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Preparation method and application for S2O8<2->/ZrO2-SiO2 solid acid catalyst

A solid acid catalyst and carrier technology, applied in the preparation of organic compounds, physical/chemical process catalysts, carboxylate preparation, etc., can solve the problems of easy-to-corrosion equipment, many side reactions, easy coloring of products, etc., and achieve good selectivity , High catalytic activity, avoiding the effect of high equipment requirements

Inactive Publication Date: 2018-12-07
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The direct esterification method mostly uses a homogeneous acid as a catalyst, but this leads to problems such as easy-to-corrosion equipment, many side reactions, easy coloring of the product, and difficulty in separating the catalyst from the product.

Method used

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  • Preparation method and application for S2O8&lt;2-&gt;/ZrO2-SiO2 solid acid catalyst
  • Preparation method and application for S2O8&lt;2-&gt;/ZrO2-SiO2 solid acid catalyst
  • Preparation method and application for S2O8&lt;2-&gt;/ZrO2-SiO2 solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Dissolve 16.10 g of zirconium oxychloride octahydrate with 72.92 g of deionized water, add it into a three-necked flask equipped with mechanical stirring, stir vigorously and adjust the pH to about 2 with concentrated ammonia water, add 20.03 g of silica sol, and crystallize at 75 ° C Add concentrated ammonia water until complete precipitation, crystallize for 3 hours, filter with suction to obtain a solid precipitate, wash with deionized water 3 times, each time 200mL, dry at 100°C to constant weight, grind, and Calcined in the furnace at 500°C for 5h to obtain ZrO 2 -SiO 2 The carrier was then impregnated with 29.53g of 1.5mol / L ammonium persulfate for 24h, dried and ground, and calcined in a muffle furnace at 500°C for 5h to obtain S 2 o 8 2- / ZrO 2 -SiO 2 A solid acid catalyst, wherein the molar ratio n (Zr:Si) of zirconium to silicon is 1:2.

[0022] This catalyst is used to catalyze the direct esterification reaction that the raw material molar ratio is MAA:...

Embodiment 2

[0024] The basic preparation method is the same as in Example 1, and the difference is that the zirconium oxychloride octahydrate add-on is 14.49g, and the silica sol add-on is 27.04g, wherein said zirconium, silicon molar ratio n (Zr: Si) is 1: 3.

[0025] This catalyst is used to catalyze the direct esterification reaction that the raw material molar ratio is MAA:2EY=1.3:1, and the catalyst consumption is 5% of raw material gross mass, and the water carrying agent consumption is 15% of raw raw material gross mass, and the polymerization inhibitor consumption is 0.5% of the total mass of raw materials, the reaction temperature is 155°C, the reaction time is 8h, the conversion rate of 2EY is 92.68%, and the yield of MED is 91.92%.

Embodiment 3

[0027] The basic preparation method is the same as in Example 1, and the difference is that the zirconium oxychloride octahydrate add-on is 12.88g, and the silica sol add-on is 32.04g, wherein said zirconium, silicon molar ratio n (Zr: Si) is 1: 4.

[0028] This catalyst is used to catalyze the direct esterification reaction that the raw material molar ratio is MAA:2EY=1.3:1, and the catalyst consumption is 5% of raw material gross mass, and the water carrying agent consumption is 15% of raw raw material gross mass, and the polymerization inhibitor consumption is 0.5% of the total mass of raw materials, the reaction temperature is 155°C, the reaction time is 8h, the conversion rate of 2EY is 99.58%, and the yield of MED is 93.81%.

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Abstract

The invention relates to a preparation method and application for a S2O8<2-> / ZrO2-SiO2 solid acid catalyst. The preparation method includes adjusting the pH value of a soluble zirconium salt solution,and adding silica sol under heating and violent stirring; filtering sediment after crystallization is performed for a certain time; removing soluble salt by washing with deionized water; performing drying and roasting to obtain a carrier; and performing soaking for a certain time by using an ammonium persulfate solution with a certain concentration after grinding so that a catalyst can be prepared through drying and roasting. The catalyst is used for catalyzing the esterification of methacrylic acid (MAA) with diethylene glycol monoethyl ether (2EY) to synthetize di(ethylene glycol) ethyl ether methacrylate (MED), the conversion rate of the 2EY is 99.58%, and the yield of the MED is 93.81%. The advantages of the preparation method are that the catalyst has a strong acid active center, cancatalyze the direct esterification of the methacrylic acid with alcohol, and is high in catalytic activity; and the catalyst is easy to separate from products and can be repeatedly used, and belongsto an environmentally friendly green chemical catalyst.

Description

technical field [0001] The invention relates to a catalyst for preparing methacrylate by direct esterification, in particular to a S 2 o 8 2- / ZrO 2 -SiO 2 Solid acid catalyst, and used for the direct esterification reaction of methacrylic acid and diethylene glycol ether to synthesize diethylene glycol ether methacrylate. The invention belongs to the technical fields of catalyst preparation and fine chemicals. Background technique [0002] The chemical structure of methacrylate photocurable monomers contains functional groups such as unsaturated carbon-carbon double bonds, ether bonds, and carbonyl groups. It has multifunctional characteristics such as copolymerization and miscibility, and has fast curing speed, low irritation, and strong dilution. It is widely used in the synthesis of copolymers, and the products have excellent performance in water resistance, weather resistance, heat resistance and other aspects. In the United States, Europe, Japan and other countri...

Claims

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Application Information

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IPC IPC(8): B01J27/02C07C67/08C07C69/54
CPCB01J27/02C07C67/08C07C69/54
Inventor 郭登峰钱婷婷刘准章泽洲张皓文黄飞龙李瑞萍
Owner CHANGZHOU UNIV
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