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Method for preparing 2,6-dichlorotoluene through catalytic chlorination of 2-chlorotoluene with loaded type molecular sieve

A technology of dichlorotoluene and chlorotoluene, which is applied in the field of preparing 2,6-dichlorotoluene by catalytic chlorination of 2-chlorotoluene with loaded molecular sieves, which can solve the problem of low reaction conversion rate and yield, unfavorable industrial production, and difficulty in industrialization Large and other problems, to achieve the effect of easy product separation, low cost, and easy operation

Inactive Publication Date: 2015-08-19
NANJING ZHONGTENG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Post-processing is difficult and industrialization is difficult
[0008] On the whole, the existing production method of 2,6-dichlorotoluene has complex process, harsh reaction conditions, low reaction conversion rate and yield, high cost, difficult post-processing and other deficiencies, which are unfavorable for its industrial production

Method used

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  • Method for preparing 2,6-dichlorotoluene through catalytic chlorination of 2-chlorotoluene with loaded type molecular sieve
  • Method for preparing 2,6-dichlorotoluene through catalytic chlorination of 2-chlorotoluene with loaded type molecular sieve
  • Method for preparing 2,6-dichlorotoluene through catalytic chlorination of 2-chlorotoluene with loaded type molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Preparation of Fe-L molecular sieve Add 145.6g of KOH to 486mL of water, then add 15.6g of Al(OH) 3 , reacted at 120°C for 3h, and cooled to room temperature to obtain potassium metaaluminate alkali solution. Prepare a certain amount of silica sol aqueous solution, slowly add the above-mentioned potassium metaaluminate solution to the silica sol aqueous solution dropwise, the amount of silica sol added in the raw material conforms to the molar ratio SiO 2 :Al 2 o 3 =30:1. The reaction was carried out at 40°C. After 10h, the mixture was placed in a hydrothermal kettle and crystallized at 150°C for 168h. Wash the prepared L-type molecular sieves with different silicon-aluminum ratios with distilled water to neutrality, dry them at 120°C for 12 hours, and set aside.

[0023] 0.815g (5mmol) FeCl 3 and 10.0 g of L-type molecular sieves were added into a 100 mL three-necked flask filled with 50 mL of distilled water, heated to 80° C., and stirred for 4 h. The sample...

Embodiment 2

[0032] Adopt the same method of implementation 1 to prepare Fe-L type molecular sieve, 2-chlorotoluene chlorination reaction step is the same as embodiment 1, keep the silicon-aluminum ratio of L type molecular sieve constant, change Fe loading capacity to be 0.2mmol / g, 0.5 mmol / g, 1.0mmol / g, the influence of Fe-L molecular sieve catalysts with different Fe loadings on the chlorination process of 2-chlorotoluene can be obtained, as shown in Table 2:

[0033] Table 2 Effect of Fe-L molecular sieve catalysts with different Fe loadings on the chlorination of 2-chlorotoluene

[0034]

[0035] It can be seen from Table 2 that, from the perspective of comprehensive raw material conversion rate and product selectivity, the loading amount of Fe is 1.0 mmol / g is better. Example 3

Embodiment 3

[0036] Adopt the same method of implementing 1 to prepare Fe-L type molecular sieve, 2-chlorotoluene chlorination reaction step is the same as embodiment 1, change the consumption of Fe-L type molecular sieve to be 1.0g, 5.0g, can obtain catalyst consumption to 2-chlorine The impact of toluene chlorination process, as shown in Table 3:

[0037] Table 3 Effect of catalyst dosage on the chlorination reaction of 2-chlorotoluene

[0038]

[0039] It can be seen from Table 3 that the increase of the catalyst dosage is beneficial to the improvement of the conversion rate of raw materials, but when the catalyst dosage is 3%, the conversion ratio is high, and the selectivity of 2,6-DCT will decrease when the catalyst dosage is continued to increase.

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Abstract

The invention discloses a method for preparing 2,6-dichlorotoluene through catalytic chlorination of 2-chlorotoluene with a loaded type molecular sieve; according to the method, the Fe-L type molecular sieve is used as a catalyst, Cl2 is used as a chlorinating agent, and selectivity chlorination of 2-chlorotoluene is carried out by a liquid phase chlorination method. The preparation method is simple in process and mild in reaction conditions; the used Fe-L type molecular sieve is good in catalytic activity and good in stability, is easily separated from the product, and can significantly improve the selectivity of 2,6-dichlorotoluene; and the method has quite high industrial application value.

Description

technical field [0001] The invention belongs to the field of organic synthesis and relates to a preparation method of 2,6-dichlorotoluene, in particular to a method for preparing 2,6-dichlorotoluene by catalyzing the chlorination of 2-chlorotoluene with a loaded molecular sieve. Background technique [0002] 2,6-Dichlorotoluene is an important fine chemical raw material, which can be widely used in the manufacture of fungicides, insecticides, herbicides, dyes and pigments, pharmaceuticals and other chemical products. 2,6-dichlorobenzaldehyde can be obtained by using 2,6-dichlorotoluene, which can be further processed to produce pharmaceutical intermediate 2,6-dichlorobenzaldehyde oxime, dicloxacillin for medicine, etc.; 2,6- Dichlorotoluene can also be obtained through ammonia oxidation to produce 2,6-dichlorobenzonitrile, which can be further processed into pesticide herbicide grass gram, fluorine-containing urea insecticides, etc. [0003] There are many synthesis techniq...

Claims

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Application Information

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IPC IPC(8): C07C25/02C07C17/12B01J29/63
Inventor 钟华陆敏山陈秀珍刘巧宝
Owner NANJING ZHONGTENG CHEM
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