Method for synthesizing titanium silicon zeolite material
A technology of titanium silicalite and zeolite, which is applied in the field of synthetic titanium silicalite materials, can solve the problems of poor activity stability, easy deactivation, low activity of titanium silicalite, etc., and achieve increased selectivity of reaction products, reduced preparation costs, and good The effect of catalytic activity stability
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[0031] Example 1
[0032] 20 grams of silicalite S-1 was added to the tetrapropylammonium hydroxide aqueous solution and stirred and mixed uniformly, then tetrabutyl titanate was added and mixed to obtain a mixture composition: silicalite (g): titanium source (mol ): Alkali source (mole): Water (g) = 100:0.2:0.2:600. Then it was put into a stainless steel sealed reactor and hydrothermally treated at a temperature of 150°C and autogenous pressure for 48 hours. The resultant was filtered, washed with water, dried naturally, and calcined at 550°C for 5 hours to obtain titanium silicalite material A. Its XRD phase diagram is as figure 1 As shown in (B), it is similar to the comparative example; the Fourier infrared spectrum is shown as figure 2 As shown in (b), similar to the comparative example, at 960cm -1 There is an infrared absorption peak that is not found in the all-silicon molecular sieve nearby, indicating that the titanium has entered the molecular sieve framework, 960cm -...
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[0033] Example 2
[0034] Add 20 grams of silicalite S-1 to the sodium hydroxide aqueous solution and stir and mix uniformly, then add tetrapropyl titanate and mix evenly to obtain the composition of the mixture: silicalite (g): titanium source (mole): alkali Source (mole): water (g) = 100:5.0:1.2:3500. Then put it into a stainless steel sealed reactor, hydrothermally heat it at a temperature of 180°C and autogenous pressure for 24 hours, filter the resultant, wash with water, dry naturally, and calcinate at 550°C for 5 hours to obtain titanium silicalite material B. The XRD phase diagram is as figure 1 As shown in (C), it is similar to the comparative example; the Fourier infrared spectrum is shown as figure 2 As shown in (c), similar to the comparative example, the infrared spectrum is at 960 cm -1 There is an infrared absorption peak near the silicon molecular sieve, indicating that the titanium has entered the molecular sieve frame, 960cm -1 Absorption peak and 550cm -1 Abso...
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[0035] Example 3
[0036] Add 20 grams of silica zeolite S-1 to the tetrapropyl ammonium hydroxide aqueous solution and stir and mix uniformly, then add tetraethyl titanate and mix, to obtain a mixture composition: silica zeolite (g): titanium source (mole ): Alkali source (mole): Water (g) = 100:2.0:1.0:1200. Then it was put into a stainless steel sealed reactor and hydrothermally treated at a temperature of 150°C and autogenous pressure for 48 hours. The resultant was filtered, washed with water, dried naturally, and calcined at 550°C for 5 hours to obtain titanium silicalite material C. In the ultraviolet-visible spectrum, there is a strong absorption band near the wavelength of 210nm, but no absorption near 340nm, indicating that all titanium enters the framework, and no non-framework titanium is produced. Its infrared spectrum 960cm -1 Absorption peak and 550cm -1 Absorption peak intensity ratio I 960 / I 550 The data are listed in Table 1.
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