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Preparation method of 2, 5-tetrahydrofuran dimethanol

A technology of tetrahydrofuran dimethanol and furan dimethanol, which is applied in the field of preparation of 2,5-tetrahydrofuran dimethanol, can solve the problems of laboriousness, low product concentration, slow fermentation process, etc., and achieve easy large-scale implementation, easy post-processing, fast The effect of reaction speed

Inactive Publication Date: 2020-06-05
ZHEJIANG SUGAR ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main method of traditional preparation of 2,5-tetrahydrofuran dimethanol is microbial method, but this method has a slow fermentation process, uncontrollable conversion process, low conversion rate and low product concentration, which seriously affects the scale. And the products required for separation and production are usually extremely complicated, and it is also a difficult problem to upgrade the level to high capacity / or reduce the number of reactions
At the same time capacity is used at scale. Fermentation processes generate considerable waste streams, which can be quite laborious to dispose of in a renewable manner.

Method used

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  • Preparation method of 2, 5-tetrahydrofuran dimethanol
  • Preparation method of 2, 5-tetrahydrofuran dimethanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Add 10g of BHMF and 600ml of absolute ethanol into a beaker, and stir evenly at room temperature. The concentration of the ethanol solution of BHMF is 1.05mM;

[0057] (2) Transfer the solution prepared in step (1) to a 1000ml autoclave. Add 0.25g of 5wt% Pd / C into the reactor, and the mass ratio of the substrate BHMF to the catalyst is 40:1;

[0058] (3) Close the lid of the autoclave, start stirring with 1000rpm, after three vacuum / nitrogen cycles, make the autoclave at 2MpaH 2 The pressure was increased and the temperature was raised to 50°C. After 2 hours, the hydrogen pressure was raised to 4Mpa and the temperature was raised to 70°C. Autoclave continued to keep stirring under this condition for 2 hours;

[0059] (4) After cooling to room temperature, the pressure was released, and the contents in the autoclave were analyzed by GC, and the results are shown in Table 1.

[0060] The reaction result of table 1 embodiment 1

[0061] Example THFDM y...

Embodiment 2

[0063] (1) Add 5g of BHMF and 600ml of absolute ethanol in a beaker, stir evenly at room temperature, wherein the concentration of the ethanol solution of BHMF is 2.1mM;

[0064] (2) Transfer the solution prepared in step (1) to a 1000ml autoclave. Add 0.25g of 5wt% Pd / C into the reactor, and the mass ratio of the substrate BHMF to the catalyst is 40:1;

[0065] (3) Close the lid of the autoclave, start stirring with 1000rpm, after three vacuum / nitrogen cycles, make the autoclave at 2MpaH 2 The pressure was lowered and the temperature increased to 50°C. After 2 hours, the hydrogen pressure increased to 4 MPa, and the temperature increased to 70°C. The autoclave was continued under these conditions with stirring for an additional 2 hours.

[0066] (4) After cooling to room temperature, the pressure was released, and the contents in the autoclave were analyzed by GC, and the results are shown in Table 2.

[0067] The reaction result of table 2 embodiment 2

[0068] ...

Embodiment 3

[0071] (1) Add 10g of BHMF and 600ml of absolute ethanol into a beaker, and stir evenly at room temperature. The concentration of the ethanol solution of BHMF is 0.525mM.

[0072] (2) Transfer the solution prepared in step (1) to a 1000ml autoclave. Add 0.125g of 5wt% Pd / C into the reactor, and the mass ratio of the substrate BHMF to the catalyst is 80:1.

[0073] (3) Close the lid of the autoclave, start stirring with 1000rpm, after three vacuum / nitrogen cycles, make the autoclave at 2MpaH 2 The pressure was lowered and the temperature increased to 50°C. After 2 hours, the hydrogen pressure increased to 4 MPa, and the temperature increased to 70°C. The autoclave was continued under these conditions with stirring for an additional 2 hours.

[0074] (4) After cooling to room temperature, the pressure was released, and the contents in the autoclave were analyzed by GC, and the results are shown in Table 3.

[0075] The reaction result of table 3 embodiment 3

[0076] ...

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Abstract

The invention provides a preparation method of 2, 5-tetrahydrofurandimethanol, which at least comprises the following steps: contacting a raw material containing 2, 5-furandimethanol with a catalyst,and reacting in a hydrogen-containing atmosphere to obtain 2, 5-tetrahydrofurandimethanol; wherein the catalyst comprises a carrier and an active component, the active component is loaded on the carrier; wherein the active component comprises active metal elements; wherein the active metal elements comprise at least one of palladium, platinum, ruthenium, nickel and rhodium; and the carrier comprising carbon material. The method for preparing the 2, 5-tetrahydrofuran dimethanol is high in activity and high in selectivity, and the reaction raw material 2,5-tetrahydrofuran dimethanol can also beprepared from 5-hydroxymethylfurfural which is a renewable source.

Description

technical field [0001] The application relates to a preparation method of 2,5-tetrahydrofuran dimethanol, which belongs to the field of chemical industry. Background technique [0002] In recent years, in the face of deteriorating environmental problems, cheap and environmentally friendly materials have become more and more in demand, with particular attention being paid to materials that can be obtained from renewable sources, i.e. by biological activities such as planting, farming or harvesting. The resulting material. [0003] In the field of polymer materials, it is widely used as a key industrial material, under the modern industry composed of synthetic plastics, fibers, rubber, coatings and adhesives, etc., 2,5-tetrahydrofuran dimethanol, as a core can be Useful precursors for the synthesis of industrially useful chemicals such as drugs, herbicides, stabilizers, bioplastics, and polymers have also received considerable attention. The main method of traditional prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/42
CPCC07D307/42
Inventor 王磊方乾全金海涛张建杨勇卢国文
Owner ZHEJIANG SUGAR ENERGY TECH CO LTD
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