Process for producing titanium-silicon zeolite microcapsule

A technology of titanium silicalite and silicon titanium, which is applied in the field of preparation of titanium silicalite microcapsules, can solve the problems of inability to form cavities above 100nm, low crystallinity, low titanium content of TS-1 molecular sieve, etc.

Active Publication Date: 2009-05-13
CHINA PETROLEUM & CHEM CORP +1
View PDF1 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is that there is low titanium content in TS-1 molecular sieve in the prior art, and there is no mention of carrying out alkali treatment to TS-1 molecular sieve, but there is low crystallinity when modifying ZSM-5 molecular sieve with alkali treatment method , the problem that the cavity above 100nm cannot be formed and the surface layer has a shell-like structure microcapsule, and a new preparation method of titanium silicalite microcapsule is provided

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～6

[0014] Treat silicon-titanium molar ratio SiO with a concentration of 0.8 mol / L sodium carbonate solution at a temperature of 80°C 2 / TiO 2 40, 80, 160, particle size 0.4, 2.0, 8.0, 20.0 μm TS-1 molecular sieve raw powder for 32 hours, washed, dried and then roasted at a temperature of 550 ° C to obtain the desired modified zeolite molecular sieve.

Embodiment 7～11

[0016] Treat silicon-titanium molar ratio SiO with a concentration of 0.1, 0.8, 2 mol / L sodium carbonate, sodium hydroxide or magnesium hydroxide solution at a temperature of 20, 60, 80 °C 2 / TiO 2 100, TS-1 zeolite molecular sieve raw powder with a particle size of 0.4 μm for 12, 32, and 48 hours, washed, dried, and then roasted at a temperature of 550° C. to obtain the desired modified zeolite molecular sieve.

Embodiment 12

[0018] The modified zeolite molecular sieves prepared in Examples 1 to 11 and Comparative Examples 1 to 2 were used to measure XRD on a Japanese Rigaku D / max-1400 X-ray diffractometer, and to carry out low-temperature nitrogen adsorption-desorption on a TriStar3000 physical adsorption instrument For research, the specific surface area of ​​the material is calculated by the BET method, and the pore size distribution and pore volume are calculated according to the BJH formula. The element composition of molecular sieves was carried out on a P-4010 inductively coupled plasma optical emission spectrometer. The results are listed in Table 1 and Table 2.

[0019] Table 1 Nitrogen adsorption-desorption results

[0020] Example 1 2 3 4 5 6 SiTi molar ratio SiO 2 / TiO 2 40 80 160 80 40 80 Molecular sieve particle size / μm 0.4 8.0 8.0 0.4 20.0 20.0 TiO before treatment 2 Mass percentage content / w% 3.22 1.64 0.62 1.64 3.22 1.64 Trea...

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

No PUM Login to view more

Abstract

The invention relates to a method for preparing titanium silicalite microcapsules, and mainly solves the problems in the prior art, for example, the content of titanium in TS-1 molecular sieve is low, the TS-1 molecular sieve is not treated with alkali, and when the ZSM-5 molecular sieve is modified by alkali treatment, the crystallization degree is low and the microcapsule with more than 100 nm cavities and having a shell-like structure on the surface is not obtained. In order to overcome the problems, the technical scheme is as follows: the titanium silicalite microcapsules are obtained by treating TS-1 crude powders (the Si/Ti molar ratio (calculated as SiO2/TiO2) ranges from 20 to 500 and the particle size ranges from 0.4 Mum to 20 Mum) with 0.4 mol/L to 5.0 mol/L of a solution of at least one alkali selected from sodium hydroxide, magnesium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate and sodium bicarbonate, at a temperature ranging from 20 DEG C to 90 DEG C for a time period ranging from 1 hour to 48 hours; and the volume of cavities with a size in the range from 100nm to 160nm accounts for 20% to 70% of the total volume of cavities with a size more than 2 nm. The titanium silicalite microcapsules are applied to the industrial production of catalytic oxidationof macromolecules.

Description

technical field [0001] The invention relates to a preparation method of titanium silicalite microcapsules. Background technique [0002] Titanium-silicon molecular sieve is a new type of catalytic material developed in the past ten years. It can catalyze various organic oxidation reactions with high activity and high selectivity under normal pressure and low temperature without causing environmental pollution. It is a new type of catalyst with the characteristics of "atom economy" in the field of green chemical technology in the 21st century. TS-1 has a titanium-containing heteroatom molecular sieve with an MFI structure, and has both the catalytic effect of titanium and the type-selective effect of ZSM-5 molecular sieve (Zhao Peiqing, Peng Zhiguang, Xia Chungu, Molecular Catalysis, 2006, 4:322). The researchers believe that the main factor affecting the catalytic oxidation activity of TS-1 molecular sieve is the content of framework titanium. Too much titanium source in th...

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 Applications(China)
IPC IPC(8): B01J29/89
Inventor 梅长松谢在库温鹏宇刘红星方敬东赵昱
Owner CHINA PETROLEUM & CHEM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap