CN102399126A - Method for preparing high purity tetrafluoromethane through combination of rectification and adsorption - Google Patents
Method for preparing high purity tetrafluoromethane through combination of rectification and adsorption Download PDFInfo
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- CN102399126A CN102399126A CN2011104250680A CN201110425068A CN102399126A CN 102399126 A CN102399126 A CN 102399126A CN 2011104250680 A CN2011104250680 A CN 2011104250680A CN 201110425068 A CN201110425068 A CN 201110425068A CN 102399126 A CN102399126 A CN 102399126A
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- gas
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- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 13
- XWCDCDSDNJVCLO-UHFFFAOYSA-N Chlorofluoromethane Chemical compound FCCl XWCDCDSDNJVCLO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000010574 gas phase reaction Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 36
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 23
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 19
- 239000000126 substance Substances 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000002594 sorbent Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 abstract description 11
- 239000000047 product Substances 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 8
- 239000006227 byproduct Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- VBKNTGMWIPUCRF-UHFFFAOYSA-M potassium;fluoride;hydrofluoride Chemical compound F.[F-].[K+] VBKNTGMWIPUCRF-UHFFFAOYSA-M 0.000 abstract 1
- 231100000331 toxic Toxicity 0.000 abstract 1
- 230000002588 toxic effect Effects 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- AFYPFACVUDMOHA-UHFFFAOYSA-N chlorotrifluoromethane Chemical compound FC(F)(F)Cl AFYPFACVUDMOHA-UHFFFAOYSA-N 0.000 description 5
- 238000009835 boiling Methods 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920002449 FKM Polymers 0.000 description 1
- 229910000792 Monel Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing high purity tetrafluoromethane through combination of rectification and adsorption. The method is mainly characterized in that: equipment for generating tetrafluoromethane continuously supplies the tetrafluoromethane, and fluorochloromethane and potassium bifluoride are subjected to gas-phase reaction to form the tetrafluoromethane. In the method for preparing the high purity tetrafluoromethane, a raw material preparation system, a tetrafluoromethane gas preparation system and a liquefying and gasifying system for the tetrafluoromethane purified through combination of rectification and adsorption. The method has the advantages that: the product has high yield and high purity (99.0-99.9 percent), has a few impurities which are easy to separate; and besides the product, other harmful and toxic byproducts are absent, the operation is convenient, and the method is an ideal technology for preparing the high purity tetrafluoromethane.
Description
Technical field
The present invention relates to a kind of alkanes Chemicals, particularly a kind of rectifying and adsorption combined mode prepare the Technology of high-purity tetrafluoromethane method, are suitable for the synthetic tetrafluoromethane of chemical industry
Background technology
tetrafluoro-methane is incombustible colourless, tasteless high pressure liquefied gas.Tetrafluoro-methane is the maximum plasma etch gases of consumption in the present microelectronics industry; In the electron device surface cleaning; The production of solar cell; Laser technology, gas phase insulation, cryogenic refrigeration, leak check agent, control cosmic rocket attitude, the aspects such as stain remover during printed wiring is produced are also used in a large number.Because its chemicalstability, tetrafluoro-methane can be used for Metal smelting, for example: copper, stainless steel, carbon steel, aluminium, Monel etc.; Also can be used for plastic industry; As: viton, X 050, also can be widely used in silicon, silicon-dioxide, silicon nitride, the etching of thin-film materials such as phosphorosilicate glass and tungsten is in the electron device surface cleaning.Original technology can not continuous production, the equipment fluctuation of service, and energy consumption is high, and product purity is low
Summary of the invention
problem to be solved by this invention is that overcome the deficiency of prior art, prior art can not be produced high-purity tetrafluoromethane, and present technique provides the high-purity tetrafluoromethane method of a kind of preparation Technology.This technology not only technology is reasonable, and preparation is simple, and is that the tetrafluoromethane purity of producing is brought up to 5N (99.999%), and has solved problem of environmental pollution.
The technical scheme that the present invention adopts is:
A kind of method that adopts rectifying and adsorption combined mode to produce high-purity tetrafluoromethane is characterized in that, at catalyzer CrO
2
F
2
Fluidized-bed, supply with thick tetrafluoromethane (300-350 kilogram/hour) continuously by the equipment that tetrafluoromethane takes place, carry out gas-phase reaction with fluorochloromethane and hydrogen fluoride and prepare tetrafluoromethane, through the high-purity tetrafluoromethane of multistage reacted;
Wherein the 1st section reaction is to be filled with CrO
2
F
2
Make CF in the fluidized-bed reactor of catalyzer
3
Cl and HF reaction, 200-600 ℃ of reaction down, or CrF
3
3H
2
O is at O
2
Exist to heat down in 350-750 ℃ down and make; CF3Cl is controlled at 1:2-8 with the amount of substance ratio of HF, and gas space velocity is 10-150h
-1
, temperature of reaction is 380-420 ℃, the gas of the 1st section generation gets into the 2nd section reaction after washing, alkali cleaning, drying;
In the 2nd section reaction, feed HF again, make CF
3
Cl is controlled at 1:0.3-5 with the amount of substance ratio of HF, and gas space velocity is at 10 ~ 300h
-1
, temperature of reaction is constant; Can make unreacted CF in this way
3
The Cl x is controlled at 15 * 10
-6
Below, product has higher purity;
In rectifying, adsorb, select to adsorb the sorbent material of removing these impurity, be about to distillation and make up, make total impurities be lower than 1 * 10 with absorption
-6
, produce high-purity tetrafluoromethane of 99.999%.
More detailed the disclosing of
the present invention adopts rectifying and adsorption combined mode to produce the Technology of high-purity tetrafluoromethane method; Mainly be to supply with thick tetrafluoromethane continuously by the equipment that tetrafluoromethane takes place; Carry out gas-phase reaction with fluorochloromethane and hydrogen fluoride (HF) and prepare tetrafluoromethane; Since fluorochloromethane fluoridize corresponding methane difficulty, therefore reaction is many carries out having under the condition of catalyzer, catalyzer uses the compound that contains Cr usually.Technology through the high-purity tetrafluoromethane of multistage reacted.The 1st section reaction is in the fluidized-bed reactor that is filled with the CrO2F2 catalyzer, to make CF3Cl and HF reaction, and reaction formula is following:
CF
3
Cl?+?HF
CF
4
?+?HCl
Catalyst system therefor can pass through Cr (III) oxyhydroxide and HF reacts down at 200-600 ℃, or CrF
3
3H
2
O is at O
2
Exist to heat down in 350-750 ℃ down and make.CF
3
Cl is controlled at 1 with the amount of substance ratio of HF: (2-8), gas space velocity is 10 ~ 150h
-1
, temperature of reaction is 380-420 ℃.The gas of the 1st section generation gets into the 2nd section reaction after washing, alkali cleaning, drying.
In the 2nd section reaction, feed HF again, make CF3Cl and the amount of substance ratio of HF be controlled at 1: (0.3-5), gas space velocity is at 10 ~ 300h
-1
, temperature of reaction is constant.Can make unreacted CF3Cl x be controlled at 15 * 10 in this way
-6
Below, product has higher purity.According to the foreign matter content of rough tetrafluoromethane, will contain low boiling point component and (C such as H2, N2, O2, Ar, CO, CH4
2
H
5
) 2O, CH
3
Cl, C
2
H
5
High boiling point compositions such as Cl, B4H10, B5H9, B5H11 are particularly near BF
3
The rough BF3 of impurity such as the CO2 that is difficult to fractionation by distillation of boiling point, C2H6 adsorbs in rectifying, selects to adsorb the sorbent material of removing these impurity, is about to distillation and makes up with absorption, makes total impurities be lower than 1 * 10
-6
, produce high-purity tetrafluoromethane of 99.999%.
by raw material preparation system → tetrafluoromethane gas preparation system, → liquefaction of rectifying and adsorption combined purifying tetrafluoromethane, carburetion system constitutes the high-purity tetrafluoromethane method technology of preparation.Its advantage is that product yield is high, purity high (99.0% ~ 99.9%), and the few and separate easily of impurity except that product itself, does not have other harmful, deleterious by products, operates more conveniently yet, is the desirable technique that high-purity tetrafluoromethane prepares.
The advantage that preparation method of the present invention had is:
(1) present method can continous-stable the purification tetrafluoro-methane, solved the drawback that can not stablize purification of original batch fractionating.
(2) integrated continuous rectification can better utilised cold and heat, makes production cost lower.
Steady quality behind
(3) continuous production can large-scale industrial production.
Description of drawings
Fig. 1 produces the technical process of high-pure carbon tetrafluoride for the absorption-low temperature rectification method
Wherein
1, the 2-adsorber; The 3-low-temperature fractionating tower; The 4-surge tank; The 5-molding machine; The 6-condensing surface
The 7-cryogenic heat exchanger; 8-ethene surge tank; The 9-vacuum pump; The 10-compressor.
Embodiment:
The present invention is explained below in conjunction with embodiment in
; The scheme of embodiment described here; Do not limit the present invention; One of skill in the art can make improvements and change according to spirit of the present invention, and described these improvement and variation all should be regarded as within the scope of the invention, and scope of the present invention and essence are limited claim.
Embodiment 1
At the fluidized-bed of catalyzer CrO2F2, supply with thick tetrafluoromethane (300 kilograms/hour) continuously by the equipment that tetrafluoromethane takes place, carry out gas-phase reaction with fluorochloromethane and hydrogen fluoride and prepare tetrafluoromethane, through the high-purity tetrafluoromethane of multistage reacted;
Wherein the 1st section reaction is in the fluidized-bed reactor that is filled with the CrO2F2 catalyzer, to make CF3Cl and HF reaction, and 200 ℃ of reactions down, or CrF33H2O heats under 350 ℃ under O2 and makes; CF
3
Cl is controlled at 1:2 with the amount of substance ratio of HF, and gas space velocity is 10-150h
-1
, temperature of reaction is 380 ℃, the gas of the 1st section generation gets into the 2nd section reaction after washing, alkali cleaning, drying;
In the 2nd section reaction, feed HF again, make CF
3
Cl is controlled at 1:0.3 with the amount of substance ratio of HF, and gas space velocity is at 10 ~ 300h
-1
, temperature of reaction is constant; Can make unreacted CF in this way
3
The Cl x is controlled at 15 * 10
-6
Below, product has higher purity; In rectifying, adsorb, select to adsorb the sorbent material of removing these impurity, be about to distillation and make up, make total impurities be lower than 1 * 10 with absorption
-6
, produce high-purity tetrafluoromethane of 99.999%.
At catalyzer CrO
2
F
2
Fluidized-bed, supply with thick tetrafluoromethane (350 kilograms/hour) continuously by the equipment that tetrafluoromethane takes place, carry out gas-phase reaction with fluorochloromethane and hydrogen fluoride and prepare tetrafluoromethane, through the high-purity tetrafluoromethane of multistage reacted;
Wherein the 1st section reaction is to be filled with CrO
2
F
2
Make CF in the fluidized-bed reactor of catalyzer
3
Cl and HF reaction, 600 ℃ of reactions down, or CrF
3
3H
2
O is at O
2
Exist to heat down in 750 ℃ down and make; CF
3
Cl is controlled at 1:8 with the amount of substance ratio of HF, and gas space velocity is 10-150h
-1
, temperature of reaction is 420 ℃, the gas of the 1st section generation gets into the 2nd section reaction after washing, alkali cleaning, drying;
In the 2nd section reaction, feed HF again, make CF
3
Cl is controlled at 1:5 with the amount of substance ratio of HF, and gas space velocity is at 10 ~ 300h
-1
, temperature of reaction is constant; Can make unreacted CF in this way
3
The Cl x is controlled at 15 * 10
-6
Below, product has higher purity; In rectifying, adsorb, select to adsorb the sorbent material of removing these impurity, be about to distillation and make up, make total impurities be lower than 1 * 10 with absorption
-6
, produce high-purity tetrafluoromethane of 99.999%
Claims (1)
1. method that adopts rectifying and adsorption combined mode to produce high-purity tetrafluoromethane; It is characterized in that; Fluidized-bed at catalyzer CrO2F2; By the equipment 300-350 kilogram that tetrafluoromethane takes place/hour supply with thick tetrafluoromethane continuously, carry out gas-phase reaction with fluorochloromethane and hydrogen fluoride and prepare tetrafluoromethane, through the high-purity tetrafluoromethane of multistage reacted;
Wherein the 1st section reaction is to be filled with CrO
2F
2Make CF in the fluidized-bed reactor of catalyzer
3Cl and HF reaction, 200-600 ℃ of reaction down, or CrF
33H
2O is at O
2Exist to heat down in 350-750 ℃ down and make; CF
3Cl is controlled at 1:2-8 with the amount of substance ratio of HF, and gas space velocity is 10-150h
-1, temperature of reaction is 380-420 ℃, the gas of the 1st section generation gets into the 2nd section reaction after washing, alkali cleaning, drying;
In the 2nd section reaction, feed HF again, make CF
3Cl is controlled at 1:0.3-5 with the amount of substance ratio of HF, and gas space velocity is at 10 ~ 300h
-1, temperature of reaction is constant; Can make unreacted CF in this way
3The Cl x is controlled at 15 * 10
-6Below, product has higher purity;
In rectifying, adsorb, select to adsorb the sorbent material of removing these impurity, be about to distillation and make up, make total impurities be lower than 1 * 10 with absorption
-6, produce high-purity tetrafluoromethane of 99.999%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104250680A CN102399126A (en) | 2011-12-19 | 2011-12-19 | Method for preparing high purity tetrafluoromethane through combination of rectification and adsorption |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104250680A CN102399126A (en) | 2011-12-19 | 2011-12-19 | Method for preparing high purity tetrafluoromethane through combination of rectification and adsorption |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102399126A true CN102399126A (en) | 2012-04-04 |
Family
ID=45881833
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104250680A Pending CN102399126A (en) | 2011-12-19 | 2011-12-19 | Method for preparing high purity tetrafluoromethane through combination of rectification and adsorption |
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| Country | Link |
|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664502A (en) * | 2012-09-07 | 2014-03-26 | 佛山市华特气体有限公司 | Octafluoropropane purifying method |
| CN103951543A (en) * | 2014-04-18 | 2014-07-30 | 佛山市华特气体有限公司 | Device and method for purifying trifluoromethane |
| CN108529589A (en) * | 2018-06-21 | 2018-09-14 | 山东重山光电材料股份有限公司 | A kind of method of industrialized production fluorinated carbon material |
| CN111099957A (en) * | 2019-12-26 | 2020-05-05 | 福建德尔科技有限公司 | Purification system and method for electronic-grade carbon tetrafluoride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4264530A (en) * | 1979-02-26 | 1981-04-28 | Daikin Kogyo Co., Ltd. | Process for preparing high purity tetrafluoromethane |
| EP0690147A1 (en) * | 1994-07-01 | 1996-01-03 | Haldor Topsoe A/S | Process for the electrochemical fluorination of a hydrocarbon substratum |
| CN1561318A (en) * | 2000-04-28 | 2005-01-05 | 昭和电工株式会社 | Method of purifying tetrafluoromethane and utilization thereof |
| CN101541673A (en) * | 2006-05-31 | 2009-09-23 | 纳幕尔杜邦公司 | Process for purifying perfluorinated products |
-
2011
- 2011-12-19 CN CN2011104250680A patent/CN102399126A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4264530A (en) * | 1979-02-26 | 1981-04-28 | Daikin Kogyo Co., Ltd. | Process for preparing high purity tetrafluoromethane |
| EP0690147A1 (en) * | 1994-07-01 | 1996-01-03 | Haldor Topsoe A/S | Process for the electrochemical fluorination of a hydrocarbon substratum |
| CN1561318A (en) * | 2000-04-28 | 2005-01-05 | 昭和电工株式会社 | Method of purifying tetrafluoromethane and utilization thereof |
| CN101541673A (en) * | 2006-05-31 | 2009-09-23 | 纳幕尔杜邦公司 | Process for purifying perfluorinated products |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103664502A (en) * | 2012-09-07 | 2014-03-26 | 佛山市华特气体有限公司 | Octafluoropropane purifying method |
| CN103664502B (en) * | 2012-09-07 | 2015-09-23 | 佛山市华特气体有限公司 | A kind of octafluoropropane purification process |
| CN103951543A (en) * | 2014-04-18 | 2014-07-30 | 佛山市华特气体有限公司 | Device and method for purifying trifluoromethane |
| CN103951543B (en) * | 2014-04-18 | 2016-04-20 | 广东华特气体股份有限公司 | A kind of trifluoromethane purification devices and purification process |
| CN108529589A (en) * | 2018-06-21 | 2018-09-14 | 山东重山光电材料股份有限公司 | A kind of method of industrialized production fluorinated carbon material |
| CN108529589B (en) * | 2018-06-21 | 2024-04-26 | 山东重山光电材料股份有限公司 | Industrial production method of fluorocarbon material |
| CN111099957A (en) * | 2019-12-26 | 2020-05-05 | 福建德尔科技有限公司 | Purification system and method for electronic-grade carbon tetrafluoride |
| CN111099957B (en) * | 2019-12-26 | 2021-04-13 | 福建德尔科技有限公司 | Purification system and method for electronic-grade carbon tetrafluoride |
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Application publication date: 20120404 |