Method for catalyzing cycloalkane by utilizing Sn-containing Ti-Si molecular sieve

A molecular sieve catalyzed oxidation of naphthenes and cycloalkanes, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, and the preparation of oxygenated compounds by oxidation of hydrocarbons, can solve the problems of difficult purification, short service life, difficult recovery, etc., and achieve the goal of overcoming the production process complex effects

Active Publication Date: 2015-03-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But peroxyacid oxidizing agent also has bigger shortcoming: (1) can produce a large amount of organic carboxylic acid (salt) wastes after finishing the reaction, has bigger impact on environment, and it is difficult to recycle or handle; (2) separation of reaction products , purification is more difficult, selectivity is low, atom economy is relatively poor, does not meet the basic principles of green chemistry; (3) organic peroxyacids need to use high-concentration hydrogen peroxide in the production process, the property is unstable, the production cost is higher, and It is more dangerous during transportation, storage and operation, thus limiting its application in industrial production
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 catalyzing cycloalkane by utilizing Sn-containing Ti-Si molecular sieve
  • Method for catalyzing cycloalkane by utilizing Sn-containing Ti-Si molecular sieve
  • Method for catalyzing cycloalkane by utilizing Sn-containing Ti-Si molecular sieve

Examples

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Effect test

preparation Embodiment 1

[0040] This example illustrates the synthesis process of TS-1 molecular sieve and the synthesis process of tin-containing titanium silicon molecular sieve according to the method of Zeolites, 1992, Vol.12, pages 943-950.

[0041] 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...

preparation Embodiment 2

[0043] 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.

[0044] 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.

[0045] According to X-ray diffraction analysis, it is a titanium-silicon molecula...

Embodiment 1

[0048]Weigh 2.3 grams of tin-containing titanium-silicon molecular sieve Sn-TS-1 (the mass percent of Sn is 1.2wt%, in terms of oxides, the same below) catalyst is loaded in a 100ml three-necked flask, then add a magnetic stirrer, 4.21 grams Cyclopentane, 3.6 grams of water and 23ml of 30% hydrogen peroxide, the molar ratio of cyclopentane to hydrogen peroxide is 1:4. 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 is controlled at about 80° C., and after 6 hours of reaction, the conversion rate of cyclopentane is 20.65%, and the selectivity of forming the corresponding δ-lactone is 26.79%. The selectivity for 5-hydroxypentanoic acid was 35.17%, and the selectivity for glutaric acid was 33.23%.

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Abstract

The invention provides a method for catalyzing cycloalkane by utilizing a Sn-containing Ti-Si molecular sieve. The method is characterized in that reaction is carried out in the presence of a catalyst under the conditions that molar ratio of cycloalkane to solvent to hydrogen peroxide is 1: (0-50): (0.2-20), temperature is 5-200 DEG C and pressure is 0.1-3.0MPa and products are recovered, wherein the mass ratio of the catalyst to cycloalkane is 1: (5-300) and the catalyst is a secondarily synthesized Sn-containing Ti-Si molecular sieve.

Description

technical field [0001] The present invention relates to a catalytic method for cycloalkane, and more specifically relates to a method for oxidizing cycloalkane with hydrogen peroxide. Background technique [0002] ε-caprolactone has the advantages of low viscosity, easy processing, and low VOC content. It is used as oligomer and denaturant in the process, which can improve the toughness, low temperature characteristics and reactivity and other functionalities; in terms of coatings, it is used as an improvement in solvents and latex coatings for automotive primers, surface coatings and various building materials. It can improve the toughness of the coating film, improve the low-temperature characteristics, reactivity, and increase the crosslinking density; in terms of adhesives, it can be used to improve the bonding properties of hot-melt adhesives and solvent-based adhesives; in resin modification On the one hand, it can be used to improve softness, fluidity, low temperatur...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C27/16C07D309/30C07D313/04C07C51/31C07C59/01C07C55/14C07C55/12B01J29/89
CPCY02P20/582
Inventor 朱斌林民夏长久龙立华邹飞艳舒兴田汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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