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Catalyst for methylbenzene directional chlorination reaction and preparation method thereof

A chlorination reaction and catalyst technology, applied in the field of catalyst and its preparation, can solve the problems of low activity of L-type zeolite, easy collapse of pore structure, large amount of catalyst, etc., achieve high activity and p-chlorotoluene selectivity, and simple preparation method , the effect of improving stability

Inactive Publication Date: 2014-07-02
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the use of L-type zeolite in toluene chlorination reaction faces two important problems: 1) L-type zeolite has low activity, which leads to a large amount of catalyst; 2) under long-term acidic conditions, its pore structure is easy to collapse and its stability is poor

Method used

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  • Catalyst for methylbenzene directional chlorination reaction and preparation method thereof
  • Catalyst for methylbenzene directional chlorination reaction and preparation method thereof
  • Catalyst for methylbenzene directional chlorination reaction and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] According to K 2 O:Al 2 o 3 : SiO 2 :H 2 O=9.3:1:20:412 molar ratio of raw materials, weigh 54g of potassium hydroxide solid and 7.6g of aluminum hydroxide powder, put them in a 500ml round bottom flask, add 262g of deionized water, and reflux at 120°C for 0.5h After dissolving and cooling to room temperature, the aluminum alkali solution was transferred to a 500ml polytetrafluoroethylene beaker. Under vigorous stirring conditions, 145.6 g of 40 wt % silica sol was added dropwise. After stirring at room temperature for 1 h, a gel was obtained.

[0027] Transfer the above gel into a stainless steel autoclave lined with polytetrafluoroethylene, place it in an oven at 170°C for static crystallization for 6 hours, centrifuge, wash with hot water at 100°C until the supernatant is neutral, and store the sample at 100°C After drying for 12 hours, a white powder sample was obtained, and the sample was recorded as K 9 -L. The samples were characterized by X-ray diffracti...

Embodiment 2

[0033] According to K 2 O:Al 2 o 3 : SiO 2 :H 2 O=9.3:1:20:412 molar ratio of raw materials, weigh 54g of potassium hydroxide solid and 7.6g of aluminum hydroxide powder, put them in a 500ml round bottom flask, add 262g of deionized water, and reflux at 120°C for 0.5h After dissolving and cooling to room temperature, the aluminum alkali solution was transferred to a 500ml polytetrafluoroethylene beaker. Under vigorous stirring conditions, 145.6 g of 40 wt % silica sol was added dropwise. After stirring at room temperature for 1 h, a gel was obtained.

[0034] Transfer the above gel into a stainless steel autoclave lined with polytetrafluoroethylene, place it in an oven at 170°C for static crystallization for 6 hours, centrifuge, wash with hot water at 100°C until the supernatant is neutral, and store the sample at 100°C After drying for 12 hours, a white powder sample was obtained, and the sample was recorded as K 9 -L. The samples were characterized by X-ray diffracti...

Embodiment 3

[0040] According to K 2 O:Al 2 o 3 : SiO 2 :H 2 O=9.3:1:20:412 molar ratio of raw materials, weigh 54g of potassium hydroxide solid and 7.6g of aluminum hydroxide powder, put them in a 500ml round bottom flask, add 262g of deionized water, and reflux at 120°C for 0.5h After dissolving and cooling to room temperature, the aluminum alkali solution was transferred to a 500ml polytetrafluoroethylene beaker. Under vigorous stirring conditions, 145.6 g of 40 wt % silica sol was added dropwise. After stirring at room temperature for 1 h, a gel was obtained.

[0041] Transfer the above gel into a stainless steel autoclave lined with polytetrafluoroethylene, place it in an oven at 170°C for static crystallization for 6 hours, centrifuge, wash with hot water at 100°C until the supernatant is neutral, and store the sample at 100°C After drying for 12 hours, a white powder sample was obtained, and the sample was recorded as K 9 -L. The samples were characterized by X-ray diffracti...

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Abstract

The invention relates to a catalyst for methylbenzene directional chlorination reaction and a preparation method thereof. The catalyst is L-shaped zeolite, the grain size of the catalyst is between 400-500 nm, the molar ratio of K to Na in the zeolite is more than or equal to 2.6, and the molar ratio of silicon to aluminum is 5.7-8. The preparation method of the catalyst comprises the following steps: adding potassium hydroxide and aluminum hydroxide into water, backwardly flowing and dissolving at a temperature of 100-120 DEG C and cooling; then adding silica sol into aluminum-alkaline solution under the situation of vigorous agitating, agitating for 0.5-1 hour at a room temperature and carrying out hydrothermal crystallization to obtain KL-shaped zeolite; roasting and carrying out ion exchange to obtain a KNaL-shaped zeolite catalyst; and dealuminizing KNaL-shaped zeolite to prepare KNaL-shaped zeolite with high silicon / aluminum ratio. The preparation method of the catalyst has the advantages of simplicity, easiness in realization, high chlorotoluene yield and higher industrial application value.

Description

technical field [0001] The invention relates to a catalyst for directional chlorination of toluene and a preparation method thereof. Background technique [0002] Chlorotoluene is an important class of fine chemical raw materials, which can be used as raw materials to synthesize a variety of medicines, pesticides, dyes, etc., and its development makes toluene chlorination one of the important choices for chlor-alkali enterprises to take the road of refinement. Monochlorotoluene includes three isomers of o-, m-, and p-chlorotoluene, among which p-chlorotoluene is the most widely used, and the other two products are relatively less in demand and relatively low in price. Usually monochlorotoluene is obtained by toluene chlorination technology, using chlorine gas as the chlorination agent, in the traditional Lewis acid-catalyzed toluene chlorination reaction, monochlorinated products are mainly ortho-para products, of which o-chlorotoluene accounts for about 65% %, p-chlorotolu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/60C07C17/12C07C25/02
Inventor 钟依均王彦方肖强
Owner ZHEJIANG NORMAL UNIVERSITY
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