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Highly active solid catalyst for preparing ketal and application thereof

A catalyst and ketal technology, which is applied in the direction of molecular sieve catalysts, physical/chemical process catalysts, carbon-based compound preparation, etc., can solve the problems of low catalyst activity and unmodified molecular sieves, and achieve high selectivity, stable surface properties, High conversion effect

Active Publication Date: 2006-05-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disclosed a kind of method for synthesizing formal as CN1301688A, make catalyst with common HZSM-5 molecular sieve, synthesize formal under normal pressure, its main problem is that molecular sieve is not modified, and the catalyst activity when synthesizing formal is relatively low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Embodiment 1. Preparation of catalyst

[0010] 1 kg of artificially synthesized ZSM-5 molecular sieve was treated with 4 kg of 0.5-2 mol / L hydrochloric acid solution, under strong stirring, and the temperature was controlled at 60-90 ° C for 1 hour, then the supernatant liquid was poured out, and the Add 4 kilograms of 0.5-2mol / L hydrochloric acid solution to repeat the treatment 2-4 times, wash and dry, hydrothermally treat at 400-600°C under normal pressure for 0.5-2 hours, and then roast it at 400-600°C for 4 Stand by after hours. The specific conditions and results are shown in Table 1.

[0011] catalyst

Embodiment 2

[0013] Add 0.2mol cyclohexanone and 0.3mol ethylene glycol mixed solution in the 200 milliliter three-neck flask that is equipped with reflux condenser, water trap, thermometer, then add the molecular sieve catalyst of 1 gram, add water-carrying agent (benzene) 40 mL, the reaction flask was placed in a 90°C constant temperature water bath, and refluxed for 0.5 hours under stirring. When the water separated from the water separator no longer increased, the reaction ended. After cooling, the yield of ethylene glycol ketal was 91%.

Embodiment 3

[0015] In the 200 milliliters of there-necked flasks that are equipped with reflux condenser, water trap, thermometer, add 0.2mol cyclohexanone and 0.4mol ethylene glycol mixed solution, then add the molecular sieve catalyst of 1.5 grams, then add water-carrying agent (benzene) 30 mL, the reaction flask was placed in a 90°C constant temperature water bath, and refluxed for 1 hour under stirring. When the water separated from the water separator no longer increased, the reaction ended. After cooling, the yield of ethylene glycol ketal was 92%.

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PUM

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Abstract

The invention discloses a high-active solid catalyst for preparing ketal and its application method. The inventive catalyst uses the ZSM-5 molecular screen as raw material to be processed with acid treatment and hydrothermal treatment to attain the catalyst with better activity and stability for preparing ketal. When using said catalyst to prepare ketal, user can utilize the discontinuous or continuous operation, while the mole ratio of ketone and ethanol is 1:4-1:10, the collection rate of ketal is higher than 90%, and the catalyst will not change its reaction activity more than 10 times.

Description

technical field [0001] The invention relates to a highly active ZSM-5 molecular sieve catalyst used in the condensation reaction of ketones and alcohols to synthesize ketals, and the application of the catalyst in the synthesis of ketals. Background technique [0002] Ketal compounds are new types of fragrance compounds developed in the past ten years. They have the characteristics of floral fragrance superior to parent ketones, long-lasting fragrance, various types of fragrance, and stable chemical properties. Ketals are also commonly used in carbonyl protection or reaction intermediates in organic synthesis, and are sometimes used as reaction solvents. [0003] The commonly used catalysts for ketal synthesis reactions are inorganic acids (such as H 2 SO 4 , HCl, H 3 PO 4 etc.), but the disadvantages of many side reactions, strong corrosion and easy pollution of the environment limit its use. Recent studies have shown that some solid acids, SnCl 4 , FeCl 3 , niobic a...

Claims

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Application Information

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IPC IPC(8): B01J29/40C07C45/00
Inventor 汪群海
Owner CHINA PETROLEUM & CHEM CORP