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Multi-stage pore molecular sieve, preparation method thereof and application thereof in synthesis of diaminodiphenylmethane derivative

A diaminodiphenylmethane and microporous molecular sieve technology, which is applied in molecular sieve catalysts, amino compound preparation, chemical instruments and methods, etc., can solve the problems of easy coking of catalysts, poor selectivity of diaminodiphenylmethane derivatives, and short service life. , to achieve the effect of reducing by-products such as polymers, high product yield and prolonging service life

Inactive Publication Date: 2018-08-03
JIANGSU QINGQUAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Purpose of the invention: In view of the deficiencies of traditional microporous molecular sieves, such as the poor selectivity of the target product diaminodiphenylmethane derivatives, the catalyst is easy to coke, and the short life is short, the purpose of the present invention is to provide a multi-level porous molecular sieve, its preparation Method and its application in catalytic synthesis of diaminodiphenylmethane derivatives

Method used

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  • Multi-stage pore molecular sieve, preparation method thereof and application thereof in synthesis of diaminodiphenylmethane derivative
  • Multi-stage pore molecular sieve, preparation method thereof and application thereof in synthesis of diaminodiphenylmethane derivative
  • Multi-stage pore molecular sieve, preparation method thereof and application thereof in synthesis of diaminodiphenylmethane derivative

Examples

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Embodiment 1

[0027] 10.0g of Hβ molecular sieve and 250mL of NaOH and NaOH with a total concentration of 0.3mol / L 2 CO 3 (Molar ratio 3 / 7) mixed lye was added to a 500mL flask, stirred at 95°C for 2h, after cooling down to room temperature, the mixture was filtered, washed with water until neutral, then exchanged twice with ammonia, and finally calcined , to obtain a hierarchically porous Hβ molecular sieve.

Embodiment 2

[0029] 10.0g HZSM-5 molecular sieve and 250mL total concentration of 0.3mol / L NaOH and Na 2 CO 3 (Molar ratio 3 / 7) mixed lye was added to a 500mL flask, stirred at 95°C for 2h, after reaching room temperature, the mixture was filtered, washed with water until neutral, then exchanged twice with ammonia, and finally calcined , to obtain the hierarchical porous HZSM-5 molecular sieve.

Embodiment 3

[0031] 10.0g HY molecular sieve and 250mL total concentration of 0.4mol / L tetramethylammonium hydroxide and Na 2 CO 3 (Molar ratio 1 / 4) mixed lye was added to a 500mL flask, stirred at 105°C for 2h, and after cooling down to room temperature, the mixture was filtered, washed with water until neutral, then exchanged twice with ammonia, and finally calcined , to obtain a multi-level porous HY molecular sieve.

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Abstract

The invention discloses a multi-stage pore molecular sieve, a preparation method thereof and application thereof in the synthesis of a diaminodiphenylmethane derivative. The multi-stage pore molecularsieve is a micropore-mesopore composite molecular sieve, the micropore diameter is less than 2nm, and the mesopore diameter is 2nm to 50nm. A molecular sieve and aqueous alkali are fed according to aproportion and heated to sufficiently react, and after filtration, washing, drying, ammonia exchange and calcination, the multi-stage pore molecular sieve is obtained. The multi-stage pore molecularsieve adopted by the invention is used in the catalytic synthesis of the diaminodiphenylmethane derivative, the product yield is high, byproducts, such as polymers, are greatly reduced, and moreover,a catalyst can be repetitively used. The process is a simple, environment-friendly and high-efficient catalytic synthesis process for the diaminodiphenylmethane derivative, and has a good industrial application prospect.

Description

technical field [0001] The invention relates to a multi-stage pore molecular sieve, its preparation method and its application in the synthesis of diaminodiphenylmethane derivatives, such as MDA, MDT, MOCA, MBTBA, H256, etc., belonging to the technical field of fine chemicals. Background technique [0002] Diaminodiphenylmethane derivatives are important chemical raw materials and are widely used in industry. Diaminodiphenylmethane (MDA) is an important intermediate for the production of diphenylmethane diisocyanate (MDI), and MDI is an important raw material for the production of polyurethane (PU). 3,3'-Dimethyl-4,4-'diaminodiphenylmethane (MDT) is often used as H-class insulating material, polyurethane resin adhesive film agent, glass fiber lubricant, epoxy resin curing agent and polyimide Amine material monomer, etc. 3,3'-dichloro-4,4'-diaminodiphenylmethane (MOCA) can be used as a vulcanizing agent for castable polyurethane rubber, a crosslinking agent for polyurethane...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/70B01J29/40B01J29/08B01J35/10C07C209/78C07C211/52C07C211/50
CPCC07C209/78B01J2229/38B01J35/613B01J35/635B01J35/633B01J35/615C07C211/52C07C211/50
Inventor 徐铁勇汤廷翔许晓龙陈昞志王长锦卢满意
Owner JIANGSU QINGQUAN CHEM CO LTD