CN106397176A - Production method of sodium phenoxyacetate - Google Patents
Production method of sodium phenoxyacetate Download PDFInfo
- Publication number
- CN106397176A CN106397176A CN201610769629.1A CN201610769629A CN106397176A CN 106397176 A CN106397176 A CN 106397176A CN 201610769629 A CN201610769629 A CN 201610769629A CN 106397176 A CN106397176 A CN 106397176A
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- CN
- China
- Prior art keywords
- sodiumphenoxyacetate
- production method
- solution
- sodium
- chloroacetic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/367—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of functional groups containing oxygen only in singly bound form
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
An embodiment of the invention discloses a production method of sodium phenoxyacetate. The production method comprises steps as follows: (1), raw materials including 38 parts by weight of chloroacetic acid and 50 parts by weight of water are weighed, chloroacetic acid is dissolved in water, and a chloroacetic acid solution is cooled to 0 DEG C; (2), a saturated sodium carbonate solution is added to the chloroacetic acid solution during stirring at the temperature of 0 DEG C until the pH value of the solution is 7-8; (3), 26 parts by weight of phenol and 50 parts by weight of water are added to the mixed solution, a 35% sodium hydroxide solution is added until the pH value is 12, and the mixed solution is heated to 92 DEG C and subjected to a reaction for 0.5 h; (4), the mixed solution is subjected to suction filtration, solids obtained through filtration are washed and dried, and required sodium phenoxyacetate is obtained. The original production technology is improved, by the aid of a simple measure of cooling, hydrolysis of chloroacetic acid is effectively inhibited, the yield of sodium phenoxyacetate is increased, the quantity of impurities in sodium phenoxyacetate is greatly reduced, and the difficulty in purification and impurity removal of a sodium phenoxyacetate product is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of chemical products, more particularly, to a kind of production method of sodiumphenoxyacetate.
Background technology
The conversion ratio of the sodiumphenoxyacetate that the production method of existing sodiumphenoxyacetate is produced only has 70% about, mainly
The reason be the chloroacetic hydrolysis of raw material, not only reduce the conversion ratio of raw material, and in prepared sodiumphenoxyacetate join
A large amount of impurity are entered so that purification sodiumphenoxyacetate also becomes difficult.So reducing chloroacetic hydrolysis is to improve phenoxy acetic acid
Sodium yield and the important means of product quality.
Content of the invention
Embodiment of the present invention technical problem to be solved is, the conversion ratio for sodiumphenoxyacetate is not high, and produces
The situation of thing impurity angle is it is proposed that a kind of production method of sodiumphenoxyacetate.
In order to solve above-mentioned technical problem, embodiments provide a kind of production method of sodiumphenoxyacetate, this one
The production method planting sodiumphenoxyacetate includes：(1) raw material are weighed according to following weight portion：Monoxone 38, water 50；By monoxone
It is dissolved in the water, and chloroacetic acid solution is cooled to 0 DEG C；(2), under conditions of keeping chloroacetic acid solution to be 0 DEG C, stir one
While being added thereto to saturated sodium carbonate solution, the pH value to solution is 7～8；(3) weight portion is added to be 26 again in mixed liquor
Phenol and 50 water, and add 35% sodium hydroxide solution to be 12 to pH, be heated to 92 DEG C and react 0.5 hour；(4) to mixing
Liquid suction filtration, and to filtering the solid washing drying obtaining, obtain required sodiumphenoxyacetate.
Wherein, carry out gas shield using nitrogen in step (3).
Wherein, appropriate reducing agent is added to avoid phenol oxidized in step (3).
Wherein, reducing agent is sodium sulfite, and weight portion is 0.26.
Implement the embodiment of the present invention, have the advantages that：Present invention improves over original production technology, by cooling
This simple measure, effectively inhibits chloroacetic hydrolysis, not only increases the yield of sodiumphenoxyacetate, and greatly
Decrease the amount of impurity in sodiumphenoxyacetate, reduce the difficulty of the purification removal of impurities of sodiumphenoxyacetate product.
Brief description
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
Have technology description in required use accompanying drawing be briefly described it should be apparent that, drawings in the following description be only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, acceptable
Other accompanying drawings are obtained according to these accompanying drawings.
Fig. 1 is a kind of flow chart of the production method of sodiumphenoxyacetate that the present invention provides.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of not making creative work
Embodiment, broadly falls into the scope of protection of the invention.
Refer to Fig. 1, Fig. 1 is a kind of structural representation of the production method of sodiumphenoxyacetate that the present invention provides.A kind of
The production method of sodiumphenoxyacetate comprises the steps：
In step sl, raw material are weighed according to following weight portion：Monoxone 38, water 50；Monoxone is dissolved in the water,
And chloroacetic acid solution is cooled to 0 DEG C.
In step s 2, under conditions of keeping chloroacetic acid solution to be 0 DEG C, stir and be added thereto to unsaturated carbonate
Sodium solution, the pH value to solution is 7～8.
In step s3, then add the phenol that weight portion is 26 and 50 water in mixed liquor, and add 35% hydrogen-oxygen
Changing sodium solution back flow reaction to pH is 12, is heated to 92 DEG C and reacts 0.5 hour.
In step s 4, to mixed liquor suction filtration, and to filtering the solid washing drying obtaining, obtain required phenoxy acetic acid
Sodium.
According to experiment, with the reduction of solution temperature, the degree of chloroacetic hydrolysis also reduces so that sodiumphenoxyacetate
Yield improves, experimental result such as following table：
| Temperature/DEG C | 55 | 15 | 0 |
| Yield/% | 53 | 80 | 85 |
When continuing to reduce mixeding liquid temperature to during less than 0 DEG C, mixed liquor can become sticky or even solidification, affects chloroethene on the contrary
Acid and the reaction of sodium carbonate.So considering with reference to yield and production efficiency, in step sl, temperature during neutralization reaction is adopted
With 0 DEG C.
In addition it is also necessary to avoid phenol to be gone bad by the dioxygen oxidation of in the air in step S3 of production process.Generally there are two kinds
Method：The first is to adopt gas shield, typically takes nitrogen to carry out gas shield；Second is to add reducing agent to avoid phenol
Oxidized, add weight portion to be 0.26 sodium sulfite as reducing agent in mixed liquor.
Implement the embodiment of the present invention, have the advantages that：Present invention improves over original production technology, by cooling
This simple measure, effectively inhibits chloroacetic hydrolysis, not only increases the yield of sodiumphenoxyacetate, and greatly
Decrease the amount of impurity in sodiumphenoxyacetate, reduce the difficulty of the purification removal of impurities of sodiumphenoxyacetate product.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvement made etc., should be included within the scope of the present invention.
Claims (4)
1. a kind of production method of sodiumphenoxyacetate it is characterised in that a kind of production method of described sodiumphenoxyacetate include with
Lower step：
(1) raw material are weighed according to following weight portion：Monoxone 38, water 50；Monoxone is dissolved in the water, and monoxone is molten
Liquid is cooled to 0 DEG C；
(2), under conditions of keeping chloroacetic acid solution to be 0 DEG C, stir and be added thereto to saturated sodium carbonate solution, extremely molten
The pH value of liquid is 7～8；
(3) add the phenol that weight portion is 26 and 50 water again in mixed liquor, and add 35% sodium hydroxide solution to pH
For 12, it is heated to 92 DEG C and reacts 0.5 hour；
(4) to mixed liquor suction filtration, and to filtering the solid washing drying obtaining, obtain required sodiumphenoxyacetate.
2. a kind of production method of sodiumphenoxyacetate according to claim 1 is it is characterised in that use in step (3)
Nitrogen carries out gas shield.
3. a kind of production method of sodiumphenoxyacetate according to claim 1 is it is characterised in that add in step (3)
Appropriate reducing agent avoids phenol oxidized.
4. a kind of production method of sodiumphenoxyacetate according to claim 3 is it is characterised in that described reducing agent is sulfurous
Sour sodium, weight portion is 0.26.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610769629.1A CN106397176A (en) | 2016-08-30 | 2016-08-30 | Production method of sodium phenoxyacetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610769629.1A CN106397176A (en) | 2016-08-30 | 2016-08-30 | Production method of sodium phenoxyacetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106397176A true CN106397176A (en) | 2017-02-15 |
Family
ID=58002240
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610769629.1A Pending CN106397176A (en) | 2016-08-30 | 2016-08-30 | Production method of sodium phenoxyacetate |
Country Status (1)
| Country | Link |
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| CN (1) | CN106397176A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151152A (en) * | 2014-07-16 | 2014-11-19 | 东北大学 | Ternary-cycle type no-waste-free preparing method for phenoxyacetic acid |
| CN105622396A (en) * | 2014-10-27 | 2016-06-01 | 浙江新安化工集团股份有限公司 | 2,4-dichlorophenoxyacetic acid preparation method |
-
2016
- 2016-08-30 CN CN201610769629.1A patent/CN106397176A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151152A (en) * | 2014-07-16 | 2014-11-19 | 东北大学 | Ternary-cycle type no-waste-free preparing method for phenoxyacetic acid |
| CN105622396A (en) * | 2014-10-27 | 2016-06-01 | 浙江新安化工集团股份有限公司 | 2,4-dichlorophenoxyacetic acid preparation method |
Non-Patent Citations (3)
| Title |
|---|
| 刘卫聪等: "除草剂2，4-D水相后氯化合成工艺优化研究", 《山东化工》 * |
| 曾振芳等: "苯氧乙酸合成工艺研究", 《广州化工》 * |
| 邓忠明等: "苯氧乙酸钠合成工艺研究", 《湖北化工》 * |
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Application publication date: 20170215 |