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1,4-hexaethyl butanediamine hydroxide, preparation method and application

A technology of butanediamine hydroxide and hexaethyldibromobutylamine, applied in 1 field, can solve problems such as high price, difficult preparation, unfavorable industrial production, etc., and achieve the effects of reducing synthesis price, simple synthesis process and low price

Inactive Publication Date: 2017-10-10
WUHAN INST OF PHYSICS & MATHEMATICS CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The templating agent involved in the above method is difficult to prepare and expensive, so it is also unfavorable for industrial production

Method used

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  • 1,4-hexaethyl butanediamine hydroxide, preparation method and application
  • 1,4-hexaethyl butanediamine hydroxide, preparation method and application
  • 1,4-hexaethyl butanediamine hydroxide, preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0034] 1,4-hexaethylbutanediamine hydroxide (1,4-(C 2 h 5 ) 3 NC 4 h 8 N(C 2 h 5 ) 3 (OH) 2 ), its preparation method comprises:

[0035] 1) Mix triethylamine and 1,4-dibromobutane in acetone solution, heat under reflux for 24 hours to obtain a yellowish solid, wash the solid with acetone until white, and the obtained white solid is 1,4-hexaethyldi Bromobutylamine;

[0036]2) Dissolve the white solid powder of 1,4-hexaethyldibromobutylamine in water to obtain a clear solution, and obtain 1,4- Hexaethylbutylenediamine Hydroxide.

[0037] In step 1), the molar ratio of triethylamine to 1,4-dibromobutane is 2.4:1, and the molar ratio of triethylamine to acetone is 0.5:1;

[0038] In step 2), the molar ratio of water to 1,4-hexaethyldibromobutylamine is 60:1;

[0039] The production cycle of the above method for preparing 1,4-hexaethyl butanediamine hydroxide is no more than 48 hours, and the yield of 1,4-hexaethyl dibromobutylamine is 86%. 1,4-hexaethyl hydroxide The...

Embodiment 2

[0041] 1,4-hexaethylbutanediamine hydroxide (1,4-(C 2 h 5 ) 3 NC 4 h 8 N(C 2 h 5 ) 3 (OH) 2 ), its preparation method comprises:

[0042] 1) Mix triethylamine and 1,4-dibromobutane in acetone solution, heat under reflux for 24 hours to obtain a yellowish solid, wash the solid with acetone until white, and the obtained white solid is 1,4-hexaethyldi Bromobutylamine;

[0043] 2) Dissolve the white solid powder of 1,4-hexaethyldibromobutylamine in water to obtain a clear solution, and obtain 1,4- Hexaethylbutylene diamine hydroxide ( figure 1 ), for Examples 4-7.

[0044] In step 1), the molar ratio of triethylamine to 1,4-dibromobutane is 2.2:1, and the molar ratio of triethylamine to acetone is 0.5:1;

[0045] In step 2), the molar ratio of water to 1,4-hexaethyldibromobutylamine is 65:1;

[0046] The above-mentioned method prepares 1, the production period of 4-hexaethyl butanediamine hydroxide is no more than 48 hours, and the productive rate of 1, 4-hexaethyl di...

Embodiment 3

[0048] 1,4-hexaethylbutanediamine hydroxide (1,4-(C 2 h 5 ) 3 NC 4 h 8 N(C 2 h 5 ) 3 (OH) 2 ), its preparation method comprises:

[0049] 1) Mix triethylamine and 1,4-dibromobutane in acetone solution, heat under reflux for 24 hours to obtain a yellowish solid, wash the solid with acetone until white, and the obtained white solid is 1,4-hexaethyldi Bromobutylamine;

[0050] 2) Dissolve the white solid powder of 1,4-hexaethyldibromobutylamine in water to obtain a clear solution, and obtain 1,4- Hexaethylbutylenediamine Hydroxide.

[0051] In step 1), the molar ratio of triethylamine to 1,4-dibromobutane is 2.0:1, and the molar ratio of triethylamine to acetone is 0.8:1;

[0052] In step 2), the molar ratio of water to 1,4-hexaethyldibromobutylamine is 100:1;

[0053] The production cycle of the above method for preparing 1,4-hexaethyl butanediamine hydroxide is no more than 48 hours, and the yield of 1,4-hexaethyl dibromobutylamine is 80%. 1,4-hexaethyl hydroxide T...

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Abstract

The invention discloses 1,4-hexaethyl butanediamine hydroxide, a preparation method and an application. Trimethylamine and 1,4-dibromobutane are mixed in an acetone solution and heated under reflux, faint yellow solids are obtained and washed with acetone to white, and obtained white solids are 1,4-hexaethyl dibromobutylamine; the white 1,4-hexaethyl dibromobutylamine solid powder is dissolved in water, a clear solution is obtained and exchanges with anions of strong basic quaternary ammonium I anion exchange resin (201*7), and 1,4-hexaethyl butanediamine hydroxide is obtained. 1,4-hexaethyl butanediamine hydroxide can serve as a novel organic amine template to be used for synthesizing a Beta molecular sieve, the synthesis cost is reduced, and a novel route for synthesizing a high-silica molecular sieve by replacing tetraethylammonium hydroxide is provided. The obtained Beta molecular sieve has good crystallinity and high silica-alumina ratio.

Description

technical field [0001] The present invention relates to the synthesis technology of aluminosilicate zeolite molecular sieves, in particular to 1,4-hexaethyl butanediamine hydroxide and its preparation method and application. 1,4-hexaethyl butanediamine hydroxide can be used as an organic amine template Preparation of Beta Zeolite. Background technique [0002] Beta zeolite was first synthesized (USP308069) by the U.S. Mobil Corporation in 1967 by hydrothermal crystallization in a strongly alkaline system of tetraethylammonium hydroxide. Because of its unique three-dimensional 12-membered ring intersection channel structure and good thermal and hydrothermal stability, Beta zeolite is used as a catalyst in hydrocracking, hydroisomerization, dewaxing, aromatic hydrocarbon alkylation, olefin hydration, etc. It exhibits excellent catalytic performance in refining and petrochemical processes, and is an important industrial zeolite molecular sieve. [0003] In many methods of syn...

Claims

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Application Information

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IPC IPC(8): C07C211/63C07C209/00C01B39/04
CPCC07C211/63C01B39/04
Inventor 刘小龙徐君邓风
Owner WUHAN INST OF PHYSICS & MATHEMATICS CHINESE ACADEMY OF SCI
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