CN113816845B - 三氟乙酸的制备方法 - Google Patents
三氟乙酸的制备方法 Download PDFInfo
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- CN113816845B CN113816845B CN202111197866.2A CN202111197866A CN113816845B CN 113816845 B CN113816845 B CN 113816845B CN 202111197866 A CN202111197866 A CN 202111197866A CN 113816845 B CN113816845 B CN 113816845B
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- solid
- liquid separation
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- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 238000004519 manufacturing process Methods 0.000 title description 10
- 239000007788 liquid Substances 0.000 claims abstract description 87
- 238000006243 chemical reaction Methods 0.000 claims abstract description 66
- 238000000926 separation method Methods 0.000 claims abstract description 66
- 238000001125 extrusion Methods 0.000 claims abstract description 25
- 239000012530 fluid Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 11
- -1 alkali metal trifluoroacetate Chemical class 0.000 claims abstract description 10
- 239000007791 liquid phase Substances 0.000 claims abstract description 9
- 239000007790 solid phase Substances 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 47
- 239000007789 gas Substances 0.000 claims description 35
- 239000000047 product Substances 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 18
- 230000008569 process Effects 0.000 claims description 16
- 239000012263 liquid product Substances 0.000 claims description 14
- CUNPJFGIODEJLQ-UHFFFAOYSA-M potassium;2,2,2-trifluoroacetate Chemical compound [K+].[O-]C(=O)C(F)(F)F CUNPJFGIODEJLQ-UHFFFAOYSA-M 0.000 claims description 11
- 238000004821 distillation Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 230000005484 gravity Effects 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 7
- 230000009471 action Effects 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 150000001340 alkali metals Chemical class 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 3
- UYCAUPASBSROMS-AWQJXPNKSA-M sodium;2,2,2-trifluoroacetate Chemical compound [Na+].[O-][13C](=O)[13C](F)(F)F UYCAUPASBSROMS-AWQJXPNKSA-M 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 2
- VFRSADQPWYCXDG-LEUCUCNGSA-N ethyl (2s,5s)-5-methylpyrrolidine-2-carboxylate;2,2,2-trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F.CCOC(=O)[C@@H]1CC[C@H](C)N1 VFRSADQPWYCXDG-LEUCUCNGSA-N 0.000 claims 3
- 238000013019 agitation Methods 0.000 claims 1
- 239000012467 final product Substances 0.000 claims 1
- 239000011541 reaction mixture Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 description 39
- 238000003756 stirring Methods 0.000 description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- 239000000243 solution Substances 0.000 description 15
- 238000007599 discharging Methods 0.000 description 7
- 239000012265 solid product Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000012047 saturated solution Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- JTNCEQNHURODLX-UHFFFAOYSA-N 2-phenylethanimidamide Chemical compound NC(=N)CC1=CC=CC=C1 JTNCEQNHURODLX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000009969 flowable effect Effects 0.000 description 2
- 238000003682 fluorination reaction Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910000343 potassium bisulfate Inorganic materials 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000008247 solid mixture Substances 0.000 description 2
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- DCEPGADSNJKOJK-UHFFFAOYSA-N 2,2,2-trifluoroacetyl fluoride Chemical compound FC(=O)C(F)(F)F DCEPGADSNJKOJK-UHFFFAOYSA-N 0.000 description 1
- 206010006784 Burning sensation Diseases 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 201000008197 Laryngitis Diseases 0.000 description 1
- 208000007101 Muscle Cramp Diseases 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 206010037423 Pulmonary oedema Diseases 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 208000005392 Spasm Diseases 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 206010047924 Wheezing Diseases 0.000 description 1
- WETWJCDKMRHUPV-UHFFFAOYSA-N acetyl chloride Chemical compound CC(Cl)=O WETWJCDKMRHUPV-UHFFFAOYSA-N 0.000 description 1
- 239000012346 acetyl chloride Substances 0.000 description 1
- JUCMRTZQCZRJDC-UHFFFAOYSA-N acetyl fluoride Chemical class CC(F)=O JUCMRTZQCZRJDC-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 210000000621 bronchi Anatomy 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- ABDBNWQRPYOPDF-UHFFFAOYSA-N carbonofluoridic acid Chemical compound OC(F)=O ABDBNWQRPYOPDF-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 238000003541 multi-stage reaction Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 210000001533 respiratory mucosa Anatomy 0.000 description 1
- 208000013220 shortness of breath Diseases 0.000 description 1
- 231100000075 skin burn Toxicity 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- WROMPOXWARCANT-UHFFFAOYSA-N tfa trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F.OC(=O)C(F)(F)F WROMPOXWARCANT-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 1
- QGEACRIKUUTESN-UHFFFAOYSA-K tripotassium triacetate Chemical compound [K+].[K+].[K+].CC([O-])=O.CC([O-])=O.CC([O-])=O QGEACRIKUUTESN-UHFFFAOYSA-K 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims (16)
Priority Applications (1)
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CN202111197866.2A CN113816845B (zh) | 2021-10-14 | 2021-10-14 | 三氟乙酸的制备方法 |
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CN202111197866.2A CN113816845B (zh) | 2021-10-14 | 2021-10-14 | 三氟乙酸的制备方法 |
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CN113816845A CN113816845A (zh) | 2021-12-21 |
CN113816845B true CN113816845B (zh) | 2024-04-16 |
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CN202111197866.2A Active CN113816845B (zh) | 2021-10-14 | 2021-10-14 | 三氟乙酸的制备方法 |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3894082A (en) * | 1972-01-07 | 1975-07-08 | Kali Chemie Ag | Process of making trifluoroacetic acid |
CN110872226A (zh) * | 2019-12-05 | 2020-03-10 | 常熟三爱富中昊化工新材料有限公司 | 三氟乙酸的制备工艺 |
CN216440607U (zh) * | 2021-10-14 | 2022-05-06 | 常熟三爱富中昊化工新材料有限公司 | 用于产生固液化学反应的反应系统 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB625098A (en) * | 1945-10-01 | 1949-06-22 | Walter Norman Haworth | Improvements in or relating to the production of trifluoroacetic acid |
-
2021
- 2021-10-14 CN CN202111197866.2A patent/CN113816845B/zh active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3894082A (en) * | 1972-01-07 | 1975-07-08 | Kali Chemie Ag | Process of making trifluoroacetic acid |
CN110872226A (zh) * | 2019-12-05 | 2020-03-10 | 常熟三爱富中昊化工新材料有限公司 | 三氟乙酸的制备工艺 |
CN216440607U (zh) * | 2021-10-14 | 2022-05-06 | 常熟三爱富中昊化工新材料有限公司 | 用于产生固液化学反应的反应系统 |
Non-Patent Citations (1)
Title |
---|
全氟羧酸的合成方法;窦若岸等;《有机氟工业》(第4期);第31-46页 * |
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CN113816845A (zh) | 2021-12-21 |
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TA01 | Transfer of patent application right |
Effective date of registration: 20221026 Address after: No.10 Xingyu Road, Haiyu Town, Changshu City, Suzhou City, Jiangsu Province 215522 Applicant after: CHANGSHU 3F ZHONGHAO NEW CHEMICAL MATERIALS Co.,Ltd. Applicant after: CHANGSHU 3F ZHENFU NEW MATERIALS Co.,Ltd. Applicant after: Shanghai Huayi sanaifu New Material Co.,Ltd. Address before: No.10 Xingyu Road, Haiyu Town, Changshu City, Suzhou City, Jiangsu Province 215522 Applicant before: CHANGSHU 3F ZHONGHAO NEW CHEMICAL MATERIALS Co.,Ltd. Applicant before: Changshu san'ai Fuyuan New Material Co.,Ltd. Applicant before: Shanghai Huayi sanaifu New Material Co.,Ltd. |
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