Method for synthesizing ZSM-5 molecular sieve
A technology of ZSM-5 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems such as ineffective treatment of mother liquor, and achieve the effect of reducing synthesis cost and reducing pollution
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[0022] Preparation of standard sample: Dissolve 0.56 g of NaOH (chemically pure) in 28 g of deionized water, add 1.34 g of Al under stirring 2 (SO 4 ) 3 18H 2 O and 1.46 grams of n-butylamine (chemically pure), then add 12 grams of 40-120 mesh silica gel (produced by Qingdao Ocean Chemical Factory) to obtain a mixture. The mixture was placed in a sealed stainless steel reaction kettle, hydrothermally crystallized at 170° C. for 24 hours, and the product was obtained after cooling. The product was filtered, washed, and dried to obtain a standard sample. The XRD crystal phase diagram of the standard sample is as follows figure 1 Shown, show that this standard sample is ZSM-5 molecular sieve.
[0023] In addition, the mother liquor produced during the preparation of titanium-silicon molecular sieves used in each embodiment of the present invention is the mother liquor obtained by the following method:
Embodiment 1
[0026] This example illustrates the synthesis method of the ZSM-5 molecular sieve of the present invention.
[0027] To 11.3 grams of water glass solution (containing 3.5% by weight of Na 2 O, 10 wt% SiO 2 ), add 5 grams of mother liquor for preparing titanium-silicon molecular sieves, and then add 1.3 grams of aluminum sulfate aqueous solution (containing 2.5% by weight of Al 2 o 3 ), and then use 20% sulfuric acid solution to adjust the pH value to 11.5 to obtain a reaction mixture. In the reaction mixture, the molar ratio of SiO 2 / Al 2 o 3 =72, Na 2 O / SiO 2=0.27,H 2 O / SiO 2 =36. SiO 2 Based on the weight of the total silicon source in the reaction mixture, the content of the silicon source from the mother liquor is 18% by weight, and the content of the external silicon source is 82% by weight.
[0028] Then the reaction mixture was hydrothermally crystallized in an autoclave at 180° C. for 20 hours, cooled to room temperature after the crystallization was compl...
Embodiment 2
[0030] This example illustrates the synthesis method of the ZSM-5 molecular sieve of the present invention.
[0031] 3.2 grams of silica sol (containing 30% by weight SiO 2 ), add 0.13 gram of sodium hydroxide and 10 gram of mother liquor for preparing titanium-silicon molecular sieve, then add 1.3 gram of aluminum sulfate aqueous solution (containing 2.5% by weight Al 2 o 3 ) to obtain a reaction mixture. In the reaction mixture, the molar ratio of SiO 2 / Al 2 o 3 =50, Na 2 O / SiO 2 =0.1,H 2 O / SiO 2 =43. SiO 2 Based on the weight of the total silicon source in the reaction mixture, the content of the silicon source from the mother liquor is 34% by weight, and the content of the external silicon source is 66% by weight.
[0032] Then the reaction mixture was hydrothermally crystallized in an autoclave at 180° C. for 30 hours, cooled to room temperature after the crystallization was completed, filtered, and the filter cake obtained after filtration was baked at 120° C...
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