Polyester polycondensation catalyst and preparation method and application thereof
A polycondensation catalyst and catalyst technology, applied in the field of polyester polycondensation catalyst and its preparation and application, can solve problems affecting product performance, achieve the effects of suppressing side reactions, high brightness, and improving activity
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[0024] Example 1. Preparation of polyester polycondensation catalyst
[0025] Take 5 mL of concentrated hydrochloric acid, 10 mL of ethanol, mix with 19.6 g of ethyl orthosilicate (TEOS) at room temperature, and stir for 1 hour to obtain the product A SiO 2 Sol.
[0026] Mix 2.5 g of tetrabutyl titanate and 10 mL of concentrated hydrochloric acid at room temperature, and stir at room temperature for 1 hour to obtain the product BTiO 2 Sol.
[0027] The product A SiO 2 Sol and product B TiO 2 The sol was mixed and stirred at 50°C for 12 hours to obtain the product CTiO 2 / SiO 2 Sol.
[0028] At 80℃, the product C TiO 2 / SiO 2 The sol was dried under vacuum to obtain catalyst D.
[0029] The product C TiO 2 / SiO 2 The sol was freeze-dried to obtain catalyst E.
[0030] The product C TiO 2 / SiO 2 The sol is placed in a semi-permeable membrane and placed in deionized water to remove Cl - , Get catalyst F.
[0031] The product C TiO 2 / SiO 2 React with 0.3 g of caprolactam to obtain catalyst G...
Example Embodiment
[0034] Example 2: Preparation of polyester polycondensation catalyst
[0035] Take 5 mL of concentrated hydrochloric acid, 10 mL of ethanol, mix with 19.6 g of ethyl orthosilicate (TEOS) at room temperature, and stir for 1 hour to obtain the product A SiO 2 Sol.
[0036] Take 2.5g TiCl 4 Add 20ml EG dropwise at 0℃, and pass in dry NH 3 The gas is prepared according to the Nelles method provided in the following literature, but the product is not hydrolyzed, and then it is supported on SiO 2 Above the sol: Li Dacheng, Zhou Dali, Chen Chaozhen, etc. Synthesis of Titanium Ethoxide and Preparation of TiO by Hydrolysis 2 Research on Micropowder[J]. Functional Materials, 1995, 26(3):278-282.
[0037] In the above preparation steps, quickly add the resulting product to A to obtain TiO 2 / SiO 2 Sol J.
[0038] J was freeze-dried under vacuum to obtain catalyst K.
[0039] Treat J with a low-temperature hydrothermal method, with a hydrothermal temperature of 50-200°C and a hydrothermal time of ...
Example Embodiment
[0046] Example 3. Application of polyester polycondensation catalyst as a catalyst in the preparation of polyester materials
[0047] The steps for preparing PET polyester material using the polyester polycondensation catalyst provided in Example 1 of the present invention are as follows:
[0048] Take 86.4 g of terephthalic acid and 32.3 g of ethylene glycol, and carry out esterification under the conditions of a pressure of 0.3 MPa and a temperature of 220-250° C. until the theoretical value of water is evaporated. 1 mg of one of the catalysts prepared in Example 1 (catalyst D-I) was added to obtain PET material N-S, respectively. The polycondensation time and product properties are shown in Table 2.
[0049] It can be seen from the data in Table 2 that the electron binding energy of titanium and the particle size of the catalyst greatly affect the activity of the catalyst: for catalysts D, E, and F, the particle size decreases in order, the activity increases, and the product per...
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