Gaseous phase etherifying production method of complex ether with mixed phenol methanol

A mixed phenol and etherification technology, applied in the field of catalysis, can solve problems such as poor economy and high hydrogen consumption

Active Publication Date: 2019-06-28
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional coal tar processing technology is the hydrogenation of coal tar to p

Method used

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  • Gaseous phase etherifying production method of complex ether with mixed phenol methanol
  • Gaseous phase etherifying production method of complex ether with mixed phenol methanol
  • Gaseous phase etherifying production method of complex ether with mixed phenol methanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0127] The preparation process of the catalyst is as follows: 120 grams of ZSM-5 molecular sieve with a molar silicon-aluminum ratio of 20 is mixed with 60 grams of diatomaceous earth and 100 grams of silica sol containing 20% ​​by weight of silicon dioxide, and an appropriate amount of 10% dilute Nitric acid is used as extrusion aid to extrude strips. Dry at 120°C and bake at 500°C for 10 hours. The above catalyst is cut into 1-3mm to prepare columnar catalyst precursor A0. A1 was obtained by steaming 20 grams of A0 in a 100% steam atmosphere for 10 hours at a temperature of 350°C and calcining at 550°C for 3 hours. Add 50ml weight content, 5% phosphoric acid aqueous solution to 20 grams of A1, soak at 30 ℃ for 4 hours. Drying at 120°C and calcining at 550°C for 10 hours prepared Catalyst A, wherein the molecular sieve content was 60%.

Embodiment 2

[0129] The preparation process of the catalyst is as follows: 170 grams of ZSM-5 molecular sieve with a molar silicon-aluminum ratio of 30 is mixed with 30 grams of alumina, and an appropriate amount of 10% dilute nitric acid is added as an extrusion aid to extrude. Dry at 120°C and bake at 700°C for 4 hours. Above-mentioned catalyst is cut into 1~3mm and makes columnar catalyst parent body B0. The parent body catalyst B0 of 20 grams carries out steam treatment in 100% steam atmosphere for 1 hour, and treatment temperature is 700 ℃, and 550 ℃ roasts 3 hours and makes B1, will Add 50ml of 3% by weight phosphoric acid solution to 20 grams of B1 and soak at room temperature for 10 hours. Dry at 120°C and calcinate at 600°C for 2 hours to prepare Catalyst B. The molecular sieve content in the catalyst is 85%.

Embodiment 3

[0131] The preparation process of the catalyst is as follows: 200 grams of ZSM-5 molecular sieve with a molar silicon-aluminum ratio of 40 is mixed with 20 grams of diatomaceous earth, 100 grams of silicon dioxide and 30% silica sol by weight, and an appropriate amount of 10% dilute nitric acid is added as an extrusion aid Extrusion molding. Dry at 120°C and bake at 550°C for 4 hours. The above-mentioned catalyst was cut into 1-3 mm to obtain columnar catalyst matrix D0. The matrix catalyst D0 sample of 20 grams was impregnated with barium nitrate solution aqueous solution for 24 hours, dried at 120°C, and roasted at 600°C for 3 hours. The weight percentage of barium oxide in the catalyst was 0.1% To prepare D1, 20 grams of D1 was steam treated for 10 hours in a 100% steam atmosphere, the treatment temperature was 350°C, and roasted at 550°C for 3 hours to obtain D2, 20 grams of D2 was added to 50ml, with a weight content of 10% Nitric acid solution, soak at room temperature ...

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Abstract

The invention discloses a gaseous phase etherifying production method of complex ether with mixed phenol methanol. The method at least comprises the following steps: feeding a mixture containing mixedphenol and methanol through a reaction zone containing an etherifying catalyst, and reacting to obtain ether. The method for producing complex ether with mixed phenol and methanol uses mixed phenol and methanol as raw materials, has the etherified product selectivity of over 98 percent, has good catalyst stability, does not have equipment corrosion in the production process, is an environment-friendly catalyst, and has an excellent industrial application prospect.

Description

technical field [0001] The application relates to a method for producing mixed ethers by vapor-phase etherification of mixed phenols and methanol, which belongs to the field of catalysis. Background technique [0002] Medium and low temperature coal tar contains a large amount of phenolic compounds, especially phenol and cresol, which are deoxygenated and converted during the hydrogenation upgrading process, resulting in reduced added value, increased hydrogen consumption, and reduced economic efficiency. The traditional solution is to cut out the phenol oil fraction with the most phenol content from coal tar, and then separate the phenolic compounds from the phenol oil to obtain high value-added fine chemicals. However, this method produces a large amount of acid-base waste liquid during the phenol extraction process, which not only has hidden dangers of environmental pollution, but also increases the cost of acid-base waste liquid treatment. In addition, the phenol obtain...

Claims

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Application Information

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IPC IPC(8): C07C41/09C07C43/04B01J29/40B01J29/70B01J37/08B01J37/28B01J37/02
Inventor 王坤院刘中民
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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