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A kind of dehydrogenation catalyst and the method for manufacturing delta-valerolactone

A dehydrogenation catalyst, copper-based catalyst technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve the problem of short service life of catalysts, difficult product separation, The catalyst is easy to sinter and other problems, so as to improve the selectivity, simplify the product separation process, and achieve the effect of good physical structure and performance.

Active Publication Date: 2020-07-28
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The existing methods for preparing δ-valerolactone require the dehydrogenation reaction of 1,5-pentanediol to be completed under a specific high temperature condition, and the reaction is guaranteed to be a gas phase dehydrogenation reaction. If the temperature is lower, the reaction conversion rate will However, under the high temperature conditions introduced by the above-mentioned patents, although a good conversion rate can be achieved, there are by-products such as n-valeric acid in the reaction product, the product is not easy to separate, the catalyst is easy to sinter, and the catalyst has short service life.

Method used

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  • A kind of dehydrogenation catalyst and the method for manufacturing delta-valerolactone
  • A kind of dehydrogenation catalyst and the method for manufacturing delta-valerolactone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Catalyst preparation:

[0043] Weigh 102g of Al 2 o 3 (1mol), mix it with 100ml of aqueous urea (CO(NH 2 ) 2 : 0.005mol) mixed evenly, placed in a 2L autogenous autoclave, kept at 90°C for 24h, then added 700ml of Mg(NO 3 ) 2 (0.02mol) aqueous solution, and heated up to 130°C, kept for 24h, washed with deionized water, dried at 120°C, and then roasted at 450°C for 8h to obtain LDHs-modified alumina composite MaterialLDHs-Al 2 o 3 .

[0044] Prepare a certain concentration of Cu(NO 3 ) 2 (where Cu(NO 3 ) 2 The amount of substance is an aqueous solution of 0.085mol), and then 100g of the LDHs-Al prepared above 2 o 3 into Cu(NO 3 ) 2 After fully shaken in the aqueous solution, place it in a water bath constant temperature shaker for 24 hours, keep the temperature of the water bath at about 70°C during this period, and shake at a rate of 130-140r / min. The obtained sample was washed 3-5 times with deionized water at room temperature, dried at 120°C, and then ...

Embodiment 2

[0051] Catalyst preparation:

[0052] With embodiment 1, difference is that alkaline substance CO(NH 2 ) 2 The dosage is 0.014mol, Mg(NO 3 ) 2 The dosage is 0.08mol, Cu(NO 3 ) 2 The dosage is 0.42mol, the prepared catalyst precursor is 131.2g, and the estimated active component copper loading is 23.7%.

[0053] Preparation of δ-valerolactone:

[0054] Same as in Example 1, the difference is that the carrier gas is replaced by hydrogen, and the reaction conditions are replaced by an absolute pressure of 0.009 MPa and 240°C. Intermittent sampling is carried out GC analysis to reaction liquid, can find out that after reaction carries out 20h, reaction enters steady state, and wherein reaction conversion rate reaches 99.6%, δ-valerolactone selectivity reaches 96.5%, and n-valeric acid is not found in by-product. After the device has been continuously operated for 1000 hours, there is no significant difference between the composition of the reaction liquid and the compositio...

Embodiment 3

[0056] Catalyst preparation:

[0057] With embodiment 1, difference is that alkaline substance CO(NH 2 ) 2 The dosage is 0.01mol, Mg(NO 3 ) 2 The dosage is 0.05mol, Cu(NO 3 ) 2 The dosage is 0.22mol, the prepared catalyst precursor is 116.1g, and the estimated active component copper loading is 13.9%.

[0058] Preparation of δ-valerolactone:

[0059] Same as in Example 1, the difference is that the carrier gas is replaced by nitrogen, and the reaction conditions are replaced by an absolute pressure of 0.005 MPa and 220°C. Intermittent sampling was carried out on the reaction liquid for GC analysis. It can be seen that after the reaction was carried out for 18 hours, the reaction entered a steady state, wherein the reaction conversion rate reached 99.9%, and the δ-valerolactone selectivity reached 98.5%. After the device has been continuously operated for 500 hours, there is no significant difference between the composition of the reaction liquid and the composition afte...

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Abstract

The invention provides a dehydrogenation catalyst and a method for producing δ-valerolactone, which solves the shortcomings of other methods such as high reaction temperature and easy deactivation of the catalyst, and has the advantages of low reaction temperature, long catalyst life, and high reaction conversion rate. High selectivity and other advantages, suitable for industrial production. Specifically, under negative pressure conditions, 1,5-pentanediol is used as a raw material and a carrier gas is mixed and then sequentially entered into a vaporizer and a reactor filled with a dehydrogenation catalyst. At a reaction temperature of 170-250°C, Under the action of dehydrogenation catalyst, 1,5-pentanediol is converted into δ-valerolactone, wherein the dehydrogenation catalyst is prepared by impregnation method, and the carrier is aluminum oxide whose surface is modified by layered double metal hydroxides (LDHs) , the active component is copper.

Description

technical field [0001] The invention relates to a dehydrogenation catalyst and a method for producing δ-valerolactone. Background technique [0002] δ-valerolactone, also known as 1,5-valerolactone, delta-valerolactone, tetrahydro-2H-2-pyrone, tetrahydro-o-pyrone, tetrahydrocoumarin, the English name is Delta -Valerolactone, abbreviated as DVL, is a cyclic lactone compound similar to caprolactone, with a molecular weight of 100.12, a boiling point of 230°C, and a molecular formula of C 5 h 8 o 2 , a colorless transparent liquid at room temperature. The specific structural formula is as follows. [0003] [0004] δ-valerolactone is a multi-purpose chemical intermediate, and it is used in different fields, mainly used to replace caprolactone in ink and coating additives, and valerolactone is used in the production of ink and coating additives instead of caprolactone Compared with the products produced only with caprolactone, the inks and coatings of our products have t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D309/30B01J23/72B01J35/10
CPCC07D309/30B01J23/002B01J23/72B01J2523/00B01J35/60B01J2523/17B01J2523/22B01J2523/31
Inventor 刘运海胡江林赵荣刚宋延方杨洋于学丽陈长生曾伟杨恒东丁可王坤黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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