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

A method for rapidly synthesizing high-titanium-content titanium-silicon molecular sieve ts-1 under normal pressure using crystallization mother liquor

A titanium-silicon molecular sieve, TS-1 technology, applied in chemical instruments and methods, molecular sieves and alkali exchange compounds, crystalline aluminosilicate zeolites, etc., to achieve the effects of increasing titanium content, avoiding pollution, and reducing the cost of synthetic equipment

Active Publication Date: 2022-03-22
DALIAN UNIV OF TECH
View PDF11 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] So far, in any published literature, there is no research report on the rapid synthesis of TS-1 molecular sieve at normal pressure and temperature below 100 °C, especially the rapid synthesis of TS with high titanium content under such conditions -1 molecular sieve, a research report on the rapid synthesis of the TS-1 molecular sieve by recycling the mother liquor

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
  • A method for rapidly synthesizing high-titanium-content titanium-silicon molecular sieve ts-1 under normal pressure using crystallization mother liquor
  • A method for rapidly synthesizing high-titanium-content titanium-silicon molecular sieve ts-1 under normal pressure using crystallization mother liquor
  • A method for rapidly synthesizing high-titanium-content titanium-silicon molecular sieve ts-1 under normal pressure using crystallization mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Inject 0.378 g of butyl titanate into a glass vial filled with 19.2 g of absolute ethanol and ultrasonically mix. Gained mixed liquid is added to 3.0g white carbon black (amorphous SiO 2 ) for 15 minutes and dried in a vacuum oven. Then add 12.0 g of tetrapropylammonium hydroxide aqueous solution with a concentration of 25 wt.% and grind it into a clear and transparent liquid. Pour the liquid into a self-made double-layer glass crystallizer with a volume of 25ml and a volume of 95°C circulating water. A reflux condenser is installed on the crystallizer. The resulting solid was isolated by ultracentrifugation. The obtained solid was dried and calcined in air at 500° C. for 4 hours to measure ultraviolet diffuse reflectance and XRD. The resulting 7.9g mother liquor was used for the next TS-1 molecular sieve synthesis.

Embodiment 2

[0039] Example 1 was repeated, but instead of 3.0 g of silica and 0.378 g of butyl titanate in Example 1, 2.24 g of silica and 0.282 g of butyl titanate were used. The mixed aqueous solution of the tetrapropyl ammonium hydroxide of 7.9 gram mother liquors, 2.83 gram 25wt.% tetrapropyl ammonium hydroxide, 1.27 gram 50wt.% by embodiment 1 gained 12.0g concentration in the replacement embodiment 1 is 25wt.% aqueous solution of tetrapropylammonium hydroxide. Change the crystallization time to 30 hours. The obtained mother liquor of about 7.9 g is used for the next TS-1 molecular sieve synthesis.

Embodiment 3

[0041] Example 2 was repeated, but the mother liquor obtained in Example 1 was replaced by the mother liquor obtained in Example 2.

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 discloses a method for rapidly crystallizing and synthesizing a titanium-silicon molecular sieve TS‑1 with uniform size and small grains and high titanium content under normal pressure. Compared with the TS-1 molecular sieve synthesis technology reported in the present invention, the TS-1 molecular sieve preparation technology proposed by the present invention has the following advantages: (1) Crystallization at 90-99.5°C under normal pressure at 24-60 The rapid synthesis of TS-1 molecular sieves with high titanium content can be achieved within hours, and this method is especially suitable for the large-scale production of TS-1 molecular sieves; (2) The template agent can be recycled, so it can not only greatly reduce the production cost of TS-1 molecular sieves (3) no inorganic alkali is used; (4) the utilization rate of silicon and titanium is close to 100%; (5) the synthesized TS-1 molecular sieve crystals have uniform size and relatively small crystal grains. Small (150-200nm), as a catalyst or catalyst carrier, it is more conducive to the mass transfer and diffusion of reactants and products.

Description

technical field [0001] The invention belongs to a method for preparing molecular sieves, in particular to a method for rapidly synthesizing TS-1 molecular sieves with high titanium content under normal pressure and low temperature conditions. Background technique [0002] Titanium silicate molecular sieve TS-1 is widely used as a catalyst in many reactions, such as ammoximation of cyclohexanone, epoxidation of alkenes, oxidation of alcohols, partial oxidation of alkanes, hydroxylation of benzene and phenol, and methanol to alkenes reaction. [0003] Titanium silicate molecular sieve TS-1 was first reported by Taramasso et al. (U.S. Patent 4,410,501) in 1983. [0004] In 2016, Chen Lihua et al. (CN104058423B) disclosed a method of hydrothermal crystallization at 100-130°C in a hydrothermal kettle using ethyl orthosilicate as the silicon source and titanium isopropoxide or butyl titanate as the titanium source. 10-12h Synthesis of TS-1 technology. [0005] In 2016, Xiong Gu...

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): C01B39/08
CPCC01B39/085C01P2002/72C01P2002/84C01P2004/62
Inventor 王新平张乐鉴朱晓晓
Owner DALIAN UNIV OF TECH
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