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Method for preparing alkylphenol products and method for effectively governing wastewater

A technology for alkylphenols and phenolic compounds, which is applied in the field of preparation of highly selective ortho-substituted alkylphenol product mixtures, can solve problems such as emissions, and achieve the effect of facilitating recycling

Active Publication Date: 2014-06-18
山东三丰新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Before rectification, the organoaluminum catalyst needs to be removed from the alkylphenol product mixture, which effectively solves the discharge problem of phenol-containing wastewater in the process of removing the organoaluminum catalyst

Method used

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  • Method for preparing alkylphenol products and method for effectively governing wastewater
  • Method for preparing alkylphenol products and method for effectively governing wastewater

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Add 600 grams of phenol, Metal aluminum scrap 4.0 grams, replace the air in the reactor with nitrogen. Turn on the heating power supply to slowly heat up the material in the kettle. When the temperature in the kettle rises to 50°C, start stirring and adjust the stirring speed to 80-100 rpm; when the temperature rises to 98-102°C, adjust the stirring speed to 300-350 rpm and slowly raise the temperature to 140-165°C Phenol and metal aluminum scraps start to react and release hydrogen, and the pressure in the kettle gradually increases. When it reaches 0.1 MPa, the automatic control valve is slightly opened manually, and the hydrogen is released, and the temperature is 165-180 ° C. Control it at 0.1~0.2 MPa, wait until the metal aluminum chips in the kettle are completely dissolved, and the reaction is completed. Reduce the temperature in the reactor to 130°C, stop stirring, open the vent valve to return to normal pressure, add 15 grams of activated carbon, replace the ...

Embodiment 2

[0068] The suspension-like water layer contained in the 500mL graduated cylinder in Example 1 was settled at 25-50°C for 24 hours, the supernatant was poured out, and the remaining precipitate was filtered to obtain the clear liquid and filter cake, and 276 grams of the clear liquid were combined. The mass fraction of calcium oxide is 0.4%. Add water and calcium oxide to prepare 300 grams of 3.8% calcium oxide aqueous solution for subsequent use.

[0069] In the low-pressure reactor A, add 600 grams of phenol and 3.0 grams of metal aluminum chips, and replace the air in the reactor with nitrogen. Turn on the heating power supply to slowly heat up the material in the kettle. When the temperature in the kettle rises to 50°C, start stirring and adjust the stirring speed to 80-100 rpm; when the temperature rises to 98-102°C, adjust the stirring speed to 300-350 rpm and slowly raise the temperature to 140-165°C Phenol and metal aluminum scraps start to react and release hydrogen,...

Embodiment 3

[0072] The suspension-like water layer contained in the 500mL graduated cylinder in Example 2 was settled at 25-50°C for 32 hours, the supernatant was poured out, and the remaining sediment was filtered to obtain the clear liquid and filter cake, and 260 grams of the clear liquid were combined. The mass fraction of calcium oxide is 0.6%. Add water and calcium oxide to prepare 300 grams of 6.4% calcium oxide aqueous solution for subsequent use.

[0073]In the low-pressure reactor A, add 600 grams of phenol and 5.0 grams of metal aluminum chips, and replace the air in the reactor with nitrogen. Turn on the heating power supply to slowly heat up the material in the kettle. When the temperature in the kettle rises to 50°C, start stirring and adjust the stirring speed to 80-100 rpm; when the temperature rises to 98-102°C, adjust the stirring speed to 300-350 rpm and slowly raise the temperature to 140-165°C Phenol and aluminum scraps start to react and release hydrogen, and the p...

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Abstract

The invention relates to a method for preparing high-selectivity ortho-substituent alkylphenol product mixed liquid, in particular to a method for preparing the mixed liquid containing ortho-substituent alkylphenol products. In the method, phenol and isobutene are used as raw materials, phenoxyl aluminum is used as catalysts, and homogeneous catalytic alkylation reaction is adopted. A low-pressure process method is adopted for preparing organo-aluminum compound catalysts, and impurities in the catalysts are effectively removed, so the high-selectivity ortho-substituent alkylphenol product mixed liquid is obtained in the catalytic alkylation reaction process. The phenoxyl aluminum catalysts are decomposed, inorganic aqueous alkali prepared from alkaline-earth metal oxide takes reaction with aluminum hydroxide hydrates, aluminum salt mixtures insoluble in water are generated, a water layer in a suspending liquid state is formed in a still standing state, and the water layer is removed through sedimentation and filtration. Therefore, the obtained process water can be cyclically used, the goal of effectively governing wastewater discharge is reached, and an oil layer is the alkylphenol product mixed liquid after the catalyst removal.

Description

technical field [0001] The invention relates to a method for preparing a highly selective ortho-substituted alkylphenol product mixture. Specifically, it involves using phenol and isobutylene as raw materials, using aluminum phenoxide as a catalyst, and homogeneously catalyzing an alkylation reaction to prepare a mixed liquid containing an ortho-substituted alkylphenol product, and an effective treatment method for the generated waste water. Background technique [0002] The catalytic reaction of phenol or phenolic compounds with olefin alkylating agents is an electrophilic substitution reaction of the alkylating agent on the aromatic ring, and the hydroxyl group is used as the first type of substituent, so that the reaction product is mainly a pair of phenolic hydroxyl groups. The isomer whose position and two ortho positions are substituted by an alkylating agent, after completing one alkyl substitution, the aromatic ring is deactivated, and after being substituted by two ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/06C07C37/11B01J31/14
Inventor 杜飞郭静波陆网军郭澄马龙
Owner 山东三丰新材料有限公司
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