O-cresol isomerization catalyst, preparing method of o-cresol isomerization catalyst and method for catalyzed synthesis of mixture of m-cresol and p-cresol through o-cresol isomerization catalyst

A catalyst, o-cresol technology, applied in its preparation, o-cresol isomerization catalyst, and synthesis of m-p-cresol, which can solve the problems of low selectivity, short life, and low activity of m-p-cresol

Active Publication Date: 2015-09-23
HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Based on this, it is necessary to provide a high-activity, long-life, intermediate O-c

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0042] The preparation method of the o-cresol isomerization catalyst of one embodiment, comprises the following steps:

[0043] S110, using cetyltrimethylammonium bromide (CTAB) as a template, adding a silicon source, an aluminum source, an alkali source and deionized water and stirring to obtain a mixed solution.

[0044] Wherein, the silicon source is selected from at least one of silica sol, tetraethyl orthosilicate and white carbon black. The aluminum source is aluminum sulfate, sodium metaaluminate or aluminum nitrate. The alkali source is sodium hydroxide.

[0045] Convert the added amount of the above aluminum source into Al 2 o 3 The amount of addition, the addition of silicon source is converted into SiO 2 The amount of Al added, then Al 2 o 3 with SiO 2 The molar ratio of CTAB to SiO is 0.02~0.035:1 2 The molar ratio of NaOH to SiO is 0.08~0.30:1 2 The molar ratio is 0.15~0.2:1.

[0046] S120, adjusting the pH value of the above mixed solution to 10-11.5, a...

Embodiment 1

[0073] (1) Preparation of H-type MCM-41 / ZSM-5 composite molecular sieve

[0074] Using 17.5 g of cetyltrimethylammonium bromide as a template, 60 g of silica sol, 3.65 g of aluminum nitrate, 2.28 g of sodium hydroxide and 450 g of deionized water were added and stirred to obtain a mixed solution.

[0075] The pH value of the above mixture was adjusted to 11 with sulfuric acid with a mass concentration of 50%, and crystallized at 100° C. for 12 hours to obtain a silicon-aluminum precursor.

[0076] Mix the above-mentioned silicon aluminum precursor with tetrapropylammonium bromide, crystallize at 125°C, pH=9.5 for 48 hours, filter, wash, dry, and roast to obtain Na-type MCM-41 / ZSM-5 composite molecular sieve.

[0077] Weigh 10 g of the above-mentioned Na-type MCM-41 / ZSM-5 composite molecular sieve, dissolve it in 1000 ml of ammonium nitrate aqueous solution (0.5 mol / L) and mix, perform ion exchange at 80 ° C for 4 hours, filter, wash, dry, and roast to obtain H Type MCM-41 / ZSM...

Embodiment 2

[0084] (1) Preparation of H-type MCM-41 / ZSM-5 composite molecular sieve

[0085] Using 17.5 g of cetyltrimethylammonium bromide as a template, 60 g of silica sol, 3.65 g of aluminum nitrate, 2.28 g of sodium hydroxide and 450 g of deionized water were added and stirred to obtain a mixed solution.

[0086] The pH value of the above mixture was adjusted to 11 with sulfuric acid with a mass concentration of 50%, and crystallized at 100° C. for 12 hours to obtain a silicon-aluminum precursor.

[0087] Mix the above-mentioned silicon aluminum precursor with tetrapropylammonium bromide, crystallize at 125°C, pH=9.5 for 72 hours, filter, wash, dry, and roast to obtain Na-type MCM-41 / ZSM-5 composite molecular sieve.

[0088] Weigh 10 g of the above-mentioned Na-type MCM-41 / ZSM-5 composite molecular sieve, dissolve it in 1000 ml of ammonium nitrate aqueous solution (0.5 mol / L) and mix, perform ion exchange at 80 ° C for 4 hours, filter, wash, dry, and roast to obtain H Type MCM-41 / ZSM...

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Abstract

The invention provides an o-cresol isomerization catalyst. The o-cresol isomerization catalyst comprises, by mass, 65%-95% of H-type MCM-41/ZSM-5 composite molecular sieves and 5%-35% of binders. The invention further provides a preparing method of the o-cresol isomerization catalyst and a method for catalyzed synthesis of a mixture of m-cresol and p-cresol through the o-cresol isomerization catalyst. The preparing method of the o-cresol isomerization catalyst includes the steps that a silicon source, an aluminum source and the like serve as raw materials firstly, hexa decyl trimethyl ammonium bromide and tetra propyl ammonium ammonium bromide serve as templates under the alkaline condition so as to synthesize Na-type composite molecular sieves with a two-step crystallization method, then the H-type composite molecular sieves are synthesized through ion exchange, and finally the H-type composite molecular sieves and the binders are mixed and molded. The o-cresol isomerization catalyst has the higher activity and the higher stability, and the selectivity of the mixture of the m-cresol and the p-cresol can be obviously improved, and the o-cresol isomerization catalyst is suitable for a fixed bed reactor.

Description

technical field [0001] The invention relates to an o-cresol isomerization catalyst, in particular to an o-cresol isomerization catalyst, a preparation method thereof and a method for catalytically synthesizing m-p-cresol by using the o-cresol isomerization catalyst. Background technique [0002] m-p-cresol is a mixture of m-cresol and p-cresol in a certain proportion. It is an important chemical intermediate and is widely used in the fields of pesticides, plastics, medicine, enameled wire varnish, etc. For example, high-purity m-cresol can be obtained by isobutylene reaction method and urea complex crystallization method, while high-purity m-cresol and p-cresol can be obtained by adsorption separation method. [0003] In the last century, the way people obtained m-p-cresol was mainly natural separation method, that is, separation from coal tar. Separation from coal tar can obtain phenol, o-cresol, m-p-cresol and xylenol, etc. However, due to limited resources and complex p...

Claims

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Application Information

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IPC IPC(8): B01J29/80C07C37/00C07C39/07
Inventor 彭伟才黄华衷晟佘喜春谢琼玉郑香兰尹笃林
Owner HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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