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Method and supported catalyst for preparing 4-alkoxyvalerate by liquid-phase hydrogenation

A technology of supported catalyst and alkoxyvalerate, which is applied in the direction of metal/metal oxide/metal hydroxide catalyst, molecular sieve catalyst, catalyst activation/preparation, etc., can solve the problem of high cost and achieve simple operation and high energy efficiency. The effect of low consumption and high yield of target product

Active Publication Date: 2021-10-15
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the method proposed by the above-mentioned prior art, the catalytic reaction to prepare 4-alkoxyvaleric acid esters with gamma-valerolactone as a starting material needs to be carried out at a relatively high temperature (greater than 160° C.), and high temperatures can easily lead to excessive The reaction produces other by-products
In addition, using gamma-valerolactone as a raw material has a high cost, and the yield of the product 4-alkoxyvalerate needs to be further improved.

Method used

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  • Method and supported catalyst for preparing 4-alkoxyvalerate by liquid-phase hydrogenation
  • Method and supported catalyst for preparing 4-alkoxyvalerate by liquid-phase hydrogenation
  • Method and supported catalyst for preparing 4-alkoxyvalerate by liquid-phase hydrogenation

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Experimental program
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Effect test

Embodiment 1

[0042] The preparation of embodiment 1 supported palladium catalyst:

[0043] Disperse the carrier activated carbon evenly in the aqueous solution, and take an appropriate amount of PdCl according to the required mass ratio 2 The solution was added to the carrier aqueous solution, stirred evenly at room temperature and then adjusted to pH Pd 2+ Precipitation is complete, add sodium borohydride (Pd 2+ : Sodium borohydride=1:15, mol ratio) and continued to stir for 2 hours. The gained solution is filtered and dried, and the supported palladium catalyst is prepared, and the palladium metal nanoparticles are evenly distributed on the carrier (as attached figure 1 shown).

[0044]Sodium borohydride is used as reducing agent in this embodiment. In the method of the present invention, in other embodiments, the reducing agent can also be hydrazine hydrate or hydrogen, both of which can achieve the same effect.

Embodiment 2

[0045] Example 2 Loaded Pd-SiO 2 Preparation of / C catalyst:

[0046] First, weigh 1g of activated carbon, disperse it evenly in the ethanol solution, measure the required amount of tetraethyl orthosilicate as the silicon source, drop it into the activated carbon solution drop by drop, stir for 12 hours, and wait until the tetraethyl orthosilicate is completely hydrolyzed. Suction filtration, drying in an oven at 80°C for 12h, and then taking it out and putting it into a tube furnace for calcination at 500°C for 2h with a heating rate of 3°C / min. Get SiO 2 / C, with this as a carrier, the same method as in Example 1 supports metal palladium.

[0047] In this example, tetraethyl orthosilicate was used to prepare the silica-modified carrier. In other embodiments, supports modified by common oxides such as cerium oxide, aluminum oxide, titanium oxide, and niobium oxide can also be prepared, and the same method is used to prepare supported catalysts.

[0048] Sodium borohydride...

Embodiment 3

[0049] Embodiment 3 ethyl levulinate hydrogenation reaction

[0050] Use the catalyst prepared in Example 1 to prepare ethyl 4-ethoxyvalerate by liquid-phase hydrogenation of ethyl levulinate, and load catalyst 0.5Pd / C (Pd:C=0.5% in a 100ml reactor lining) , mass ratio), the consumption is about 15% (accounting for ethyl levulinate mass percent), adding raw material ethyl levulinate, solvent ethanol, the solvent dilution ratio is about 30:1 (ethanol: ethyl levulinate, volume ratio), the reaction temperature was 140°C, and the reaction was carried out for 4 hours under a hydrogen pressure of 0.5 MPa, the conversion rate of ethyl levulinate was 16%, and the selectivity of the target product was >99%.

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Abstract

The invention discloses a method for hydrogenating 4-alkoxyvaleric acid esters by using biomass-derived platform compounds levulinic acid esters as raw materials. The method adopts a supported metal palladium catalyst and H-beta molecular sieves to carry out one-step hydrogenation etherification of levulinic acid ester compounds in an alcoholic solution to obtain the described 4-alkoxyvaleric acid ester, and the conversion rate of raw materials is >99% %, the product selectivity is as high as 96%. The invention also discloses the preparation method of the supported catalyst and its application in the hydrogenation reaction of levulinic acid ester. The technical route proposed by the invention has the beneficial characteristics of simple and convenient operation, high yield of target product and low energy consumption.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a method for preparing 4-alkoxyvalerate by liquid-phase hydrogenation, in particular to a method for directly hydrogenating levulinic acid ester compounds as raw materials to produce high-purity 4-alkoxy A method for valerate esters, and the supported catalysts required for the process. Background technique [0002] Biomass-based ether compounds are widely used and can be directly used as fuel additives or intermediates in the pharmaceutical industry. 4-Alkoxyvalerate, as an ether compound of biomass derivatives, has potential application value in the production and application fields of petrochemical products, such as solvents, spices, food additives and transportation fuel additives. The currently reported preparation route is mainly an acid-catalyzed etherification method. Generally, γ-valerolactone is used as a raw material, and 4-alkoxyvaleric acid esters are synthesized und...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/708C07C67/31B01J23/44B01J29/72B01J37/03B01J37/16B01J37/08
Inventor 关业军崔倩倩龙银双吴鹏
Owner EAST CHINA NORMAL UNIV
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