2550-06-3Relevant articles and documents
Dendritic polarizing agents for DNP SENS
Liao, Wei-Chih,Ong, Ta-Chung,Gajan, David,Bernada, Florian,Sauvée, Claire,Yulikov, Maxim,Pucino, Margherita,Schowner, Roman,Schwarzw?lder, Martin,Buchmeiser, Michael R.,Jeschke, Gunnar,Tordo, Paul,Ouari, Olivier,Lesage, Anne,Emsley, Lyndon,Copéret, Christophe
, p. 416 - 422 (2016)
Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy (DNP SENS) is an effective method to significantly improve solid-state NMR investigation of solid surfaces. The presence of unpaired electrons (polarizing agents) is crucial for DNP, but it has drawbacks such as leading to faster nuclear spin relaxation, or even reaction with the substrate under investigation. The latter can be a particular problem for heterogeneous catalysts. Here, we present a series of carbosilane-based dendritic polarizing agents, in which the bulky dendrimer can reduce the interaction between the solid surface and the free radical. We thereby preserve long nuclear T′2 of the surface species, and even successfully enhance a reactive heterogeneous metathesis catalyst.
Preparation method of 3-chloropropyltrichlorosilane
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Paragraph 0003; 0024-0028, (2021/07/14)
The invention relates to a preparation method of 3-chloropropyl trichlorosilane, and belongs to the field of synthesis of silane coupling agents. According to the invention, by taking chloropropene and trichlorosilane raw materials, biopolymer wool as a ligand to synthesize a Wool-Pt catalyst and organic amines as an auxiliary agent, 3-chloropropyltrichlorosilane is prepared under normal pressure. The preparation method provided by the invention has the advantages of simple operation, high reaction activity, good selectivity, high product yield, low catalyst use cost, low energy consumption, safety, environmental protection and the like, and accords with industrial production.
Continuous production process and device for γ - chloropropyltrichlorosilane
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Paragraph 0060-0091, (2021/09/29)
The invention provides a continuous production process and device for γ -chloropropyltrichlorosilane, which comprises the following steps: respectively metering trichlorosilane and chloropropene into a reactor after being metered, and adding a catalyst. The first Crude products generated in the reactor are processed by a catalyst recovery device to obtain second crude products and a catalyst, the catalyst is returned to the reactor, second crude products are conveyed to first separation units. The second Crude product was separated by first separation units to give γ - chloropropyltrichlorosilane and propyltrichlorosilane. To the method and the device, trichlorosilane and chloropropene are continuously conveyed to the reactor for reaction, unreacted raw materials and the catalyst are returned to the reactor, and products and byproducts are separated and taken out. γ.
METHOD FOR THE DEHYDROGENATION OF DICHLOROSILANE
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Paragraph 0094, (2021/06/22)
Dichlorosilane and trichlorosilane are dehydrogenated at elevated temperature in the presence of an ammonium or phosphonium salt as a catalyst, and a halogenated hydrocarbon or hydrogen halide. The method may be used to synthesize organochlorosilane.
The ligand bidentate phosphine rhodium complex and its manufacturing method, and a hydrosilylation of allyl halide using a rhodium complex compound having a bidentate phosphine (by machine translation)
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Paragraph 0047-0048, (2020/09/16)
In the manufacture of a catalyst can be used as a complex 3 - [be] halo propyl silane and manufacturing method, a method for manufacturing 3 - halo propyl silane efficiently. [Solution] a rhodium complex catalyst or the like is used as a specific formula is obtained. [Drawing] no (by machine translation)
Method for producing chloropropyltrichlorosilane
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Paragraph 0038-0049; 0053-0059, (2020/03/14)
The invention provides an industrial production method of trichloro(3-chloropropyl)silane. A trichloro(3-chloropropyl)silane addition reaction coarse product is used as reaction substrates; the raw material reactants of chloropropene and trichlorosilane a
Method for preparing organic silicon by passage reaction device
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Paragraph 0048, (2016/10/17)
The invention provides a method for preparing organic silicon by a passage reaction device. Under the condition of main catalysts Z, hydrogen-containing silane X and an unsaturated compound Y are introduced into the passage reaction device; hydrosilylation reaction is performed to prepare the organic silicon, wherein the hydrogen-containing silane X has the structure being HSiRR'Cl, in the formula, R and R' are independently C1 to C16 alkyl or alkoxy; a=1, 2 or 3; b, c and d are respectively and independently 0, 1, 2 or 3; the unsaturated compound Y is a monoene compound or single-alkyne compound; the main catalysts Z are one or several mixed ones of single-component complexes or multi-component complexes of Pt, Pd, Rh, Ru, Cu, Ag, Au or Ir; the passage surface in which reaction flow contacts is subjected to inactivation treatment by an activating agent Z. The problems of long reaction period, poor stability and the like of large-sized reaction equipment are solved; the problem that mixing, pre-reaction and afterreaction are separated and are performed in multi-unit equipment is solved.
A γ-chloro propyl trichlorosilane synthesis method
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Paragraph 0025; 0026, (2017/05/12)
The invention discloses a synthesis method of gamma-chloropropyltrichlorosilane. In the method, trichlorosilane and chloropropene are used as raw materials, and a chloroplatinic acid-phenothiazine-organic amine complex is used as a catalyst. The method comprises the synthesis steps of firstly, adding the chloroplatinic acid-phenothiazine-organic amine complex as a catalyst into a pressure reaction kettle, dropwise adding two reaction materials, namely trichlorosilane and chloropropene, into the pressure reaction kettle at the reaction temperature of 100-180 DEG C through an overhead tank, and finishing the synthesis of the gamma-chloropropyltrichlorosilane after reacting at the temperature of 100-180 DEG C for 10-60min, wherein the dropwise adding time of the trichlorosilane and the chloropropene is 1.5-2.5h, and the inner pressure of the reaction kettle is 0.3-1.1MPa. The synthesis method of the gamma-chloropropyltrichlorosilane, disclosed by the invention, has the characteristics of short reaction time, high production efficiency, low material loss, high product yield and the like.
N-heterocyclic cabeen platinum a carboxylic acid metal salt complex integrated catalyst and preparation method thereof
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Paragraph 0102; 0103, (2017/08/15)
The invention relates to the field of organic high-molecular chemistry and discloses an N-heterocyclic carbene platinum complex metal carboxylate integrated catalyst and a preparation method thereof. The preparation method includes following steps: (1) carrying out a reaction between alkyl imidazole and halogenated carboxylic acid to obtain a carboxylic acid functionalized imidazolium salt; (2) carrying out a reaction with chlorides of ferrous, copper, zinc, calcium or magnesium to obtain a imidazole-based ionic liquid containing carboxylates containing the ferrous, the copper, the zinc, the calcium or the magnesium; (3) preparing an N-heterocyclic carbene ligand from the ionic liquid under effect of potassium tert-butyl alcohol; and (4) carrying out a reaction with a Karstedt catalyst to prepare the N-heterocyclic carbene platinum complex metal carboxylate integrated catalyst. The catalyst is high in selectivity, is free of generation of platinum black precipitation, is easy to separate and can be recycled.
Gamma-chloropropyltrichlorosilane production method and system
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Paragraph 0045; 0046; 0047; 0048; 0049; 0050; 0051; 0052, (2016/10/10)
The invention provides a gamma-chloropropyltrichlorosilane production method and system. The production system comprises a tubular reactor, a tank reactor of which an inlet is communicated with an outlet of the tubular reactor and a first outlet is communicated with a first inlet of the tubular reactor, and a rectification device of which an inlet is communicated with a second outlet of the tank reactor. Compared with the existing production system, the production system provided by the invention returns a part of a crude product in the tank reactor to the tubular reactor and an activated catalyst starts a reaction so that a catalyst starting process is avoided, reaction time is shortened and a catalyst use amount is reduced. A part of the crude product in the tank reactor is returned to the tubular reactor and a temperature in the tubular reactor is kept by heat so that energy consumption is reduced. Through control of a reaction temperature in the tubular reactor, reaction selectivity is improved. A reaction temperature in the tank reactor is improved so that the reaction is full.