Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Nanometer sn-β molecular sieve and its preparation method and the method of phenol hydroxylation reaction

A beta molecular sieve and molecular sieve technology, applied in the field of beta molecular sieve, can solve the problems of easy deep oxidation, etc., and achieve the effect of less skeleton defects, large specific surface area and small particle size

Active Publication Date: 2019-08-06
JIANGXI NORMAL UNIV
View PDF7 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Phenol hydroxylation is the main method for preparing catechol and hydroquinone. This method mainly uses titanium-silicon molecular sieve TS-1 as a catalyst, but because its pore size is only about 0.55 nanometers, the diffusion of reaction products is inhibited. They Easy deep oxidation to generate quinone

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Nanometer sn-β molecular sieve and its preparation method and the method of phenol hydroxylation reaction
  • Nanometer sn-β molecular sieve and its preparation method and the method of phenol hydroxylation reaction
  • Nanometer sn-β molecular sieve and its preparation method and the method of phenol hydroxylation reaction

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0025] The invention provides a kind of preparation method of nanometer Sn-beta molecular sieve, comprises the following steps:

[0026] (1) In the presence of an aqueous solvent, mix the silicon source, the tin source, the structure-directing agent and the alkali source in proportion to obtain a gel-like mixed solution, adjust the pH value of the mixed solution to 9.5-13.8, and place the mixed solution in Crystallize at a temperature of 150-220°C for 5-28 days, separate and roast to obtain a crystallized product;

[0027] (2) mixing the crystallization product, cobalt salt and / or nickel salt in an aqueous solvent in proportion to obtain a reaction solution, and reacting the reaction solution at a temperature of 180-220° C. for 2-10 hours to obtain a molecular sieve precursor;

[0028] (3) mixing the molecular sieve precursor and the sulfur-containing medium in a water-containing solvent, and reacting at a temperature of 80-140° C. for 1-6 hours to obtain nano Sn-β molecular s...

Embodiment 1

[0058] Under stirring conditions, tetraethyl orthosilicate, sodium stannate, tetraethylammonium hydroxide and hydrazine hydrate are mixed in water, and the molar ratio of each substance in the formed mixed solution is SiO 2 :Sn:Structure directing agent:H 2 O=1:0.012:1.3:100, stir until the solution is gel, add potassium tert-butoxide to adjust the pH value of the solution to 12.6, then transfer the solution to a polytetrafluoroethylene reactor, the total volume of the mixed solution is 65% of the capacity of the reactor, crystallized at a temperature of 190°C for 5 days, separated and roasted to obtain a crystallized product;

[0059] The crystallization product, cobalt sulfate, and nickel nitrate are in weight ratio: crystallization product: Co 2+ : Ni 2+ = 1:1:1 dissolved in water to obtain a mixed solution, transfer the mixed solution into a polytetrafluoroethylene reactor, react at a temperature of 180°C for 10 hours, and obtain a pink precursor; add the precursor to so...

Embodiment 2

[0062] Under stirring conditions, tetraethoxysilane, tin sulfate, tetraethylammonium iodide and sodium ethylate are mixed in water, and the molar ratio of each substance in the formed mixed solution is SiO 2 :Sn:Structure directing agent:H 2 O=1:0.01:1.0:10, stir until the solution is gel-like, add ammonia water to adjust the pH value of the solution to 11.7, then transfer the solution into a polytetrafluoroethylene reactor, the total volume of the mixed solution is the capacity of the reactor 65%, crystallized at 180°C for 10 days, separated and roasted to obtain a crystallized product;

[0063] The crystallization product, cobalt nitrate, and nickel sulfate are in weight ratio: crystallization product: Co 2+ : Ni 2+ =1:0.5:1.5 dissolved in water to obtain a mixed solution, transfer the mixed solution into a polytetrafluoroethylene reactor, and react at a temperature of 190°C for 4 hours to obtain a pink precursor; add the precursor to thiourea In the aqueous solution, the...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
specific surface areaaaaaaaaaaa
Login to View More

Abstract

The present invention relates to the technical field of β molecular sieves, and discloses a nano-Sn-β molecular sieve and a preparation method thereof and a method for phenol hydroxylation reaction. The preparation method of the nano-Sn-β molecular sieve comprises the following steps: (1) in the presence of an aqueous solvent , mixing the silicon source, the tin source, the structure directing agent and the alkali source to obtain a mixed solution, adjusting the pH value of the mixed solution to 9.5-13.8, performing a crystallization reaction on the mixed solution, separating and roasting to obtain a crystallized product; (2 ) mixing the crystallization product, cobalt salt and / or nickel salt in an aqueous solvent in proportion to obtain a reaction solution, and reacting the reaction solution at a temperature of 180-220° C. for 2-10 hours to obtain a molecular sieve precursor; (3 ) mixing the molecular sieve precursor and the sulfur-containing medium in an aqueous solvent, and performing a hydrothermal reaction to obtain a nano-Sn-β molecular sieve. The composite nano Sn-β molecular sieve is prepared by the above method, and the product has uniform particle size, large specific surface area and few skeleton defects, and has good catalytic performance in phenol hydroxylation reaction.

Description

technical field [0001] The invention relates to the technical field of beta molecular sieves, in particular to a nanometer Sn-beta molecular sieve, a preparation method thereof, and a phenol hydroxylation reaction method. Background technique [0002] Heteroatom molecular sieves refer to molecular sieves with non-silicon and aluminum elements in their skeleton structure. The introduction of heteroatoms not only regulates the acidity and surface properties of zeolite catalysts, but also makes them have special catalytic properties. Titanium-silicon molecular sieve TS-1 is a molecular sieve with a four-coordinate titanium framework, and its appearance marks the beginning of the synthesis and application of heteroatom molecular sieves. [0003] β molecular sieves are stacking fault symbiosis composed of three structurally distinct but closely related polymorphs. It has a three-dimensional twelve-membered ring channel structure, in which the channels in the [100] and [010] dire...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/48C01B39/06B82Y40/00B01J29/04C07C37/60C07C39/08
CPCY02P20/52
Inventor 王宝荣谢贤清陈飞彪郭晓红雷志伟廖维林
Owner JIANGXI NORMAL UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products