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Method for forming amination catalyst

A molding method and catalyst technology, applied in the direction of physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve problems such as insufficient bonding, poor overall selectivity, and low strength of shaped catalysts, so as to improve mechanical strength, Reduce the effect of side effects

Active Publication Date: 2013-04-03
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It uses anatase TiO with relatively weak acidity 2 As a forming aid, and for TiO 2 Modified, but still not completely eliminated anatase TiO 2 The occurrence of side reactions caused by modification treatment of TiO 2 In the process, it is necessary to introduce metal components, which will cause side reactions such as dehydrogenation and deamination. Therefore, the overall selectivity of the reaction is still poor; in addition, due to the anatase TiO 2 The bonding effect is not enough, and the strength of the shaped catalyst is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] According to the method described in CN102000602A, adopt following weight percentage to implement:

[0028] Component A 6%

[0029] Anatase TiO 2 30%

[0030] Component B 64%

[0031] Where component A is Pb(NO 3 ) 2 ; Component B is dealuminated H-ZSM-5, its SiO 2 / Al 2 o 3 The molar ratio was 150.

[0032] The molding method of cyclic amine catalyst is implemented according to the following steps:

[0033] a) Prepare 200mL of Pb(NO 3 ) aqueous solution, the TiO of 60g anatase 2 Add to the aqueous solution, add 40mL ammonium dihydrogen phosphate aqueous solution with a solubility of 0.74mol / L to the above aqueous solution under stirring, soak for 8h at a temperature of 80°C, filter, wash and dry to obtain impregnated TiO 2 .

[0034] b) the TiO obtained by impregnating step a) 2 Mixed with 128g of component B, uniformly granulated, pressed into shape, and calcined at 450°C for 8h to obtain cyclic amine catalyst I.

Embodiment 2

[0036] The molding formula of the amination catalyst of the present invention is implemented according to the following weight percentages:

[0037] Component A 60%

[0038] Component B 35%

[0039] Component C 5%

[0040] Among them, component A is molecular sieve catalyst powder; component B is phosphorous acid; component C is Tianqing powder.

[0041] The shaping method of amination catalyst comprises the steps:

[0042] Step 1: Preparation of molecular sieve catalyst powder:

[0043] Add H-ZSM-5 into 0.1Mol / L hydrochloric acid solution, heat and reflux for 2 hours, wherein the solid-to-liquid volume ratio of H-ZSM-5 and hydrochloric acid solution is 1:4, filter, wash, and dry to obtain dealuminated H- ZSM-5, its SiO 2 / Al 2 o 3 The molar ratio was 150.

[0044] Step 2: Preparation of amination catalyst:

[0045] (1) Select raw materials according to the following mass percentages: molecular sieve catalyst powder prepared in step 1: 60%; phosphorous acid: 35%; Tian...

Embodiment 3

[0048] The molding formula of the amination catalyst of the present invention is implemented according to the following weight percentages:

[0049] Component A 90%

[0050] Component B 5%

[0051] Component C 5%

[0052] Among them, component A is molecular sieve catalyst powder; component B is hypophosphorous acid; component C is Tianqing powder.

[0053] The shaping method of amination catalyst comprises the steps:

[0054] Step 1: Preparation of molecular sieve catalyst powder:

[0055]Add H-ZSM-5 into 0.1Mol / L hydrochloric acid solution, heat and reflux for 2 hours, wherein the solid-to-liquid volume ratio of H-ZSM-5 and hydrochloric acid solution is 1:4, filter, wash, and dry to obtain dealuminated H- ZSM-5, its SiO 2 / Al 2 o 3 The molar ratio was 350.

[0056] Step 2: Preparation of amination catalyst:

[0057] (1) Select raw materials according to the following mass percentages: molecular sieve catalyst powder prepared in step 1: 90%; hypophosphorous acid: 5%;...

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Abstract

The invention discloses a method for forming an amination catalyst. At first, a forming formula of the amination catalyst comprises 60%-90% of component A, 5%-35% of component B and 5% of component C, wherein the component A is molecular sieve based catalyst powder, and the molecular sieve based catalyst powder A is prepared by the following method: H-ZSM-5 is added into 0.1mole / liter hydrochloric acid solution to be subjected to heating reflux for 2 hours, wherein the solid-liquid volume ratio of the H-ZSM-5 to the hydrochloric acid solution is 1:4, after filtering, cleaning and drying are performed, dealuminized H-ZSM-5 is obtained, and the molar ratio of SiO2 to Al2O3 is 150-350; the component B is a phosphorous acid or hypophosphorous acid compound; and the component C is sesbania cannabina Pers or methyl cellulose. The components A, B and C are mixed uniformly according to the forming formula, the mixture is granulated, tabletted or extruded and is calcinated for 6 hours at 530 DEG C, so that a formed amination catalyst finished product is obtained.

Description

technical field [0001] The invention relates to a molding method of an amination catalyst, in particular to a molding method of an amination catalyst for synthesizing ethyleneamine compounds through the condensation reaction of ethanolamine and ammonia. Background technique [0002] In the process of synthesizing ethyleneamines with amine compounds as raw materials, various acidic oxides and modified zeolite molecular sieves are used as catalysts, which is a method widely used in this field, but the influence of catalyst molding methods on amination reactions is not known. Not enough attention has been paid. [0003] CN101406845A discloses a molding method of an amination catalyst. The hydrogen-type mordenite treated with an alkali metal is mixed with alumina, titanium oxide, ethanolamine titanate dodecyl alcohol ester evenly, and after aging, it is extruded and tabletted. Or rolling ball forming. Due to the use of acidic alumina as a forming aid in this forming method, it...

Claims

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Application Information

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IPC IPC(8): B01J29/40
Inventor 赵锋伟吕剑杨建明梅苏宁余秦伟魏阿宝王伟李亚妮李春迎何飞崔文华
Owner XIAN MODERN CHEM RES INST
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