoric acid of phosphate fertilizer industry by-product and made.
3. the production method of ammonium bifluoride with high purity according to claim 1 is characterized in that, 40～80 ℃ of air stream dryings of dry employing described in the step (3).
4. the production method of ammonium bifluoride with high purity according to claim 1 is characterized in that, filtrate described in the step (3) is used for the described Neutral ammonium fluoride saturated solution of preparation steps (1) after reclaiming.
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| CN2010101090628A CN101898769B (en) | 2010-02-11 | 2010-02-11 | Method for producing high-purity ammonium bifluoride |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2012193074A (en) * | 2011-03-16 | 2012-10-11 | Seiko Epson Corp | Separation method and separation apparatus |
| CN102491370B (en) * | 2011-12-02 | 2013-11-13 | 瓮福（集团）有限责任公司 | Method for producing ammonium bifluoride by recovering fluorine resource from fluorine-containing silicon slag |
| CN102530991B (en) * | 2012-02-28 | 2013-08-07 | 瓮福（集团）有限责任公司 | Preparation method of ammonium bifluoride |
| CN103803584B (en) * | 2012-11-08 | 2016-03-02 | 福建省邵武市永飞化工有限公司 | Ammonium bifluoride preparation method |
| CN102976356B (en) * | 2012-12-17 | 2015-01-14 | 贵州省化工研究院 | Method for preparing high-quality ammonium hydrogen fluoride from fluorine and silicon compound |
| CN103145147B (en) * | 2013-03-28 | 2016-02-17 | 瓮福（集团）有限责任公司 | A kind of method of Liquid preparation methods ammonium bifluoride with high purity |
| CN106044796A (en) * | 2016-06-29 | 2016-10-26 | 福建天福化工有限公司 | Preparation method of high-purity flaky ammonium bifluoride |
| CN111036065B (en) * | 2019-12-30 | 2022-05-20 | 天津市长芦化工新材料有限公司 | Device for removing hydrogen fluoride and using method thereof |
| CN116477577A (en) * | 2023-01-10 | 2023-07-25 | 衢州市鼎盛化工科技有限公司 | Method for preparing anhydrous hydrogen fluoride by recycling low-concentration hydrofluoric acid |
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2010
- 2010-02-11 CN CN2010101090628A patent/CN101898769B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 张梅.氟硅酸法制氟化氢铵联产优质白炭黑工艺研究.《无机盐工业》.2010,第42卷(第1期),第55页第1栏第1行至第56页第1栏第21行. * |
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