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Preparation method of n,n'-bis(dimethylaminoalkyl)urea-α,ω-dihalogenated alkyl copolymer

A technology of dimethylaminoalkyl and dihalogenated alkyl, which is applied in the field of preparation of cationic quaternary ammonium salt polymers, can solve the problems of difficult reaction control, large process fluctuation, etc., and achieves improved performance, accelerated reaction rate, and easy realization. Effect

Active Publication Date: 2015-12-23
湖北吉和昌化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the possibility of terminating the reaction is mentioned above, in the case of polymers, the control of the reaction is extremely difficult, and the addition of monohalogenated alkanes or acids can cause large process fluctuations

Method used

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  • Preparation method of n,n'-bis(dimethylaminoalkyl)urea-α,ω-dihalogenated alkyl copolymer
  • Preparation method of n,n'-bis(dimethylaminoalkyl)urea-α,ω-dihalogenated alkyl copolymer
  • Preparation method of n,n'-bis(dimethylaminoalkyl)urea-α,ω-dihalogenated alkyl copolymer

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Put 600g of urea, 180g of water, and 2080g of N,N'-dimethylaminopropylamine into the flask, and add 3g of Zn and ZnCl 2 Using a microwave reactor to raise the temperature to 100°C for reflux reaction, the microwave frequency is 200Hz, and nitrogen gas is blown at the same time for 6 hours, and the nitrogen flow rate is 1L / min. At this temperature, the excess unreacted N,N'-di Methaminopropylamine and decompose unreacted urea, add activated carbon accounting for 0.3% of the total weight percentage of N,N'-dimethylaminopropylamine and stir for 30 minutes, filter to obtain 2278g of N,N'-bis(dimethylaminoalkyl ) urea, the tail gas in the reaction process is absorbed by a dilute sulfuric acid device; the product color is light yellow transparent liquid, and the product content is 99.3%.

[0024] Mix N,N'-bis(dimethylaminoalkyl)urea and water in equal quantities, raise the temperature to 70°C, start to drop α,ω-dichloroethyl ether, N,N'-bis(dimethylamino Alkyl) urea and α, ω...

Embodiment 2

[0026] Put 600g of urea, 180g of water, and 2040g of N,N'-dimethylaminopropylamine into the flask, and add 2g of Al and AlCl 3 Using a microwave reactor to heat up to 100°C for reflux reaction, the microwave frequency is 300Hz, and nitrogen gas is blown at the same time for 5 hours, and the nitrogen flow rate is 3L / min. At this temperature, the excess unreacted N,N'-di Aminopropylamine and decompose unreacted urea, add activated carbon accounting for 0.5% of the total weight of N,N'-dimethylaminopropylamine and stir for 30 minutes, filter to obtain N,N'-bis(dimethylaminoalkyl)urea , The tail gas in the reaction process is absorbed by a dilute sulfuric acid device; the product color is light yellow transparent liquid, and the product content is 99.5%.

[0027] Mix N,N'-bis(dimethylaminoalkyl)urea and water in equal quantities, raise the temperature to 80°C, and start to drop α,ω-dichloroethyl ether, N,N'-bis(dimethylamino Alkyl) urea and α, ω-dichloroethyl ether are in a molar...

Embodiment 3

[0029] Put 600g of urea, 180g of water, and 2100g of N,N'-dimethylaminopropylamine into the flask, and add 5g of Al and AlCl 3 Using a microwave reactor to raise the temperature to 100°C for reflux reaction, the microwave frequency is 250Hz, while blowing nitrogen gas for 4 hours, the nitrogen flow rate is 5L / min, and the excess unreacted N,N'-distillate is distilled under reduced pressure at this temperature Aminopropylamine and decompose unreacted urea, add activated carbon accounting for 0.2% of the total weight of N,N'-dimethylaminopropylamine and stir for 30 minutes, filter to obtain N,N'-bis(dimethylaminoalkyl)urea , The tail gas in the reaction process is absorbed by a dilute sulfuric acid device; the product color is light yellow transparent liquid, and the product content is 99.5%.

[0030] Mix N,N'-bis(dimethylaminoalkyl)urea and water in equal quantities, raise the temperature to 90°C, start to drop α,ω-dichloroethyl ether, N,N'-bis(dimethylamino Alkyl) urea and α,...

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Abstract

The invention discloses a preparation method of an N, N'-bis(dimethylamino alkyl) ureido-alpha, omega-dihalo alkyl copolymer. According to the invention, a microwave heating method is adopted for reacting so as to obviously increase the reaction rate, shorten the reaction time and lower the reaction temperature. By adding a mixture of catalysts Zn and ZnCl2 or a mixture of Al and AlCl3, the condition that the color of a product is darkened by the oxidization of the N, N'-dimethylaminopropylamine can be effectively avoided; meanwhile, the reaction can be effectively accelerated. By introducing nitrogen gas, the condition that the color of the product is darkened by the oxidization of the product can be further avoided; meanwhile, ammonia produced by the reaction is exhausted, so that the reaction is accelerated. A dropwise adding method is adopted during polymerization reaction, so that the reaction temperature runaway phenomenon can be avoided; meanwhile, the characteristic viscosity of the polymer is regulated by controlling the dropwise adding speed, so that the molecular weight distribution of the product can be effectively controlled.

Description

technical field [0001] The present invention relates to the preparation method of cationic quaternary ammonium salt polymer for zincate zinc plating, specifically refers to a kind of N,N'-bis(dimethylaminoalkyl)urea-α,ω-dihalogenated alkyl copolymer method of preparation. Background technique [0002] Over the years, N,N'-bis(dimethylaminopropyl)urea-α,ω-dihaloalkyl copolymers have found wide application as electroplating additives. At present, it is mainly used as a brightener, leveling agent and refiner in alkaline galvanizing and zinc alloys, which can significantly improve the performance of metal deposition, and can obtain uniformly distributed coatings in a wide range of current densities, and The formation of air bubbles, which is common during zinc deposition, can be avoided. [0003] EP2099268 mentions that the polymer is also an important leveling agent in the copper plating solution; in the pretreatment process of some integrated circuit boards, the copolymer ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/00
Inventor 杨威陈彰评宋文超付远波周世骏李玉梁明瑞涛高成
Owner 湖北吉和昌化工科技有限公司
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