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Ternary-cycle type no-waste-free preparing method for phenoxyacetic acid

A technology of phenoxyacetic acid and sodium phenoxyacetic acid, which is applied in the chemical industry, can solve the problems of waste water pollution and low yield, achieve high conversion rate and improve efficiency

Inactive Publication Date: 2014-11-19
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the problems of low yield and large amount of waste water polluting the environment in the existing production process of phenoxyacetic acid, the present invention improves in three aspects, one is to use a catalyst to improve the efficiency of the reaction; the other is to use the condensation mother liquor The high conversion rate of phenol is realized by the circulation and phenol washing solvent circulation; the third is to use the condensation mother liquor water circulation, hydrochloric acid gas acidification + acidification mother liquor circulation to solve the waste water problem in production

Method used

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  • Ternary-cycle type no-waste-free preparing method for phenoxyacetic acid
  • Ternary-cycle type no-waste-free preparing method for phenoxyacetic acid
  • Ternary-cycle type no-waste-free preparing method for phenoxyacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Add 38.4mL of water and 29.76g of chloroacetic acid into a 250mL single-necked flask and stir to dissolve, then add 16.7g of sodium carbonate solid to make the solution pH=6, and obtain a sodium chloroacetate solution;

[0046] Drop into 150mL chlorobenzene in 500mL there-necked flask, drop into 33.84g phenol, dropwise add 36g mass concentration while stirring and be the sodium hydroxide solution of 40%, make solution pH=12, obtain sodium phenoxide solution;

[0047] Heat and reflux the three-necked flask, keep the solution temperature at 91±1°C, add 0.1 g of catalyst (ferrous chloride-EDTA-sodium iodide), and then add the sodium chloroacetate solution obtained from the above reaction dropwise into the flask, approximately Add for 30 minutes, reflux for 1 hour after the dropwise addition, and keep the system pH=11.5~12; after the reaction, cool the flask to 40°C, add 5mL of concentrated hydrochloric acid with a mass concentration of 30% dropwise to make the system pH=7 ...

Embodiment 2

[0051] Add 51.2g of the condensed mother liquor water and 29.76g of chloroacetic acid separated in Example 1 into a 250mL single-necked flask, stir and dissolve, add 16.7g of sodium carbonate solid to the inside to make the solution pH=6, and obtain a sodium chloroacetate solution;

[0052] Get the remaining 28.8g of the condensation mother liquor water separated in Example 1, add 14.4g of solid sodium hydroxide to obtain a sodium hydroxide solution, which is used to regenerate and wash the mother liquor in the next cycle;

[0053] In the 500mL there-necked flask, drop into the condensation mother liquor that embodiment 1 separates and obtain, drop into 28.2g phenol, stir, then add the phenol extracting liquid caustic soda in embodiment 1, make pH=12 in the system, obtain sodium phenolate solution;

[0054] Add 0.014 g of ferrous chloride, the catalyst component, and add the sodium chloroacetate solution obtained above into the three-necked flask at one time. After the addition...

Embodiment 3

[0060] Add 59.5mL of water and 29.77g of chloroacetic acid into a 250mL single-necked flask and stir to dissolve, then add 16.70g of sodium carbonate solid to make the solution pH = 6, and obtain a sodium chloroacetate solution;

[0061] Drop into 200mL toluene in 500mL there-necked flask, drop into 35.25g phenol, dropwise add 46.88g mass concentration while stirring and be the sodium hydroxide solution of 32%, make solution pH=12, obtain sodium phenoxide solution;

[0062] Heat and reflux the three-necked flask, keep the solution temperature at 94±1°C, add 0.1 g of catalyst (ferrous chloride-EDTA-sodium iodide), and dropwise add the sodium chloroacetate solution obtained from the above reaction into the flask, about For 40 minutes, reflux for 2 hours after the dropwise addition, and keep the system pH=11-11.5; after the reaction, cool the flask to 30°C, add 6mL of concentrated hydrochloric acid with a mass concentration of 36% dropwise, to make the system pH=5; Suction filtra...

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Abstract

In order to solve problems that an existing phenoxyacetic acid production process of low yield and environment pollution caused by a great deal of generated wastewater, the invention provides a ternary-cycle type no-waste-free preparing method for phenoxyacetic acid. The method is characterized by being a production process which takes ferrous chloride-EDTA (Ethylene Diamine Tetraacetic)-sodium iodide as a catalyst and adopts a ternary-cycle mode. The method comprises the following steps: in two phases of a water phase and an organic phase, condensing sodium phenate and sodium chloroacetate to generate sodium phenoxyacetate, wherein the sodium phenate is excessive, and excessive phenol is dissolved in a solvent for being cycled to realize mother liquor circulation; washing the sodium phenoxyacetate in a solvent to recycle entrained phenol to realize washing liquor circulation; producing the phenoxyacetic acid from the sodium phenoxyacetate by virtue of a four-phase reaction, cooling and crystallizing to realize acidification circulation. The method disclosed by the invention can be used for realizing effective separation of the sodium chloride and the phenoxyacetic acid, and is free of wastewater in the whole process; and moreover, the yield in the circulating process can be over 98%.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a "three-cycle" method for preparing phenoxyacetic acid without waste water. Background technique [0002] Phenoxyacetic acid is a very important chemical. It and its downstream products are widely used pesticides and pharmaceutical products. It has a long history of use. Years of use have proved that it has the characteristics of low toxicity, high efficiency and good safety. , is widely accepted. However, the production process of these chemicals is still relatively backward, and most of them are still in the state of their original production process, which has many disadvantages such as low yield, high waste discharge, and large amount of wastewater. [0003] The synthetic method of phenoxyacetic acid mainly adopts the Williamson synthetic method, and various new synthetic methods have also been developed in recent years such as phase transfer catalysis etc. [Journal of Northwe...

Claims

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Application Information

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IPC IPC(8): C07C51/367C07C51/02C07C51/42C07C59/70
CPCB01J31/26B01J2531/842C07C51/02C07C51/41C07C59/70
Inventor 孙宏滨齐轩尚兴翠李媛媛
Owner NORTHEASTERN UNIV
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