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Method for catalyzing 2,5-dichlorotoluene reaction by modified H type molecular sieve

A dichlorotoluene and molecular sieve technology, which is applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of restricting the development and research of downstream products, serious corrosion of reaction equipment, and large consumption of catalysts. Ease of control, low cost of raw materials, and simple reaction steps

Active Publication Date: 2017-06-13
MINGGUANG FEIZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 2,6-dichlorotoluene has a wide range of uses, but currently there is no domestic manufacturer specializing in the production of 2,6-dichlorotoluene, mainly relying on imports, which seriously restricts the development and research of its downstream products
The preparation methods of 2,4-dichlorotoluene generally include: p-chlorotoluene directional chlorination method, p-\o-chlorotoluene method, 3-chloro-4-toluidine method, etc., but these methods face product separation difficulties, many wastes, Disadvantages such as severe corrosion to reaction equipment and large catalyst consumption

Method used

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  • Method for catalyzing 2,5-dichlorotoluene reaction by modified H type molecular sieve
  • Method for catalyzing 2,5-dichlorotoluene reaction by modified H type molecular sieve
  • Method for catalyzing 2,5-dichlorotoluene reaction by modified H type molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] By changing the amount of loaded metal, we can know the effect of metal loading on the reaction of 2,5-dichlorotoluene catalyzed by the modified H-type molecular sieve, as shown in Table 1:

[0034] Table 1 The effect of the amount of loaded metal on the conversion rate of raw materials and product selectivity

[0035]

[0036] Note: PhCl is chlorobenzene, DCB is dichlorobenzene, 2,6-DCT is 2,6-dichlorotoluene, 2,4-DCT is 2,4-dichlorotoluene, Xylene dichloride is dichloroxylene, 3 , 4-DCT is 3,4-dichlorotoluene, 2,3-DCT is 2,3-dichlorotoluene.

[0037] When the metallic Cu loading is 10%, the reaction temperature is 350 °C, and the carrier gas is N 2 , the volumetric space velocity of the raw material solution is 0.4hr -1 , the conversion rate of 2,5-dichlorotoluene was 26.35%, the selectivity of dichlorobenzene was 46.79%, the selectivity of 2,6-dichlorotoluene was 11.96%, the selectivity of 2,4-dichlorotoluene The selectivity of 3,4-dichlorotoluene is 1.97%.

...

Embodiment 2

[0040] 2, the process of 5-dichlorotoluene solid-liquid phase reaction adopts the method identical with embodiment 1, Cu10%-Hβ (25), carrier gas is N 2 , the volumetric space velocity of the raw material solution is 0.4hr -1 , but changing the reaction temperature to 310°C, 330°C, and 370°C, we can see the effect of the reaction temperature on the isomerization reaction process of 2,5-dichlorotoluene catalyzed by the modified H-type molecular sieve, as shown in Table 3:

[0041]The influence of table 3 reaction temperature on raw material conversion rate and product selectivity

[0042]

[0043] Note: PhCl is chlorobenzene, DCB is dichlorobenzene, 2,6-DCT is 2,6-dichlorotoluene, 2,4-DCT is 2,4-dichlorotoluene, Xylene dichloride is dichloroxylene, 3 , 4-DCT is 3,4-dichlorotoluene, 2,3-DCT is 2,3-dichlorotoluene.

[0044] When the reaction temperature is 350°C, the conversion rate of 2,5-dichlorotoluene is 26.35%, the selectivity of dichlorobenzene is 46.79%, the selectivit...

Embodiment 3

[0047] The process of isomerization of 2,5-dichlorotoluene adopts the same method as in Example 1, Cu10%-Hβ(25), the reaction temperature is 350°C, and the volumetric space velocity of the raw material solution is 0.4hr -1 , but change the type of carrier gas to H 2 , it can be seen that the type of carrier gas affects the isomerization reaction process of 2,5-dichlorotoluene catalyzed by the modified H-type molecular sieve, as shown in Table 3:

[0048] Table 3 The effect of the type of carrier gas on the conversion rate of raw materials and product selectivity

[0049]

[0050] When the carrier gas is hydrogen, the conversion rate of 2,5-dichlorotoluene is 33.44%, the selectivity of dichlorobenzene is 38.07%, the selectivity of 2,6-dichlorotoluene is 15.22%, and the selectivity of 2,4-dichlorotoluene is 33.44%. The selectivity of chlorotoluene was 18.56%, and the selectivity of 3,4-dichlorotoluene was 2.90%.

[0051] The experimental results show that the modified H-typ...

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Abstract

The invention relates to a method for catalyzing 2, 5-dichlorotoluene reaction by a modified H type molecular sieve, and belongs to the technical field of chlorotoluene derivatives. The method comprises the following steps: dissolving Cu(NO3)2 3H2O into distilled water, fully mixing and stirring with an H type molecular sieve after completely dissolving, standing for 12 hours under a condition that the environment temperature is 110 DEG C after standing and drying, and drying in a muffle furnace of which the temperature is 400 DEG C for 2 hours; performing a modified molecular sieve, grinding, sieving, and selecting sieved molecular sieve particles as a catalyst; filling a constant-temperature zone of a fixed bed reactor with the catalyst; conveying raw materials to the fixed bed reactor through a constant flow pump, and continuously bringing rapidly vaporized raw material steam in the constant-temperature zone into a catalyst bed layer through a gas; finally collecting a product through water bath condensation. According to the method disclosed by the invention, the modified H type molecular sieve is adopted as the catalyst, no toxicity and no harm exist, better stability and higher catalytic activity are obtained, cyclic and repeated utilization can be carried out, and sustained industrial production is facilitated.

Description

technical field [0001] The invention relates to a method for catalyzing the reaction of 2,5-dichlorotoluene with a modified H-type molecular sieve, which belongs to the technical field of chlorotoluene derivatives and also belongs to the technical field of molecular sieve applications. Background technique [0002] Chlorotoluene is an important fine chemical raw material, widely used in medicine, pesticides, dyes and so on. The market demand for chlorotoluene has changed greatly, which makes the research on the technology of isomer adjustment of chlorotoluene have a good prospect for industrialization. In recent years, using it as a raw material, a variety of intermediates such as new pesticides, medicines, and dyes have been developed and synthesized successively. Most of these intermediates have good market prospects, and many of them have become hot development products. The huge development space in the downstream market has promoted the production and development of ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/37C07C25/02B01J29/76
CPCB01J29/7615B01J2229/18C07C17/37C07C25/02
Inventor 翟楚殷恒波李继泰
Owner MINGGUANG FEIZHOU NEW MATERIAL
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