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Catalyst for synthesizing isopropamide products, preparation method and application

A catalyst, propylamine technology, applied in reductive alkylation preparation, chemical instruments and methods, physical/chemical process catalysts and other directions, can solve the problems of reducing the service life of the catalyst, the conversion rate of the ammoniation reaction is not high, affecting the activity of the catalyst, etc. , to achieve the effect of long catalyst life, high target conversion rate and good selectivity

Active Publication Date: 2011-09-07
ZHEJIANG XINHUA CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is feasible to consider the above two methods from the perspective of process design, but there are big problems in actual production: firstly, the composition of the circulating liquid is far more than the three substances of isopropyl alcohol, diisopropylamine and water, and also includes isopropylamine, acetone, For substances such as isopropylidene amine, a pure nickel-based catalyst cannot convert the circulating fluid into isopropylamine with a high conversion rate and high selectivity; on the other hand, the presence of a large amount of water affects the activity of the catalyst, resulting in The conversion rate of the ammoniation reaction is not high, and the service life of the catalyst is reduced at the same time, resulting in a vicious cycle of the system

Method used

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  • Catalyst for synthesizing isopropamide products, preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0032] 82.24 g Ni(NO 3 ) 2 ·6H 2 O, 217.32 g Co(NO 3 ) 2 ·6H 2 O, 12.54 g Fe(NO 3 ) 3 ·6H 2 O, 13.96 g Cu(NO 3 ) 2 ·6H 2 O, 1.26 g Ru(NO 3 ) 2 ·6H 2 O was mixed with 350 milliliters of deionized water (the mass ratio of Ni / Co / Fe / Cu / Ru was 8.5:22:1:1.5:0.16), and 133.68 grams of diatomaceous earth was added and mixed with 0.3 molar concentration Na 2 CO 3 Co-precipitation by solution co-current method, control the pH value to 9.0, age for 4 hours under stirring at 75-90°C, filter the precipitate and wash it repeatedly with deionized water until it is almost neutral, and then put the washed precipitate at 120°C After drying for 6 hours, roast at 400°C for 6 hours to obtain an oxidized mixture of Ni-Co-Fe-Cu-Ru. The oxidized mixture is ground into a powder (referred to as dry material) by a ball mill, and an appropriate amount of nitric acid is added to the powder. Ionized water is used to make wet materials, the addition of nitric acid is 1.2w% of the dry materia...

Embodiment 6

[0036] Use the catalyzer that embodiment 1-5 prepares, add 160 gram catalyzers on the reactor (reactor inner diameter 20mm, long 550mm) of small-scale continuous hydrogenation reaction device, after 8 hours with hydrogen reduction in the scope of 350-450 ℃, pass Enter the reaction raw material (isopropylamine circulation liquid: ammonia: hydrogen=2.4: 8.3: 11.3) to carry out hydrogenation amination reaction, reaction temperature 145 ℃, reaction pressure 1.3MPa, space velocity 0.5h -1 , the conversion rate of circulating fluid is 90%, and the total selectivity of mono- and diisopropylamine is 98% (wherein mono-isopropylamine is 64%, and diisopropylamine is 34%).

Embodiment 7

[0038] On the reaction device of embodiment 6, use the catalyst of embodiment 6 to carry out hydrogenation ammonification reaction, raw material feed ratio is still isopropylamine circulation liquid: ammonia: hydrogen=2.4: 8.3: 11.3, reaction temperature 175 ℃, reaction pressure 1.3MPa, air speed 0.5h -1 , the conversion rate of circulating liquid is 95%, and the total selectivity of mono- and diisopropylamine is 96.6% (wherein mono-isopropylamine is 45%, and diisopropylamine is 51.6%).

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Abstract

The invention relates to a catalyst for synthesizing isopropamide products by utilizing isopropamide circulation fluid, a preparation method and an application thereof. The catalyst provided by the invention is composed of mixed oxide of Ni, Co, Fe, Cu and Ru and diatomite, and the catalyst has excellent catalytic activity and selectivity and good stability. By adopting the catalyst and process method provided by the invention, the conversion rate of isopropamide circulation fluid is high, the selectivity of mono isopropylamine and diisopropylamine products is high, and the life of the catalyst is long.

Description

technical field [0001] The invention relates to a catalyst for synthesizing isopropylamine series products with isopropylamine circulating liquid, a preparation method and application thereof. technical background [0002] Isopropylamine is an important fine chemical intermediate, which belongs to low-carbon fatty amine products. Widely used as synthetic pesticides (such as herbicide atrazine, promethazine, glyphosate isopropylamine salt, insecticide isofenphos-methyl, fungicide iprodione, etc.), medicine (such as xinlegan, endolamine , Indolol, Chlorophylline, etc.), dye intermediates, and also widely used in rubber industry, water treatment industry, light industry, textile, daily chemical, leather and other industries. [0003] There are two production methods of isopropylamine, i.e. isopropanol gas-phase ammoniation method and acetone hydrogenation method. During the production process of acetone hydroammoniation, a large amount of circulating liquid containing isoprop...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C211/06C07C209/26
Inventor 兰昭洪王晓明王卫民徐利红谢自强
Owner ZHEJIANG XINHUA CHEM
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