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A safe and low-energy-consumption forming method of titanium-silicon molecular sieve spray

A technology of titanium-silicon molecular sieve and molding method, which is applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., and can solve problems such as low feed rate, difficulty in mixing uniformly, and high spray temperature

Active Publication Date: 2018-01-02
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, it is not easy to mix evenly with the original powder spray, and it is easy to block the nozzle
However, spraying with concentrated crystallization liquid or crystallization liquid and the original powder filter cake requires a higher spray temperature and a lower feed rate because the crystallization liquid contains more difficult-to-volatile organic compounds, which not only increases energy Consumption will also lead to safety hazards such as carbonization or explosion of organic matter

Method used

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  • A safe and low-energy-consumption forming method of titanium-silicon molecular sieve spray
  • A safe and low-energy-consumption forming method of titanium-silicon molecular sieve spray
  • A safe and low-energy-consumption forming method of titanium-silicon molecular sieve spray

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 (preparation of titanium silicon molecular sieve crystallization solution and titanium silicon molecular sieve raw powder)

[0026] According to the method described in "Zeolites, 1992, Vol.12: 943-950", the nano-sized TS-1 molecular sieve crystallization solution was prepared.

[0027] Mix 382.5 g of tetraethyl orthosilicate with 178.5 g of tetrapropylammonium hydroxide, add 1046.6 g of distilled water, mix and hydrolyze at normal pressure and 60 °C for 1.0 h to obtain a hydrolysis solution of tetraethyl orthosilicate , slowly added a solution consisting of 18.7 g tetrabutyl titanate and 85 g anhydrous isopropanol under vigorous stirring, and stirred the resulting mixture at 75 °C for 3 h to obtain a clear transparent colloid. Put this into a stainless steel sealed reaction kettle, crystallize at a constant temperature at 170 °C for 72 h, and then quench it to obtain a crystallization solution of nano-sized titanium-silicon molecular sieve.

[0028] A small ...

Embodiment 2

[0029] Embodiment 2 (preparation of titanium silicon molecular sieve cluster)

[0030] Take 800 g of the titanium-silicon molecular sieve crystallization solution obtained in Example 1, add 16.8 g of a pre-agglomeration aid polyacrylamide solution with a mass fraction of 1‰, stir for a period of time, and add dilute nitric acid to adjust the pH of the crystallization solution to 7. Then suction filtration and separation can obtain millimeter-sized titanium-silicon molecular sieve clusters.

[0031] A small amount of titanium-silicon molecular sieve clusters was taken and dried overnight at 120 °C. Analysis showed that the mass fraction of titanium-silicon molecular sieve clusters was 30%. After calcining in air atmosphere at 550 ℃ for 6 h, the titanium-silicon molecular sieve raw powder was obtained. The obtained sample was subjected to XRD analysis, and there were five characteristic diffraction peaks with diffraction angles 2θ=7.8°, 8.8°, 23.2°, 23.8°, and 24.3°.

Embodiment 3

[0032] Embodiment 3 (titanium silicon molecular sieve cluster spray)

[0033] Take 74.1 g of the millimeter-sized titanium-silicon molecular sieve cluster obtained in Example 2, add 5.44 g of silica sol (mass fraction 30%), 1.146 g of white carbon black, and 19.33 g of citric acid aqueous solution (pH value is 3-5), and the slurry solidifies The content is 25%, and then beat evenly. The slurry was sprayed under the conditions of an inlet temperature of 190 °C, an outlet temperature of 70 °C, and a feed rate of 18 g / min.

[0034] The formed particles were calcined under programmed temperature conditions, the heating rate was 5 ℃ / min, and the calcination was performed at 230 ℃ for 20 min, at 350 ℃ for 60 min, and at 720 ℃ for 3 h in an air atmosphere. The shaped titanium-silicon molecular sieve particle A is prepared. The photographs were characterized by SEM scanning electron microscope as figure 1 As shown, the shape of the formed titanium-silicon molecular sieve is circula...

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Abstract

The invention provides a safe and low-energy consumption molding method of titanium silicon molecular sieve spray. The method of the present invention is to pre-agglomerate the hydrothermally synthesized titanium-silicon molecular sieve crystallization liquid into millimeter-sized clusters by first adding auxiliary agents, separating out most of the organic matter such as water and template agents, and then dispersing the pre-agglomerated clusters into In an acidic aqueous solution, it is sprayed at a lower inlet temperature and a higher feed rate to cause secondary dehydration, agglomeration into micron-sized particles, and then roasting to obtain a spherical TS‑1 catalyst. The invention not only solves the problems of uneven mixing and clogging of nozzles when spraying raw powder, but also solves potential safety hazards such as carbonization or explosion of organic matter caused by high inlet and outlet temperatures when the crystallized liquid is concentrated and sprayed.

Description

technical field [0001] The invention relates to a safe and low-energy-consumption forming method of titanium-silicon molecular sieve spraying. Background technique [0002] Since Taramasso first synthesized titanium-silicon molecular sieve catalysts in 1983, the molecular sieves have excellent catalytic properties for the epoxidation of alkenes, the oxidation of alkanes, the oxidation of alcohols, the hydroxylation of phenols and benzene, etc. It is one of the research hotspots of new materials for green chemical technology. Titanium-silicon molecular sieves have the advantages of catalytic oxidation activity, high product selectivity, and mild reaction conditions when used in ammoximation reactions, and are considered to be typical representatives of environmentally friendly catalysts. [0003] Patent EP0200260 studies the formation of titanium-silicon molecular sieve catalysts, first using SiO 2 Wrap titanium-silicon molecular sieve crystals, and then spray molding to ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89
CPCB01J29/89B01J35/51
Inventor 王向宇叶晓雪高鑫刘杨青薛艳温贻强常中华
Owner ZHENGZHOU UNIV
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