CN116621131A - Method and device for recycling sodium difluorophosphate synthetic tail gas - Google Patents
Method and device for recycling sodium difluorophosphate synthetic tail gas Download PDFInfo
- Publication number
- CN116621131A CN116621131A CN202310693830.6A CN202310693830A CN116621131A CN 116621131 A CN116621131 A CN 116621131A CN 202310693830 A CN202310693830 A CN 202310693830A CN 116621131 A CN116621131 A CN 116621131A
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- China
- Prior art keywords
- gas
- sodium
- difluorophosphate
- tail gas
- condenser
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- 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.)
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- KBVUALKOHTZCGR-UHFFFAOYSA-M sodium;difluorophosphinate Chemical compound [Na+].[O-]P(F)(F)=O KBVUALKOHTZCGR-UHFFFAOYSA-M 0.000 title claims abstract description 31
- 238000004064 recycling Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- ODZPKZBBUMBTMG-UHFFFAOYSA-N sodium amide Chemical compound [NH2-].[Na+] ODZPKZBBUMBTMG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 18
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 15
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 12
- SAEOCANGOMBQSP-UHFFFAOYSA-N diazanium;fluoro-dioxido-oxo-$l^{5}-phosphane Chemical compound [NH4+].[NH4+].[O-]P([O-])(F)=O SAEOCANGOMBQSP-UHFFFAOYSA-N 0.000 claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 8
- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000009833 condensation Methods 0.000 claims abstract description 5
- 230000005494 condensation Effects 0.000 claims 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 claims abstract description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 4
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 24
- 238000010521 absorption reaction Methods 0.000 claims description 15
- 238000004821 distillation Methods 0.000 claims description 14
- 238000003860 storage Methods 0.000 claims description 11
- 238000001179 sorption measurement Methods 0.000 claims description 8
- 230000002194 synthesizing effect Effects 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000012459 cleaning agent Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 150000001447 alkali salts Chemical class 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229910000000 metal hydroxide Inorganic materials 0.000 claims description 3
- 150000004692 metal hydroxides Chemical class 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- SDTMFDGELKWGFT-UHFFFAOYSA-N 2-methylpropan-2-olate Chemical compound CC(C)(C)[O-] SDTMFDGELKWGFT-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 230000018044 dehydration Effects 0.000 description 7
- 238000006297 dehydration reaction Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- OBCUTHMOOONNBS-UHFFFAOYSA-N phosphorus pentafluoride Chemical compound FP(F)(F)(F)F OBCUTHMOOONNBS-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/087—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms
- C01B21/092—Compounds containing nitrogen and non-metals and optionally metals containing one or more hydrogen atoms containing also one or more metal atoms
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/455—Phosphates containing halogen
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a method and a device for recycling sodium difluorophosphate synthesis tail gas, which belong to the technical field of sodium difluorophosphate synthesis, wherein ammonium fluoride and phosphoric acid are used for preparing ammonium difluorophosphate, ammonium difluorophosphate and sodium tert-butoxide are reacted for preparing sodium difluorophosphate, tert-butoxide and ammonia, the sodium difluorophosphate synthesis tail gas contains ammonia and vaporized tert-butoxide, the ammonia reacts with alkali liquor to generate sodium amide, the sodium amide and the tert-butoxide are heated to be separated by gas liquid, the vaporized tert-butoxide is recycled by condensation, and a small amount of residual ammonia in gas is adsorbed by active carbon.
Description
Technical Field
The invention belongs to the technical field of sodium difluorophosphate synthesis, and particularly relates to a method and a device for recycling tail gas generated in sodium difluorophosphate synthesis.
Background
In recent years, along with the development of new energy by the national successive departure policy, the targets of carbon peak, carbon neutralization and the like are simultaneously provided, the new energy industry is entering a high-speed development period, and the lithium ion battery has a huge application market in the fields of electric automobiles, energy storage batteries, digital electronic products and the like.
Compared with the preparation of sodium difluorophosphate by a phosphorus pentafluoride gas method, the synthesis of ammonium difluorophosphate is easier to realize, the synthesis of ammonium difluorophosphate does not need to use a high-pressure sealing tube and high temperature, only needs to be heated slightly at the beginning under the atmospheric condition, the reaction can be triggered, and the higher yield can be obtained.
However, the effective components in the tail gas generated by preparing sodium difluorophosphate in the prior art cannot be recycled, so that the problems of low raw material utilization rate and increased production cost are caused.
Disclosure of Invention
To solve the problems set forth in the background art. The invention provides a method for recycling tail gas generated in synthesizing sodium difluorophosphate, which has the characteristics of simple structure and high recycling rate.
The invention also provides a device for recycling the tail gas generated in the synthesis of sodium difluorophosphate.
In order to achieve the above purpose, the present invention provides the following technical solutions: according to the method, ammonium fluoride and phosphoric acid are prepared to obtain ammonium difluorophosphate, the ammonium difluorophosphate reacts with sodium tert-butoxide to obtain sodium difluorophosphate, tert-butoxide and ammonia gas, the sodium difluorophosphate synthesis tail gas contains ammonia gas and vaporized tert-butoxide, the ammonia gas reacts with alkali liquor to generate sodium amide, the sodium amide and the tert-butoxide are heated to be separated into gas and liquid, the vaporized tert-butoxide is recovered through condensation, and a small amount of ammonia gas remained in the gas is adsorbed through activated carbon.
Further, the temperature at which the tertiary butanol and the sodium amide are condensed is 20-80 ℃.
Further, the alkali liquor is one or more aqueous solutions of metal hydroxide, alkali weak acid salt, basic salt and active metal oxide, and one of the reaction equations is as follows: 2nh3+2naoh→2h2o+2nanh2.
Further, after the alkali liquor reacts with ammonia gas, separating liquid, dehydrating and distilling to obtain the sodium amide which can be used for synthesizing the cleaning agent.
Further, the distillation temperature is 210 ℃ to 400 ℃.
Further, a synthetic tail gas recycle device of sodium difluorophosphate, including synthetic tail gas transfer line, the gas outlet of synthetic tail gas transfer line is connected with first condenser, the gas outlet of first condenser is connected with the absorption tower, the gas outlet of absorption tower is connected with the second condenser, the gas outlet of second condenser is connected with active carbon adsorption device, active carbon adsorption device's gas outlet is connected with the exhaust line, the liquid outlet of absorption tower is connected with gas-liquid separator, gas-liquid separator's gas outlet is connected with the third condenser, the liquid outlet of third condenser is connected with the holding vessel, the side of holding vessel is connected with the refrigerator, the liquid outlet of gas-liquid separator is connected with the dehydration tower, the liquid outlet of dehydration tower is connected with the distillation column, the liquid outlet of distillation column is connected with the fourth condenser, the side of distillation column is provided with the holding vessel.
Further, a reflux tower is arranged between the second condenser and the absorption tower.
Further, a heater is arranged on the side edge of the gas-liquid separator, and the heating temperature range of the heater is 0-100 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention solves the problems of low utilization rate of raw materials and environmental pollution of tail gas in the prior art, can recycle the catalyst tertiary butanol for preparing sodium difluorophosphate by treating the tail gas, greatly reduces raw material cost, reduces environmental pollution, reacts ammonia with alkali liquor, and obtains the sodium amide for synthesizing the cleaning agent by separating liquid, dehydrating and distilling, thereby realizing the recycling of the synthesized tail gas.
Drawings
FIG. 1 is a schematic diagram of a device for recycling sodium difluorophosphate synthesis tail gas;
in the figure: 1. a synthetic tail gas transfer line; 2. a first condenser; 3. an absorption tower; 4. a second condenser; 5. an activated carbon adsorption device; 6. an exhaust line; 7. a reflux column; 8. a third condenser; 9. a storage tank; 10. a refrigerator; 11. a heater; 12. a gas-liquid separator; 13. a dehydration tower; 14. a distillation column; 15. a fourth condenser; 16. a storage tank.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, the present invention provides the following technical solutions: the method for recycling the tail gas of the sodium difluorophosphate synthesis comprises the steps of preparing ammonium difluorophosphate from ammonium fluoride and phosphoric acid, preparing sodium difluorophosphate, tertiary butanol and ammonia gas by reacting the ammonium difluorophosphate with the tertiary butanol, generating sodium amide by reacting the ammonia gas with alkali liquor, heating the sodium amide and the tertiary butanol, separating the heated gas from the vaporized tertiary butanol, condensing and recovering the vaporized tertiary butanol, and adsorbing a very small amount of ammonia gas remained in the gas by activated carbon.
In the invention, the condensation temperature of tertiary butanol and sodium amide is 20-80 ℃.
In the invention, the alkali liquor is one or more aqueous solutions of metal hydroxide, alkali weak acid salt, basic salt and active metal oxide, and one of the reaction equations is as follows: 2nh3+2naoh→2h2o+2nanh2.
In the invention, after the alkali liquor reacts with ammonia gas, the sodium amide which can be used for synthesizing the cleaning agent is obtained through liquid separation, dehydration and distillation.
In the present invention, the distillation temperature is 210-400 ℃.
The invention further discloses a sodium difluorophosphate synthetic tail gas recycling device, which comprises a synthetic tail gas conveying pipeline 1, wherein an air outlet of the synthetic tail gas conveying pipeline 1 is connected with a first condenser 2, an air outlet of the first condenser 2 is connected with an absorption tower 3, an air outlet of the absorption tower 3 is connected with a second condenser 4, an air outlet of the second condenser 4 is connected with an activated carbon adsorption device 5, an air outlet of the activated carbon adsorption device 5 is connected with an exhaust pipeline 6, a liquid outlet of the absorption tower 3 is connected with a gas-liquid separator 12, an air outlet of the gas-liquid separator 12 is connected with a third condenser 8, a liquid outlet of the third condenser 8 is connected with a storage tank 9, a side edge of the storage tank 9 is connected with a refrigerator 10, a liquid outlet of the gas-liquid separator 12 is connected with a dehydration tower 13, a liquid outlet of the dehydration tower 13 is connected with a distillation tower 14, a liquid outlet of the distillation tower 14 is connected with a fourth condenser 15, and a storage tank 16 is arranged on a side edge of the distillation tower 14.
In the present invention, a reflux column 7 is provided between the second condenser 4 and the absorption column 3.
In the invention, the side of the gas-liquid separator 12 is provided with a heater 11, and the heating temperature of the heater 11 is in the range of 0-100 ℃.
The working principle and the using flow of the invention are as follows: when the invention is used, the tertiary butanol gas with ammonia and vaporization enters from the synthetic tail gas conveying pipeline 1, the ammonia and the tertiary butanol enter into the absorption tower 3 through the first condenser 2 for cooling and condensing, the ammonia reacts with alkali liquor in the absorption tower 3 to generate sodium amide, the gas is condensed through the second condenser 4, the gas is adsorbed by the activated carbon adsorption device 5, then the gas is discharged from the exhaust pipeline 6, the sodium amide and the tertiary butanol enter into the gas-liquid separator 12, the heater 11 heats the tertiary butanol to vaporize, the tertiary butanol is condensed and collected into the storage tank 9 through the third condenser 8, the refrigerator 10 refrigerates, the tertiary butanol in the storage tank 9 is in a low temperature state, the tertiary butanol is conveniently stored, the sodium amide is dehydrated through the dehydration tower 13, and distilled through the distillation tower 14, so that the purity of the sodium amide is improved, and the sodium amide is stored in the storage tank 16 after being condensed through the fourth condenser 15, and the recovery and the reutilization of the synthetic tail gas are realized.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for recycling tail gas generated in synthesizing sodium difluorophosphate is characterized by comprising the following steps: ammonium fluoride and phosphoric acid are prepared to obtain ammonium difluorophosphate, the ammonium difluorophosphate reacts with sodium tert-butoxide to obtain sodium difluorophosphate, tert-butanol and ammonia, ammonia and vaporized tert-butanol are contained in the tail gas generated by synthesizing sodium difluorophosphate, the ammonia reacts with alkali liquor to generate sodium amide, the sodium amide and the tert-butanol are heated to be separated into gas and liquid, the vaporized tert-butanol is recovered through condensation, and a small amount of residual ammonia in the gas is adsorbed through activated carbon.
2. The method for recycling sodium difluorophosphate synthesis tail gas according to claim 1, wherein the method comprises the following steps: the condensation temperature of the tertiary butanol and the sodium amide is 20-80 ℃.
3. The method for recycling sodium difluorophosphate synthesis tail gas according to claim 1, wherein the method comprises the following steps: the alkali liquor is one or more aqueous solutions of metal hydroxide, alkali weak acid salt, basic salt and active metal oxide, and one of the reaction equations is as follows: 2nh3+2naoh→2h2o+2nanh2.
4. The method for recycling sodium difluorophosphate synthesis tail gas according to claim 1, wherein the method comprises the following steps: after the alkali liquor reacts with ammonia gas, separating liquid, dehydrating and distilling to obtain the sodium amide which can be used for synthesizing the cleaning agent.
5. The method for recycling sodium difluorophosphate synthesis tail gas according to claim 1, wherein the method comprises the following steps: the distillation temperature is 210-400 ℃.
6. The method for recycling sodium difluorophosphate synthesis tail gas according to any one of claims 1 to 5, characterized by comprising the following steps: the sodium difluorophosphate synthetic tail gas recycling device comprises a synthetic tail gas conveying pipeline, wherein a first condenser is connected with a gas outlet of the synthetic tail gas conveying pipeline, an absorption tower is connected with a gas outlet of the first condenser, a second condenser is connected with a gas outlet of the absorption tower, an activated carbon adsorption device is connected with a gas outlet of the activated carbon adsorption device, a gas exhaust pipeline is connected with a gas outlet of the absorption tower, a gas-liquid separator is connected with a gas outlet of the gas-liquid separator, a third condenser is connected with a liquid outlet of the third condenser, a storage tank is connected with a side edge of the storage tank, a dehydrating tower is connected with a liquid outlet of the dehydrating tower, a distillation tower is connected with a fourth condenser, and a storage tank is arranged on the side edge of the distillation tower.
7. The sodium difluorophosphate synthesis tail gas recycling apparatus according to claim 6, wherein: a reflux tower is arranged between the second condenser and the absorption tower.
8. The sodium difluorophosphate synthesis tail gas recycling apparatus according to claim 6, wherein: the side of the gas-liquid separator is provided with a heater, and the heating temperature of the heater ranges from 0 ℃ to 100 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310693830.6A CN116621131A (en) | 2023-06-12 | 2023-06-12 | Method and device for recycling sodium difluorophosphate synthetic tail gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310693830.6A CN116621131A (en) | 2023-06-12 | 2023-06-12 | Method and device for recycling sodium difluorophosphate synthetic tail gas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116621131A true CN116621131A (en) | 2023-08-22 |
Family
ID=87597347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310693830.6A Withdrawn CN116621131A (en) | 2023-06-12 | 2023-06-12 | Method and device for recycling sodium difluorophosphate synthetic tail gas |
Country Status (1)
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|---|---|
| CN (1) | CN116621131A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117771873A (en) * | 2023-11-15 | 2024-03-29 | 上海开鸿环保科技有限公司 | Method for recycling fluorobenzene synthesis tail gas pollution components based on activated carbon assisted denitration |
-
2023
- 2023-06-12 CN CN202310693830.6A patent/CN116621131A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117771873A (en) * | 2023-11-15 | 2024-03-29 | 上海开鸿环保科技有限公司 | Method for recycling fluorobenzene synthesis tail gas pollution components based on activated carbon assisted denitration |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20230822 |
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