Silica-nitrilotriacetic acid-platinum catalyst and preparation method and use thereof

A nitrilotriacetic acid, silica technology, applied in physical/chemical process catalysts, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc. Problems such as low availability and affecting catalytic effect

Inactive Publication Date: 2018-05-29
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the supported platinum catalysts reported in many articles use inorganic materials modified with sulfur, phosphorus and other groups as the supporting materials. These catalysts are unstable at high temperatures due to the presence of

Method used

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  • Silica-nitrilotriacetic acid-platinum catalyst and preparation method and use thereof
  • Silica-nitrilotriacetic acid-platinum catalyst and preparation method and use thereof
  • Silica-nitrilotriacetic acid-platinum catalyst and preparation method and use thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] The preparation of the silicon dioxide supported platinum catalyst modified by polyamino polycarboxylate material, concrete steps are as follows:

[0071] Step 1. Amino functional modification of the basic solid-carrying material silica: SiO 2 Place in 6M hydrochloric acid and reflux at 60°C for 6 hours. After the reaction, wash with distilled water until neutral, and dry in a blast drying oven to obtain acidified silica gel. Take the acidified silica gel and place it in a vacuum drying oven at 130°C for 3h activation to obtain activated SiO 2 . Weigh 5g activated SiO 2Place in a three-necked flask filled with 50mL of toluene, add 7mL of APTES, namely 3-aminopropyltriethoxysilane, and stir mechanically at 110°C for 24h; product, and the product was placed in a 70 ° C forced air drying oven for 24 hours to obtain amino-bonded silica gel (APSG).

[0072] Step 2, discuss the preparation of three intermediates:

[0073] The first: silicon dioxide - diethyltriaminepenta...

Embodiment 2

[0081] To the IR of related substance in embodiment 1, 1 HNMR, 13 CNMR, TEM, EDS and XPS characterization: The structure of DTPAD was preliminarily confirmed by IR method. Such as Figure 4 As shown, 1816, 1770, 1641cm -1 The appearance of characteristic peaks such as the preliminary verification of the structure of the product; DTPAD was dissolved in DMSO for 1 HNMR and 13 Characterization of CNMR, DTPAD 1 HNMR such as Figure 5 As shown, 2.96(d,4H), 3.15(s,4H), 3.47(s,8H), 3.75(s,1H) and DTPAD 13 CNMR such as Figure 6 As shown, 49.47(2C), 51.48(2C), 54.81(4C), 168.90(1C), 172.57(4C), the results further verified the structure of DTPAD. Figure 7 The results compared to SiO 2 , SiO 2 -NH 2 , SiO 2 -DTPA, SiO2 2 - the difference in the IR absorption peaks of DTPA-Pt, Figure 8 compared to SiO 2 , SiO 2 -NH 2 , SiO 2 -NTA, SiO 2 -IR absorption peaks of NTA-Pt, SiO 2 , SiO 2 -NH 2 , SiO 2 -SA, SiO 2 - The IR absorption peaks of SA-Pt are different as F...

Embodiment 3

[0083] Measure three parts of 0.01mol 1-hexene respectively in centrifuge tubes, and add them respectively according to the preparation method of the present invention. During the immobilization process of platinum, mechanically stir under the protection of nitrogen, the solvent is ethanol, and the immobilization temperature is below 78°C. Prepared SiO 2 -DTPA-Pt (with a Pt content of 2.8×10 -3 mmol), SiO 2 -NTA-Pt (with a Pt content of 2.3×10 -3 mmol), SiO 2 -SA-Pt (with a Pt content of 2.9×10 -3 mmol), after activation at 60°C for 30 minutes, add 0.018 mol of methyl dichlorosilane, seal and add a condensing device, and continue to react for 4 hours. After the reaction, cool to room temperature, take the supernatant, and perform membrane filtration , GC test, GC results such as Figure 20 As shown, compared with the GC retention time of n-hexylmethyldichlorosilane standard substance, it can be preliminarily determined that the product is the target product n-hexylmethyld...

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Abstract

The invention discloses a silica-nitrilotriacetic acid-platinum catalyst and a preparation method and use thereof. The preparation method mainly comprises modifying SiO2-NH2 with NTA to obtain SiO2-NTA, and immobilizing platinum. The immobilization catalyst is successfully used for a hydrosilylation reaction of chain olefins (such as 1-heptene, 1-hexene, 1-octene, 1-decene, 1-dodecene, 1-tetradecene, 1-hexadecene and 1-octadecene) and methyl dichlorosilane, and a hydrosilylation reaction of cyclic olefin (such as norbornene), styrene, 2-hexene and methyl dichlorosilane.

Description

technical field [0001] The invention relates to the technical field of platinum catalyst preparation, in particular to the preparation and application of a green polyamino polycarboxylate material modified silica-supported platinum catalyst, especially to a silica-nitrilotriacetic acid-platinum catalyst, preparation Methods and uses. Background technique [0002] Platinum metal catalysts, as a class of heavy metal catalysts with a wide range of applications and a large amount, have been widely concerned by researchers at home and abroad. They are mainly used to catalyze important chemical reactions such as hydrosilylation, hydrogenation, and oxidation. industrial application value. Among them, the hydrosilylation reaction refers to the addition reaction between organic or inorganic Si-H bonds and unsaturated multiple bonds, which can form Si-C bonds to synthesize organosilicon compounds with grafted functional groups on carbon atoms. One of the important methods of silicon...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07F7/14
CPCB01J31/0271B01J31/0237B01J31/0254B01J2231/323C07F7/14
Inventor 李优鑫包建民邵冬云
Owner TIANJIN UNIV
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