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Method for synthesizing raw material bromopropane of profenofos with profenofosby products

A technology of profenofos and by-products, which is applied in the field of profenofos by-products to synthesize bromopropane raw material of profenofos, which can solve the problems of high toxicity, failure to meet discharge standards, and inability to directly biochemically

Active Publication Date: 2017-01-04
山东科源化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are more than ten domestic enterprises producing, and about 6 to 7 tons of by-product wastewater are produced for each ton of products produced. Due to the heavy color, odor, and high toxicity, the by-product wastewater cannot be directly biochemical. It must be pretreated first, otherwise it cannot be processed. Discharge
In recent years, although there have been reports on the treatment of this waste water in China, the focus is on how to recover bromine from the waste water of the bromination process section, but there has been no report on the use of trimethylethylamine bromide in the by-product waste water to synthesize bromopropane, the raw material of profenofos

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Synthesis of bromopropane as raw material of profenofos by using profenofos by-product

[0021] n-propanol: 420kg;

[0022] Profenofos by-product: 1870kg, (wherein trimethylethylamine bromide: 66.0%, bromine: 31.4%), the mol ratio of n-propanol and trimethylethylamine bromide is 1:1.05;

[0023] Concentrated sulfuric acid: 770kg, the molar ratio of n-propanol to concentrated sulfuric acid is 1:1.1.

[0024] Reaction steps:

[0025] (1) Under the action of the dehydrating agent concentrated sulfuric acid, the profenofos by-product reacts with n-propanol to obtain a mixed solution containing bromopropane;

[0026] (2) above-mentioned mixed solution is left standstill, separates out oil base layer, i.e. separating liquid for the first time;

[0027] (3) add 200kg of water to the separation liquid for the first time, wash, neutralize and adjust the pH value to 6, let stand, and separate the oil base layer, that is, the separation liquid for the second time;

[0028] (4)...

Embodiment 2

[0031] Synthesis of bromopropane as raw material of profenofos by using profenofos by-product

[0032] n-propanol: 420kg;

[0033] Profenofos by-product: 1925kg, (wherein trimethylethylamine bromide: 67.2%, bromine: 32%), the mol ratio of n-propanol and trimethylethylamine bromide is 1:1.1;

[0034] Concentrated sulfuric acid: 805kg, the molar ratio of n-propanol to concentrated sulfuric acid is 1:1.15.

[0035] Reaction steps:

[0036] (1) Under the action of the dehydrating agent concentrated sulfuric acid, the profenofos by-product reacts with n-propanol to obtain a mixed solution containing bromopropane;

[0037] (2) above-mentioned mixed solution is left standstill, separates out oil base layer, i.e. separating liquid for the first time;

[0038] (3) add 220kg of water to the separation liquid for the first time, wash, neutralize and adjust the pH value to be 6, leave standstill, separate the oil base layer, that is, the separation liquid for the second time;

[0039]...

Embodiment 3

[0042] Synthesis of bromopropane as raw material of profenofos by using profenofos by-product

[0043] n-propanol: 420kg;

[0044] Profenofos by-product: 1945kg, (wherein trimethylethylamine bromide: 69.5%, bromine: 33.1%), the mol ratio of n-propanol and trimethylethylamine bromide is 1:1.15;

[0045] Concentrated sulfuric acid: 840kg, the molar ratio of n-propanol to concentrated sulfuric acid is 1:1.2.

[0046] Reaction steps:

[0047] (1) Under the action of the dehydrating agent concentrated sulfuric acid, the profenofos by-product reacts with n-propanol to obtain a mixed solution containing bromopropane;

[0048] (2) above-mentioned mixed solution is left standstill, separates out oil base layer, i.e. separating liquid for the first time;

[0049] (3) add 240kg of water to the separation liquid for the first time, wash, neutralize and adjust the pH value to be 6, leave standstill, separate the oil base layer, that is, the separation liquid for the second time;

[005...

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Abstract

The invention relates to a method for synthesizing the raw material bromopropane of profenofos with profenofos byproducts. According to the method, brominated trimethylamine in profenofos synthesis byproducts is recycled and synthesized into bromopropane with n-propanol, and synthesized bromopropane can be recycled for synthesizing profenofos. The method comprises the following steps that firstly, under the action of a dehydrating agent concentrated sulfuric acid, profenofos byproducts react with n-propanol, and a mixed solution containing bromopropane is obtained; secondly, the mixed solution is subjected to standing, an oil-base layer is separated out, and a primary separation solution is obtained; thirdly, water is added into the primary separation solution for washing and neutralizing, standing is carried out, an oil-base layer is separated out, and a secondary separation solution is obtained; fourthly, the secondary separation solution is distilled and purified, and the end product bromopropane is obtained. According to the method, bromine in wastewater is extracted while the profenofos byproducts are treated, and the bromine resource is recycled. The purity of bromopropane synthesized with the method can reach 98.5%, and the recycling rate of bromine reaches 83% or above.

Description

technical field [0001] The invention relates to the field of processing pesticide synthesis by-products, in particular to a method for synthesizing bromopropane as a raw material of profenofos by using profenofos by-products. Background technique [0002] Profenofos, also known as bromochlorphos and polyfenfos, is a pesticide variety developed by Ciba-Geigy in the late 1970s. It has high activity against resistant pests, especially the resistant cotton bollworm. This variety was listed by the state in 2005 as one of the varieties to replace highly toxic organophosphorus pesticides, and has a good development prospect. [0003] At present, there are more than ten domestic enterprises producing, and about 6 to 7 tons of by-product wastewater are produced for each ton of product produced. Due to the heavy color, odor, and high toxicity, the by-product wastewater cannot be directly biochemical. It must be pretreated first, otherwise it cannot be used. Discharge. In recent year...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/16C07C19/075
CPCC07C17/16C07C19/075
Inventor 刘旭东张明宇提云恒
Owner 山东科源化工有限公司
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