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
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[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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