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A method for simultaneously preparing methallyl alcohol and acetal by using sn-beta catalysts

A technology of methallyl alcohol and methacrolein, applied in chemical instruments and methods, molecular sieve catalysts, carbon-based compound preparation, etc., can solve problems such as high temperature and pressure, low yield, environmental pollution, etc., and achieve separation Convenience, high activity, and high stability

Active Publication Date: 2020-07-03
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Alkaline hydrolysis has become one of the most important methods for producing methallyl alcohol, but there are certain problems: a large amount of alkaline reagents and organic solvents need to be added in the hydrolysis process, higher temperature and pressure are required, and the impact on the environment Higher contamination and lower yield due to presence of by-product ether
Up to now, there is not yet a method for simultaneously preparing methallyl alcohol and acetal without high temperature and high pressure and easy separation.

Method used

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  • A method for simultaneously preparing methallyl alcohol and acetal by using sn-beta catalysts
  • A method for simultaneously preparing methallyl alcohol and acetal by using sn-beta catalysts
  • A method for simultaneously preparing methallyl alcohol and acetal by using sn-beta catalysts

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Experimental program
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Effect test

Embodiment 1

[0035] 1) Sn-β preparation method: at 373K with 65-68% HNO 3 H-β was dealuminated for 20h, the 65-68% HNO 3 The formula ratio with H-β is 20ml:1g, the obtained powder is washed and dried, and physically ground with tin acetate for 20min, the ratio of the powder and tin acetate is 5:1, and then in the tube furnace, air is used as the flow The atmosphere was calcined at 823K for 3h to obtain Sn-β-type catalyst, which was Sn-β.

[0036] 2) Sn-β-Ar preparation method: at 373K with 65-68% HNO 3H-β was dealuminated for 20h, the 65-68% HNO 3 The formula ratio with H-β is 20ml:1g, the obtained powder is washed and dried, and physically ground with tin acetate for 20min. The mass ratio of the powder and tin acetate is 5:1. calcined at 823K for 3h in a flowing atmosphere, and then calcined at 823K for 3h with air as a flowing atmosphere to obtain Sn-β-type catalyst, which is Sn-β-Ar.

[0037] 3) Sn-β-Ar-Na preparation method: Sn-β-Ar was prepared according to the above method, and t...

Embodiment 2

[0040] The method of simultaneously preparing methallyl alcohol and acetal can be carried out in a 10ml round-bottomed flask equipped with a condensing reflux tube, a thermocouple, a stirrer, a heater, and the like. Specifically, 2.8 mmol of methacrolein and 80 mmol of ethanol were added to a 10 ml round-bottomed flask, and 0.2 g of Sn-β catalyst Sn-β was added. Using methacrolein as a substrate, ethanol as a solvent and a hydrogen source, heating to 77 ° C, reflux reaction for 2h, to obtain methallyl alcohol and acetal.

[0041] The product after the reaction was filtered and qualitatively analyzed by GC-MS (HP-5 capillary column 30m×0.25mm×0.25μm), gas chromatography (Thermo Trace 1310, HP-5 capillary column 30m×0.25mm×0.25μm) hydrogen flame ionization detector for quantitative analysis. The activity evaluation results of the catalysts are shown in Table 1. Based on methacrolein, the conversion of methacrolein was 69.9%, and the yields of methallyl alcohol and acetal were ...

Embodiment 3

[0043] In a 10ml round-bottomed flask, add 1.8mmol methacrolein, 80mmol ethanol, add 0.2g Sn-β catalyst Sn-β, use methacrolein as substrate, ethanol as solvent and hydrogen source, heat to 77°C, Reflux reaction for 2h to obtain methallyl alcohol and acetal.

[0044] The product after the reaction was filtered and qualitatively analyzed by GC-MS (HP-5 capillary column 30m×0.25mm×0.25μm), gas chromatography (Thermo Trace 1310, HP-5 capillary column 30m×0.25mm×0.25μm) hydrogen flame ionization detector for quantitative analysis. The activity evaluation results of the catalysts are shown in Table 1. Based on methacrolein, the conversion of methacrolein was 76.6%, and the yields of methallyl alcohol and acetal were 42.8% and 50.6%, respectively.

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Abstract

The invention discloses a method for preparing methallyl alcohol and aldehyde acetal simultaneously by using Sn-beta catalysts. The method comprises the following steps: dealuminizing an H-beta molecular sieve serving as a parent, and grinding and roasting the H-beta molecular sieve and stannum acetate to obtain the Sn-beta catalyst Sn-beta; obtaining the Sn-beta catalysts Sn-beta-Ar and Sn-beta-Ar-Na by aftertreatment methods of Ar pretreatment and Na exchange so as to reduce stannum species outside a skeleton and the B acid content of the catalysts and further improve the catalytic activity and selectivity; and preparing two important chemical products methallyl alcohol and aldehyde acetal simultaneously at low temperature by using the above Sn-beta catalysts, taking methylacrolein as a substrate and taking ethanol as a solvent and a hydrogen source. The Sn-beta catalysts have high activity, and the methallyl alcohol with the yield being 90 percent and the aldehyde acetal with the yield being 96 percent can be obtained; the catalysts have high stability and is not deactivated after being circulated for many times; the reaction is conducted at low temperature without high temperature and high pressure; and the reaction system is a multiphase reaction system, and the catalysts and the products are separated simply and conveniently.

Description

technical field [0001] The invention belongs to the technical field of preparation of methallyl alcohol and acetal, and in particular relates to a method for simultaneously preparing methallyl alcohol and acetal by using a Sn-β catalyst. Background technique [0002] Methallyl alcohol is an important organic intermediate used in the synthesis of fragrances, resins, etc. Synthesis of methallyl alcohol polyoxyethylene ether (HPEG) with methallyl alcohol and ethylene oxide as raw materials for a new generation of high-performance concrete water reducing agent. Methallyl alcohol can synthesize methacrylic acid and its esters, and can also synthesize allyl-containing esters with other organic acids. It has important applications in polymerizing monomers and surfactants. [0003] The traditional method for preparing methallyl alcohol takes 2-methylallyl chloride as the starting material, and adopts the alkaline hydrolysis method to produce methallyl alcohol. US2072015, US2323781...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/70C07C41/56C07C43/303C07C29/141C07C33/03
CPCB01J29/7057B01J2229/183C07C29/141C07C41/56C07C45/512C07C43/303C07C33/03C07C47/06
Inventor 万绍隆胡文达王勇
Owner XIAMEN UNIV
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