Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

A kind of method for synthesizing 1,6-hexanediol by gas-phase hydrogenation of dimethyl adipate

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

Active Publication Date: 2011-12-07
WANHUA CHEM GRP CO LTD +1
View PDF13 Cites 10 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of method for synthesizing 1,6-hexanediol by gas-phase hydrogenation of dimethyl adipate
  • A kind of method for synthesizing 1,6-hexanediol by gas-phase hydrogenation of dimethyl adipate
  • A kind of method for synthesizing 1,6-hexanediol by gas-phase hydrogenation of dimethyl adipate

Examples

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 later 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 calci...

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 0 di...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
poweraaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for synthesizing 1,6-hexanediol by gas-phase hydrogenation of dimethyl adipate. The preparation of the hydrogenation catalyst used in the method comprises the following steps: adding a mesoporous silicon oxide carrier and a copper-containing Aqueous salt solution, stirred, evaporated to dryness by microwave, dried by microwave and calcined to obtain hydrogenation catalyst. In addition, the preparation of the protective bed used to remove the impurity gas in hydrogen in the method of the present invention comprises the following steps: active carbon carrier, and alkali metal salt or / and alkaline earth metal calcium salt are formulated into an aqueous solution in proportion, stirred, microwave evaporated to dryness, microwave dried Roasting under the protection of an inert gas; a high-performance guard bed is obtained, which contains: 5-90wt% activated carbon, 10-95wt% potassium oxide and calcium oxide, and the method of the invention greatly improves the physical properties and catalytic performance of the catalyst.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com