CN103819332A - Preparation method for trichloroacrylic acid - Google Patents
Preparation method for trichloroacrylic acid Download PDFInfo
- Publication number
- CN103819332A CN103819332A CN201410059143.XA CN201410059143A CN103819332A CN 103819332 A CN103819332 A CN 103819332A CN 201410059143 A CN201410059143 A CN 201410059143A CN 103819332 A CN103819332 A CN 103819332A
- Authority
- CN
- China
- Prior art keywords
- preparation
- acid
- hexachloropropylene
- dilute sulphuric
- temperature
- Prior art date
- 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.)
- Pending
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/16—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation
- C07C51/305—Preparation of carboxylic acids or their salts, halides or anhydrides by oxidation with sulfur or sulfur-containing compounds
Abstract
A technical solution adopted by the invention is a preparation method for trichloroacrylic acid. The preparation method takes hexachloropropylene and dilute sulphuric acid as raw materials and comprises the steps of mixing the raw materials; carrying out a heating reflux reaction with stirring; extracting with dichloroethane when a temperature is reduced to below 50 DEG C; removing dichloroethane by distillation under a normal temperature and at a temperature of 100 DEG C; and finally distilling out a product under a reduced pressure. The preparation method is simple, and is in no use of chlorine gas with high toxicity, low in raw material cost and high in product yield and purity. Determination shows that a melting point of trichloroacrylic acid is 72-74 DEG C; and gas phase and liquid phase analysis are identical with those of a standard sample.
Description
Technical field
The invention belongs to chemical industry preparation field, especially the preparation method of tri chloropropene acid.
Background technology
Less to preparing the method research of tri chloropropene acid in prior art, preparation method's complexity, and generally use chlorine as raw material, chlorine has high toxicity, and producers' health is existed to certain potential safety hazard.Therefore, develop a kind of preparation method simple, select nontoxic or to the less material of people's Health hazard as raw material, be one of this area problem demanding prompt solution.
Summary of the invention
The present invention overcomes in prior art will, using high toxicity chlorine as the deficiency of raw material of preparing tri chloropropene acid, provide a kind of preparation method of tri chloropropene acid.
The technical solution adopted in the present invention is, a kind of preparation method of tri chloropropene acid, take hexachloropropylene and dilute sulphuric acid as raw material, under stirring after mixing, carry out heating reflux reaction, then treating that temperature is reduced to is less than 50 ℃, with ethylene dichloride extraction, at 100 ℃ of normal pressures, to steam except ethylene dichloride, finally decompression steams product.
As preferably, described dilute sulphuric acid massfraction is 20%, and dilute sulphuric acid and hexachloropropylene mass ratio are 2:1.
As preferably, described heating reflux reaction condition to be reflux reflux after without hexachloropropylene to gas chromatographic analysis again 1h.
The invention has the beneficial effects as follows: preparation method of the present invention is simple, do not use highly toxic chlorine, raw materials cost is low, and product yield and purity are high.
Embodiment
Embodiment
25g hexachloropropylene, 50g20% sulfuric acid (massfraction) are added in the four-hole boiling flask of 150ml with agitator, prolong, thermometer, reflux refluxes 1 hour after without hexachloropropylene to gas chromatographic analysis again, then reduce temperature to being less than 50 ℃, add the extraction of 10g ethylene dichloride, air distillation to temperature reaches 100 ℃, and then decompression steams product, obtains 15g, content 98.7%, yield 85%.
Claims (3)
1. a preparation method for tri chloropropene acid, is characterized in that: take hexachloropropylene and dilute sulphuric acid as raw material, under stirring, carry out heating reflux reaction after mixing, then treating that temperature is reduced to is less than 50 ℃, with ethylene dichloride extraction, at 100 ℃ of normal pressures, to steam except ethylene dichloride, finally decompression steams product.
2. the preparation method of tri chloropropene acid according to claim 1, is characterized in that: described dilute sulphuric acid massfraction is 20%, and dilute sulphuric acid and hexachloropropylene mass ratio are 2:1.
3. the preparation method of tri chloropropene acid according to claim 1, is characterized in that: described heating reflux reaction condition to be reflux reflux after without hexachloropropylene to gas chromatographic analysis again 1h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410059143.XA CN103819332A (en) | 2014-02-20 | 2014-02-20 | Preparation method for trichloroacrylic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410059143.XA CN103819332A (en) | 2014-02-20 | 2014-02-20 | Preparation method for trichloroacrylic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103819332A true CN103819332A (en) | 2014-05-28 |
Family
ID=50754669
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410059143.XA Pending CN103819332A (en) | 2014-02-20 | 2014-02-20 | Preparation method for trichloroacrylic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103819332A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032199A (en) * | 1987-09-23 | 1989-04-05 | 赫彻斯特股份公司 | The preparation method of fluorate acrylic acid and derivative thereof |
| CN1972890A (en) * | 2004-06-25 | 2007-05-30 | 和光纯药工业株式会社 | Method for deuterating haloacrylic acid or its salt |
-
2014
- 2014-02-20 CN CN201410059143.XA patent/CN103819332A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032199A (en) * | 1987-09-23 | 1989-04-05 | 赫彻斯特股份公司 | The preparation method of fluorate acrylic acid and derivative thereof |
| CN1972890A (en) * | 2004-06-25 | 2007-05-30 | 和光纯药工业株式会社 | Method for deuterating haloacrylic acid or its salt |
Non-Patent Citations (2)
| Title |
|---|
| 杨挺: "氯乙酸合成方法探讨", 《贵阳金筑大学学报》, no. 03, 31 December 2000 (2000-12-31), pages 98 - 100 * |
| 韩佳骏等: "三氯乙烯水解法制备一氯乙酸的研究", 《太化科技》, no. 1, 31 December 1995 (1995-12-31), pages 13 - 15 * |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140528 |