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Method for preparing 1,6-hexylene glycol through dimethyl adipate gas-phase hydrogenation

A technology of dimethyl adipate and hexanediol, which is applied in the field of organic synthesis and catalyst preparation, can solve the problems of poor selectivity of noble metal catalysts, harsh catalytic reaction conditions, and complicated preparation processes, so as to increase the number of effective active sites and reduce Pressure requirement, effect of improving catalytic ability

Active Publication Date: 2017-09-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Its prominent feature is that the method overcomes the complex preparation process of the composite oxide catalyst used in the hydrogenation of dimethyl adipate to prepare hexanediol, the harsh conditions of the catalytic reaction, and the disadvantages that the reaction needs to be carried out at high temperature, high pressure and low space velocity, and Poor selectivity and high cost of noble metal catalysts have obvious economic and social benefits

Method used

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  • Method for preparing 1,6-hexylene glycol through dimethyl adipate gas-phase hydrogenation
  • Method for preparing 1,6-hexylene glycol through dimethyl adipate gas-phase hydrogenation
  • Method for preparing 1,6-hexylene glycol through dimethyl adipate gas-phase hydrogenation

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Experimental program
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Effect test

Embodiment 1

[0030] Cu / HPS catalyst I with a mass fraction of Cu of 20% was firstly prepared according to the above method.

[0031]The operation steps are as follows: prepare 100ml of 1mol / L HCl solution, put it into a 250ml flask and bathe it to 15°C. 1gF127, 2.5gKCl and 1.2gTMB were added sequentially. Stir at 15°C for 1h. 4.16g TEOS was added dropwise to the flask. Then stirred at 15°C for 24h. The suspension was transferred to a stainless steel crystallization kettle for crystallization at 100°C for 24h. Filter the crystallized liquid, dry the filter cake and bake it at 500°C to obtain a white solid that is hierarchical porous SiO 2 Carrier (HPS).

[0032] Weigh an appropriate amount of carrier, take 0.774g Cu(NO 3 ) 2 ·3H 2 O and 2.7ml of ammonia water are configured into copper ammonia solution, and 0.82g of HPS carrier is added and 2.7ml of water is added. After aging at room temperature for 4 hours, the temperature was raised to distill ammonia until the pH of the solutio...

Embodiment 2

[0039] Prepare 100ml of 1mol / L HCl solution and add it to a 250ml flask in a water bath to 15°C. 1gF127, 2.5gKCl and 1.2gTMB were added sequentially. Stir at 15°C for 1h. 4.16 g of TEOS was added dropwise to the flask. Then stirred at 15°C for 24h. The suspension was transferred to a stainless steel crystallization kettle for crystallization at 140°C for 24h. The crystallized liquid is filtered, and the filter cake is dried and calcined at 500°C. The obtained white solid is hierarchically porous SiO 2 Carrier HPS.

[0040] Weigh an appropriate amount of carrier, take 0.857gCu(NO 3 ) 2 ·3H 2 O and 2.9ml ammonia water are configured into copper ammonia solution, add 0.908g HPS carrier and add 2.9ml water. After aging at room temperature for 4 hours, the temperature was raised to distill ammonia until the pH of the solution was less than 7. After filtering and washing, the obtained filter cake was dried. Roast at 400°C for 4h. The prepared catalyst with a loading capa...

Embodiment 3

[0046] Prepare 100ml of 1mol / L HCl solution and add it to a 250ml flask in a water bath to 15°C. 1gF127, 2.5gKCl and 1.2gTMB were added sequentially. Stir at 15°C for 1h. 4.16 g of TEOS was added dropwise to the flask. Then stirred at 15°C for 24h. The suspension was transferred to a stainless steel crystallization kettle for crystallization at 100°C for 24h. The crystallized liquid is filtered, and the filter cake is dried and calcined at 500°C. The obtained white solid is hierarchical porous SiO 2 Carrier HPS.

[0047] Weigh an appropriate amount of carrier, take 0.944gCu(NO 3 ) 2 ·3H 2 O and 3.3ml of ammonia water are configured into copper ammonia solution, and 1g of HPS carrier is added and 3.3ml of water is added. After aging at room temperature for 4 hours, the temperature was raised to distill ammonia until the pH of the solution was less than 7. After filtering and washing, the obtained filter cake was dried. Roast at 400°C for 4h. The prepared catalyst wi...

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Abstract

The invention provides a method for preparing 1,6-hexylene glycol through dimethyl adipate gas-phase hydrogenation. The method comprises the following steps: by taking a hierarchical pore SiO2 molecular sieve as a carrier, loading a copper-based catalyst, mixing gasified dimethyl adipate with hydrogen, putting the mixture into a fixed bed reactor for reaction under a certain condition, a 1,6-hexylene glycol-containing liquid phase product is obtained. According to the method provided by the invention, by taking the SiO2 molecular sieve with ordered meso pores and micro pores as the carrier, the dispersity of copper serving as an active component is substantially promoted, and the number of effective active sites of the catalyst is increased; moreover, due to the adoption of an ammonia distillation method, the copper is loaded on the mesoporous silicon oxide molecular sieve, so that high dispersion of the catalyst is realized; furthermore, the ordered meso pores of the hierarchical pore SiO2 molecular sieve is retained, and the catalysis capacity is improved.

Description

technical field [0001] The invention relates to a high-performance method for preparing 1,6-hexanediol by gas-phase hydrogenation of dimethyl adipate, belonging to the field of organic synthesis and catalyst preparation. Background technique [0002] 1,6-Hexanediol is an important fine chemical raw material that has been gradually paid attention to in recent years. It is widely used in polyurethane, polyester, coatings, light curing agents, pharmaceutical intermediates and other fields. New cornerstone. The polyurethane prepared with 1,6-hexanediol can improve the hydrolysis weakness and enhance the durability of polyester polyurethane, and the polyester prepared with 1,6-hexanediol and 4,4-dicarboxydiphenylsulfonic acid , with high tensile strength, high elasticity and excellent solvent resistance and swelling resistance, especially suitable for photographic film base. In the medical field, 1,6-dibromohexane, which is prepared from 1,6-hexanediol, is used to synthesize in...

Claims

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Application Information

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IPC IPC(8): C07C29/149C07C31/20B01J29/03
CPCB01J29/0333B01J29/0356B01J2229/186C07C29/149C07C31/20
Inventor 赵玉军郭子原马新宾王胜平
Owner TIANJIN UNIV
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