CN110092354A - Fluorite adds the method for silica hydrothermal calcine processing and manufacturing anhydrous hydrogen fluoride - Google Patents
Fluorite adds the method for silica hydrothermal calcine processing and manufacturing anhydrous hydrogen fluoride Download PDFInfo
- Publication number
- CN110092354A CN110092354A CN201810092466.7A CN201810092466A CN110092354A CN 110092354 A CN110092354 A CN 110092354A CN 201810092466 A CN201810092466 A CN 201810092466A CN 110092354 A CN110092354 A CN 110092354A
- Authority
- CN
- China
- Prior art keywords
- hydrogen fluoride
- melamine
- solution
- diafiltration
- syria
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000010436 fluorite Substances 0.000 title claims abstract description 12
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 title claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title abstract description 11
- 229910000040 hydrogen fluoride Inorganic materials 0.000 title abstract description 11
- 238000004519 manufacturing process Methods 0.000 title description 3
- 239000007789 gas Substances 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 12
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 10
- 238000011026 diafiltration Methods 0.000 claims abstract description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 10
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims abstract description 10
- VBKNTGMWIPUCRF-UHFFFAOYSA-M potassium;fluoride;hydrofluoride Chemical compound F.[F-].[K+] VBKNTGMWIPUCRF-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000011698 potassium fluoride Substances 0.000 claims abstract description 8
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims abstract description 7
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 7
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 7
- 229910001634 calcium fluoride Inorganic materials 0.000 claims abstract description 5
- 235000003270 potassium fluoride Nutrition 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 5
- 239000002002 slurry Substances 0.000 claims abstract description 5
- 239000003337 fertilizer Substances 0.000 claims abstract description 4
- HSWVOAHDTZACBD-UHFFFAOYSA-N hydron;1,3,5-triazine-2,4,6-triamine;fluoride Chemical compound F.NC1=NC(N)=NC(N)=N1 HSWVOAHDTZACBD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- RNMCQEMQGJHTQF-UHFFFAOYSA-N 3,5,6,7-tetrahydrotetrazolo[1,5-b][1,2,4]triazine Chemical compound N1CCN=C2N=NNN21 RNMCQEMQGJHTQF-UHFFFAOYSA-N 0.000 claims description 2
- 239000000428 dust Substances 0.000 claims description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims 1
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 1
- 238000001816 cooling Methods 0.000 claims 1
- 239000003546 flue gas Substances 0.000 claims 1
- 238000005829 trimerization reaction Methods 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- -1 halide salt Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- 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
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/192—Preparation from fluorspar
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Removal Of Specific Substances (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Cab-O-sil is added in Fluorspar Powder, is allowed to CaF2、SiO2Mole ratio be 1: 1, it is placed in electric furnace, it is passed through water vapour and produces hydrogen fluoride in 800-900 degree Celsius roasting, furnace gas first passes through gravitational settling dedusting, it is passed through melamine slurry again and hydrogen fluoride generates hydrogen fluoride melamine complex salt crystal body, it is reacted again with potassium fluoride solution through diafiltration, generate potassium bifluoride solution and melamine, the latter is returned and goes to react with the HF in furnace gas before this process, the former condensing crystallizing diafiltration is dried to solid, it is placed in thermal decomposition releasing hydrogen fluoride in 400 degree of electric furnaces Celsius and is condensed into anhydrous hydrogen fluoride product, the potassium fluoride for decomposing generation returns to wiring solution-forming before this process and reacts again with hydrogen fluoride melamine double salt, the solid of roaster discharge is through levigate as high-quality siliceous fertilizer.
Description
Technical field
The present invention is the manufacturing technology of anhydrous hydrogen fluoride, is to belong to halide salt hydrothermal calcine technology neck city.
Background material
Fluorite produces anhydrous hydrogen fluoride, is enriching sulfuric acid decomposition technique both at home and abroad, yet there are no so far and sulfuric acid is not added and obtains
To the technology of anhydrous hydrogen fluoride.
Summary of the invention
1, by CaF2H5/SiO2Equal gram molecules hydro-thermal reaction principle is added and fluorite CaF in Fluorspar Powder2It is equimolar
SiO2Cab-O-sil.
2, mixture is steam roasting 1 hour logical at 800 1 900 degree Celsius
3, roaster gas is first passed through into gravitational dust collection, enters back into and reacts generation HF, C in melamine slurry with HF3H6N6,
nH2O complex salt crystal body, the moisture content in furnace gas are discharged with gaseous state and liquid
4, complex salt crystal body generates potassium bifluoride solution and melamine is solid through diafiltration and certain density kF solution reaction
Body, the latter return to front and react with the HF in furnace gas.
5, by KHF2Solution condensing crystallizing is dry, is placed in 400 degree of electric furnaces Celsius and thermally decomposes, and the HF condensation of generation is
AHF product, the KF return front for decomposing generation are modulated into kF solution and react again with double salt.
6, by the solid of roaster discharge through levigate as high-quality siliceous fertilizer.
Detailed description of the invention
Fig. 1 is that fluorite adds silica hydrothermal calcine to fabricate anhydrous hydrogen fluoride process flow diagram
By CaF2、SiO2Equal gram molecules hydro-thermal reaction principle is added and fluorite CaF in Fluorspar Powder2Equimolar SiO2's
Cab-O-sil.It is mixed into 800 1 900 degree of electric furnaces Celsius and is passed through steam roasting 1 hour, the furnace gas of generation passes through gravitational settling
It is passed through reaction in melamine slurry liquid after dedusting and generates HF, C3H6N6, nH2O complex salt crystal body, after diafiltration by its with it is certain dense
The KF solution reaction of degree generates potassium bifluoride solution and melamine, the latter's diafiltration return before this process again with the HF in furnace gas
It reacts, is placed in 400 degree of electric furnace Celsius and thermally decomposes after the concentrated crystallizing and drying of potassium bifluoride solution, the hydrogen fluoride of generation is through cold
Solidifying to become AHF product, the potassium fluoride for thermally decomposing generation is reacted with double salt again back to wiring solution-forming before this process.
Embodiment
Take 1000 grams of CaF2SiO is added in=97% Fluorspar Powder2=98% Cab-O-sil 761.6g, stirs evenly, merging
Lead to steam roasting 1 hour in Celsius 850 native 5 degree of electric furnaces, roaster gas first passes through gravity settling basin, enters back into melamine slurry
Expect that reactor generates hydrogen fluoride melamine complex salt crystal body, through diafiltration, its fluorination nak response for being 20% with concentration is generated
Potassium bifluoride solution simultaneously releases melamine, returns after the latter's diafiltration and goes to react with the HF in furnace gas before this process, generation
The concentrated crystallizing and drying of potassium bifluoride solution obtains solid KHF2, it is put into 400 degree of electric furnaces Celsius and thermally decomposes, the gas of generation
It is 99.96% mass is 472.8 grams of AHF that body condensation, which is purity, and the KF for decomposing generation, which is returned, is fitted on into solution before this process
It is reacted with double salt, the sizing of roaster discharge is carefully high-quality siliceous fertilizer.
Product quality analysis (weight %)
Claims (7)
1. pressing CaF2、SiO2Equal gram molecules hydrothermal calcine reaction principle is added and fluorite CaF in Fluorspar Powder2Equimolar SiO2
Cab-O-sil.
2. being put into 800-900 degree electric furnace Celsius, lead to steam roasting 0.5-1 hours.
3. the flue gas come out from roaster enters trimerization after first passing through gravitational dust collection according to the method that claim 2 Syria is stated
Cyanamide slurry liquid generates HF, C3H6N6, nH2O double salt is fixed up.
4. being reacted again with certain density potassium fluoride solution according to double salt in the method that claim 3 Syria is stated through diafiltration, generate
Potassium bifluoride solution simultaneously releases melamine.
5. according to the method that claim 4 Syria is stated the HF gone before this process with furnace gas will be returned to after melamine diafiltration
Reaction, solution condensing crystallizing diafiltration it is dry potassium bifluoride solid.
6. according to the method that claim 5 Syria is stated, by potassium bifluoride be placed in heat resolve in 400 degree of electric furnaces Celsius go out it is pure
HF gas, is condensed into AHF product, and the potassium fluoride of generation returns to wiring solution-forming before this process and goes to answer with hydrogen fluoride melamine
The anti-Me of salt.
7. it is high-quality siliceous fertilizer that the solid of roaster discharge is levigate through cooling according to the method that claim 2 Syria is stated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810092466.7A CN110092354A (en) | 2018-01-29 | 2018-01-29 | Fluorite adds the method for silica hydrothermal calcine processing and manufacturing anhydrous hydrogen fluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810092466.7A CN110092354A (en) | 2018-01-29 | 2018-01-29 | Fluorite adds the method for silica hydrothermal calcine processing and manufacturing anhydrous hydrogen fluoride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110092354A true CN110092354A (en) | 2019-08-06 |
Family
ID=67441979
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810092466.7A Pending CN110092354A (en) | 2018-01-29 | 2018-01-29 | Fluorite adds the method for silica hydrothermal calcine processing and manufacturing anhydrous hydrogen fluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110092354A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0514701B2 (en) * | 1984-06-07 | 1993-02-25 | Tokuyama Soda Kk | |
| CN101269816A (en) * | 2008-05-16 | 2008-09-24 | 夏克立 | Method for producing fluorine series compounds and white carbon black |
| CN107188145A (en) * | 2016-03-14 | 2017-09-22 | 姚鼎文 | The method that one kind makes industrial potassium dihydrogen phosphate with hydrochloric acid decomposing medium and low grade, melamine complex salt crystal legal system |
-
2018
- 2018-01-29 CN CN201810092466.7A patent/CN110092354A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0514701B2 (en) * | 1984-06-07 | 1993-02-25 | Tokuyama Soda Kk | |
| CN101269816A (en) * | 2008-05-16 | 2008-09-24 | 夏克立 | Method for producing fluorine series compounds and white carbon black |
| CN107188145A (en) * | 2016-03-14 | 2017-09-22 | 姚鼎文 | The method that one kind makes industrial potassium dihydrogen phosphate with hydrochloric acid decomposing medium and low grade, melamine complex salt crystal legal system |
Non-Patent Citations (1)
| Title |
|---|
| 张邦建等: "《食品卫生检测技术》", 海洋出版社 * |
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Application publication date: 20190806 |