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 deactivated lead-containing guard bed is also a difficult problem

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

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1. Preparation of guard bed

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

[0046] 5 g of pretreated coal-based activated carbon was impregnated in 25 mL of K 2 CO 3 and CaCO 3 In a solution of 1 mol / liter respectively, stir in a stirrer for 4 hours, then evaporate to near dryness in a microwave oven with 500W intermittent power, and cool to room temperature; 2 CO 3 and CaCO 3 Put the activated carbon into a quartz glass tube with a sieve plate, and pass nitrogen protection under the tube to prevent the activated carbon from oxidizing and burning. Place the quartz tube in a reaction furnace for calc...

Embodiment 2

[0055] 1. Preparation of guard bed

[0056] The coal-based activated carbon after the pretreatment of 5 grams of embodiment 1 is impregnated in 25 milliliters of K 2 CO 3 and CaCO 3 In a solution of 3mol / L respectively, stir in a stirrer for 4 hours, then evaporate to nearly dryness in a microwave oven with 500W intermittent power, dry for 30 minutes under microwave radiation (120°C), and cool to room temperature; 2 CO 3 and CaCO 3 The activated carbon is loaded into a quartz glass tube with a sieve plate, and the tube is protected by nitrogen to prevent the oxidative combustion of the activated carbon. The quartz tube is placed in a reaction furnace at 350°C for 4 hours. After the calcination, continue to cool to room temperature with nitrogen, and then granulate , that is, 30.7wt% activated carbon, 43.5wt% K 2 A guard bed of O and 25.8 wt% CaO.

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

[0058] Tetraethyl orthosilicate (TEOS), cetyltrimethylammonium bromide (CTAB), s...

Embodiment 3

[0065] 1. Preparation of guard bed:

[0066] The coal-based activated carbon after the pretreatment of 5 grams of embodiment 1 is impregnated in 25 milliliters of K 2 CO 3 and CaCO 3 In the solutions of 1 mol / L and 3 mol / L respectively, stir in a stirrer for 4 hours, then evaporate to nearly dryness in a microwave oven with 500W intermittent power, dry for 30 minutes under microwave radiation (120°C), and cool to room temperature; K 2 CO 3 and CaCO 3 Put the activated carbon into a quartz glass tube with a sieve plate, and pass nitrogen protection under the tube to prevent the activated carbon from oxidizing and burning. Place the quartz tube in a reaction furnace for calcination at 350°C for 4 hours. After the calcination, continue to pass nitrogen to cool to room temperature, granulate and fill , that is, 43.2wt% activated carbon, 20.4wt% K 2 A guard bed of O and 36.4 wt% CaO.

[0067] 2. Preparation of hydrogenation catalyst

[0068] 16.0 g Cu(NO 3 ) 2 ·3H 2 O di...

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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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