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Preparation technology and device of cyclohexanedimethanol

A technology of cyclohexane dimethanol and dialkyl cyclohexene dicarboxylate, which is applied in the field of preparation of cyclohexane dimethanol, which can solve the problem of uneven catalyst distribution, slow liquid phase replacement, and limited liquid holding capacity of sieve trays And other issues

Active Publication Date: 2018-05-29
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the structure of the tray is simple, the liquid holding capacity of the sieve tray is limited, the catalyst is unevenly distributed, and the catalyst wears and leaks greatly, which affects the plate efficiency and reaction effect.
CN01114953 discloses a catalytic rectification tray with a gas riser, the catalyst is scattered at the bottom of the tray, the gas riser is higher than the height of the catalyst, and gas-liquid mass transfer elements such as float valves and bubble caps are installed on the upper part of the gas riser. The liquid flows in one direction in the horizontal direction, the catalyst is unevenly distributed, the reaction liquid cannot pass through the catalyst bed, there are problems such as slow liquid phase replacement, stagnation zone and dead zone, and the reaction effect is affected

Method used

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  • Preparation technology and device of cyclohexanedimethanol
  • Preparation technology and device of cyclohexanedimethanol
  • Preparation technology and device of cyclohexanedimethanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0093] Preparation of Hollow Molecular Sieve Supported Heteropolyacid Catalyst

[0094] Solution configuration: configure tetrapropylammonium hydroxide and NaNO with concentrations of 0.3 and 0.3 mol / L respectively 3 of aqueous solution. Take 1 kg of pure silicon-type molecular sieve S-1 (Dalian University of Technology Qiwangda Chemical Technology Co., Ltd.) with a particle diameter of 120 nm, put it in 5 L of the alkali solution configured above, and keep stirring at 170 ° C for 24 hours; Wash with distilled water, then dry at 100°C under normal pressure for 2 hours, and bake at 500°C for 4 hours in an air atmosphere. Na with a molar ratio of 12:1 2 WO 4 and Na 2 SiO 3 A total of 20g was dissolved in 5L of distilled water, and the above-prepared molecular sieve was placed in the heteropolyacid solution, and the temperature was controlled at 90°C. With stirring, phosphoric acid was continuously added dropwise until the pH value = 1, and the stirring reaction was continue...

Embodiment 2

[0098] Preparation of Hollow Molecular Sieve Supported Heteropolyacid Catalyst

[0099] Solution configuration: configure tetrapropylammonium hydroxide and NaNO with concentrations of 0.3 and 0.3 mol / L respectively 3 of aqueous solution. Take 1 kg of pure silicon-type molecular sieve S-1 (Dalian University of Technology Qiwangda Chemical Technology Co., Ltd.) with a particle diameter of 300 nm, place it in 5 L of the alkali solution configured above, and keep stirring at 170 ° C for 24 hours; Wash with distilled water, then dry at 100°C under normal pressure for 2 hours, and bake at 500°C for 4 hours in an air atmosphere. Na with a molar ratio of 12:1 2 WO 4 and Na 2 SiO 3 A total of 40g was dissolved in 5L of distilled water, and the above-prepared molecular sieve was placed in the heteropoly acid solution, and the temperature was controlled at 90°C. With stirring, phosphoric acid was continuously added dropwise until the pH value = 1, and the stirring reaction was conti...

Embodiment 3DA

[0102] Embodiment 3DA synthesis

[0103] A drainage loop reactor with a volume of 2L is used, the inner diameter of the loop is 10mm, and the diameter of the drainage nozzle is 0.5mm. Add 500ml of dimethyl muconate prepared in the above steps and 5ml of methanol into a 2L drainage loop reactor, fill with ethylene to 3.0MPa at room temperature, preheat to 120°C, maintain the temperature of the system and then fill with CO 2 To 8MPa and add ethylene to maintain the system pressure, react for 10h, take a sample and send it to GC analysis, the conversion rate of dimethyl muconate is about 97%, and the yield of the product cyclohexene dicarboxylate is 92.4% based on dimethyl muconate .

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Abstract

The invention discloses a preparation technology and device of cyclohexanedimethanol. Cyclohexanedimethanol is prepared from biomaterial muconic acid as a raw material through an esterification reaction, a Diels-Alder reaction and a hydrogenation reaction. The complete biomaterial muconic acid is used in the route, use of petrochemical resources is significantly reduced, hydrogen consumption is low, and the reaction yield is high.

Description

technical field [0001] The invention relates to a process and device for preparing cyclohexanedimethanol, in particular to a new method and device for preparing cyclohexanedimethanol based on bio-based muconic acid as a raw material. technical background [0002] Cyclohexanedimethanol (CHDM) is an important aliphatic dihydric alcohol. Due to its cycloalkane structure, it can obtain higher crystallinity and durability than commonly used aliphatic dihydric alcohols when synthesizing polyester. Temperature performance, which has developed very rapidly in recent years, is a polyester raw material diol urgently recommended by the country's 13th Five-Year Plan. The traditional industrial preparation route of CHDM is to prepare terephthalic acid based on fossil raw materials through esterification and hydrogenation. The main raw material of this traditional route is terephthalic acid (PTA), which is a large-tonnage petrochemical product, which is mainly used to synthesize polyeste...

Claims

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Application Information

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IPC IPC(8): C07C29/149C07C35/08C07C67/08C07C69/602B01J29/03
CPCB01J29/03B01J2229/186C07C29/149C07C67/08C07C67/347C07C35/08C07C69/75C07C69/602Y02P20/10Y02P20/54
Inventor 何岩乔小飞刘俊贤宋明炎董龙跃赵一鸣黎源
Owner WANHUA CHEM GRP CO LTD
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