CN102417436A - Method for preparing high-purity trifluoromethane by adopting low-temperature batch rectification process - Google Patents
Method for preparing high-purity trifluoromethane by adopting low-temperature batch rectification process Download PDFInfo
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- CN102417436A CN102417436A CN2011104234194A CN201110423419A CN102417436A CN 102417436 A CN102417436 A CN 102417436A CN 2011104234194 A CN2011104234194 A CN 2011104234194A CN 201110423419 A CN201110423419 A CN 201110423419A CN 102417436 A CN102417436 A CN 102417436A
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- Prior art keywords
- trifluoromethane
- purity
- chcl
- temperature
- adsorber
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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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- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000002808 molecular sieve Substances 0.000 claims abstract description 10
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims description 14
- 238000005194 fractionation Methods 0.000 claims description 9
- BAPZCSMFCUVUHW-UHFFFAOYSA-N dichloro(fluoro)methane Chemical compound F[C](Cl)Cl BAPZCSMFCUVUHW-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N CHCl3 Substances ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 abstract 3
- 239000000047 product Substances 0.000 description 5
- 238000007323 disproportionation reaction Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000002594 sorbent Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 125000004773 chlorofluoromethyl group Chemical group [H]C(F)(Cl)* 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- VOPWNXZWBYDODV-UHFFFAOYSA-N Chlorodifluoromethane Chemical compound FC(F)Cl VOPWNXZWBYDODV-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229920004449 Halon® Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- BCDGQXUMWHRQCB-UHFFFAOYSA-N glycine methyl ketone Natural products CC(=O)CN BCDGQXUMWHRQCB-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002620 method output Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance 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 trifluoromethane by adopting a low-temperature batch rectification process. The raw material trifluoromethane enters a molecular sieve adsorber at a certain flow rate under the condition of a certain temperature and pressure. In adsorbing CHCl3And CCl2F2Then introducing into a low-temperature rectifying still, performing batch rectification at-155 deg.C to-84 deg.C to remove CHCl3、O2、N2And the like, thereby obtaining high-purity CHF3 with the purity of more than 99.99 percent. The process is reasonable, the preparation is simple, and the method is the simplest and most convenient and ideal technology for preparing the high-purity trifluoromethane.
Description
Technical field
The invention belongs to the organic intermediate preparing technical field, relate to the preparation method of high-purity trifluoromethane, say so more specifically and adopt the method for the high-purity trifluoromethane of low temperature batch fractionating prepared.
Background technology
Trifluoromethane is claimed fluoroform again, is a kind of colourless, little flavor, and nonconducting gas is the ideal Halon substitute.
Mainly contain two big purposes, the one, be used for the etching of computingmachine silicon chip, the one, as fire-fighting medium.As the abundantest so far hydrogen fluorine carbide; The mean lifetime that trifluoromethane exists in atmosphere is about 260 years; Its caloric receptivity is equivalent to 11700 times of carbonic acid gas; Original technology is to adopt electrolytic process, electrolysis acetic acid, acetone or methylamine electrolysis production trifluoromethane in anhydrous hydrofluoric acid, and energy consumption is too high.
Summary of the invention
Problem to be solved by this invention is, overcomes the shortcoming of the trifluoromethane of can not purifying of prior art, and a kind of method that adopts the high-purity trifluoromethane of low temperature batch fractionating prepared is provided.
Preparing method of the present invention is following:
A kind of method that adopts the high-purity trifluoromethane of low temperature batch fractionating prepared is characterized in that:
(1) under the working method of closed loop, the raw material trifluoromethane under-155 ℃ to-84 ℃ temperature and 0.3-0.5MPA pressure condition, is got into molecular sieve adsorber with the 50ml/min flow and removes CHCl
3And CCl2F
2
(2) introduce in the low temperature fractionation still, carry out batch fractionating, remove CHCl at-155 ℃ to-84 ℃
3, O
2, N
2Impurity obtains high-purity freonll-11 CHF more than 99.99%
3
The preparation method who is more preferably is:
(1) the raw material trifluoromethane gets into molecular sieve adsorber with the 50ml/min flow and removes CHCl under-155 ℃ to-84 ℃ temperature and 0.3-0.5MPA pressure condition
3And CCl2F
2
(2) introduce in the low temperature fractionation still, carry out batch fractionating, remove CHCl at-100 ℃ to-84 ℃
3, O
2, N
2Impurity obtains high-purity freonll-11 CHF more than 99.99%
3
The present invention adopts low temperature batch fractionating technology, through the working method of closed loop, prepares high-purity trifluoromethane.The raw material trifluoromethane gets in the molecular sieve adsorber with certain flow under certain temperature and pressure condition.At absorption CHCl
3And CCl
2F
2After, introduce in the low temperature fractionation still, between-155 ℃ to-84 ℃, carry out batch fractionating, remove CHCl
3, O
2, N
2Deng impurity, thereby obtain high-purity CHF more than 99.99%
3, be collected in the aluminum alloy container with the liquid nitrogen deep method.
Raw material trifluoromethane gas (50ml/min) gets into (1) through pipeline, and dress 3A molecular sieve adsorbs CHCl in (2) adsorber, adsorber
3And CCl
2F
2, the absorption back gets into (3) low-temperature fractionating tower, removes CHCl through after the rectifying
3, O
2, N
2Impurity; Rectifying tower (3) leans on condensing surface (6) that the phegma cold is provided; Lean on cryogenic heat exchanger (7) to come heat exchange, the cold of cryogenic heat exchanger leans on compressor (10), vacuum pump (9); Ethene surge tank (8) provides cold, and high-purity trifluoromethane product gets into product surge tank (4) back entering diaphragm type compressor (5) and fills.Wherein trifluoromethane fills and refers to: be collected in the aluminum alloy container with the liquid nitrogen deep method.
The present invention adopts the high-purity trifluoromethane of low temperature batch fractionating prepared compared with prior art, has the following advantages:
(1) this method earning rate is high, and method is simple, and non-pollutant discharge belongs to a loop production.
(2) present method will be strict controlled in rectifying between-155 ℃ to-84 ℃, just can obtain high-purity trifluoromethane.
(3) raw material is simple and easy to, and reacting balance is reliable, is fit to heavy industrialization.
Description of drawings
Fig. 1 produces the technical process of high-purity trifluoromethane 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:
Below in conjunction with embodiment the present invention is described; 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
Adopt Freon 22 catalytic disproportionation reaction process to prepare the method for trifluoromethane:
(1) the raw material trifluoromethane gets into molecular sieve adsorber with the 50ml/min flow and removes CHCl under-84 ℃ of temperature and 0.3MPA pressure condition
3And CCl2F
2
(2) introduce in the low temperature fractionation still, carry out batch fractionating, remove CHCl at-155 ℃ to-84 ℃
3, O
2, N
2Impurity obtains high-purity freonll-11 CHF more than 99.99%
3
Embodiment 2
(1) the raw material trifluoromethane gets into molecular sieve adsorber with the 50ml/min flow and removes CHCl under-100 ℃ of temperature and 0.5MPA pressure condition
3And CCl2F
2
(2) introduce in the low temperature fractionation still, carry out batch fractionating, remove CHCl at-100 ℃ to-84 ℃
3, O
2, N
2Impurity obtains high-purity freonll-11 CHF more than 99.99%
3
Embodiment 3
(1) the raw material trifluoromethane gets into molecular sieve adsorber with the 50ml/min flow and removes CHCl under-120 ℃ of temperature 0.4MPA pressure conditions
3And CCl2F
2
(2) introduce in the low temperature fractionation still, carry out batch fractionating, remove CHCl at-100 ℃ to-110 ℃
3, O
2, N
2Impurity obtains high-purity freonll-11 CHF more than 99.99%
3
(1) CHClF
2Under certain temperature (120 ℃) and pressure (0.5MPA) condition, get in the one-level disproportionation reactor with certain flow (flow is 50ml/min).Its reaction product is removed CHCl through first-stage condenser
3After, unreacted CHClF
2Getting into second stage disproportionation reactor further reacts;
(2) product that comes out from the secondary disproportionation reactor is removed CHCl through secondary condenser
3And CCl2F
2After, introduce in the low temperature fractionation still, carry out batch fractionating at-100 ℃ to-84 ℃, remove CHCl
3, O
2, N
2Impurity obtains high-purity CHF more than 99.99%
3
Embodiment 4
(1) the raw material trifluoromethane gets into molecular sieve adsorber with the 50ml/min flow and removes CHCl under-125 ℃ to-135 ℃ temperature and 0.35MPA pressure condition
3And CCl2F
2
(2) introduce in the low temperature fractionation still, carry out batch fractionating, remove CHCl at-100 ℃ to-84 ℃
3, O
2, N
2Impurity obtains high-purity freonll-11 CHF more than 99.99%
3
Embodiment 4
With reference to accompanying drawing 1, raw material trifluoromethane gas (50ml/min) gets into (1) through pipeline, and dress 3A molecular sieve adsorbs CHCl in (2) adsorber, adsorber
3And CCl
2F
2, the absorption back gets into (3) low-temperature fractionating tower, removes CHCl through after the rectifying
3, O
2, N
2Deng impurity; Rectifying tower (3) leans on condensing surface (6) that the phegma cold is provided; Lean on cryogenic heat exchanger (7) to come heat exchange, the cold of cryogenic heat exchanger leans on compressor (10), vacuum pump (9); Ethene surge tank (8) provides cold, and high-purity trifluoromethane product gets into product surge tank (4) back entering diaphragm type compressor (5) and fills.Yield 80% to 90% can be purified to 99.999% trifluoromethane gas.
Embodiment 5
Comparison test:
High-purity trifluoromethane of ordinary method preparation: the method in usefulness is that absorption method is produced high-purity trifluoromethane now; This method is trifluoromethane to be introduced have in the equipment of sorbent material; Utilize the selective adsorption of sorbent material to trifluoromethane, vacuumize remove other impurity after, heating discharges trifluoromethanes to 200 degree sorbent materials and reclaims; This method output capacity is low excessively, and cost is high.
Method of the present invention
The first step: the raw material trifluoromethane is introduced in the adsorber, interior dress 3A and the 4A molecular sieve property selected absorption muriate and other impurity, two above an adsorption devices are used alternatingly;
Second step: introduce in the rectifying still through the gas of absorption, adopt cryogenic rectification method, intermittently under the 45ml/min situation, pressure 0.35MPA, temperature is purified under-130 ℃ of situation, can obtain high-purity 99.995% trifluoromethane;
The 3rd step: final product gets into compressor and fills steel cylinder through behind the surge tank.
The trifluoromethane quality examination situation of the present invention's preparation:
| Project | Technical indicator |
| Purity | 99.995% |
| Moisture content | ≤0.1 |
| Acidity | ≤ 0.1 |
| Evaporation residue | 0.001% |
| Suspended substance or throw out | Invisible |
| Muriate | Qualified |
| Non-condensable gases in the gas phase | ---。 |
Claims (3)
1. method that adopts the high-purity trifluoromethane of low temperature batch fractionating prepared is characterized in that:
(1) under the working method of closed loop, the raw material trifluoromethane under-155 ℃ to-84 ℃ temperature and 0.3-0.5MPA pressure condition, is got into molecular sieve adsorber with the 50ml/min flow and removes CHCl
3And CCl2F
2
(2) introduce in the low temperature fractionation still, carry out batch fractionating, remove CHCl at-155 ℃ to-84 ℃
3, O
2, N
2Impurity obtains high-purity freonll-11 CHF more than 99.99%
3
2. the preparation method of the said high-purity trifluoromethane of claim 1 is characterized in that:
Raw material trifluoromethane gas (50ml/min) gets into (1) through pipeline, and dress 3A molecular sieve adsorbs CHCl in (2) adsorber, adsorber
3And CCl
2F
2, the absorption back gets into (3) low-temperature fractionating tower, removes CHCl through after the rectifying
3, O
2, N
2Impurity; Rectifying tower (3) leans on condensing surface (6) that the phegma cold is provided; Lean on cryogenic heat exchanger (7) to come heat exchange, the cold of cryogenic heat exchanger leans on compressor (10), vacuum pump (9); Ethene surge tank (8) provides cold, and high-purity trifluoromethane product gets into product surge tank (4) back entering diaphragm type compressor (5) and fills.
3. the preparation method of the said high-purity trifluoromethane of claim 2, wherein trifluoromethane fills and refers to: be collected in the aluminum alloy container with the liquid nitrogen deep method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104234194A CN102417436A (en) | 2011-12-16 | 2011-12-16 | Method for preparing high-purity trifluoromethane by adopting low-temperature batch rectification process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104234194A CN102417436A (en) | 2011-12-16 | 2011-12-16 | Method for preparing high-purity trifluoromethane by adopting low-temperature batch rectification process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102417436A true CN102417436A (en) | 2012-04-18 |
Family
ID=45942107
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104234194A Pending CN102417436A (en) | 2011-12-16 | 2011-12-16 | Method for preparing high-purity trifluoromethane by adopting low-temperature batch rectification process |
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| Country | Link |
|---|---|
| CN (1) | CN102417436A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103721357A (en) * | 2012-10-11 | 2014-04-16 | 中国石油化工集团公司 | Method for reducing fire hazard danger of device |
| 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 |
| CN112694387A (en) * | 2020-12-30 | 2021-04-23 | 广东华特气体股份有限公司 | Difluoromethane purification method |
| CN112920012A (en) * | 2021-01-29 | 2021-06-08 | 福建德尔科技有限公司 | Novel preparation method of electronic grade CHF3 |
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|---|---|---|---|---|
| EP0727629A2 (en) * | 1995-02-16 | 1996-08-21 | Praxair Technology, Inc. | Cryogenic rectification system for fluorine compound recovery |
| CN100999437A (en) * | 2006-12-22 | 2007-07-18 | 山东东岳化工有限公司 | Recovery method of trifluoromethane |
| CN101863734A (en) * | 2010-06-22 | 2010-10-20 | 石平湘 | Method for purifying carbon tetrafluoride |
-
2011
- 2011-12-16 CN CN2011104234194A patent/CN102417436A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0727629A2 (en) * | 1995-02-16 | 1996-08-21 | Praxair Technology, Inc. | Cryogenic rectification system for fluorine compound recovery |
| CN100999437A (en) * | 2006-12-22 | 2007-07-18 | 山东东岳化工有限公司 | Recovery method of trifluoromethane |
| CN101863734A (en) * | 2010-06-22 | 2010-10-20 | 石平湘 | Method for purifying carbon tetrafluoride |
Non-Patent Citations (3)
| Title |
|---|
| 《低温与特气》 19961231 孙福楠等 吸附-低温精馏法生产高纯四氟化碳的探讨 第37-39页 , 第4期 * |
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| 彭立培等: "三氟化氮纯化方法综述", 《全国特种气体第十二次年会 》, 31 December 2008 (2008-12-31), pages 52 - 57 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103721357A (en) * | 2012-10-11 | 2014-04-16 | 中国石油化工集团公司 | Method for reducing fire hazard danger of device |
| 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 |
| CN112694387A (en) * | 2020-12-30 | 2021-04-23 | 广东华特气体股份有限公司 | Difluoromethane purification method |
| CN112920012A (en) * | 2021-01-29 | 2021-06-08 | 福建德尔科技有限公司 | Novel preparation method of electronic grade CHF3 |
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Application publication date: 20120418 |