CN103896717A - Purification method for trifluoromethane - Google Patents
Purification method for trifluoromethane Download PDFInfo
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- CN103896717A CN103896717A CN201210578821.4A CN201210578821A CN103896717A CN 103896717 A CN103896717 A CN 103896717A CN 201210578821 A CN201210578821 A CN 201210578821A CN 103896717 A CN103896717 A CN 103896717A
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Abstract
The invention provides a purification method for high-purity trifluoromethane. The method comprises the following steps: carrying out condensation and separation on a reaction product by using latent heat of a reaction raw material HCFC-22 and then carrying out two-stage rectification so as to obtain HFC-23 with content of more than 99.99%. The method provided by the invention enables the prepared product to have high purity and has the advantages of low energy consumption and smooth, steady and safe generation technology.
Description
Technical field
The present invention designs the method for purification of a kind of HFC, especially relates to the method for purification of a kind of high-purity HFC.
Background technology
Trifluoromethane, claims again fluoroform, is a kind of colourless, micro-taste, and non-conductive gas, is desirable Halon substitute.Mainly contain two large purposes, the one, in semiconductor industry, be used in the plasma etching (plasma etching) of silicon-dioxide and silicon nitride.The 2nd, use as refrigeration agent or fire-fighting medium.
In common process, adopt difluorochloromethane and anhydrous hydrofluoric acid to prepare in the technique of trifluoromethane at 200 ℃～350 ℃, reacting rear material gas temperature is higher, can increase difficulty to the subsequent disposal of by-product hydrochloric acid, so need to lower the temperature to it by heat exchange, conventional cool-down method has graphite heat exchanger or falling film absorption etc., these cool-down methods not only need a large amount of refrigerants to carry out heat exchange, and cooling-down effect is not good.
Ordinary method, after rectification and purification, obtains trifluoromethane content 99.9%, and the content of difluorochloromethane reaches 50ppm.Remain at present in certain difficulty for preparing high-purity trifluoromethane of content more than 99.99%.
Summary of the invention
For prior art deficiency, the invention provides a kind of method of purification of high-purity trifluoromethane, first utilize the latent heat of reaction raw materials HCFC-22 to carry out condensation separation to reaction product, then obtain more than 99.99% HFC-23 of content through two stage rectification.
For reaching goal of the invention the technical solution used in the present invention be:
A method of purification for trifluoromethane, comprises the following steps:
(1) in reactor (1), add the feed stream (9) containing HCFC-22 and anhydrous hydrogen fluoride, under fluorination catalyst effect, HCFC-22 and anhydrous hydrogen fluoride gas-phase reaction generate HFC-23, form reacting product stream (10);
(2) reacting product stream (10) is after condensing works (2) condensation, and the logistics (11) containing HFC-23, HCl, HCFC-22 and HF is formed on top, and the logistics (12) containing chloroform and a small amount of HF is formed on bottom;
(3) after logistics (11) is dry by water wash column (3) washing, soda-wash tower (4) alkali cleaning and moisture eliminator (5) successively, obtain the logistics (15) containing HFC-23 and a small amount of HCFC-22 and chloroform;
(4) logistics (15) is added to No. 1 rectifying tower (6) rectifying, rectification temperature is-5～40 ℃, rectifying pressure is 1.0～3.0MPa, tower top place forms the logistics (16) containing HFC-23 and a small amount of HCFC-22 and chloroform, tower reactor place forms the logistics (17) containing HCFC-22 and chloroform, and logistics (17) intermittent cycle is to reactor (1);
(5) logistics (16) is added to No. 2 rectifying tower (7) rectifying, rectification temperature is-5～30 ℃, rectifying pressure is 1.0～3.0MPa, tower top place obtains HFC-23 logistics (18), after drying device (8) is dry, obtain finished product HFC-23(20), tower reactor place forms the logistics (19) containing HCFC-22 and a small amount of chloroform, and intermittent cycle is to reactor (1).
Generate the HFC-23 stage at above-mentioned HCFC-22 and anhydrous hydrogen fluoride reaction, after raw material HCFC-22 and anhydrous hydrogen fluoride vaporization mix, entering reactor (1) reacts, temperature of reaction is preferably 200～350 ℃, reaction pressure is preferably 5～15KPa, obtains content and reach 85%-95%, the temperature crude product HFC-23 80-120 ℃ of left and right after reaction.Gas phase fluorination catalyzer is preferably AlF
3.
After fluoridation finishes, reacting product stream (10) passes into condensing works (2), i.e. HCFC-22 interchanger, carries out condensation separation, carries out heat exchange by the latent heat of vaporization of HCFC-22 material, reaches vaporization raw material HCFC-22 and the object to crude product HFC-23 cooling.Crude product HFC-23 temperature after heat exchange can be reduced to 5～25 ℃, and in temperature-fall period, constantly has condenses to separate out, and the liquid of separating out is mainly containing the logistics (12) of chloroform and a small amount of HF, and flow is 0.2～0.8Kg/h.
The logistics (11) obtaining after condensation separation obtains the logistics (15) containing HCFC-23 and a small amount of HCFC-22 and chloroform after being dried by water wash column (3) washing, soda-wash tower (4) alkali cleaning and moisture eliminator (5) successively.The object that scale is washed is to reclaim the high boiling material such as chloroform, unnecessary HF and by-product HCl, in the logistics obtaining after scale is washed and is dried (15), and HFC-23 content approximately 93～98%.Moisture eliminator (5) is preferably sulphuric acid desiccator, and the moisture content of dry rear logistics (15) is 50～300PPM.
After scale is washed, is dried, logistics (15) enters two stage rectification process.The opening for feed of No. 1 rectifying tower (6) and No. 2 rectifying tower (7) is all positioned at tower body under rectifying tower.The rectification temperature of No. 1 rectifying tower (6) is-5～40 ℃, be preferably 0～30 ℃, rectifying pressure is 1.0～3.0MPa, be preferably 1.5～2.5MPa, tower top place forms the logistics (16) containing HFC-23 and a small amount of HCFC-22 and chloroform, tower reactor place forms the logistics (17) containing HCFC-22 and chloroform, and logistics (17) continues to participate in reaction according to growing amount intermittent cycle to reactor (1).After No. 1 rectifying tower (6) separates, in logistics (16), the content of HFC-23 reaches more than 99.9%.The rectification temperature of No. 2 rectifying tower (7) is-5～30 ℃, be preferably 0～25 ℃, rectifying pressure is 1.0～3.0MPa, be preferably 1.5～2.5MPa, tower top place obtains HFC-23 logistics (18), tower reactor place forms the logistics (19) containing HCFC-22 and a small amount of chloroform, and logistics (19) continues to participate in reaction according to growing amount intermittent cycle to reactor (1).After No. 2 rectifying tower (7) separate, in HFC-23 logistics (18), the content of HFC-23 reaches more than 99.99%.
Logistics (18) is finally by the dry moisture of removing of super-dry device (8), the high-purity HFC-23 product that obtain exceeding 99.99%, impurity HCFC-22 content is less than 10ppm, water content is less than 10ppm.Moisture eliminator (8) is preferably 4A mole sieve drier.
Method of purification provided by the invention compared with prior art, has the following advantages:
(1) adopt the latent heat of vaporization of raw material HCFC-22 as the refrigerant of HFC-23 crude product, do like this high boiling material such as roughing out trichloromethane of can lowering the temperature to HFC-23 on the one hand, reduce the workload of follow-up rectifying; Can also remove on the other hand organism and F in by-product hydrochloric acid
-, improved the quality of hydrochloric acid; Can also reach the object of the vaporization to raw material HCFC-22, reduce the process that adopts conventional steam heating HCFC-22, reduce energy consumption;
(2) the rectifying mode of employing two-stage tandem, production technique is more steady, and rectification effect is better, is more conducive to prepare high-purity HFC-23;
(3) the high-purity HFC-23 product that can obtain exceeding 99.99%, impurity HCFC-22 content is less than 10ppm, water content is less than 10ppm.
Accompanying drawing explanation
Fig. 1 is process flow sheet, wherein:
Equipment:
1, reactor, 2, condensing works, 3, water wash column, 4, soda-wash tower, 5, moisture eliminator, 6, No. 1 rectifying tower, 7, No. 2 rectifying tower, 8, moisture eliminator.
Logistics:
9, containing the feed stream of HCFC-22 and anhydrous hydrogen fluoride, 10, reacting product stream, 11, containing HFC-23, HCl, the logistics of HCFC-22 and HF, 12, containing the logistics of chloroform and a small amount of HF, 13, containing HCFC-23 and a small amount of HCl, HF, HCFC-22, the logistics of chloroform, 14, containing the logistics of HCFC-23 and a small amount of HCFC-22 and chloroform, 15, containing the logistics of HCFC-23 and a small amount of HCFC-22 and chloroform, 16, containing the logistics of HFC-23 and a small amount of HCFC-22 and chloroform, 17, containing the logistics of HCFC-22 and chloroform, 18, be essentially the logistics of HFC-23, 19, containing the logistics of HCFC-22 and a small amount of chloroform, 20, HFC-23 logistics.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described, but does not limit the invention to these embodiments.One skilled in the art would recognize that the present invention contained all alternativess, improvement project and the equivalents that within the scope of claims, may comprise.
Embodiment 1
Raw material HCFC-22 and HF pass into reactor (1) reaction with the speed of 140Kg/h and the speed of 35Kg/h respectively, temperature of reaction is 200 ℃, pressure is 5Kpa, form reacting product stream (10), reacting product stream (10) after interchanger condensation, obtain temperature be 5 ℃ containing the logistics (11) of HFC-23, HCl, HCFC-22 and HF.Logistics (11), through water wash column (3) washing, reclaims 0.8Kg/h high boiling material, and wherein approximately 90% is chloroform.Again through alkali cleaning and dry after obtain the logistics (15) containing HFC-23 and a small amount of HCFC-22 and chloroform, wherein to account for the quality percentage composition of logistics (15) be approximately 93% to HFC-23.Rectifying is carried out in logistics (15) tower body charging from No. 1 rectifying tower (6), control rectification temperature 15 ℃ of left and right, pressure is in 2.4MPa left and right, and tower top place forms the logistics (16) containing HFC-23 and a small amount of HCFC-22 and chloroform, and tower reactor place forms the logistics (17) containing HCFC-22 and chloroform.Logistics (17) continues to participate in reaction according to the step reactor (1) that is circulated to of turnout.Logistics (16) continues tower body charging from No. 2 rectifying tower (7) and carries out rectifying, controls rectification temperature 10 ℃ of left and right, and pressure is in 2.2MPa left and right, and tower top place obtains HFC-23 logistics (18), and tower reactor place forms the logistics (19) containing HCFC-22 and a small amount of chloroform.Logistics (19) continues to participate in reaction according to the step reactor (1) that is circulated to of turnout.Logistics (18) closes in groove by 4A mole sieve drier (8) absorption, and obtaining content is more than 99.99% HFC-23 high purity product, and HCFC-22 content is lower than 8ppm, and water content is lower than 6ppm.
Embodiment 2
Raw material HCFC-22 and HF pass into reactor (1) reaction with the speed of 150Kg/h and the speed of 40Kg/h respectively, temperature of reaction is 260 ℃, pressure is 9Kpa, form reacting product stream (10), reacting product stream (10) after interchanger condensation, obtain temperature be 15 ℃ containing the logistics (11) of HFC-23, HCl, HCFC-22 and HF.Logistics (11), through water wash column (3) washing, reclaims 0.4Kg/h high boiling material, and wherein approximately 95% is chloroform.Again through alkali cleaning and dry after obtain the logistics (15) containing HFC-23 and a small amount of HCFC-22 and chloroform, wherein to account for the quality percentage composition of logistics (15) be approximately 96% to HFC-23.Rectifying is carried out in logistics (15) tower body charging from No. 1 rectifying tower (6), control rectification temperature 7 ℃ of left and right, pressure is in 2.2MPa left and right, and tower top place forms the logistics (16) containing HFC-23 and a small amount of HCFC-22 and chloroform, and tower reactor place forms the logistics (17) containing HCFC-22 and chloroform.Logistics (17) continues to participate in reaction according to the step reactor (1) that is circulated to of turnout.Logistics (16) continues tower body charging from No. 2 rectifying tower (7) and carries out rectifying, controls rectification temperature 5 ℃ of left and right, and pressure is in 2.0MPa left and right, and tower top place obtains HFC-23 logistics (18), and tower reactor place forms the logistics (19) containing HCFC-22 and a small amount of chloroform.Logistics (19) continues to participate in reaction according to the step reactor (1) that is circulated to of turnout.Logistics (18) closes in groove by 4A mole sieve drier (8) absorption, and obtaining content is more than 99.99% HFC-23 high purity product, and HCFC-22 content is lower than 6ppm, and water content is lower than 6ppm.
Embodiment 3
Raw material HCFC-22 and HF pass into reactor (1) reaction with the speed of 170Kg/h and the speed of 50Kg/h respectively, temperature of reaction is 350 ℃, pressure is 15Kpa, form reacting product stream (10), reacting product stream (10) after interchanger condensation, obtain temperature be 25 ℃ containing the logistics (11) of HFC-23, HCl, HCFC-22 and HF.Logistics (11), through water wash column (3) washing, reclaims 0.4Kg/h high boiling material, and wherein approximately 92% is chloroform.Again through alkali cleaning and dry after obtain the logistics (15) containing HFC-23 and a small amount of HCFC-22 and chloroform, wherein to account for the quality percentage composition of logistics (15) be approximately 98% to HFC-23.Rectifying is carried out in logistics (15) tower body charging from No. 1 rectifying tower (6), control rectification temperature 3 ℃ of left and right, pressure is in 1.9MPa left and right, and tower top place forms the logistics (16) containing HFC-23 and a small amount of HCFC-22 and chloroform, and tower reactor place forms the logistics (17) containing HCFC-22 and chloroform.Logistics (17) continues to participate in reaction according to the step reactor (1) that is circulated to of turnout.Logistics (16) continues tower body charging from No. 2 rectifying tower (7) and carries out rectifying, controls rectification temperature 0 ℃ of left and right, and pressure is in 1.6MPa left and right, and tower top place obtains HFC-23 logistics (18), and tower reactor place forms the logistics (19) containing HCFC-22 and a small amount of chloroform.Logistics (19) continues to participate in reaction according to the step reactor (1) that is circulated to of turnout.Logistics (18) closes in groove by 4A mole sieve drier (8) absorption, and obtaining content is more than 99.99% HFC-23 high purity product, and HCFC-22 content is lower than 7ppm, and water content is lower than 5ppm.
Claims (9)
1. a method of purification for trifluoromethane, is characterized in that comprising the following steps:
(1) in reactor (1), add the feed stream (9) containing HCFC-22 and anhydrous hydrogen fluoride, under fluorination catalyst effect, HCFC-22 and anhydrous hydrogen fluoride gas-phase reaction generate HFC-23, form reacting product stream (10);
(2) reacting product stream (10) is after condensing works (2) condensation, and the logistics (11) containing HFC-23, HCl, HCFC-22 and HF is formed on top, and the logistics (12) containing chloroform and a small amount of HF is formed on bottom;
(3) after logistics (11) is dry by water wash column (3) washing, soda-wash tower (4) alkali cleaning and moisture eliminator (5) successively, obtain the logistics (15) containing HFC-23 and a small amount of HCFC-22 and chloroform;
(4) logistics (15) is added to No. 1 rectifying tower (6) rectifying, rectification temperature is-5～40 ℃, rectifying pressure is 1.0～3.0MPa, tower top place forms the logistics (16) containing HFC-23 and a small amount of HCFC-22 and chloroform, tower reactor place forms the logistics (17) containing HCFC-22 and chloroform, and logistics (17) intermittent cycle is to reactor (1);
(5) logistics (16) is added to No. 2 rectifying tower (7) rectifying, rectification temperature is-5～30 ℃, rectifying pressure is 1.0～3.0MPa, tower top place obtains HFC-23 logistics (18), after drying device (8) is dry, obtain finished product HFC-23(20), tower reactor place forms the logistics (19) containing HCFC-22 and a small amount of chloroform, and intermittent cycle is to reactor (1).
2. according to the method for purification of trifluoromethane claimed in claim 1, it is characterized in that, in described step (1), temperature of reaction is 200～350 ℃, reaction pressure 5～15KPa, fluorination catalyst is AlF
3.
3. according to the method for purification of trifluoromethane claimed in claim 1, it is characterized in that utilizing the latent heat of vaporization of HCFC-22 to carry out condensation in described step (2), the temperature of the logistics (11) obtaining after condensation is 5～25 ℃.
4. according to the method for purification of trifluoromethane claimed in claim 1, it is characterized in that the moisture content of the logistics (15) forming in described step (3) is 50～300PPM.
5. according to the method for purification of trifluoromethane claimed in claim 1, it is characterized in that in described step (3), moisture eliminator (5) is sulphuric acid desiccator.
6. according to the method for purification of trifluoromethane claimed in claim 1, it is characterized in that in described step (5), moisture eliminator (8) is 4A mole sieve drier.
7. according to the method for purification of trifluoromethane claimed in claim 1, the rectification temperature that it is characterized in that No. 1 rectifying tower (6) in described step (4) is 0～30 ℃, and rectifying pressure is 1.5～2.5MPa.
8. according to the method for purification of trifluoromethane claimed in claim 1, the rectification temperature that it is characterized in that No. 2 rectifying tower (6) in described step (4) is 0～25 ℃, and rectifying pressure is 1.5～2.5MPa.
9. according to the method for purification of trifluoromethane claimed in claim 1, it is characterized in that the opening for feed of described No. 1 rectifying tower (6) and No. 2 rectifying tower (7) is positioned at tower body under rectifying tower.
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| CN201210578821.4A CN103896717B (en) | 2012-12-27 | 2012-12-27 | A kind of method of purification of trifluoromethane |
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| CN201210578821.4A CN103896717B (en) | 2012-12-27 | 2012-12-27 | A kind of method of purification of trifluoromethane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111072447A (en) * | 2018-10-19 | 2020-04-28 | 中化蓝天氟材料有限公司 | Method for reducing acidity and moisture in fluorine-containing alkane |
| CN112851465A (en) * | 2021-01-27 | 2021-05-28 | 福建德尔科技有限公司 | Preparation of electronic grade CHF using novel catalysts3Novel preparation method of |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105080A (en) * | 1985-07-01 | 1986-12-31 | 浙江省化学工业研究所 | The improvement preparation method of trifluoromethane |
| CN1263795A (en) * | 2000-03-18 | 2000-08-23 | 浙江莹光化工有限公司 | Fluorinating catalyst for preparing fluoroparaffin |
| CN1938248A (en) * | 2003-10-17 | 2007-03-28 | 霍尼韦尔国际公司 | Method of producing hydrofluorocarbons |
-
2012
- 2012-12-27 CN CN201210578821.4A patent/CN103896717B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85105080A (en) * | 1985-07-01 | 1986-12-31 | 浙江省化学工业研究所 | The improvement preparation method of trifluoromethane |
| CN1263795A (en) * | 2000-03-18 | 2000-08-23 | 浙江莹光化工有限公司 | Fluorinating catalyst for preparing fluoroparaffin |
| CN1938248A (en) * | 2003-10-17 | 2007-03-28 | 霍尼韦尔国际公司 | Method of producing hydrofluorocarbons |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111072447A (en) * | 2018-10-19 | 2020-04-28 | 中化蓝天氟材料有限公司 | Method for reducing acidity and moisture in fluorine-containing alkane |
| CN112851465A (en) * | 2021-01-27 | 2021-05-28 | 福建德尔科技有限公司 | Preparation of electronic grade CHF using novel catalysts3Novel preparation method of |
| CN112851465B (en) * | 2021-01-27 | 2023-03-10 | 福建德尔科技股份有限公司 | Preparation of electronic grade CHF using a catalyst 3 Preparation method of (1) |
| 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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Effective date of registration: 20190726 Address after: 310051 Binjiang District Jiangnan Road, Zhejiang, No. 96, No. Co-patentee after: Sinochem Blue Sky Fluorine Material Co., Ltd. Patentee after: Sinochem Lantian Co., Ltd. Address before: 310051 Binjiang District Jiangnan Road, Zhejiang, No. 96, No. Co-patentee before: ZHEJIANG CHEMICAL INSTITUTE TECHNOLOGY CO., LTD. Patentee before: Sinochem Lantian Co., Ltd. |