Preparation and application of a green and environmentally friendly immobilized platinum catalyst
A platinum catalyst, a green and environmentally friendly technology, used in catalytic reactions, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. The effect of large specific surface area and high mechanical strength
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Embodiment 1
[0051] SiO 2 -The preparation of EDTA-Pt catalyst, step is as follows:
[0052] Step 1. Preparation of ethylenediaminetetraacetic dianhydride (EDTAD): Weigh 20 g of ethylenediaminetetraacetic acid (EDTA) into a 100 mL three-necked flask; add 34 mL of pyridine and 26 mL of acetic anhydride to the three-necked flask in sequence, Mechanically stirred and refluxed at 65°C for 24 hours; after the reaction, suction filtered to obtain a solid product, which was washed with ether and dried to obtain the crude EDTAD; put the crude EDTAD in a 100 mL Erlenmeyer flask, and add 55 mL of acetic anhydride, After stirring intermittently for 30 min, after suction filtration, wash with acetic anhydride, then wash twice with diethyl ether, drain, and vacuum dry at 65°C to obtain EDTAD, as figure 1 shown in .
[0053] Step 2. Functional modification of the basic immobilized material silica: put the silica gel in 6 M hydrochloric acid and reflux at 60 °C for 6 h. After the reaction, wash with wa...
Embodiment 2
[0057] To the IR, EDS, EDS of related product in embodiment 1 1 HNMR characterization: The structure of EDTAD was preliminarily confirmed by KBr pellet method. Such as image 3 Shown, 1810, 1761, 1127, 1072, 1008 cm -1 The appearance of other characteristic peaks preliminarily verified the structure of the product. EDTAD was dissolved in DMSO for 1 HNMR characterization, such as Figure 4 As shown, the results of d 3.71 (s, 8H), 2.67 (s, 4H) further verified the structure of EDTAD. By comparing SiO 2 , SiO 2 -EDTA, SiO 2 - The difference in the IR absorption peak of EDTA-Pt, Figure 5 Results Preliminary verification successfully carried out functional modification and immobilization on silica gel. Using EDS on SiO 2 -EDTA-Pt for further verification as Figure 6 As shown, the appearance of C, H, O, N, Cl, Pt and other elements further indicates that the modification and immobilization of silica gel are successful.
Embodiment 3
[0059] Measure 5 parts of 0.01 molmol 1-hexene respectively and place them in centrifuge tubes, and respectively add SiO 2 -EDTA-Pt (Pt content is 0.01 ×10 -4 mol), activated at 40 °C, 50 °C, 60 °C, 70 °C, and 80 °C for 30 min respectively; 0.0102 mol of methyl dichlorosilane was added, sealed and equipped with a condensing device, and the reaction was continued for 4 h; after the reaction, Cool to room temperature, take supernatant, carry out membrane filtration, GC test, GC result is as follows Figure 7 shown. Compared with the GC retention time of n-hexylmethyldichlorosilane standard substance, it can be initially determined that the product is the target product, and the results are as follows Figure 8 shown. product by 1 H NMR further confirmed that it was the target product n-hexylmethyldichlorosilane, and the yield could reach the maximum yield of 88.0% at 60 ℃. 1 H NMR results as Figure 9 shown. 1 H NMR (CDCl 3) δ: 1.50 (m, 2H), 1.38 (dt, 2H), 1.30 (dd, 4H)...
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