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A novel method for synthesizing 3,4-dichlorobenzonitrile

A technology for dichlorobenzonitrile and p-chlorobenzonitrile, which is applied in the field of chlorinated benzonitrile synthesis, can solve problems such as large supply of raw materials, and achieve the effects of promoting production, simple control and improving utilization rate

Active Publication Date: 2018-08-03
HUBEI JUNTAI PHARMA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above-mentioned synthetic techniques have their own characteristics, but there are certain shortcomings. The most important problem is that there is a big problem in the supply of raw materials. Therefore, a new method for the synthesis of 3,4-dichlorobenzonitrile is developed.

Method used

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  • A novel method for synthesizing 3,4-dichlorobenzonitrile
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  • A novel method for synthesizing 3,4-dichlorobenzonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Soak 100 parts of coconut shell activated carbon in 50 parts of water containing 1 part of ferric chloride, 0.4 part of zinc chloride, and 0.6 part of manganese chloride, fully stir and absorb, soak and age for 24 hours, dry the water in it, and put Coconut shell activated carbon loaded with catalyst was filled into a tubular reactor and heated to 200°C for 4 hours of activation. Then continue heating. After the temperature of the catalyst in the tubular reactor reaches 240°C, feed the molten p-chlorobenzonitrile, mixed chlorine and nitrogen in a ratio of 1:2.1:4 to ensure that the reaction temperature is at 240-245°C, the typical ratio of the obtained crude material is shown in Table 1. Table I

[0034] p-Chlorobenzonitrile

[0035] After distillation treatment, 3,4-dichlorobenzonitrile with a purity of 99% can be obtained, with a molar yield of 60% and a composite molar yield of 67%. The melting point of 3,4-dichlorobenzonitrile is 70-71°C.

Embodiment 2

[0037] Soak 100 parts of coconut shell activated carbon in 50 parts of water containing 0.8 parts of ferric chloride, 0.8 parts of zinc chloride, and 0.6 parts of manganese chloride, fully stir and absorb, soak and age for 24 hours, and dry the water in it. Coconut shell activated carbon loaded with catalyst was filled into a tubular reactor and heated to 200°C for 4 hours of activation. Then continue heating. After the temperature of the catalyst in the tubular reactor reaches 235°C, feed the melted p-chlorobenzonitrile and mixed chlorine and nitrogen uniformly according to the ratio of 1:2.1:4 to ensure that the reaction temperature is at 235-240°C, the typical ratio of the crude material obtained is shown in Table 2.

[0038] Table II

[0039] p-Chlorobenzonitrile

[0040] After distillation treatment, 3,4-dichlorobenzonitrile with a purity of 99% can be obtained with a molar yield of 56% and a composite molar yield of 62.5%.

Embodiment 3

[0042] Soak 100 parts of coconut shell activated carbon in 50 parts of water containing 1 part of ferric chloride, 0.4 part of zinc chloride, and 0.6 part of manganese chloride, fully stir and absorb, soak and age for 24 hours, dry the water in it, and put Coconut shell activated carbon loaded with catalyst was filled into a tubular reactor and heated to 200°C for 4 hours of activation. Then continue heating. After the temperature of the catalyst in the tubular reactor reaches 240°C, feed the melted p-chlorobenzonitrile and mixed chlorine and nitrogen uniformly according to the ratio of 1.1:2.1:4 to ensure that the reaction temperature is at 240-245°C, the typical ratio of the crude material obtained is shown in Table 3.

[0043] Table three

[0044] p-Chlorobenzonitrile

[0045] After distillation treatment, 3,4-dichlorobenzonitrile with a purity of 99% can be obtained, with a molar yield of 58.5% and a composite molar yield of 65.3%.

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Abstract

The invention discloses a novel method for synthesizing 3,4-dichlorobenzonitrile.The method comprises the steps that chlorobenzonitrile and chlorine serve as the raw materials, a tubular reactor serves as reaction equipment, and 3,4-dichlorobenzonitrile is synthesized in one step at the temperature of 200-280 DEG C under the action of a catalyst.According to the method, chlorobenzonitrile which is low in price and sufficient in supply serves as the main raw material, 3,4-dichlorobenzonitrile is synthesized in one step through chlorine chlorination under the action of the catalyst at certain temperature.The method has the advantages that control is easy, the raw materials are easy to obtain, the cost is low, and the method is suitable for industrialization.

Description

technical field [0001] The invention relates to a method for synthesizing dichlorobenzonitrile, in particular to a novel method for synthesizing 3,4-dichlorobenzonitrile, which belongs to the technical field of chlorinated benzonitrile synthesis. Background technique [0002] Generally speaking, 3,4-dichlorobenzonitrile is an important intermediate of the pesticide cyhalofop-ethyl, which is the only aryloxyphenoxypropionic acid herbicide that is highly safe for rice, so 3,4-Dichlorobenzonitrile has great application value in the field of pesticides, and its synthesis method has attracted more and more attention. [0003] Specifically, there are many synthetic methods for 3,4-dichlorobenzonitrile, which can be divided into the following types according to different starting materials: [0004] like figure 1 , a kind of 3,4-dichlorotoluene as raw material, under the action of a catalyst to synthesize 3,4-dichlorotoluene by ammoxidation, this method is adopted by most of the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/30C07C255/50
CPCC07C253/30C07C255/50
Inventor 邱远龙张俊涛王唯石家伟谭哲
Owner HUBEI JUNTAI PHARMA CHEM
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