ETS-10 titanium silicalite molecular sieve modification method

A titanium-silicon molecular sieve and modification technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of low product crystallinity, low Al content, and many factors that limit the amount of Al introduction.

Active Publication Date: 2013-02-13
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the ETS-10 titanium-silicon molecular sieve containing Al is synthesized by the direct synthesis method, the synthe...

Method used

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  • ETS-10 titanium silicalite molecular sieve modification method
  • ETS-10 titanium silicalite molecular sieve modification method
  • ETS-10 titanium silicalite molecular sieve modification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Get two parts of 20.00g of the original powder of ETS-10 titanium silicon molecular sieve, add 200.00g deionized water respectively, under the condition of stirring, then add 1.67g NaOH particles respectively (at this time the alkali concentration is about 0.2mol / L), get two mixed slurries;

[0054] After the two mixed slurries were stirred evenly, they were respectively placed in a water bath at 90°C, and the stirring was continued for 1h and 2h respectively;

[0055] Filter the obtained two slurries, wash the solid product repeatedly until the pH of the washing liquid is less than 9, and then place the solid product at 120°C for 12 hours to obtain the ETS-10 titanium silicon molecular sieve modified by alkali treatment. They are marked as AT-1 and AT-2 respectively, and their pore structure data are shown in Table 2, and their nitrogen adsorption-desorption isotherms and pore distribution curves are shown in Table 2, respectively. Figure 2a with Figure 2b shown. ...

Embodiment 2

[0059] Take two parts of 20.00g of ETS-10 titanium silicon molecular sieve raw powder, add 200.00g of deionized water respectively, and add 4.17g of NaOH particles respectively under the condition of stirring (at this time, the alkali concentration is about 0.5mol / L);

[0060] After the two mixed slurries were stirred evenly, they were respectively placed in a water bath at 90°C, and the stirring was continued for 1h and 2h respectively;

[0061] Filter the obtained two slurries, wash the solid product repeatedly until the pH of the washing liquid is less than 9, and then place the solid product at 120°C for 12 hours to obtain the ETS-10 titanium silicon molecular sieve modified by alkali treatment. They are respectively marked as AT-3 and AT-4, and their pore structure data are shown in Table 3, and their nitrogen adsorption-desorption isotherms and pore distribution curves are shown in Table 3, respectively. Figure 3a with Figure 3b shown.

[0062] table 3

[0063] ...

Embodiment 3

[0065] Get five parts of 20.00g of the original powder of ETS-10 titanium silicon molecular sieve, add 200.00g of deionized water respectively, under the condition of stirring, then add 1.67g, 3.33g, 5.00g, 6.67g, 8.33g of NaOH particles (this Alkali concentration corresponds to 0.2mol / L, 0.4mol / L, 0.6mol / L, 0.8mol / L, 1.0mol / L respectively);

[0066] After stirring the five mixed slurries evenly, place them in a water bath at 90°C and continue stirring for 1 hour respectively;

[0067] Filter the obtained five slurries, wash the solid product repeatedly until the pH of the washing liquid is less than 9, and then place the solid product at 120°C for 12 hours to obtain the ETS-10 titanium-silicon molecular sieve modified by alkali treatment. They are respectively marked as AT-5, AT-6, AT-7, AT-8, and AT-9, and their pore structure data are shown in Table 4, and their nitrogen adsorption-desorption isotherms and pore distribution curves are shown in Table 4, respectively. Figur...

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Abstract

The invention relates to an ETS-10 titanium silicalite molecular sieve modification method. The ETS-10 titanium silicalite molecular sieve modification method provided by the invention comprises the following steps: alkali treatment modification: carrying out alkali treatment modification of EST-10 titanium silicalite molecular sieve raw powder through adopting an alkaline solution, filtering, washing, and drying to obtain alkali treatment modified ETS-10 titanium silicalite molecular sieve; and realuminated modification treatment: carrying out realuminated modification treatment of the alkali treatment modified ETS-10 titanium silicalite molecular sieve through adopting an aluminum salt solution or an aluminate solution, filtering, washing, drying, and roasting to obtain the alkali treatment modification and realuminated modification treated ETS-10 titanium silicalite molecular sieve. The modification method provided by the invention adopts the alkali treatment modification and the realuminated modification treatment of the EST-10 titanium silicalite molecular sieve raw powder to be carried out, so the surface phase of the EST-10 titanium silicalite molecular sieve is rich in titanium and aluminum, abundant meso-structures are introduced, and the skeletal acidity is improved.

Description

technical field [0001] The invention relates to a method for modifying a titanium-silicon molecular sieve, in particular to a method for modifying an ETS-10 titanium-silicon molecular sieve, and belongs to the technical field of molecular sieve modification. Background technique [0002] ETS-10 titanium silicon molecular sieve was first reported and synthesized by Kuznicki et al. of Engelhard Company in 1989 (USP 4853202). The framework of ETS-10 titanium silicate molecular sieve is composed of six coordination (TiO 6 ) 2- and four-coordinated (SiO 4 ) structures together to form the largest twelve-membered ring microporous channel structure (0.49 × 0.76nm). Among them, the hexacoordinated (TiO 6 ) 2- The structure has two negative charges, so ETS-10 has ion exchange properties and can introduce acidity, which is compatible with neutral four-coordinated (TiO 4 ) are very different. The total specific surface area of ​​ETS-10 titanium silicon molecular sieve is general...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 申宝剑李景郭巧霞张兴全张志华赵野田然张文成郭金涛温广明王甫村
Owner PETROCHINA CO LTD
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