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Catalyst for synthesizing amide and method for synthesizing N-mercaptoethyl-3-sulfydryl-propanamide

A technology for synthesizing amides and catalysts, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of N-mercaptoethyl-3-mercapto-propionamide The synthetic method has no problems such as reports, and achieves the effects of reducing the generation of by-products, controlling molecular weight, and having high product purity

Active Publication Date: 2014-12-10
SHANGHAI DONGSHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] But, there is no report about the synthetic method of N-mercaptoethyl-3-mercapto-propionamide

Method used

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  • Catalyst for synthesizing amide and method for synthesizing N-mercaptoethyl-3-sulfydryl-propanamide
  • Catalyst for synthesizing amide and method for synthesizing N-mercaptoethyl-3-sulfydryl-propanamide
  • Catalyst for synthesizing amide and method for synthesizing N-mercaptoethyl-3-sulfydryl-propanamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1, prepare SO 4 2- / TiO 2 -ZnO Mixed Crystal Solid Acid Support Coordination Catalyst

[0062] (a) Chemical composition: 100 parts of deionized water, TiCl 4 20 parts, 20 parts of zinc nitrate, 50 parts of 25wt% ammonia water, 5 parts of sodium tetraborate, 3 parts of basic nickel carbonate, 1 part of triphenyl cobalt phosphide, and 3 parts of ferrocene.

[0063] (b) TiCl 4 1. Add zinc nitrate to deionized water. In a high-speed disperser (1500 rpm), the temperature rises to 95°C. Add ammonia water to the mixture, then add sodium tetraborate and basic nickel carbonate, and continue to keep warm for 3 hours. , stop stirring, lower to normal temperature, let stand, filter to collect the precipitate, wash with deionized water, and vacuum dry at 120°C.

[0064] (c) Calcining the product of (b) process at 850° C. for 3 hours.

[0065] (d) The product of (c) process is immersed in 10wt% sulfuric acid solution for 2 hours, and then put into 550 ° C ...

Embodiment 2

[0067] Embodiment 2, prepare SO 4 2- / TiO 2 -ZnO Mixed Crystal Solid Acid Support Coordination Catalyst

[0068] (a) Chemical composition: 100 parts of deionized water, TiCl 4 28 parts, 15 parts of zinc nitrate, 60 parts of 25wt% ammonia water, 7 parts of sodium tetraborate, 4 parts of basic nickel carbonate, 3 parts of triphenyl cobalt phosphide, and 2 parts of ferrocene.

[0069] (b) TiCl 4 1. Add zinc nitrate to deionized water. In a high-speed disperser (1500 rpm), the temperature rises to 90°C. Add ammonia water to the mixture, then add sodium tetraborate and basic nickel carbonate, and continue to keep warm for 2 hours. , stop stirring, lower to normal temperature, let stand, filter to collect the precipitate, wash with deionized water, and vacuum dry at 120°C.

[0070] (c) Calcining the product of (b) process at 900° C. for 3 hours.

[0071] (d) The product of the (c) process is immersed in a 10wt% sulfuric acid solution for 2 hours, and then baked at ...

Embodiment 3

[0073] Embodiment 3, prepare SO 4 2- / TiO 2 -ZnO Mixed Crystal Solid Acid Support Coordination Catalyst

[0074] (a) Chemical composition: 100 parts of deionized water, TiCl 4 24 parts, 19 parts of zinc nitrate, 80 parts of 25wt% ammonia water, 7 parts of sodium tetraborate, 3 parts of basic nickel carbonate, 2 parts of triphenyl cobalt phosphide, and 2 parts of ferrocene.

[0075] (b) TiCl 4 1. Add zinc nitrate to deionized water. In a high-speed disperser (1500 rpm), the temperature rises to 90°C. Add ammonia water to the mixture, then add sodium tetraborate and basic nickel carbonate, and continue to keep warm for 2 hours. , stop stirring, lower to normal temperature, let stand, filter to collect the precipitate, wash with deionized water, and vacuum dry at 120°C.

[0076] (c) Calcining the product of (b) process at 970° C. for 3 hours.

[0077] (d) The product of the (c) process is immersed in 10wt% sulfuric acid solution for 2 hours, and then baked at 64...

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Abstract

The invention provides a catalyst for synthesizing amide, especially N-mercaptoethyl-3-sulfydryl-propanamide, and a preparation method of the catalyst. The method comprises the following steps: mixing a titanium salt solution, a zinc salt solution and ammonia water, tetraborate and basic nickel carbonate, collecting precipitation, then roasting, dipping and roasting in sulfuric acid, and then mixing the roasted product with (triphenylphosphine) cobalt (I) nitro-hydride and a cyclopentadienyl iron solution. The invention further provides a method for synthesizing N-mercaptoethyl-3-sulfydryl-propanamide by using a mixed crystal solid acid carrier coordination catalyst, the synthesized N-mercaptoethyl-3-sulfydryl-propanamide can be used for the regulation of the molecular weight in polymerization, especially the addition polymerization, the molecular weight can be effectively controlled, and the production of the byproducts is reduced.

Description

technical field [0001] The invention relates to a catalyst for synthesizing amides and a method for synthesizing amides, in particular to a catalyst for synthesizing N-mercaptoethyl-3-mercapto-propionamide, a preparation method of the catalyst, and the N- Synthetic method of mercaptoethyl-3-mercapto-propionamide. Background technique [0002] In polymer synthesis chemistry, controlling the molecular weight is a very important process. By controlling the molecular weight, a variety of new polymer materials with different properties can be synthesized from the same monomer. Molecular weight regulators, as the name implies, are substances used to adjust the molecular weight of polymers. They do not affect the polymerization reaction speed, but can control the length (molecular weight) of polymer chains, that is, control the degree of polymerization or viscosity. In order to manufacture more new materials with high-tech value, many chemists seek to choose various types of molec...

Claims

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Application Information

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IPC IPC(8): B01J31/38C07C323/52C07C319/12
Inventor 施晓旦郭和森
Owner SHANGHAI DONGSHENG NEW MATERIALS
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