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Method for producing DMAPA and co-producing bis-DMAPA and tri-DMAPA

A technology of bis-dmapa and products, which is applied in chemical instruments and methods, preparation of organic compounds, molecular sieve catalysts, etc., can solve the problem that the conversion rate and selectivity are difficult to meet the requirements at the same time, the product ratio cannot be adjusted, and the catalyst utilization rate is low. problems, to achieve the effect of improving atom utilization efficiency, improving product selectivity, and reducing agglomeration

Pending Publication Date: 2022-01-07
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The production process is complex and needs to be continuously switched. The proportion of the obtained products is usually not adjustable, and the production efficiency is low. It is difficult to meet the requirements of conversion rate and selectivity at the same time. Low efficiency, low catalyst utilization, poor stability

Method used

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  • Method for producing DMAPA and co-producing bis-DMAPA and tri-DMAPA
  • Method for producing DMAPA and co-producing bis-DMAPA and tri-DMAPA
  • Method for producing DMAPA and co-producing bis-DMAPA and tri-DMAPA

Examples

Experimental program
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Effect test

Embodiment 1

[0047] The sodium aluminate and 3.5g 40wt% 7.0g 10wt% sodium hydroxide aqueous solution three-necked flask placed in water bath, with stirring at 30 ℃ 30ml of deionized water was homogeneous, 29g tetraethyl ammonium hydroxide as A three-necked flask were added template agent, and then added dropwise 8g triethanolamine agent B as a template, was heated to 30 ℃, stirred for 2 hours to obtain a clear solution. After at a rate of 1g / min was added 233g 30wt% silica sol by a peristaltic pump, was heated to 80 deg.] C for 5 hours to form a gel was transferred to a hydrothermal reaction vessel at a rate of 1.5 ℃ / min heating to 220 deg.] C, after maintaining for 300 hours and then cooled to 50 deg.] C at a rate of 0.5 ℃ / min, the crystallization will be the end of the reaction water autoclave molecular sieve crystals obtained was centrifuged, washed with deionized water and dried to a PH of 7.5,80 ℃ 12h ground to a powder, was placed in a muffle furnace under a nitrogen atmosphere at ...

Embodiment 2

[0049] The sodium aluminate and 5.0g 40wt% 6.6g 10wt% sodium hydroxide aqueous solution three-necked flask placed in water bath, with stirring at 30 ℃ 30ml of deionized water was homogeneous, 45g tetraethyl ammonium hydroxide as A three-necked flask were added template agent, and then added dropwise to 3g of polyvinyl alcohol as a template agent B, heated to 30 ℃, stirred for 2 hours to obtain a clear solution. After at a rate of 3g / min was added 164g 25wt% silica sol by a peristaltic pump, was heated to 80 deg.] C for 6 hours, the water formed in the reaction gel was transferred to the autoclave at a rate of 2 ℃ / min heating to 240 deg.] C, after maintaining 250 hours and then cooled to 50 deg.] C at a rate of 0.5 ℃ / min, the water will be crystallized in the autoclave at the end of the reaction solution obtained by centrifugal separation of the catalyst crystal, deionized water and dried to a PH of 7.5,80 ℃ 12h after milling into a powder, placed in a muffle furnace under a ...

Embodiment 3

[0051]The boric acid 6.25g 40% solution was placed in water bath three-necked flask, stir under 30 ℃, the 23g tetraethyl ammonium hydroxide as a template agent A three-necked flask was added, dropwise addition of the triethanolamine as a template 5g agent B, warmed to 40 ℃, stirred for 2 hours to obtain a clear solution. At a rate of 1.5g / min is added via a peristaltic pump 240g 40wt% silica sol was heated to 80 deg.] C for 8 hours, the water formed was transferred to the autoclave after the reaction the gel at a rate of 1 ℃ / min heating to 240 ℃ after maintaining for 300 hours and then cooled to 50 deg.] C at a rate of 0.5 ℃ / min, the water will be crystallized in the autoclave at the end of the reaction solution obtained by centrifugal separation of the catalyst crystal, deionized water was dried to PH 7.5,80 ℃ after 12h ground to a powder, was placed in a muffle furnace under a nitrogen atmosphere at a rate of 2 ℃ / min heating to 550 deg.] C, maintained 14H, at a rate of 3...

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Abstract

The invention provides a method for continuously producing DMAPA and co-producing bis-DMAPA and tri-DMAPA, which comprises the following steps: adopting two fixed bed reactors connected in series, carrying out addition on acrylonitrile and dimethylamine in a No.1 reactor to obtain an intermediate product, feeding the intermediate product into a No.2 reactor to carry out hydrodeamination reaction, and simultaneously co-producing three products of DMAPA, bis-DMAPA and tri-DMAPA in corresponding proportions; wherein a catalyst used in the No.1 reactor is an inert carrier which does not participate in the reaction, and a catalyst used in the No.2 reactor is a bimetallic catalyst immobilized on a molecular sieve. Three products of DMAPA, bis-DMAPA and tri-DMAPA with corresponding proportions can be co-produced by a one-step method, the content of the three products can reach 1: (1-2): (0.5-2), the three products can be applied or sold without subsequent reaction, the preparation process is simple, green and environment-friendly, and no three wastes are generated.

Description

Technical field [0001] The present invention belongs to petrochemical industry, particularly relates to a process for producing N, N- dimethyl-1,3-propanediamine and the co-N, N- dimethylamino method propionitrile derivative. Background technique [0002] N, N- dimethyl-1,3-propanediamine (DMAPA) is an important organic chemical raw materials, demand that the surfactant art significantly, and as intermediates for the preparation of fabric softeners, agrochemicals , flocculants and dyes, economic benefit. Which is bis (dimethylaminopropyl) amine (bis-DMAPA) and tris (dimethylaminopropyl) amine (tri-DMAPA) is equally applied to the field of promoting agents and derivatives of epoxy curing agents, these three products often used as cationic surfactants products are sold common application, with great use of space. [0003] Synthesis of DMAPA, bis-DMAPA, and tri-DMAPA product of these three processes is usually acrylonitrile and dimethylamine to Michael addition to give an intermedia...

Claims

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Application Information

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IPC IPC(8): C07C253/30C07C255/24C07C209/48C07C211/09C07C211/14B01J29/74B01J29/76B01J29/86
CPCC07C253/30C07C209/48B01J29/7615B01J29/7415B01J29/86B01J2229/18C07C255/24C07C211/09C07C211/14
Inventor 丁儒姜庆梅龚亚军刘富强迟森森李文滨王小龙唐培吉张聪颖尚永华
Owner WANHUA CHEM GRP CO LTD
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