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Tin-silicon molecular sieve and synthetic method and application thereof, and phenol hydroxylation method

A tin-silicon molecular sieve and phenol hydroxylation technology are applied in the direction of molecular sieve catalysts, chemical instruments and methods, and the preparation of organic compounds, which can solve problems such as low yield, long crystallization time of tin-silicon molecular sieves, and weak crystal guiding ability. Achieve the effects of high crystallinity, shorten hydrolysis time, and reduce dosage

Active Publication Date: 2016-01-27
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the existing technology for preparing tin-silicon molecular sieves, due to the weak crystal guiding ability of Sn itself, the crystallization time for preparing tin-silicon molecular sieves is longer, and the yield is also lower.

Method used

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  • Tin-silicon molecular sieve and synthetic method and application thereof, and phenol hydroxylation method
  • Tin-silicon molecular sieve and synthetic method and application thereof, and phenol hydroxylation method
  • Tin-silicon molecular sieve and synthetic method and application thereof, and phenol hydroxylation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Firstly, tetraethyl orthosilicate as a source of organosilicic acid and tin chloride pentahydrate as a source of tin are dissolved in an aqueous solution of tetrapropylammonium hydroxide as an alkali source template agent, wherein the molar composition of the material is organosilicon source: tin source: alkali source Templating agent: water = 100:5:10:400, organic silicon source is SiO 2 Meter, tin source as SnO 2 Meter, alkali source template with OH - After the silicon ester is hydrolyzed (the hydrolysis rate is 50%), the mixture is transferred to a sealed reactor for hydrothermal crystallization at 140°C for 6 hours. After cooling, the reactor is opened to add silica gel A to the crystallization system and mix well. SiO 2 According to the calculation, the molar ratio of the added silica gel to the organic silicon source was 1:0.2, and then the mixture was continued to crystallize in a sealed reaction vessel at a temperature of 170°C and autogenous pressure for 12 ...

Embodiment 2

[0070] Firstly, the organosilicon source tetraethyl orthosilicate and the tin source tin chloride pentahydrate are dissolved in the alkali source template agent tetrapropyl ammonium hydroxide aqueous solution, wherein the material molar composition is organosilicon source: tin source: alkali source template agent : water = 100:2:15:500, organic silicon source is SiO 2 Meter, tin source as SnO 2 Meter, alkali source template with OH - After the silicon ester (hydrolysis rate is 70%) is hydrolyzed, the mixture is transferred to a sealed reactor for hydrothermal crystallization at 140°C for 10 hours. After cooling, the reactor is opened to add silica gel B to the crystallization system and mix well. SiO 2 Calculated, the molar ratio of the added silica gel to the organic silicon source is 1:0.1, and then the mixture is continued to be crystallized in a sealed reactor at a temperature of 170°C and an autogenous pressure for 20h, and then the crystallized product is recovered acc...

Embodiment 3

[0072] Firstly, the organosilicon source tetraethyl orthosilicate and the tin source tetrabutyl stannate are dissolved in the alkali source template agent tetrapropyl ammonium hydroxide aqueous solution, wherein, the molar composition of the material is organosilicon source: tin source: alkali source template Agent: water = 100:1:20:650, organic silicon source is SiO 2 Meter, tin source as SnO 2 Meter, alkali source template with OH - After the silicon ester is hydrolyzed (the hydrolysis rate is 60%), the mixture is transferred to a sealed reactor for hydrothermal crystallization at 120°C for 8 hours, and after cooling, the reactor is opened to add silica sol with a mass fraction of 25% to the crystallization system. and mix well, wherein the molar ratio of added silica sol to organosilicon source is 1:0.5 in terms of silicon dioxide, and then continue to crystallize the mixture in a sealed reaction kettle at a temperature of 160°C and autogenous pressure for 14h, and then T...

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Abstract

The invention provides a method for synthesizing a tin-silicon molecular sieve. The method comprises: (1) hydrolyzing an organic silicon source, a tin source and an alkali source template agent to obtain a mixture A and carrying out first crystallization on the obtained mixture A; and (2) mixing the material obtained by first crystallization with an inorganic silicon source to obtain a mixture B and carrying out second crystallization on the obtained mixture B. The invention provides the tin-silicon molecular sieve synthesized through the method and an application of the molecular sieve. The invention provides a phenol hydroxylation method. By taking the inorganic silicon source which is relatively low in price as a part of, or even, a main silicon source, the use level of organosilicone esters is reduced, and the synthetic benefit is improved to a great extent. Moreover, the synthesized tin-silicon molecular sieve is high in relative crystallinity, high in catalytic oxidation activity and high in selectivity, and shows the characteristics of being high in catalytic oxidation activity and high in selectivity on hydroquinone in a probe reaction, i.e. a phenol hydroxylation reaction.

Description

technical field [0001] The present invention relates to a synthesis method of tin-silicon molecular sieve, tin-silicon molecular sieve synthesized by the synthesis method of tin-silicon molecular sieve, application of tin-silicon molecular sieve of the present invention in phenol hydroxylation and a method of phenol hydroxylation. Background technique [0002] Tin-silicon molecular sieve, such as tin-silicon molecular sieve SnS-1 with MFI crystal structure, is a new type of tin-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing transition metal element tin into the molecular sieve framework with ZSM-5 structure. SnS-1 not only has the catalytic oxidation effect of tin, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve. Since the SnS-1 molecular sieve can use non-polluting low-concentration hydrogen peroxide as an oxidant in the oxidation reaction of organic matter, it avoids the proble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/04C07C37/60C07C39/08
Inventor 史春风朱斌林民
Owner CHINA PETROLEUM & CHEM CORP
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