Production method and production system for 2,4-dichlorophenol

A production system and production method technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as high environmental protection costs, difficulty in controlling sulfur dioxide reuse, and poor product appearance.

Inactive Publication Date: 2018-08-21
SHANDONG RUNBO BIOTECH CO LTD
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  • 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 prod

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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
Comparison scheme
Effect test

Embodiment 1

[0055] supply figure 1 The production system shown; the aspect ratio of the fixed bed reactor is 10, the flow velocity of phenol is 0.2m / s; the flow velocity of sulfuryl chloride is 0.1m / s.

[0056] Dissolve 1 kg of ferric chloride in 100 kg of methanol, mix with 50 kg of polyacrylic acid ion exchange resin, reflux for 5 hours, remove methanol and then dry in vacuum to obtain a supported metal salt catalyst.

[0057] The loaded metal salt catalyst is filled into the tubes of the ceramic medium fixed-bed reactor, and sulfuryl chloride distributors are arranged between the tubes.

[0058] Mix 100kg phenol with 0.01kg dipropyl sulfide to obtain a mixed solution;

[0059] Pass the mixed liquid and sulfuryl chloride into the fixed bed reactor according to the equimolar ratio of phenol and sulfuryl chloride to carry out the chlorination reaction, and the temperature of the fixed bed reactor is controlled at 80°C through the shell-side heat exchanger.

[0060] The chlorination reac...

Embodiment 2

[0065] Continue to use the production system in Example 1.

[0066] Mix 100kg of phenol with 0.1kg of phenylene sulfide to obtain a mixed solution;

[0067] Pass the mixed liquid and sulfuryl chloride into the fixed bed reactor according to the equimolar ratio of phenol and sulfuryl chloride to carry out the chlorination reaction, and the temperature of the fixed bed reactor is controlled at 60°C through the shell-side heat exchanger.

[0068] The chlorination reaction solution continuously enters the deacidification tower to realize continuous deacidification. The tail gas of deacidification is a mixture of hydrogen chloride and sulfur dioxide, which is continuously passed into the sulfuryl chloride reactor, and continuously reacts with chlorine to generate sulfuryl chloride, which is then used for phenol chlorination and deacidification. The temperature is 80°C.

[0069] The deacidification liquid qualified for deacidification is continuously transferred to the rectificatio...

Embodiment 3

[0071] Get 0.08kg of phenylene sulfide recovered in Example 2, add it into 100kg of phenol, and mix thoroughly. Then the mixed solution and sulfuryl chloride were passed into the fixed-bed reactor in Example 2 according to the molar ratio of phenol and sulfuryl chloride to carry out the chlorination reaction, and the temperature of the fixed-bed reactor was controlled at 60° C. through a shell-side heat exchanger. Pass the mixed liquid and sulfuryl chloride into the fixed bed reactor according to the equimolar ratio of phenol and sulfuryl chloride to carry out the chlorination reaction, and the temperature of the fixed bed reactor is controlled at 120°C through the shell-side heat exchanger. The deacidification qualified deacidification liquid is continuously transferred to the rectification tower, and the phenol and ether catalysts are separated to obtain 0.9 kg of recovered phenylene sulfide catalyst and 173.0 kg of 2,4-dichlorophenol, with a content of 99.6% and a yield of 9...

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Abstract

The invention provides a production system for 2,4-dichlorophenol. The production system comprises a fixed-bed reactor, which comprises a phenol feeding port, a sulfuryl chloride feeding port and a discharge outlet, and is provided with a supported metal salt catalyst; a deacidification tower, which comprises a feed inlet, a gas discharge outlet and a liquid discharge outlet, wherein the feed inlet of the deacidification tower communicates with the discharge outlet of the fixed-bed reactor; and a rectifying tower, wherein the feed inlet of the rectifying tower communicates with the liquid discharge outlet of the deacidification tower. Compared with the prior art, the production system provided by the invention has the following advantages: the supported metal salt catalyst is fixed in thefixed-bed reactor for continuous usage and is not in a same system with phenol and a metal catalyst, so impurities in a reaction solution used in a chlorination reaction are reduced, the reaction solution can be easily separated and purified, a finally rectified substance has no solid residue, and a reaction route is clean and environment-friendly.

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): C07C37/62C07C37/68C07C37/74C07C39/30
CPCC07C37/62C07C37/685C07C37/74C07C39/30
Inventor 孙国庆侯永生陈桂元赵广理
Owner SHANDONG RUNBO BIOTECH CO LTD
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