Preparation of urylene dimethylamino-propane and dichloroethyl ether copolymer

A technology of dimethylaminopropane and dimethylaminopropylamine is applied in the field of preparation of urea-dimethylaminopropane and dichloroethyl ether copolymer, and can solve the problems of low conversion rate of dimethylaminopropane, unstable average molecular weight, and PUB color and luster. To achieve the effect of environmental friendliness, ensure product purity and color, and facilitate industrial production

Active Publication Date: 2012-11-21
武汉松石科技股份有限公司
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  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

Dimethylaminopropane conversion rate synthesized by the above-mentioned method is low (conversion rate is about 80%), and impurity content is high (containing about 20% impurity), and the PUB color and luster obtained with it is poor (documentation is recorded as reddish brown, The iodine colorimetry is between 30-100#), and the average molecular weight is unstable (2000-40000), which causes the instability of the electroplating effect
[0005] In the existing method, in the synthesis process of uridine dimethylaminopropane, there is an oxidation phenomenon in dimethylaminopropane, and urea will decompose during the synthesis process, which will cause the color to deepen, and will also cause the molecular weight to be too low in the next step of polymerization. (Molecular weight less than 2000) and excessive phenomenon

Method used

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  • Preparation of urylene dimethylamino-propane and dichloroethyl ether copolymer
  • Preparation of urylene dimethylamino-propane and dichloroethyl ether copolymer
  • Preparation of urylene dimethylamino-propane and dichloroethyl ether copolymer

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Embodiment 1

[0056] The preparation method of urethane dimethylaminopropane and dichloroether copolymer, it comprises following reaction steps:

[0057] ①. Synthesis of urea-dimethylaminopropane: add dimethylaminopropylamine: urea at a ratio of 1.8: 1 to the reactor, stir while adding, feed an inert gas into the reactor, and add a catalyst at a temperature of 100°C. Keeping the temperature for 8 hours, then raising the temperature to 140°C, recovering the ammonia gas released during the reaction (using dilute sulfuric acid to absorb ammonia gas) to obtain the crude uridine dimethylaminopropane, and then rectifying to obtain the fine urea dimethylaminopropane;

[0058] ②. Synthesis of copolymer: Put ureadimethylamidopropane: β, β-dichloroethyl ether: water into the reaction kettle at a ratio of 0.5:1:12, stir while adding, react under reflux for 13 hours, and then add Molecular weight regulator, keep warm for 3 hours, add activated carbon (the mass of activated carbon is 1-10% of the total ...

Embodiment 2

[0062] The preparation method of uridine dimethylaminopropane and dichloroether copolymer is characterized in that it comprises the following reaction steps:

[0063] ①. Synthesis of urea-dimethylaminopropane: add dimethylaminopropylamine: urea at a ratio of 2.0: 1 to the reactor, stir while adding, feed an inert gas into the reactor, and add a catalyst, the temperature is 75°C, Keeping warm for 2 hours, then raising the temperature to 140°C, recovering the ammonia gas released during the reaction to obtain the crude uridine dimethylaminopropane, and then rectifying to obtain the refined urea dimethylaminopropane;

[0064] ②. Synthesis of copolymer: put urea dimethylaminopropane: β, β-dichloroethyl ether: water into the reaction kettle at a ratio of 1.2:1:12, stir while adding, react under reflux for 21 hours, and then add Molecular weight regulator, heat preservation reaction for 1 hour, add activated carbon (the mass of activated carbon is 1-10% of the total mass of the copo...

Embodiment 3

[0068] The preparation method of urethane dimethylaminopropane and dichloroether copolymer, it comprises following reaction steps:

[0069] ①. The synthesis of urea-dimethylaminopropane: add dimethylaminopropylamine: urea at a ratio of 1.9: 1 to the reactor, stir while adding, feed an inert gas into the reactor, and add a catalyst, the temperature is 90°C, Keeping warm for 5 hours, then raising the temperature to 140°C, recovering the ammonia gas released during the reaction to obtain the crude uridine dimethylaminopropane, and then rectifying to obtain the refined urea dimethylaminopropane;

[0070] ②. Synthesis of copolymer: Put urea dimethylaminopropane: β, β-dichloroethyl ether: water into the reaction kettle at 0.9:1:12, stir while adding, react under reflux for 17 hours, then add Molecular weight regulator, heat preservation reaction for 2 hours, add activated carbon to decolorize, then distill off excess water to obtain uridine dimethylaminopropane and dichloroethyl eth...

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Abstract

The invention relates to a method for preparing a copolymer of urylene dimethylamino propane and dichlorethyl ether. The method is characterized by comprising the reaction steps as follows: the synthesis of the urylene dimethylamino propane and the synthesis of the copolymer are carried out; catalyst is a mixture of niobium hydroxide and phytic acid; the mol ratio of the niobium hydroxide and thephytic acid is 1.0-6.0:1; the dosage of the catalyst is 1-10 per thousand lity of dimethylamino propylamine; molecular weight regulator is nicotinic acid; the dosage of the nicotinic acid is 0.5-1.5 per thousand; and the invention overcomes the disadvantage that the prior preparation method has high impurity content, bad luster and unstable average molecular weight, thereby causing unstable electroplating effect. The invention has the advantages of good purity and luster, stable average molecular weight, simple synthesis technology, being friendly to the environment, low energy consumption, etc.

Description

technical field [0001] The invention relates to a preparation method of uridine dimethylaminopropane and dichloroethyl ether copolymer (PUB), which is an excellent electroplating intermediate. Background technique [0002] With the development of our country's economy and the improvement of people's awareness of environmental protection, in many industries, such as machinery, electronics, ships, instruments, light industry, etc., there is a need for an environmentally friendly and cheap plating, which is alkaline galvanizing. Since ordinary alkaline galvanizing cannot compare with cyanide galvanizing in terms of brightness, leveling, coverage and dispersion, and thickness of the coating, it is especially difficult to meet the electroplating requirements of parts with very complex geometries. The application range of the process is limited, which requires the development of new electroplating intermediates to solve this problem. [0003] As an excellent electroplating interm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00
Inventor 曾志兵周烈平邱立陈立霞陈曦刘义津孙碧新欧阳亿伟陈静胡梅邓翠萍程海霞
Owner 武汉松石科技股份有限公司
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