CN104628550B - 一种一氯醋酸制备方法 - Google Patents
一种一氯醋酸制备方法 Download PDFInfo
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- CN104628550B CN104628550B CN201310545759.3A CN201310545759A CN104628550B CN 104628550 B CN104628550 B CN 104628550B CN 201310545759 A CN201310545759 A CN 201310545759A CN 104628550 B CN104628550 B CN 104628550B
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- Prior art keywords
- monochloroacetic acid
- acid preparation
- preparation
- monochloroacetic
- sulphuric acid
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- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000001117 sulphuric acid Substances 0.000 claims abstract description 7
- 235000011149 sulphuric acid Nutrition 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims abstract description 5
- 229960002415 trichloroethylene Drugs 0.000 claims abstract description 4
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 230000007062 hydrolysis Effects 0.000 claims 1
- 238000006460 hydrolysis reaction Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 239000000376 reactant Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 239000004615 ingredient Substances 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- LXNHXLLTXMVWPM-UHFFFAOYSA-N pyridoxine Chemical compound CC1=NC=C(CO)C(CO)=C1O LXNHXLLTXMVWPM-UHFFFAOYSA-N 0.000 description 2
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 description 2
- UCTWMZQNUQWSLP-VIFPVBQESA-N (R)-adrenaline Chemical compound CNC[C@H](O)C1=CC=C(O)C(O)=C1 UCTWMZQNUQWSLP-VIFPVBQESA-N 0.000 description 1
- 229930182837 (R)-adrenaline Natural products 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 239000004099 Chlortetracycline Substances 0.000 description 1
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229960001948 caffeine Drugs 0.000 description 1
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- CYDMQBQPVICBEU-UHFFFAOYSA-N chlorotetracycline Natural products C1=CC(Cl)=C2C(O)(C)C3CC4C(N(C)C)C(O)=C(C(N)=O)C(=O)C4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-UHFFFAOYSA-N 0.000 description 1
- CYDMQBQPVICBEU-XRNKAMNCSA-N chlortetracycline Chemical compound C1=CC(Cl)=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-XRNKAMNCSA-N 0.000 description 1
- 229960004475 chlortetracycline Drugs 0.000 description 1
- 235000019365 chlortetracycline Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229960005139 epinephrine Drugs 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 229960002449 glycine Drugs 0.000 description 1
- 235000013905 glycine and its sodium salt Nutrition 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- RADKZDMFGJYCBB-UHFFFAOYSA-N pyridoxal hydrochloride Natural products CC1=NC=C(CO)C(C=O)=C1O RADKZDMFGJYCBB-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011726 vitamin B6 Substances 0.000 description 1
- 235000019158 vitamin B6 Nutrition 0.000 description 1
- 229940011671 vitamin b6 Drugs 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明公开了一种一氯醋酸的制备方法，将浓硫酸、三烷基膦按照一定比例放入密闭的反应釜中并加热至80‑85℃，根据浓硫酸的有效成分的多少慢慢加入三氯乙烯，不断搅拌，并保持温度，直至反应停止、温度自然下降至40‑50℃，静置0.5‑2小时，过滤，结晶物即为一氯醋酸。本发明方法不但反应可控，质量稳定，而且工艺简单，成本较低。
Description
技术领域
本发明涉及一种化工原料的制备方法，具体涉及一种一氯醋酸制备方法。
背景技术
一氯醋酸也称氯乙酸，被广泛应用于制造羧甲基纤维素、合成咖啡碱，是肾上腺素、氨基醋酸、维生素B6、金霉素等的重要中间体。同时，在农药制备、染料等行业也被广泛应用。传统的氯乙酸制备多沿用冰醋酸氯化法，该法原料昂贵,
产物收率低, 产品中二氯化副产物亦较多，经济上不合算，质量上不稳定。
发明内容
本发明所要解决的技术问题是针对现有技术的不足，提供一种新的一氯醋酸制备方法。
本发明所要解决的技术问题是通过以下的技术方案来实现的。本发明是一种一氯醋酸制备方法，其特点是：将浓硫酸、三烷基膦按照一定比例放入密闭的反应釜中并加热至80-85℃，根据浓硫酸的有效成分的多少慢慢加入三氯乙烯，不断搅拌，并保持温度，直至反应停止、温度自然下降至40-50℃，静置0.5-2小时，过滤，结晶物即为一氯醋酸。
与现有技术相比，本发明方法不但反应可控，质量稳定，而且工艺简单，成本较低。
具体实施方式
以下进一步描述本发明的具体技术方案，以便于本领域的技术人员进一步地理解本发明，而不构成对其权利的限制。
实施例1，一种一氯醋酸制备方法，将95%的浓硫酸100千克、三烷基膦5千克加入到密闭的反应釜中并加热至80-85℃，然后将500千克三氯乙烯缓缓注入，保持反应温度在80-85℃之间并不断搅拌，直至反应停止，然后降低温度至40-50℃，静置1小时，过滤，结晶物即为一氯醋酸。
Claims (4)
1.一种一氯醋酸制备方法，其特征在于将三氯乙烯、硫酸、三烷基膦按照一定配方比例混合，在一定温度下进行水解反应，然后经结晶、过滤而得一氯醋酸产品。
2.根据权利要求1所述的一种一氯醋酸制备方法，其特征在于所述原料配方为90-98%浓硫酸100份、三氯乙烯500份、三烷基膦5份。
3.根据权利要求1所述的一种一氯醋酸制备方法，其特征在于所述水解是在80-85℃温度条件下进行密闭反应。
4.根据权利要求1所述的一种一氯醋酸制备方法，其特征在于所述结晶时将反应物降低温度至40-50℃，静置1小时。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310545759.3A CN104628550B (zh) | 2013-11-07 | 2013-11-07 | 一种一氯醋酸制备方法 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310545759.3A CN104628550B (zh) | 2013-11-07 | 2013-11-07 | 一种一氯醋酸制备方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104628550A CN104628550A (zh) | 2015-05-20 |
| CN104628550B true CN104628550B (zh) | 2016-10-05 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310545759.3A Active CN104628550B (zh) | 2013-11-07 | 2013-11-07 | 一种一氯醋酸制备方法 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104628550B (zh) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4172957A (en) * | 1978-03-22 | 1979-10-30 | Rhone-Poulenc Industries | Production of monochloroacetyl chloride and monochloroacetic acid by hydration of trichloroethylene |
| JPH05255176A (ja) * | 1992-03-11 | 1993-10-05 | Toagosei Chem Ind Co Ltd | モノクロロ酢酸の製造方法 |
-
2013
- 2013-11-07 CN CN201310545759.3A patent/CN104628550B/zh active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4172957A (en) * | 1978-03-22 | 1979-10-30 | Rhone-Poulenc Industries | Production of monochloroacetyl chloride and monochloroacetic acid by hydration of trichloroethylene |
| JPH05255176A (ja) * | 1992-03-11 | 1993-10-05 | Toagosei Chem Ind Co Ltd | モノクロロ酢酸の製造方法 |
Non-Patent Citations (1)
| Title |
|---|
| 氯乙酸制备工艺的研究;王远明等;《化学世界》;20031125(第11期);第594-596，588页 * |
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| Publication number | Publication date |
|---|---|
| CN104628550A (zh) | 2015-05-20 |
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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Yuyang Inventor after: Fan Yuehui Inventor before: Fan Yuehui |
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| COR | Change of bibliographic data | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20160901 Address after: 601, room two, unit 50-1, Jianshe Middle Road, Haizhou District, Jiangsu, Lianyungang, 222000 Applicant after: Wang Yuyang Address before: 222000 Jiangsu Province, Lianyungang City Lianyun District high Gong Dao Xiang Gao Gong Shimamura Xishan Group No. 1 township government Applicant before: Fan Yuehui |
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| C14 | Grant of patent or utility model | ||
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| CP02 | Change in the address of a patent holder |
Address after: 222000 room 602, unit 2, building 11, Shen Yuan, Xin'an Town, Lianyungang, Jiangsu. Patentee after: Wang Yuyang Address before: 222000 Room 601, unit two, 50-1 building middle road, Haizhou District, Lianyungang, Jiangsu. Patentee before: Wang Yuyang |
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| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 222000 Room 102, unit 1, building 12, area a, yipinyuan, No. 58, Julong North Road, Haizhou District, Lianyungang City, Jiangsu Province Patentee after: Wang Yuyang Address before: Room 602, unit 2, building 11, mingguiyuan, Shencheng, Xin'an Town, Guannan County, Lianyungang City, Jiangsu Province Patentee before: Wang Yuyang |