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Forming method and forming catalyst of titanium silicon molecular sieve and its application and method for oxidation of cyclohexanone

A technology of titanium-silicon molecular sieve and molding method, which is applied in the field of cyclohexanone oxidation, can solve the problems of definite hydroxy acid selectivity, achieve high hydroxy acid selectivity, high pore volume and crush resistance, and overcome the production process complex effects

Active Publication Date: 2019-09-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it is impossible to clearly draw a technical solution with high selectivity for hydroxy acids

Method used

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  • Forming method and forming catalyst of titanium silicon molecular sieve and its application and method for oxidation of cyclohexanone
  • Forming method and forming catalyst of titanium silicon molecular sieve and its application and method for oxidation of cyclohexanone
  • Forming method and forming catalyst of titanium silicon molecular sieve and its application and method for oxidation of cyclohexanone

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Embodiment approach

[0025] According to a preferred embodiment of the present invention, the aqueous mixture also contains Al element, preferably Al 2 o 3 The content of the calculated Al element is 0.05-10% by weight. The catalyst thus obtained is used in the oxidation reaction of cyclohexanone with higher hydroxy acid selectivity.

[0026] According to the method of the present invention, as long as the above-mentioned elements are contained in the mixture, the purpose of the present invention can be achieved. The present invention has no special requirements for the raw materials of each element, which can be determined according to the type of raw material of the crystallization mother liquor, for example, the provision of silicon element The silicon source can be an organic silicon source and / or an inorganic silicon source.

[0027] Specifically, the organosilicon source can be, for example, one or more selected from the silicon-containing compounds shown in formula I,

[0028]

[0029...

Embodiment 1

[0081] (1) Titanium-silicon molecular sieve TS-1 was prepared according to the method in Example 1 of US4410501, and the crystallization mother liquor was collected. The specific operation process is:

[0082] Place 455 g of tetraethyl orthosilicate in a CO-free 2 Then, 15 g of tetraethyl titanate and 800 g of aqueous solution of tetrapropylammonium hydroxide with a concentration of 25% by weight were successively added into the reactor in the atmosphere. After stirring for 1 hour, the temperature was raised to 80-90°C and stirring was continued for 5 hours. Then, deionized water was added to the reaction solution until the total volume of the reaction solution was 1.5 L. Next, the reaction solution was transferred to a high-pressure reactor equipped with a stirring device, and after hydrothermal crystallization at 175°C for 10 days under autogenous pressure, the resulting reaction mixture was filtered to collect the crystallization mother liquor, and the filtered solid was ...

Embodiment 2

[0096] The same method as in Example 1 is used to prepare the shaped titanium-silicon molecular sieve. The difference is that in step (1), the crystallization mother liquor is concentrated to the total amount of the crystallization mother liquor, and the SiO 2 The silicon element content is 3.5% by weight, based on TiO 2 The content of titanium element is 0.09% by weight, expressed as NH 3 The calculated nitrogen content is 8.6% by weight, and step (2) mixes 10 g of titanium-silicon molecular sieve TS-1 prepared in step (1) with 10 g of crystallization mother liquor obtained in step (1).

[0097] Table 1 lists the crush resistance, titanium-silicon molecular sieve content, cyclohexanone conversion, and hydroxy acid selectivity of the obtained shaped titanium-silicon molecular sieve (volume average particle diameter of 81 microns).

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Abstract

The present invention relates to the field of catalyst molding, and particularly provides a titanium-silicon molecular sieve molding method, which comprises: mixing a titanium-silicon molecular sieve and a water-containing mixture, carrying out hydrothermal treatment under a sealed condition, molding the slurry obtained from the hydrothermal treatment to obtain a molding body, and calcining the molding body, wherein the water-containing mixture contains a silicon element, a titanium element and a nitrogen element, and is at least partially derived from the crystallization mother liquor of the titanium silicon molecular sieve. The present invention provides a molding catalyst prepared according to the preparation method, and applications thereof. The invention further provides a cyclohexanone oxidation method. According to the present invention, with the titanium-silicon molecular sieve molding method, the industrial waste liquid is effectively utilized, and the problems of complex process, corrosion on equipment, harmful emission and the like of the traditional process are overcome; and the molding catalyst has characteristics of high titanium-silicon molecular sieve content, high pore volume, high crushing resistance, and high selectivity to the target product.

Description

technical field [0001] The invention relates to a molding method of titanium-silicon molecular sieve, a molding catalyst obtained by the method of the invention and its application in oxidizing cyclic ketones and a method for oxidizing cyclohexanone. Background technique [0002] Hydroxy acids are an important class of chemical raw materials. For example, 6-hydroxycaproic acid is an important organic chemical raw material. It is widely used in the fields of organic synthesis and polymer materials. Its physical properties: melting point is 38-40 °C, The boiling point is 113-116°C, the density is 0.981g / ml, the refractive index is 1044, and the flash point is >110°C. Using 6-hydroxycaproic acid, 6-formylcaproic acid, ε-caprolactone, adipic acid, etc. can be prepared. Its derivative 6-hydroxyhexanoic acid ethyl ester etc. are commonly used organic chemical intermediates. [0003] At present, the raw materials for preparing 6-hydroxycaproic acid mainly include cyclohexanone...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89B01J35/10B01J37/08C07C59/01C07C51/285
CPCC07C51/285B01J29/89B01J37/08B01J2229/10B01J35/633B01J35/635C07C59/01
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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