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Synthesis of 2,4-D

A synthetic method, etherification technology, applied in 2 fields, can solve the problems of heavy pollution, unfavorable clean production, waste of water resources, etc., and achieve the effect of high conversion rate, less pollution and high yield

Inactive Publication Date: 2007-11-07
蒋亦清
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the prior art, the synthesis methods of 2,4-D include chlorination after phenol etherification, etherification after chlorination of phenol, etherification oxidation chlorination of phenol ethylene oxide, 2,4-dichloro Methods such as phenol etherification oxidation method, the above methods all produce a large amount of phenol-containing wastewater in the synthesis process, which is not conducive to clean production; moreover, the water washing method is used in the purification of the product, which not only wastes water resources, but also causes great pollution

Method used

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  • Synthesis of 2,4-D

Examples

Experimental program
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Embodiment 1

[0021] Drop into 500g saturated brine in the 1000ml four-port flask with agitation and reflux condenser (the second batch starts to use synthetic mother water) and drops into 94g of phenol (99.5% in content), 96g of chloroacetic acid (98%) is warming up to 70°C, and divides Add 85g (96%) of flaky sodium hydroxide in batches. After the addition, heat up to reflux and keep for 3-8 hours. 30g of water will be released in the later stage of heat preservation. (The water generated by the reaction) may not be dehydrated. After the reaction is over, cool to 60°C , pass in hydrogen chloride gas, adjust the system to PH = 1~2, then add 300ml of dichloroethane, static layering, keep the temperature at 30 ° C ~ 70 ° C, the lower layer is salt water, the middle layer is saturated brine, put down the salt layer, and drain Obtain the by-product sodium chloride product, the filtrate and the water layer are combined to separate the saturated brine, collect (for the next batch of applications),...

Embodiment 2

[0023] Use the mother water of Example 1 to apply mechanically, weigh 500g of the mother water and process it according to the method of Example 1 to obtain 210g of the product with a content of 98% and a yield of 93%. The reaction mother water is applied again to obtain 216g of the product with a content of 98% and a yield of 95.8%. Recycling Sodium chloride 115g.

Embodiment 3

[0025] The synthesis method is the same as Example 2. After etherification, it is acidified with hydrogen chloride or sulfuric acid, cooled to 50-85 °C, filtered, the solid is etherified, washed with a small amount of hot water to remove phenol and chloroacetic acid, and the washing water is combined into brine for the next batch. , the washed solid was dissolved in ethylene dichloride, fed with chlorine gas for reaction, and processed according to the method of Example 1 to obtain 215 g of the product, with a content of 98% and a yield of 95%.

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Abstract

The present invention relates to synthesis of 2, 4-D including the first etherification and the subsequent chlorization of phenol or the first chlorization and the subsequent etherification of phenol, and features that the etherification reaction is completed in saturated salt solution. The present invention utilizes saturated salt solution obtained through reaction and eliminating crystallized salt to replace water, and performs chlorization and separation by means of the solubility of the product in chlorinated alkane, so as to solve the problem of treating phenol containing waste water. The present invention has cyclic utilization of material, high conversion rate, high yield, less pollution, high product quality and other technological advantages.

Description

technical field [0001] The invention relates to a synthesis method of 2,4-D. Background technique [0002] 2,4-D, alias 2,4-dichlorophenoxyacetic acid, molecular formula Cl 2 C 6 h 3 OCH 2 COOH, is a white to sodium-coloured, crystalline powder substance. 2,4-D is mainly used as herbicide and plant growth agent in agriculture, and it is usually processed into sodium salt, ammonium salt or ester liquid, powder, emulsion, ointment and so on. [0003] In the prior art, the synthesis methods of 2,4-D include chlorination after phenol etherification, etherification after chlorination of phenol, etherification oxidation chlorination of phenol ethylene oxide, 2,4-dichloro Methods such as phenol etherification and oxidation method, the above-mentioned methods all produce a large amount of phenol-containing wastewater in the synthesis process, which is not conducive to clean production; and the water washing method is used in the purification of the product, which not only waste...

Claims

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Application Information

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IPC IPC(8): C07C59/135C07C59/13C07C51/00
Inventor 蒋亦清
Owner 蒋亦清
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