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Production method and production system for 2,4-dichlorophenol

A production method and technology of dichlorophenol, which is applied in the field of 2,4-dichlorophenol production method and production system, can solve problems such as affecting use and poor product appearance, and achieve simple process, low cost and high selectivity Effect

Inactive Publication Date: 2018-08-21
SHANDONG RUNBO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The Chinese patent with the publication number CN105777499A discloses a method for directional synthesis of 2,4-dichlorophenol and 2,4,6-trichlorophenol with sulfuryl chloride plus a composite catalyst. It is mentioned that 98% of 2, 4-dichlorophenol, but due to the use of expensive sulfuryl chloride, and the subsequent use of molten crystallization for separation, it will inevitably lead to the mixing of low-melting catalysts and oxidative and discolored substances during chlorination into the target product, resulting in poor appearance of the product and containing Certain impurities will affect subsequent use and make it difficult to implement industrialization

Method used

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  • Production method and production system for 2,4-dichlorophenol
  • Production method and production system for 2,4-dichlorophenol

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Add 4000kg of phenol to the 8000L chlorination kettle of the tail gas recycling device supporting phenol recovery and drying, start stirring, then add 0.4kg of dimethyl sulfide, 8kg of ferric chloride, after complete dissolution, keep the temperature at 40°C, start 100 kg of sulfuryl chloride was added dropwise as an initiator, and no fresh sulfuryl chloride was used subsequently. When sulfuryl chloride is added dropwise, tail gas containing sulfur dioxide and hydrogen chloride will overflow. After passing through the tail gas purification and recovery device, the purified mixed gas of sulfur dioxide and hydrogen chloride has a molar ratio of sulfur dioxide to hydrogen chloride of 1:1. After being measured by a flow meter, it is sent to the sulfuryl chloride synthesis process.

[0055] In the sulfuryl chloride synthesis unit, according to the molar amount of tail gas measured by the flow rate, it enters the sulfuryl chloride synthesis reactor at a molar ratio of 1:1 bet...

Embodiment 2

[0060] Add 4000kg of phenol to the 8000L chlorination kettle of the tail gas recycling device supporting phenol recovery and drying, start stirring, then add 1kg of phenylene sulfide and 8kg of ferric chloride, after complete dissolution, keep the temperature at 50°C, and start adding dropwise 150 kg of sulfuryl chloride was used as an initiator, and fresh sulfuryl chloride was no longer used in the follow-up. When sulfuryl chloride is added dropwise, tail gas containing sulfur dioxide and hydrogen chloride will overflow. After passing through the tail gas purification and recovery device, the purified mixed gas of sulfur dioxide and hydrogen chloride has a molar ratio of sulfur dioxide to hydrogen chloride of 1:1. After being measured by a flow meter, it is sent to the sulfuryl chloride synthesis process.

[0061] In the sulfuryl chloride synthesis unit, according to the molar amount of tail gas measured by the flow rate, the molar ratio of chlorine gas to mixed gas is 1.05:1...

Embodiment 3

[0066] Add 4000kg of phenol to the 8000L chlorination kettle of the tail gas recycling device supporting phenol recovery and drying, start stirring, then add 0.6kg of phenylene sulfide and 7kg of titanium tetrachloride. Add 100 kg of sulfuryl chloride as an initiator, and no fresh sulfuryl chloride will be used later. When sulfuryl chloride is added dropwise, tail gas containing sulfur dioxide and hydrogen chloride will overflow. After passing through the tail gas purification and recovery device, the purified mixed gas of sulfur dioxide and hydrogen chloride has a molar ratio of sulfur dioxide to hydrogen chloride of 1:1. After being measured by a flow meter, it is sent to the sulfuryl chloride synthesis process.

[0067] In the sulfuryl chloride synthesis unit, according to the molar amount of tail gas measured by the flow rate, it enters the sulfuryl chloride synthesis reactor at a molar ratio of 1.1:1 between chlorine gas and mixed gas for sulfuryl chloride synthesis, and ...

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Abstract

The invention provides a production method for 2,4-dichlorophenol. The production method comprises the following steps: S1) mixing an initiator, phenol and a catalyst and carrying out a reaction to obtain the chlorination tail gas of phenol and a reaction solution, wherein the initiator is sulfuryl chloride; S2) mixing the chlorination tail gas of phenol with chlorine gas for a reaction to obtainsulfuryl chloride; and S3) mixing the sulfuryl chloride with the reaction solution and carrying out a reaction to obtain the chlorination tail gas of phenol and 2,4-dichlorophenol. Compared with the prior art, the invention has the following advantages: chlorine gas is used as an initial chlorination raw material and continuously produces sulfuryl chloride through a reaction with sulfur dioxide inthe chlorination tail gas of phenol, and then the sulfuryl chloride is continuously added into the reaction solution to finally prepare 2,4-dichlorophenol; continuous reaction and tail gas recyclingflow are adopted in the invention, so high-selectivity low-cost high-yield preparation of 2,4-dichlorophenol is realized; moreover, the production method is simple in process flow and applicable to industrial production, and has great economic value and social benefits.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a production method and production system of 2,4-dichlorophenol. Background technique [0002] 2,4-Dichlorophenol is used as a solvent, pesticide and pharmaceutical intermediate for the synthesis of biben, 2,4-D, ibifos (EPBP), dukesan, glyphosate and the drug thiobisdichlorophene, The annual demand is tens of thousands of tons. [0003] The production methods of 2,4-dichlorophenol mainly include: phenol direct chlorination method, mixed phenol chlorination method, o-chlorophenol selective chlorination method, p-chlorophenol chlorination method and phenol catalytic chlorination method. [0004] The direct chlorination of phenol is a traditional production process at home and abroad. The process is simple and the cost is low. However, because the physical properties of the by-product 2,6-dichlorophenol are very close to those of 2,4-dichlorophenol, it is difficult to se...

Claims

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Application Information

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IPC IPC(8): C07C37/62C07C37/70C07C37/74C07C39/30B01J31/38B01J31/30B01J31/26C01B17/45
Inventor 孙国庆侯永生陈桂元赵广理
Owner SHANDONG RUNBO BIOTECH CO LTD
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