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A kind of preparation method of large particle diameter titanium silicon molecular sieve

A technology of titanium-silicon molecular sieve and large particle size, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve problems such as separation and recovery of difficult products, and achieve less synthesis steps and lower cost Inexpensive, uniform grain effect

Active Publication Date: 2017-12-22
JUHUA GROUP TECH CENT
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  • Claims
  • Application Information

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Problems solved by technology

[0008] The present invention aims at the deficiencies of the prior art, and provides a method for preparing a large-diameter titanium-silicon molecular sieve. The titanium-silicon molecular sieve prepared by the present invention can better solve the problem that the small-particle-diameter titanium-silicon molecular sieve is difficult to separate from the product in industry. and recovery issues, to improve catalyst reuse

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  • A kind of preparation method of large particle diameter titanium silicon molecular sieve
  • A kind of preparation method of large particle diameter titanium silicon molecular sieve
  • A kind of preparation method of large particle diameter titanium silicon molecular sieve

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preparation example Construction

[0030] The preparation method of a kind of large particle size titanium silicon molecular sieve of the present invention comprises the following steps:

[0031] 1) First, at a temperature of 30-90°C, add the inorganic silicon source to the organic template aqueous solution to form the first mixed solution. After the addition, stir with a stirrer for 0.2-2 hours, and wait for the first mixed solution to mix evenly Finally, add an inorganic titanium source to form a second mixed solution. After the addition is complete, stir with a stirrer for 0.5 to 4 hours. After the second mixed solution is evenly mixed, add an alkali source at one time to form a third mixed solution, preferably the second mixed solution. The preparation temperatures of the first mixed solution, the second mixed solution and the third mixed solution are all 40-60°C, and the SiO in the third mixed solution is molar ratio in the inorganic silicon source 2 : TiO in inorganic titanium source 2 : organic template...

Embodiment 1

[0042] 15.2g silica sol (SiO 2 content of 30%) was slowly added to tetrapropylammonium hydroxide aqueous solution, stirred at a temperature of 40°C for 30 minutes to make it evenly mixed, slowly added titanium trichloride solution, stirred for 40 minutes, then added ammonia water, stirred for 60 Minutes to obtain a mixed solution, wherein the molar ratio of silica sol: titanium trichloride: tetrapropyl ammonium hydroxide: ammonia water: water is 1:0.02:0.1:40:60. Put the above mixed solution into a sealed stainless steel reaction kettle, heat and statically crystallize at a reaction temperature of 170°C for 4 days, obtain a filter cake after filtration, then wash the filter cake with deionized water, and place the obtained filter cake at 120°C Carry out vacuum drying at high temperature, and finally roast at 550° C. for 6 hours to obtain titanium-silicon molecular sieve material A (volume average diameter is 25.9 microns, median value of particle diameter (d 50 ) is 24.3 micr...

Embodiment 2

[0044] 20.5g silica sol (SiO 2 content of 30%) was slowly added to tetrapropylammonium hydroxide aqueous solution, stirred for 1 hour at a temperature of 80°C to make it evenly mixed, slowly added titanium sulfate aqueous solution, stirred for 30 minutes, then added ammonia water, and stirred for 40 minutes to obtain The mixed solution, wherein the molar ratio of silica sol: titanium sulfate: tetrapropyl ammonium hydroxide: ammonia water: water is 1:0.015:0.08:50:50. Put the above mixed solution into a sealed stainless steel reaction kettle, heat and statically crystallize at a reaction temperature of 170°C for 6 days, obtain a filter cake after filtration, then wash the filter cake with deionized water, and place the obtained filter cake at 120°C Carry out vacuum drying at high temperature, and finally roast at 550° C. for 8 hours to obtain titanium-silicon molecular sieve material B (volume average diameter is 21.5 microns, median value of particle diameter (d 50 ) is 18.4 ...

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Abstract

The invention discloses a preparation method of a large-particle-size titanium silicon molecular sieve, which comprises the following steps: adding an inorganic silicon source into an organic template water solution at 30-90 DEG C, sufficiently stirring for 0.2-2 hours, adding an inorganic titanium source, sufficiently stirring for 0.5-4 hours, uniformly mixing, adding an alkali source at one time, and carrying out hydrothermal crystallization on the mixed solution (composed of the following components in parts by mole: 1 part of SiO2 in the inorganic silicon source, 0.01-0.03 part of TiO2 in the inorganic titanium source, 0.02-0.2 part of organic template, 20-80 parts of alkali source and 30-70 parts of alkali source) at 120-200 DEG C for 2-10 days; and filtering, washing, drying and roasting to obtain the titanium silicon molecular sieve. The titanium silicon molecular sieve catalyst prepared by the method has uniform particle size, has the average particle size of greater than 10 micrometers, and is easy for separation and recovery after reaction. The method can enhance the reutilization rate, has the advantages of fewer synthesis steps, low cost and high product quality stability, and is simple to operate.

Description

technical field [0001] The invention relates to a preparation method of a titanium-silicon molecular sieve, in particular to a preparation method of a large-diameter titanium-silicon molecular sieve. Background technique [0002] Titanium-silicon molecular sieve is the introduction of transition metal titanium atoms into the molecular sieve framework with a certain topology to form a porous crystalline material with catalytic oxidation activity. Titanium-silicon molecular sieves can be used to catalyze various organic oxidation reactions, such as olefin epoxidation, alkane partial oxidation, alcohol oxidation, phenol hydroxylation, cyclic ketone ammoxidation, etc. As an oxidant, hydrogen oxide has high reaction selectivity, relatively simple process, and has incomparable advantages of energy saving, economy, and environmental friendliness compared with traditional oxidation systems, and is considered to be a typical representative of environmentally friendly catalysts. [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
CPCC01B39/085C01P2002/82C01P2004/03C01P2004/51C01P2004/61
Inventor 马利勇李宏峰周强林晓云
Owner JUHUA GROUP TECH CENT
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