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Load type heteropoly acid catalyst for manufacturing phynol/acetone with hydrogen phosphide cumene decomposition

A cumene hydrogen peroxide, supported technology, used in molecular sieve catalysts, physical/chemical process catalysts, carbon-based compounds preparation and other directions, can solve problems such as equipment corrosion, difficult product separation, and phenol-containing wastewater polluting the environment.

Inactive Publication Date: 2008-07-16
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] The present invention provides a phenol / acetone supported heteropolyacid catalyst by decomposing cumene hydroperoxide to solve the problem of violent reaction caused by the traditional sulfuric acid catalyst in the reaction of CHP decomposition to prepare phenol / acetone, which is difficult to control. The equipment is severely corroded, a large amount of phenolic wastewater is produced to pollute the environment, the production cost is high, and the products are not easy to separate, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 5ml of modified zeolite beta, add 5ml of 20% phosphotungstic acid solution, dry in the shade and dry in an oven at 120°C for 3 hours, move it into a muffle furnace, and use the temperature programming method to raise the temperature to 200°C (the programmed temperature rise rate is 1°C / min), keep constant temperature at 200°C for 4h, and cool down to room temperature naturally.

[0032] Catalyst evaluation experiment:

[0033] Take out 2g catalyst of the present invention and join in the four-necked flask of 250ml, add 80ml acetone again, start stirring, be warming up to 55 ℃ and start to drop 23ml cumene hydroperoxide (mass concentration 88%), drop rate 1ml / min, Control the reaction temperature at 50-70°C. After the dropwise addition, continue to react within this temperature range for 3h, lower the temperature, filter, and take samples for analysis (using chemical methods to analyze the content of phenol and CHP). The analysis results are shown in Table 1 below....

Embodiment 2

[0037] Take 5ml of modified β zeolite, add 5ml of 20% phosphotungstic acid solution, dry in the oven at 120°C for 3 hours after drying in the shade, take out and add 5ml of 2% titanium sulfate solution, dry in the oven at 120°C after drying in the shade After 3 hours, move it into a muffle furnace, raise the temperature to 200°C using the temperature programming method (programmed temperature increase rate is 1°C / min), continue to keep the temperature at 200°C for 4 hours, and cool naturally to room temperature.

[0038] Catalyst evaluation experiment:

[0039] Take out 2g catalyst and join in the 250ml four-neck flask, add 80ml acetone again, start to stir, warm up to 55 ℃ and start to drop 23ml cumene hydroperoxide (mass concentration 88%), drop rate 1ml / min, control reaction The temperature was 50-70°C. After the dropwise addition, the reaction was continued within this temperature range for 3h, cooled, filtered, and sampled for analysis (using chemical methods to analyze t...

Embodiment 3

[0043] Comparative experiment using sulfuric acid as catalyst

[0044]Get 80ml of acetone and add in a 250ml four-neck flask, add 2ml of dilute sulfuric acid solution (mass concentration 5%), warm up to 55°C and start to drop 23ml of cumene hydroperoxide (mass concentration 88%), at a rate of 1ml / min , control the reaction temperature at 50-70°C, after the dropwise addition, continue to react within this temperature range for 3h, lower the temperature, neutralize to neutral with hexamethylenediamine, wash, rest and separate layers, separate the lower aqueous solution, dry, and sample Analysis (using chemical method to analyze the content of phenol and CHP), analysis results are as follows in Table 3.

[0045] table 3

[0046] name

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Abstract

The invention relates to a supported heteropolyacid catalyst used for preparing phenol / acetone through iso-propyl benzene hydrogen peroxide. The impregnation volume ratio between modified beta zeolite and 20 percent of phosphor-tungstic acid is 1: 1; firstly, the modified beta zeolite is added with phosphor-tungstic acid solution (10-30 percent) with the same volume as the modified beta zeolite, shade dried and then dried in an oven at 120 DEG C for 3h, transferred into a muffle, and heated to 200 DEG C through temperature programming with a temperature rising velocity of 1 DEG C / min, and then the temperature is maintained for 4h, finally naturally cooled to normal temperature. The invention has the advantages of quite wide adjustable acid center and acid strength, large specific surface area, good structure stability, high activity, no corrosion and pollution, easily separated products, moderate reaction conditions, low production cost and reproducibility, etc.

Description

technical field [0001] The invention belongs to a supported heteropolyacid catalyst, under the action of which, cumene hydroperoxide is decomposed to produce phenol / acetone. technical background [0002] Phenol is one of the important basic organic synthesis raw materials in the chemical industry, mainly used in the production of phenolic resin, bisphenol A, caprolactam, aniline, alkylphenol, etc. At present, the main production methods of phenol in the world are: cumene method, toluene-benzoic acid method and benzene direct oxidation method. Among them, the cumene method is the main production method of phenol in the world, accounting for about 90% of the world's total phenol production. The production process of the cumene method is: benzene and propylene react under the action of a catalyst to generate cumene, and the cumene is oxidized by air or oxygen to generate cumene hydroperoxide (abbreviated as CHP). Decomposition occurs to phenol / acetone. The catalysts used in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/70B01J27/19C07C39/04C07C37/08C07C45/53C07C49/08
CPCY02P20/52
Inventor 孙秀云张连中路大勇魏庆玲邱俊杨英杰赵胤
Owner JILIN INST OF CHEM TECH