Method for catalytically oxidizing lactone

A technology of catalytic oxidation and lactone, applied in chemical instruments and methods, oxidative preparation of carboxylic acids, molecular sieve catalysts, etc., can solve the problems of heteropolyacid catalysts with unstable properties, short service life, small specific surface, etc., and achieve catalytic oxidation Activity and catalytic activity, good stability, increased catalytic activity, and high lactone conversion

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, heteropolyacid catalysts have shortcomings such as unstable properties, small specific surface area, easy deactivation, difficult recovery and short service life, so they have not been widely promoted at present.

Method used

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  • Method for catalytically oxidizing lactone
  • Method for catalytically oxidizing lactone
  • Method for catalytically oxidizing lactone

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0034] This example illustrates the synthesis process of TS-1 molecular sieve and the synthesis process of tin-titanium-silicon molecular sieve according to the method of Zeolites, 1992, Vol.12, pages 943-950.

[0035] Mix 22.5 grams of tetraethyl orthosilicate with 7.0 grams of tetrapropylammonium hydroxide, add 59.8 grams of distilled water, mix well, and then hydrolyze at normal pressure and 60°C for 1.0 hour to obtain a hydrolysis solution of tetraethyl orthosilicate A solution consisting of 1.1 g of tetrabutyl titanate and 5.0 g of anhydrous isopropanol was slowly added under vigorous stirring, and the resulting mixture was stirred at 75° C. for 3 hours until it became a clear and transparent colloid. Put the colloid into a stainless steel sealed reaction kettle, and place it at a constant temperature of 170°C and autogenous pressure for 6 days to obtain a mixture of crystallized products; filter the mixture, wash it with water until the pH is 6-8, and dry it at 110°C Aft...

preparation example 2

[0037] Take the TS-1 molecular sieve obtained in Catalyst Preparation Example 1 according to the ratio of molecular sieve (g): sulfuric acid (mol): water (mol) = 100: 0.15: 15 and mix evenly, react at 90 ° C for 5.0 hours, and then follow the conventional method Filtration, washing and drying yielded acid-treated TS-1 molecular sieves.

[0038] The above-mentioned acid-treated TS-1 molecular sieves were mixed uniformly according to the ratio of molecular sieve (gram): triethanolamine (mol): tetrapropylammonium hydroxide (mol): water (mol) = 100: 0.20: 0.15: 180, and put into A stainless steel sealed reaction kettle was placed at a constant temperature of 190°C and autogenous pressure for 0.5 days. After cooling and pressure relief, it was filtered, washed, dried according to conventional methods, and roasted in an air atmosphere at 550°C for 3 hours to obtain a hollow structure molecular sieve.

[0039] According to X-ray diffraction analysis, it is a titanium-silicon molecula...

Embodiment 1

[0042] Weigh 2.3 grams of tin-containing hollow titanium-silicon molecular sieve Sn-HTS (SnO 2 The mass percentage is 2.6wt%, TiO 2 The mass percent is 3.2wt%) catalyst is packed in the 100ml three-neck flask, then add magnetic stirrer, 22.81 gram ε-caprolactone, 18 gram water and 23ml concentration to be the hydrogen peroxide of 30% at this moment, ε-caprolactone The molar ratio of ester to hydrogen peroxide is 1:1. The three-necked flask is placed on a temperature-controlled magnetic stirrer, and the upper part of the three-necked flask is condensed and refluxed with a condenser, and the magnetic stirrer and heating device are started to start the reaction. The reaction temperature was controlled at about 50°C. After 5 hours of reaction, the conversion rate of ε-caprolactone was 75.72%, the selectivity to 6-hydroxycaproic acid was 54.27%, and the selectivity to adipic acid was 39.61%.

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Abstract

The invention provides a method for catalytically oxidizing lactone. The method is characterized in that reaction is carried out in the presence of a catalyst under the conditions that molar ratio of lactone to solvent to hydrogen peroxide is 1: (0-80): (0.2-20), temperature is 10-200 DEG C and reaction pressure is 0.1-3.0MPa, so as to prepare corresponding hydroxyl acid and binary acid, wherein the mass ratio of the catalyst to the lactone is 1: (5-300) and the catalyst is a tin-titanium-silicon molecular sieve.

Description

technical field [0001] The present invention relates to a method for catalyzing the oxidation of lactones, more specifically to a method for oxidizing lactones with hydrogen peroxide. Background technique [0002] Hydroxy acids are important organic chemical raw materials. Taking 6-hydroxycaproic acid as an example, its melting point is 38-40°C, its boiling point is 113-116°C, its density is 0.981g / ml, its refractive index is 1.044, and its flash point is >110°C. It is an important organic chemical raw material, which has a wide range of applications in the fields of organic synthesis and polymer materials. For example, the preparation of 6-formyl caproic acid, ε-caprolactone, adipic acid, etc. Its derivative 6-hydroxyhexanoic acid ethyl ester etc. are commonly used organic chemical intermediates. US Patent USP2008306153 introduces a CH 2 Cl 2 In a solvent, using PCC (Pyridinium Chlorochromate) as an oxidant at 37°C, 6-hydroxycaproic acid is oxidized to 6-formylcapro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/31C07C59/01C07C55/14C07C55/12B01J29/89
CPCY02P20/582
Inventor 夏长久林民朱斌龙立华史春风舒兴田邹飞艳汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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