Molecular sieve based catalyst for directly preparing polymethyl benzene and preparation and usage methods thereof

A technology based on polymethylbenzene and molecular sieves, which is applied in the field of molecular sieve-based catalysts for the direct preparation of polymethylbenzenes, can solve the problems that the yield is difficult to further increase, and achieve the effects of cost reduction and environmental protection

Active Publication Date: 2016-09-28
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, due to the strong acidity of the ZSM-5 molecular sieve, while the product continues to be methylated, the process of demethylation will also occur at the same time, and the yield is difficult to further increase

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Sodium metaaluminate, silica sol, and tetraethylammonium hydroxide are added to water and mixed to form a molar composition of Na 2 O: Al 2 o 3 : SiO 2 : Templating agent: H 2 O=0.44:0.44:80:12.7:1040 mixture.

[0037] (2) The mixture was crystallized at 140° C. for 3 days in a hydrothermal kettle, cooled, washed with water, and centrifuged 3 times after taking it out to obtain a solid product. Dry at 100°C for 24h, and bake at 450°C for 10 hours in an air atmosphere to obtain sodium ZSM-12.

[0038] (3) Sodium ZSM-12 was treated with 1M ammonium nitrate (NH 4 NO 3 ) solution was mixed according to the ratio of 1g molecular sieve: 20mL solution, and ammonia exchange was carried out at 70°C. After each exchange, it was dried at 110°C and roasted at 450°C for 10 hours in an air atmosphere. Repeated 3 times to obtain hydrogen ZSM- 12 (diameter 0.03 μm, Si / Al molar ratio 40).

[0039] (4) The zinc nitrate solution of 1mol / L is impregnated on the hydrogen type ZS...

Embodiment 2

[0042] (1) Sodium metaaluminate, silicon source (sodium silicate and silica sol, mixed in any proportion), tetraethylammonium bromide are added to water, mixed to form a molar composition of Na 2 O: Al 2 o 3 : SiO 2 : Templating agent: H 2 O=0.44:1.33:100:11:1000 mixture.

[0043] (2) Put the mixture in a hydrothermal kettle for crystallization at 200° C. for 3 days, take it out, cool it, wash it with water, and centrifuge it 3 times to obtain a solid product. Dry at 110°C for 12h, and bake at 650°C for 3 hours in an oxygen atmosphere to obtain sodium ZSM-12.

[0044] (3) Sodium ZSM-12 was treated with 1M ammonium nitrate (NH 4 NO 3 ) solution was mixed according to the ratio of 1g molecular sieve: 20mL solution, and ammonia exchange was carried out at 90°C. After each exchange, it was dried at 110°C and roasted at 650°C for 3 hours in an oxygen atmosphere. Repeated 3 times to obtain hydrogen ZSM- 12 (diameter 80 μm, Si / Al molar ratio 100).

[0045] (4) Zinc nitrate of...

Embodiment 3

[0048] (1) Sodium metaaluminate, sodium silicate, template (50% tetraethylammonium hydroxide and 50% ethylenediamine) are added to water and mixed to form a molar composition of Na 2 O: Al 2 o 3 : SiO 2 : Templating agent: H 2 O=0.44:0.6:100:12:1020 mixture.

[0049] (2) The mixture was placed in a hydrothermal kettle for crystallization at 160° C. for 5 days, cooled, washed with water, and centrifuged three times after taking it out to obtain a solid product. Dry at 105°C for 18h, and bake at 550°C for 7 hours under nitrogen atmosphere to obtain sodium ZSM-12.

[0050] (3) Sodium ZSM-12 was treated with 1M ammonium nitrate (NH 4 NO 3 ) solution was mixed according to the ratio of 1g molecular sieve: 20mL solution, and ammonia exchange was carried out at 80°C. After each exchange, it was dried at 110°C and roasted for 7 hours at 550°C under nitrogen atmosphere. Repeated 3 times to obtain hydrogen ZSM- 12 (diameter 0.5 μm, Si / Al molar ratio 80).

[0051] (4) Mix and imp...

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Abstract

The invention discloses a molecular sieve based catalyst for directly preparing polymethyl benzene and preparation and usage methods thereof. The molecular sieve based catalyst for preparing the polymethyl benzene (tetramethylbenzene- hexamethylbenzene) by using CO, methanol, dimethyl ether or C1-C8 aromatic hydrocarbons and other raw materials uses a ZSM-12 molecular sieve as a main component, can form a multi-component catalyst with a metal and / or structural strengthening agent and / or a stability additive. According to a preparation method of the ZSM-12 molecular sieve and a method for preparing the multi-component catalyst by utilizing the ZSM-12 molecular sieve, the temperature is 450-520 DEG C and the weight space velocity of raw materials is 0.2-15 g / g / h in aromatization reaction, and the polymethyl benzene yield in an obtained organic liquid product is above 80%.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a molecular sieve-based catalyst for directly preparing polymethylbenzene and its preparation and use methods. Background technique [0002] Polymethylbenzene (tetramethylbenzene to hexamethylbenzene) is an important fine chemical raw material, often used as a plasticizer, a curing agent for epoxy resin, a dye or an antioxidant, and various pharmaceutical intermediates. In the traditional petrochemical route, these polymethylbenzenes are mainly obtained from the C 9 -C 12 Separation in distillates, due to its low content and many other substances with the same boiling range, the energy consumption of separation is very large. At the same time, naphtha often contains a certain amount of sulfur compounds, which will seriously affect the performance of these polymethylbenzenes. Another preparation method is alkylation with xylene etc. (reaction with methyl c...

Claims

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Application Information

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IPC IPC(8): B01J29/74B01J29/76B01J29/78B01J29/70C07C1/20C07C15/02
CPCB01J29/7034B01J29/7469B01J29/7669B01J29/7869B01J2229/18C07C1/20C07C2529/70C07C2529/74C07C2529/76C07C2529/78C07C15/02Y02P30/20Y02P30/40
Inventor 骞伟中侯一林王宁黄巍胡琼方
Owner TSINGHUA UNIV
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