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Method for preparing furandimethanol diether by catalytic furandimethanol etherification

A technology of furandimethanol diether and furandimethanol, which is applied in the field of preparation of furandimethanol diether, can solve the problems of difficult product separation, many side reactions, and low yield of diether products, and achieve improved diffusion limit, reduction of The effect of by-product formation

Active Publication Date: 2020-08-11
沈阳开拓利思科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2,5-DMF has the characteristics of high energy density, high octane number, etc., but it is only suitable as a gasoline component, and there is a molecular weight loss of nearly 30% during the conversion process from HMF to 2,5-DMF, so the atom economy Poor sex
In general, the main problems in the current process of preparing BRMF by etherification of BHMF are: the yield of the target diether product (BRMF) is not high, which increases the cost of preparation, and more importantly, a large amount of by-products generated It seriously affects the life of the catalyst and brings great difficulties to the subsequent product separation
[0005] Chinese patent 201110401610.9 discloses "a method for preparing furandimethanol dialkyl ether from sugar", which uses a microporous silica-alumina molecular sieve as a catalyst for the etherification reaction. Or the diffusion limitation of product, thereby cause side reaction more, the yield of diether product is generally low (less than 50%), follow-up separation and purification difficulty is very big

Method used

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  • Method for preparing furandimethanol diether by catalytic furandimethanol etherification
  • Method for preparing furandimethanol diether by catalytic furandimethanol etherification
  • Method for preparing furandimethanol diether by catalytic furandimethanol etherification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A preparation method for furandimethanol dimethyl ether, comprising the steps of:

[0039] S1. Get 15g of hydrothermally synthesized microporous ZSM-5 molecular sieve (for example: produced by Tianjin Nanhua Catalyst Co., Ltd.) (http: / / www.nkcatalyst.com / );

[0040] S2. Add 300ml of 0.5M HCl solution, stir and react at 50°C for 6h, filter, wash with deionized water, and dry to obtain a hierarchical porous silica-alumina molecular sieve (HP-ZSM-5-1);

[0041] S3. Take 5g of HP-ZSM-5-1 and put it into a 10ml fixed-bed reactor;

[0042] S4. The temperature of the fixed-bed reactor is raised to 65°C, and a mixed liquid is introduced. The liquid composition is: 10mol% BHMF, 90mol% methanol, and the liquid flow rate is 1.0h -1 , the product was detected by HPLC, and the yield of furandimethanol dimethyl ether (BMMF) was 99%.

[0043] figure 1 The BET test results of the HP-ZSM-5-1 sample are given, figure 2 The HPLC analysis result spectrum is given.

Embodiment 2

[0045] A preparation method for furandimethanol dimethyl ether, comprising the steps of:

[0046] S1, get 20g of hydrothermally synthesized microporous ZSM-5 molecular sieves;

[0047] S2. Add 300ml of 1M NaOH solution, stir and react at 60°C for 8h, filter, wash, and dry to obtain a hierarchical porous silica-alumina molecular sieve (HP-ZSM-5-2).

[0048] S3, get 5g HP-ZSM-5-2 and pack in 10ml fixed-bed reactor,

[0049] S4. The temperature of the fixed-bed reactor is raised to 50°C, and a mixed liquid is introduced. The liquid composition is: 10% BHMF, 90% ethanol, and the liquid flow rate is 0.5h -1 , the product was detected by HPLC, and the yield of furandimethanol diethyl ether (BEMF) was 97%.

Embodiment 3

[0051] A preparation method for furandimethanol dimethyl ether, comprising the steps of:

[0052] S1, get 10g of hydrothermally synthesized microporous Beta molecular sieve (for example: produced by international catalyst company zeolystinternational), http: / / www.zeolyst.com;

[0053] S2. Add 300ml of 0.5M HCl solution, stir and react at 60°C for 6h, filter, wash, and dry to obtain a hierarchical porous silica-alumina molecular sieve (HP-Beta-1).

[0054] S3, get 5g HP-Beta-1 and pack in 10ml fixed-bed reactor,

[0055] S4. The temperature of the fixed-bed reactor is raised to 60°C, and a mixed liquid is introduced. The liquid composition is: 10% BHMF, 90% methanol, and the liquid flow rate is 1h -1 , the product was detected by HPLC, and the yield of furandimethanol dimethyl ether (BMMF) was 98%.

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Abstract

The invention discloses a method of catalyzing etherification of furandimethanol to prepare furandimethanol diether, comprising the steps of S1, selecting microporous silicon-aluminum molecular sieve;S2, adding an acid or alkali to carry out treatment to form multilevel-pore silicon-aluminum molecular sieve with micropores and mesopores; S3, filling a fixed-bed reactor with the multilevel-pore silicon-aluminum molecular sieve of step S2; S4, introducing reaction raw liquid BHMF (2,5-bis(hydroxymethyl)furan) and alcohol to carry out etherification to obtain the finished product. The multilevel-pore silicon-aluminum molecular sieve prepared herein is applicable to esterification from 2,5-furandimethanol to 2,5-furandimethanol diether; compared with common microporous silicon-aluminum molecular sieves, the multilevel-pore silicon-aluminum molecular sieve can effectively improve the diffusion limits of a reaction process; the generation of byproducts is greatly decreased; BRMF yield reaches 85-99%, and subsequent separation is not required to acquire the finished 2,5-furandimethanol diether with purity of 95% and above after non-reacted alcohol is removed by simple distillation.

Description

technical field [0001] The invention relates to a preparation method of furandimethanol diether, in particular to a method for preparing furandimethanol diether by catalyzing the etherification of furandimethanol. Background technique [0002] With the rapid development of the global economy, the contradiction between the dwindling traditional oil resources and the increasing demand for fossil fuels is becoming more and more prominent. The use of renewable biomass resources to prepare fuels will effectively reduce the dependence on fossil fuels, thereby alleviating the above-mentioned contradictions to a certain extent, so it is of great significance. The preparation of various bio-based liquid fuels by using the direct products of photosynthesis—carbohydrates (especially six-carbon sugar carbohydrates) is the current focus of research and development at home and abroad, such as industrialized fuel ethanol and bio-fermentation to prepare bio-based chemicals Wait. Convertin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/42
CPCC07D307/42
Inventor 闫海生尹荃
Owner 沈阳开拓利思科技有限公司
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