Catalyst for synthesizing 3-buten-1-ol through 1,4-butanediol and preparation method of catalyst

A catalyst, butanediol technology, applied in the direction of chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem that affects the purity of the product 3-buten-1-ol and other problems, to achieve the effect of easy large-scale production, less by-products, and a single type

Inactive Publication Date: 2015-05-06
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existence of these by-products will seriously affect the purity of the product 3-buten-1-ol

Method used

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  • Catalyst for synthesizing 3-buten-1-ol through 1,4-butanediol and preparation method of catalyst
  • Catalyst for synthesizing 3-buten-1-ol through 1,4-butanediol and preparation method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Measure 0.2ml of tetraethyl orthosilicate, dissolve it in 100ml of alcohol-water mixture with a volume ratio of 6:1 (concentration of tetraethyl orthosilicate is 0.008mol / L), put it in a constant temperature water bath at 60°C and stir for 10 minutes , add 0.19g of acetic acid solution, and continue to stir at constant temperature for 2h to obtain a silicon solution; weigh 21.17g of zirconyl nitrate, dissolve it in 100ml of alcohol-water mixture with a volume ratio of 6:1 (the concentration of zirconyl nitrate is 0.792mol / L) , placed in a 60°C constant temperature water bath and stirred for 1 hour to obtain a zirconium solution; the prepared zirconium solution was added to a silicon solution, placed in a 60°C water bath, stirred, gelled, and aged for 30 minutes to obtain a colloid; weigh 11.81g of Ca(NO 3 ) 2 .4H 2 O is dissolved in water and prepared as Ca at a concentration of 1 mol / L 2+ Solution, simultaneously weigh 49.53g of ammonium carbonate and dissolve in wat...

Embodiment 2

[0022] Prepare the catalyst according to the method of Example 1, replace 0.2ml tetraethyl orthosilicate with 1.1369g sodium silicate nonahydrate, change the alcohol-water volume ratio of the prepared silicon solution and zirconium solution to 4:1, and replace 0.19g acetic acid solution with 0.584g of concentrated hydrochloric acid instead, after drying, roasting, and cooling to room temperature, catalyst B was obtained.

Embodiment 3

[0024] Prepare the catalyst by the method of Example 2, change the amount of zirconyl nitrate to 20.31g, replace 11.81g calcium nitrate tetrahydrate with 8.60g calcium sulfate dihydrate, replace 49.53g ammonium carbonate with 12.19g sodium carbonate, and dry , roasting, and after cooling to room temperature, catalyst C is obtained.

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Abstract

The invention provides a catalyst for synthesizing 3-buten-1-ol through 1,4-butanediol and a preparation method of the catalyst. The catalyst is a CaO-SiO2-ZrO2 catalyst prepared by combining sol-gel with deposition-precipitation through a one-pot process, wherein the content of CaO in the catalyst is 5-25wt%, and the content of SiO2 is 0-15wt%. The preparation method comprises the following steps: hydrolyzing a silicon source, hydrolyzing a zirconium source, gelling silicon-zirconium, performing calcium source deposition-precipitation and performing aftertreatment. The preparation method is simple, the operation is convenient, and large-scale production is easily realized. According to the prepared catalyst, 1,4-butanediol is catalyzed to perform selective dehydration to synthesize 3-buten-1-ol under the reaction condition of the temperature of 300-400 DEG C, the yield is 90 percent or above, and fewer reaction byproducts are produced and are easy to separate.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for catalyzing the selective dehydration of 1,4-butanediol to synthesize 3-buten-1-ol and a preparation method thereof. Background technique [0002] 3-buten-1-ol (BTO) is a kind of enol compound with double bond and hydroxyl group. It is active and can participate in various reactions. As a high value-added fine chemical, it is widely used in fine chemical fields such as plastic lenses, food flavors and petroleum processing, especially in the pharmaceutical field for the synthesis of new drugs of heterocyclic derivatives, such as: anti-tumor drugs, Anti-AIDS drugs and anti-proliferation drugs, etc. In recent years, with the rapid increase in the demand for anti-tumor drugs such as pemetrexed disodium, the market demand for BTO has also increased sharply. [0003] So far, the methods for synthesizing 3-buten-1-ol mainly include: propylene formaldehyde addition method, 3,4-epoxy-1-butene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/02C07C33/025C07C29/60
Inventor 张因赵丽丽秦晓琴赵永祥张鸿喜连晓宁
Owner SHANXI UNIV
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