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Preparation method of catalyst applied to tert-butylamine production through direct amination of isobutene and application

A catalyst and isobutylene technology, applied in the direction of physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of affecting reactants and products, blocking orifices, easy to fall on the outer surface, etc., to achieve high reactivity , low reaction pressure and temperature, high selectivity

Active Publication Date: 2016-10-26
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method provided by the present invention also solves the problem that after the molecular sieve is impregnated and loaded with F, the distribution of F on the surface of the molecular sieve is not uniform, and it is easy to fall on the outer surface and block the orifice, thereby affecting the diffusion of reactants and products in the catalyst, reducing the reactivity of the catalyst, etc. question

Method used

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  • Preparation method of catalyst applied to tert-butylamine production through direct amination of isobutene and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take by weighing 0.243 gram of ammonium fluoride, the HZSM-11 molecular sieve of 10 grams, add 6.25 grams of 40% (weight) silica sol (Na 2 (0:0.04% by weight) mixed, extruded, and dried at 120°C to obtain sample B. A mixture of 5 grams of tetrabutylammonium hydroxide and 30 grams of distilled water was added to the reaction kettle in advance, and the sample B was placed in the reaction kettle above the porous stainless steel mesh and sealed and then subjected to gas-solid phase treatment at 180° C. for 14 hours.

[0021] After the product was taken out, it was washed twice with water, dried at 120°C, and calcined at 400°C for 3 hours to obtain the catalyst as Cat-B. Defined as 100% with the XRD spectrogram feature diffraction peak intensity sum of Cat-A in Comparative Example 1, other samples (such as Cat-B, Cat-C, Cat-D, Cat-E) and its ratio obtain relative crystallinity Spend. Cat-B has a relative crystallinity of 105%.

Embodiment 2

[0023] Take by weighing 0.545 gram of ammonium fluoride, the HZSM-11 molecular sieve of 10 grams, add 12 grams of 40% (weight) silica sol (Na 2 (0:0.03% by weight) mixed, extruded, and dried at 120°C to obtain sample B; a mixture of 10 grams of tetrabutylammonium hydroxide and 20 grams of distilled water was added in advance in the reactor, and sample B was placed in the reactor to be porous Gas-solid phase treatment was carried out at 180° C. for 24 hours after sealing above the stainless steel mesh. After the product was taken out, it was washed twice with water, dried at 120°C, and calcined at 450°C for 4 hours, and the catalyst obtained was designated as Cat-C. XRD results show that the relative crystallinity of Cat-C is 120%.

Embodiment 3

[0025] Take by weighing 0.070 gram of ammonium fluoride, the HZSM-11 molecular sieve of 10 grams, add 8 grams of beer silica gel (Na 2 (0:0.02% by weight) mixed, extruded, and dried at 120°C to obtain sample C. A mixture of 4 grams of tetrabutylammonium hydroxide and 15 grams of distilled water was added to the reaction kettle in advance, and the sample C was placed in the reaction kettle above the porous stainless steel mesh and sealed and then subjected to gas-solid phase treatment at 120° C. for 90 hours. After the product was taken out, it was washed twice with water, dried at 140°C, and calcined at 350°C for 6 hours. The catalyst obtained was designated as Cat-D. XRD results showed that the relative crystallinity of Cat-D was 145%.

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Abstract

The invention provides a preparation method of catalyst applied to tert-butylamine production through direct amination of isobutene and an application. The catalyst is an overall F-ZSM-11 binder-free molecular sieve. The preparation method of the catalyst comprises steps as follows: performing hydrothermal treatment on a mixture formed by an ammonium fluoride and silica binder and an HZSM-11 molecular sieve raw powder in a tetrabutyl ammonium hydroxide aqueous solution or steam to form the overall F-ZSM-11 binder-free molecular sieve; performing further drying and roasting to prepare the needed catalyst. In a tert-butylamine production process through direct amination of isobutene, the catalyst has the characteristics of high reactivity, low reaction pressure and temperature and high target product selectivity.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, in particular to a preparation method and application of a catalyst for direct amination of isobutene to produce t-butylamine. Background technique [0002] Tertiary butylamine is an important organic chemical raw material, widely used in the fields of synthetic rubber vulcanization accelerators, drugs, pesticides, colorants, synthetic resins, surfactants and organic synthesis. [0003] There are many ways to prepare tert-butylamine, but the previous production methods, such as tert-butyl urea hydrolysis, tert-butyl amide hydrolysis, isobutylene-HCN method (Ritter method), halogenated hydrocarbon amination method and other production processes involve strong acid / strong base The use and processing of the method have serious problems of equipment corrosion and pollution, which do not meet the requirements of green chemical industry. In addition, the Ritter method also uses highly toxic HCN as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40C07C209/60C07C211/03
CPCB01J29/40B01J2229/186C07C209/60C07C211/03
Inventor 徐龙伢高尚耀张琬铄朱向学王玉忠谢素娟刘盛林
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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