Synthesis method of dichlorophenol

A synthesis method and technology of dichlorophenol are applied in the synthesis of 2,5-dichlorophenol, 2,4-dichlorophenol or 3,4-dichlorophenol, and in the field of synthesis of dichlorophenol, and can solve the problem of production environment The problems of strong odor and harsh reaction conditions can achieve the effect of less three wastes, low production cost and mild reaction conditions.

Inactive Publication Date: 2019-05-17
SHANDONG RUNBO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction temperature of this method is 150-250°C, the reaction time is usually 8-10 hours, the reaction conditions are relatively harsh, and the production environment smells large.

Method used

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  • Synthesis method of dichlorophenol
  • Synthesis method of dichlorophenol
  • Synthesis method of dichlorophenol

Examples

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preparation example Construction

[0023] The invention provides a kind of synthetic method of dichlorophenol, comprising the following steps:

[0024] S1, subjecting 1,4-dichlorobenzene to an alkylation reaction to obtain 1,4-dichloro-2-isopropylbenzene;

[0025] Or subject 1,3-dichlorobenzene to an alkylation reaction to obtain 1,3-dichloro-4-isopropylbenzene;

[0026] Or subject 1,2-dichlorobenzene to an alkylation reaction to obtain 1,2-dichloro-4-isopropylbenzene;

[0027] S2, the alkyl in the 1,4-dichloro-2-isopropylbenzene, the alkyl in the 1,3-dichloro-4-isopropylbenzene or 1,2-dichloro-4-isopropyl Alkyl groups in benzene are oxidized to obtain dichloroperoxides with a structure of formula x;

[0028] S3. Catalyzing and decomposing the dichloroperoxide respectively to obtain dichlorophenol and acetone;

[0029]

[0030] The synthesis method of dichlorophenol provided by the invention has the advantages of high product purity, less waste, simple and easy preparation, low cost, etc., and is suitable...

Embodiment 1

[0049] Take 294g of 1,4-dichlorobenzene, 170g of 2-chloropropane and 30g of aluminum trichloride into the autoclave, raise the temperature to 60°C, raise the pressure to 0.5MPa, keep the pressure for 5 hours, cool down to 25°C after the reaction is complete, and release After pressing, the obtained reaction material was washed with 200 g of water until neutral, and then dried to obtain 348.2 g of 1,4-dichlorocumene. Add 10g of 5wt% sodium carbonate solution to the oxidation reactor, pressurize the air to 0.5MPa pressure, raise the temperature to 110°C, transfer the obtained 1,4-dichloroisopropylbenzene, and oxidize it to 1,4-dichloroisopropyl Benzene peroxide, the temperature was lowered to obtain 390.6 g of the peroxide.

[0050] Add 50g acetone, 20g gained 1,4-dichlorocumene peroxide, 10g catalyst macroporous sulfonic acid resin (aperture 1mm) in the four-necked flask equipped with condenser and stirrer, put the four-necked flask Put it into a constant temperature water bat...

Embodiment 2

[0052] Take 294g of 1,3-dichlorobenzene, 170g of 2-chloropropane and 30g of solid phosphoric acid catalyst into the autoclave, raise the temperature to 50°C, raise the pressure to 0.6MPa, keep the pressure for 5 hours, cool down to 25°C after the reaction is complete, and release the pressure After completion, the obtained reaction material was washed with 200 g of water until neutral, and then dried to obtain 352.2 g of 1,3-dichlorocumene. Add 10g of 5% sodium carbonate solution to the oxidation reactor, pressurize the air to 0.5MPa, raise the temperature to 110°C, transfer the obtained 1,3-dichloroisopropylbenzene, and oxidize it into 1,3-dichloroisopropyl Benzene peroxide, the peroxide is obtained by cooling.

[0053] Add 50g acetone, 20g gained 1,3-dichlorocumene peroxide, 10g catalyst macroporous sulfonic acid resin (aperture 1.5mm) in the four-necked flask that is equipped with condenser and stirrer, the four-necked flask Put it into a constant temperature water bath, r...

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Abstract

The invention provides a synthesis method of dichlorophenol. The method comprises following steps: S1, 1,4-dichlorobenzene is subjected to an alkylation reaction, and 1,4-dichloro-2-cumene is obtained; or 1,3-dichlorobenzene is subjected to the alkylation reaction, and 1,3-dichloro-4-cumene is obtained; or 1,2-dichlorobenzene is subjected to the alkylation reaction, and 1,2-dichloro-4-cumene is obtained; S2, alkyl in 1,4-dichloro-2-cumene, alkyl in 1,3-dichloro-4-cumene or alkyl in 1,2-dichloro-4-cumene is oxidized, and dichloroperoxide with the structure represented as formula x in the description is obtained; S3, dichloroperoxide is subjected to catalytic decomposition respectively, and dichlorophenol and acetone are obtained. A product obtained with the synthesis method of dichlorophenol is high in content, few three wastes are produced, reaction conditions are mild, operation is easy, and the production cost of the product is low.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a synthesis method of dichlorophenol, specifically a synthesis method of 2,5-dichlorophenol, 2,4-dichlorophenol or 3,4-dichlorophenol. Background technique [0002] The molecular weight of dichlorophenol is 163.00. It is an important organic intermediate in industry, including 2,5-dichlorophenol, 2,4-dichlorophenol and 3,4-dichlorophenol. Among them, 2,5-dichlorophenol is an important intermediate of pesticides, medicines and dyes, nitrogen fertilizer synergist and leather antifungal agent, and is mainly used in the synthesis of herbicide dicamba. Dicamba, a herbicide, has a significant control effect on annual and perennial broad-leaved weeds. It is widely used in post-emergence weeding in fields such as cereals, corn orchards, and is widely used in developed areas. With the improvement of crop protection awareness in developing countries , the market of dicamba in de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/08C07C39/30C07C45/53C07C49/08
Inventor 孙国庆侯永生胡义山周长涛
Owner SHANDONG RUNBO BIOTECH CO LTD
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