Platinum catalyst resistant to sulfur poisoning and preparation method of platinum catalyst

A platinum catalyst, sulfur poisoning technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. It has the effect of inhibiting sulfur poisoning, stable catalyst activity and long storage period.

Active Publication Date: 2018-07-13
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the platinum catalyst will be poisoned when encountering the compound system containing S element, which will make the catalyst lose its catalytic activity. Therefore, the platinum catalyzed hydrosilylation system must strictly control the sulfur element in the system, and its use is limited.
Among them, the Pt catalyst complexes prepared by Speier catalyst and Karstedt catalyst are both homogeneous catalysts with high reactivity, but they will be poisoned when they encounter compounds containing N, P, and S elements. Loss of catalytic activity, which greatly limits the preparation of various special modified polysiloxanes by hydrosilylation
And the storage stability is poor, so it must be used up in a short time, otherwise gelation will occur, and the platinum complex will be reduced to Pt metal, which will turn black and lose its catalytic activity

Method used

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  • Platinum catalyst resistant to sulfur poisoning and preparation method of platinum catalyst
  • Platinum catalyst resistant to sulfur poisoning and preparation method of platinum catalyst
  • Platinum catalyst resistant to sulfur poisoning and preparation method of platinum catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. Pt(bphO) 2 (SEt 2 ) 2 Preparation of intermediates

[0046] In the four-necked flask equipped with a condenser tube and nitrogen inlet, feed nitrogen, add toluene (235.92g), ethanol (78.64g), 4-hydroxybiphenyl (34.00g, 0.2mol) and cis-dichlorobis(di Ethyl sulfide) platinum (II) (44.64g, 0.1mol), after stirring for 20min with a magnet, add dichloroacetic acid (0.71g) and trifluoromethanesulfonic acid (0.63g), stir for 10min, then use a peristaltic pump to control Drop distilled water (1.44g) into the reaction system at a rate of 6 drops / min, react at 80°C for 24h, cool down to room temperature, add ammonium bicarbonate (1.15g, 0.015mol) into the reaction system, and stir for 40min , filtered, and rectified by rotary distillation at 90°C for 80 minutes, weighed ethyl acetate (235.92g), took half of it and put it into the one-necked bottle after rotary steaming, filtered it with electromagnetic shock for 10 minutes, and rinsed the one-necked bottle with the remaining...

Embodiment 2

[0051] 1. Pt(bphO) 2 (SEt 2 ) 2 Preparation of intermediates

[0052] In the four-necked flask equipped with a condenser tube and nitrogen inlet, argon gas was introduced, and chloroform (168.58g), isopropanol (67.43g), 4-hydroxyethylbiphenyl (39.65g, 0.2mol) and cis- Dichlorobis(diethylsulfide)platinum (II) (44.64g, 0.1mol), after stirring for 30min with a magnet, add dichloroacetic acid (0.42g) and trifluoromethanesulfonic acid (0.42g), and stir for 10min , use a peristaltic pump to control the speed of 8 drops / min, and drop distilled water (1.17g) into the reaction system dropwise, react at a temperature of 90°C for 36h, cool to room temperature, add ammonium bicarbonate (0.55g, 0.007mol ) in the reaction system, stirred for 60 minutes, then rotary evaporated at 80°C for 80 minutes, weighed tetrahydrofuran (168.58g), took half of it and put it into the single-necked bottle after rotary steaming, filtered it with electromagnetic shock for 15 minutes, rinsed the single-nec...

Embodiment 3

[0057] 1. Pt(bphO) 2 (SEt 2 ) 2 Preparation of intermediates

[0058] In the four-necked flask that condenser tube and nitrogen inlet and constant pressure funnel are housed, pass into nitrogen, add cyclohexane (81.49g), isobutanol (48.89g), 4-(4-methylphenyl)phenol ( 36.85g, 0.2mol) and trans-dichlorobis(diethylsulfide) platinum (Ⅱ) (44.64g, 0.1mol), after stirring for 40min with a magnet, add 2-propiolic acid (0.24g) and strong acid The cationic resin (0.65g) was stirred for 30min, and distilled water (1.08g) was dripped into the reaction system at a rate of 10 drops / min controlled by a peristaltic pump. After reacting at a temperature of 80°C for 48h, the temperature was lowered to room temperature. , add ammonium bicarbonate (0.21g, 0.003mol) into the reaction system, stir for 40min, then spin evaporate at 90°C for 100min, weigh n-hexane (81.49g), take half of it and add it to the one-necked flask after spin steam, and electromagnetically Suction filtration after shaki...

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Abstract

The invention belongs to the technical field of organosilicon polymer, and discloses a platinum catalyst resistant to sulfur poisoning and a preparation method of the platinum catalyst. The platinum catalyst comprises the following molecular structural formulas (1) and (2), wherein the A group is an ether structural group containing double protonated biphenyl or derivatives of the double protonated biphenyl, and the B group is a nitrogen-containing six-membered ring pyridine structure or a derivative structural group of the nitrogen-containing six-membered ring pyridine structure. Through theprepared catalyst which is resistant to sulfur poisoning and has a specifically designed structure, not only can the defects of short storage time, inconvenient use and sufficiently sealed harsh storage conditions of of a current platinum catalyst be overcome, but also an effect of resistance to sulfur poisoning can be achieved; therefore, in a system in the presence of sulfur compounds, a strongcatalytic effect can still be achieved, and the platinum catalyst has no harsh synthesis conditions, a simple preparation process, simple steps, high production efficiency, stable products and low cost, so that industrial production of the platinum is realized.

Description

technical field [0001] The invention belongs to the technical field of organosilicon polymers, and more specifically relates to a platinum catalyst resistant to sulfur poisoning and a preparation method thereof. Background technique [0002] Since Sommer et al. discovered the hydrosilylation reaction in 1947, scientific researchers have done a lot of research and achieved great results. It is the most important synthetic route for organosilicon coupling agents and functional organosilicon compounds. In organosilicon chemistry Both occupy an important position in the organic silicon industry. Such as silicone glue, LED packaging glue, silicone pressure-sensitive adhesive, anti-stick coating, silicone rubber and special silicone oil and other fields. [0003] Transition metals are commonly used as catalysts for hydrosilylation reactions, among which platinum-gold complexes are the most active and widely used. At present, platinum complexes on the market are mainly prepared b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07F15/00
CPCB01J31/1815B01J31/2208B01J2531/828C07F15/0093
Inventor 刘珠刘晓暄苏嘉辉向洪平崔艳艳
Owner GUANGDONG UNIV OF TECH
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