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Solid base catalyst for synthesizing 4-hydroxybutyl vinyl ether and preparation method and application thereof

A technology of hydroxybutyl vinyl ether and solid base catalyst, which is applied in catalyst activation/preparation, unsaturated compound addition to prepare ether, ether preparation and other directions, can solve the problems of inability to recycle, low catalytic activity, etc., and achieves low price , the effect of high catalytic activity and simple preparation process

Active Publication Date: 2018-06-22
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for the synthesis of hydroxybutyl vinyl ether by the acetylene method, the existing solid base catalysts mainly have problems such as low catalytic activity and inability to be recycled.

Method used

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  • Solid base catalyst for synthesizing 4-hydroxybutyl vinyl ether and preparation method and application thereof
  • Solid base catalyst for synthesizing 4-hydroxybutyl vinyl ether and preparation method and application thereof
  • Solid base catalyst for synthesizing 4-hydroxybutyl vinyl ether and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Weigh 0.84g Cu(NO 3 ) 2 ·3H 2 O, 0.89g KOH and 15.69g ZrOCl 2 ·8H 2 O mixed, after fully grinding, add a certain amount of deionized water and stir evenly, dry at 120°C for 6h, roast at 500°C in air atmosphere for 4h, prepare 40mL of 0.18mol / L glucose solution, add 10 % ammonia water, adjust the pH of the solution to 10, at 90°C, the CuO-K 2 O / ZrO 2 Added to the above solution, stirred and refluxed for 1h, filtered after reaction, and dried the filter cake at 60°C for 6h to obtain Cu 2 O-K 2 O / ZrO 2 solid base catalyst.

[0047] Add 30g of 1,4-butanediol and 4.5g of the above catalyst into a 100ml three-necked flask, pass through acetylene, and control the flow rate of acetylene to 0.04L / min, start stirring, heat the oil bath to 150°C, react for 9h, use The reaction solution was analyzed by gas chromatography OV-1701, and the yield of 4-hydroxybutyl vinyl ether was 67.39%, and the total yield of by-products was lower than 0.17%.

[0048] The detection conditio...

Embodiment 2

[0060] Cu(NO 3 ) 2 ·3H 2 O, KOH and ZrOCl 2 ·8H 2 The mass of O was changed to 0.28g, 0.4g and 13.08g respectively, the glucose solution was changed to ascorbic acid solution, and Cu 2 O-K 2 O / ZrO 2 solid base catalyst.

[0061] Using the evaluation conditions of Example 1, under the above evaluation conditions, the yield of 4-hydroxybutyl vinyl ether is 60.52%, and the total yield of by-products is lower than 0.41%.

Embodiment 3

[0063] Cu(NO 3 ) 2 ·3H 2 O, KOH and ZrOCl 2 ·8H 2 O to CuSO, respectively 4 ·5H 2 O, K 2 CO 3 and Zr(NO 3 ) 4 ·5H 2 O, the drying temperature was changed to 110°C, and the same method was used to prepare Cu 2 O-K 2 O / ZrO 2 solid base catalyst.

[0064] Using the evaluation conditions of Example 1, under the above evaluation conditions, the yield of 4-hydroxybutyl vinyl ether is 62.18%, and the total yield of by-products is lower than 0.36%.

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Abstract

The invention discloses a solid base catalyst for synthesizing 4-hydroxybutyl vinyl ether and a preparation method and application thereof. The catalyst disclosed by the invention adopts zirconium dioxide (ZrO2) as a carrier and double components, i.e., Cu and K, as an active center, and the percentage by mass of each component is: 1 to 15 percent of cuprous oxide (Cu2O) as an active component, 10to 35 percent of potassium oxide (K2O) and 50 to 89 percent of ZrO2 as the carrier. The preparation method is as follows: copper salt, potassium salt and zirconium salt are mixed, sufficiently ground, added with deionized water and uniformly stirred, and after drying, roasting, liquid phase reduction and other steps, the catalyst is prepared. The process of the method is simple, operability is high, industrialized production is facilitated, and the cost is low. The prepared catalyst is used for synthesizing 4-hydroxybutyl vinyl ether by the acetylene method, the yield of target product can reach 67.39 percent, and the problems of low catalytic activity and poor selectivity existing in conventional solid base catalysts are solved.

Description

technical field [0001] The invention relates to a solid base catalyst for synthesizing 4-hydroxybutyl vinyl ether, a preparation method and application thereof, and belongs to the technical field of catalyst preparation. Background technique [0002] Vinyl ether is an important class of high polymer monomers and organic synthesis intermediates. Its homopolymers and copolymers have low toxicity, odorless, low shrinkage, high strength, high adhesion, solubility, excellent flexibility and Easy to synthesize and other characteristics, it can be used as a reactive diluent in epoxy resin, acrylic resin and unsaturated polyester systems, and also used in the production of adhesives, coatings, oil viscosity modifiers, plasticizers, lubricants, Hair sprays, elastomers, foams, insecticides and surface protection materials, etc. As an intermediate in organic synthesis, vinyl ether can be used to synthesize tetramethoxypropane, γ-picoline, 2-aminopyrimidine, and glutaraldehyde, a fungi...

Claims

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Application Information

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IPC IPC(8): B01J23/78B01J37/08C07C41/08C07C43/178
CPCB01J23/002B01J23/78B01J37/088B01J2523/00C07C41/08B01J2523/13B01J2523/17B01J2523/48C07C43/178
Inventor 王永钊赵永祥吕婷婷王晶晶魏旭晖
Owner SHANXI UNIV