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Compound containing tertiary amine derivatives, preparation method and application thereof

A technology containing tertiary amine urea and derivatives, applied in the field of fine chemicals

Inactive Publication Date: 2012-06-20
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a kind of amine catalyst with high catalytic activity, good stability and low corrosion to equipment in view of some problems existing in amine catalysts currently used for synthesizing polyurethane

Method used

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  • Compound containing tertiary amine derivatives, preparation method and application thereof
  • Compound containing tertiary amine derivatives, preparation method and application thereof
  • Compound containing tertiary amine derivatives, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 2.2 g of ethylene carbonate into a 100 mL one-necked flask, and slowly add 5.8 g of N,N-diethylethylenediamine dropwise. Place the flask in an oil bath, connect a spherical condenser and a three-way joint, use a vacuum pump to evacuate the air in the system, and fill it with nitrogen as a protective gas. The temperature of the oil bath was raised to 120°C and the reaction was stirred at reflux. The reaction was stopped after 24 hours. After the product was cooled, the product was rotary evaporated at 90° C. for 1 hour under vacuum conditions to obtain an almost colorless transparent viscous liquid. The above liquid was analyzed by HPLC-MS combined technology, and the peak with a mass-to-charge ratio of 258, the molecular ion peak with a mass-to-charge ratio of 257, and the main fragment ion peak with a mass-to-charge ratio of 158 were detected in ESI-mode. The reactants and possible products of this reaction are analyzed and compared to determine that the product c...

Embodiment 2

[0021] Dissolve 4.2 grams of α, α'-dimethylol propionic acid in 86 grams of polyoxypropylene glycol and transfer to a 250 mL round bottom flask, then slowly add 29 grams of toluene diisocyanate dropwise, and stir the reaction at 80°C for 24 hours to make a prepolymer.

[0022] Weigh 4.2 g of [(C2H5)2NCH2CH2NH]2CO prepared in Example 1 and dissolve it in 220 g of pure water, add the above-mentioned prepolymer under stirring, and continue stirring for 4 hours to obtain a white emulsion. Add 22 grams of polyacrylic acid as a thickener to the emulsion under stirring, then add 60 grams of pure water, and stir for two hours to prepare the adhesive W. The adhesive adhesive layer has good flexibility and can be used for bonding between foam plastics.

Embodiment 3

[0024] 1.5 g of urea was added into a 100 mL one-necked flask, and then 5.7 g of N-(2-aminoethyl)pyrrolidine was slowly added dropwise. Place the flask in an oil bath, connect a spherical condenser and a three-way joint, use a vacuum pump to evacuate the air in the system, and fill it with nitrogen as a protective gas. Raise the temperature of the oil bath to 140°C, stir and reflux the reaction, and use a vacuum pump to pump out the ammonia gas produced by the reaction after 2 hours, 4 hours, 8 hours, 18 hours, and 20 hours, and fill it in time. nitrogen. The reaction was stopped after 24 hours. After the product was cooled, the product was rotary evaporated at 90° C. for 1 hour under vacuum conditions to obtain a colorless transparent viscous liquid. The yield of the reaction under this condition was 88.3%. The above liquid was analyzed by HPLC-MS technology, and the peak with a mass-to-charge ratio of 254, the molecular ion peak with a mass-to-charge ratio of 253, and the ...

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Abstract

The invention relates to a compound containing tertiary amine derivatives and a preparation method. The derivatives can be used as the formula components of a catalyst and a binder for synthesizing polyurethane. The invention provides a method for synthesizing the compound containing the tertiary amine derivatives. The method comprises the following steps: mixing ethylene carbonate or urea with NH2XNR2 at a mass ratio of 1: 2; performing a constant temperature backflow reaction at 100-140 DEG C and under the condition of introducing N2 as protective gas; and separating and purifying the obtained product, thereby obtaining the compound containing the tertiary amine derivatives. When the compound is taken as the catalyst for synthesizing the polyurethane, the catalytic activity is higher. The compound is higher in boiling point, lower in toxicity and wider in application prospect.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to a compound containing tertiary urea derivatives, a preparation method and application thereof. Background technique [0002] Before 1958, the production of polyurethane foam used the prepolymer method, the so-called two-step method. Since then, due to the emergence of two types of catalysts represented by triethylenediamine and stannous octoate, one-step foaming has been rapidly promoted. [0003] The catalysts for polyurethane are mainly amines and organometallics, both of which are delayed catalysts. In addition to accelerating the reaction, these catalysts can also control the relative speed of parallel reactions, affect the fluidity of the reaction mixture, the physical and mechanical properties of the finished product and the technical parameters of the process. Among them, amines are nucleophilic catalysts, which are often regarded as mainly catalyzing the foaming reaction in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/13C07C275/14C07C273/18C08G18/18C09J11/06C08G101/00
Inventor 高峰于萍罗运柏
Owner WUHAN UNIV
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