Method for synthesizing 1,6-hexamethylene glycol by using dimethyl adipate gas phase and hydrogen

A technology of dimethyl adipate and hexanediol, which is applied in the field 1, can solve problems such as difficult treatment of lead-containing guard beds, and achieve the effects of improving physical properties and catalytic properties, strong penetration ability, and mild reaction conditions

Active Publication Date: 2009-09-16
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since lead is a heavy metal element, the treatment of the dea

Method used

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  • Method for synthesizing 1,6-hexamethylene glycol by using dimethyl adipate gas phase and hydrogen
  • Method for synthesizing 1,6-hexamethylene glycol by using dimethyl adipate gas phase and hydrogen
  • Method for synthesizing 1,6-hexamethylene glycol by using dimethyl adipate gas phase and hydrogen

Examples

Experimental program
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Example Embodiment

[0043] Example 1

[0044] 1. Preparation of guard bed

[0045] The coal-based activated carbon was first soaked in a 10% hydrochloric acid solution and stirred on a stirrer for 18 hours, then kept at a constant temperature in an oven at 100°C for 2 hours, and washed repeatedly with deionized water until it became neutral. Then, it was steamed to near dryness in a microwave oven at an intermittent power of 500W, dried under microwave radiation (120°C) for 20 minutes, and cooled and stored for use.

[0046] Immerse 5 g of pretreated coal-based activated carbon in 25 ml of K 2 CO 3 And CaCO 3 In the solution of 1 mol / L respectively, stir in a stirrer for 4 hours, then steam it in a microwave oven with an intermittent power of 500W until it is nearly dry and cool to room temperature; the adsorbed K 2 CO 3 And CaCO 3 The activated carbon is put into a quartz glass tube with a sieve plate, and nitrogen is protected under the tube to prevent the activated carbon from oxidizing and burnin...

Example Embodiment

[0054] Example 2

[0055] 1. Preparation of guard bed

[0056] Immerse 5 g of coal-based activated carbon pretreated in Example 1 in 25 ml of K 2 CO 3 And CaCO 3 In the 3mol / L solution, stir in a stirrer for 4 hours, then steam it in a microwave oven at 500W intermittent power to near dryness, dry it under microwave radiation (120°C) for 30 minutes, and cool to room temperature; the adsorbed K 2 CO 3 And CaCO 3 The activated carbon is filled into a quartz glass tube with a sieve plate. The tube is protected by nitrogen to prevent the activated carbon from oxidizing and burning. The quartz tube is calcined in a reaction furnace at 350°C for 4 hours. After the calcination is completed, continue to pass nitrogen to cool to room temperature, granulate and fill , You can get 30.7wt% activated carbon, 43.5wt% K 2 A guard bed of O and 25.8wt% CaO.

[0057] 2. Preparation of MCM-48 carrier:

[0058] Ethyl orthosilicate (TEOS), cetyl trimethyl amine bromide (CTAB), sodium hydroxide, water ...

Example Embodiment

[0064] Example 3

[0065] 1. Preparation of guard bed:

[0066] Immerse 5 g of coal-based activated carbon pretreated in Example 1 in 25 ml of K 2 CO 3 And CaCO 3 In the solution of 1 mol / L and 3 mol / L respectively, stir in a stirrer for 4 hours, then steam to near dryness in a microwave oven at 500W intermittent power, dry for 30 minutes under microwave radiation (120°C), and cool to room temperature; K 2 CO 3 And CaCO 3 The activated carbon is filled into a quartz glass tube with a sieve plate, and the bottom of the tube is protected by nitrogen to prevent the activated carbon from oxidizing and burning. The quartz tube is calcined in a reaction furnace at 350°C for 4 hours. , You can get 43.2wt% activated carbon, 20.4wt% K 2 A guard bed of O and 36.4wt% CaO.

[0067] 2. Preparation of hydrogenation catalyst

[0068] 16.0 g Cu(NO 3 ) 2 ·3H 2 O dissolved in 50 ml H 2 In O, redissolve 18.6 grams of Al(NO 3 )3 ·9H 2 O, 4.0 g Mn(Ac) 2 ·4H 2 After mixing O, stir and add 4 g of MCM-48...

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Abstract

The invention discloses a method for synthesizing 1,6-hexamethylene glycol by using dimethyl adipate gas phase and hydrogen. Preparing hydrogenation catalyst includes steps as follows: stirring, microwave evaporating to dryness, microwave drying and baking for obtaining the hydrogenation catalyst. In addition, preparing a protective bed used for removing impurity gas in hydrogen includes steps as follows: confecting an active carbon carrier, an alkali metal salt and an alkaline earth metal calcium salt to water solution in proportion, stirring, microwave evaporating, microwave drying and baking under protection of inert gases; obtaining the protection bed with high performance that contains: 5-90wt% active carbon, 10-95wt% kalium oxide and calcium oxide. The method can improve physical property and catalysis property of the catalyzer greatly.

Description

technical field [0001] The invention relates to the synthesis of 1,6-hexanediol, in particular to a method for synthesizing 1,6-hexanediol by gas-phase hydrogenation of dimethyl adipate in the presence of a catalyst. Background technique [0002] 1,6-Hexanediol is an important basic organic synthesis raw material that has developed rapidly in recent years. Due to the longer carbon chain, the polyester or polyurethane synthesized from it has more balanced physical properties than other short-chain diols, such as ethylene glycol or propylene glycol and 1,4-butanediol. . 1,6-Hexanediol is mainly used in the production of high-quality polyurethane elastomer resin, polyurethane adhesive, polyester plasticizer, UV-curable coating, high-grade water-soluble resin coating, polycarbonate, pharmaceutical intermediates And food additives, in addition, 1,6-hexanediol is also widely used in the production of hair styling agents, gelatin and plasticizers for coating in photographic films...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/149B01J23/889B01J21/04B01J21/08B01J35/10B01J37/34B01J37/08
Inventor 崔娇英李付国赵文娟黎源王鑫马德强
Owner WANHUA CHEM GRP CO LTD
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