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One-step synthesis method of polyethyleneimine

A polyethylene imine and synthesis method technology, applied in the field of polyethylene imine preparation, can solve the problems of unfavorable cost reduction, and achieve the effects of saving reaction time, avoiding high reactivity, and mild reaction conditions

Active Publication Date: 2021-10-22
上海氟聚化学产品股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] But this method requires special catalysts and high temperature and high pressure reaction conditions, which is also not conducive to cost reduction
According to statistics, the prices of the products prepared by the above methods are similar, basically around 100-180 yuan / kg

Method used

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  • One-step synthesis method of polyethyleneimine
  • One-step synthesis method of polyethyleneimine
  • One-step synthesis method of polyethyleneimine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1 Without separation and purification of monomers, the hydrochloric acid method synthesizes PEI in one step

[0050] 1. Synthesis of aminoethanol hydrogen sulfate

[0051] The reaction formula is shown in formula 5:

[0052]

[0053] Concrete reaction steps are as follows:

[0054] 1) Take 30g of ice water and add it to a beaker, place it in an ice-salt bath, keep the temperature at 4°C, stir and slowly add 60g of concentrated sulfuric acid;

[0055] 2) According to the molar ratio of sulfuric acid to 1:1, slowly add 36.6g of ethanolamine dropwise to the solution, and at the same time add ice cubes to the solution continuously, and control the solution temperature at 5-7°C for about 1 hour;

[0056] 3) After the dropwise addition is completed, transfer the reaction solution to a three-necked flask, and carry out vacuum distillation in an oil bath. The distillation temperature is initially set to 135°C, and most of the liquid is evaporated; then slowly rise ...

Embodiment 2

[0079] Embodiment 2: One-step synthesis of PEI by 1,2 dichloroethane method

[0080] Take 30 g of ice water and add it to a 500 ml three-neck flask, place it in an ice-salt bath at 4°C, stir and slowly add 100 g of concentrated sulfuric acid; slowly add 61 g of ethanolamine dropwise to the solution, while continuously adding ice cubes to the solution, The solution temperature was controlled at 20°C.

[0081] After the dropwise addition is completed, carry out vacuum distillation in the oil bath. The distillation temperature is initially set to 135°C, and most of the liquid is evaporated; then the temperature is slowly raised to 160°C, and part of the liquid is evaporated, and the solution appears cloudy at the same time. The internal temperature of the solution was 150°C. Stop heating immediately and take the three-necked flask out of the oil bath, and place it in the air to cool naturally. A white solid precipitated out, and stood for several hours until the liquid completely...

Embodiment 3

[0085] Embodiment 3: Epichlorohydrin method one-step synthetic PEI

[0086] Take 100g of ice water and add it to a 2-liter three-neck flask, place it in a 4°C ice-salt bath, stir and slowly add 400g of 98% concentrated sulfuric acid; slowly add 244g of ethanolamine dropwise to the solution, and continuously add Ice cubes, the solution temperature was controlled at 20°C.

[0087] After the dropwise addition is completed, carry out vacuum distillation in the oil bath. The distillation temperature is initially set to 135°C, and most of the liquid is evaporated; then the temperature is slowly raised to 160°C, and part of the liquid is evaporated, and the solution appears cloudy at the same time. The internal temperature of the solution is 150°C. Stop heating immediately and take the three-neck flask out of the oil bath, and place it in the air to cool naturally. A white solid precipitates out. Leave it for several hours until the liquid completely becomes a white solid;

[0088] ...

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Abstract

The invention relates to a one-step synthesis method of polyethyleneimine. The method comprises the following steps: (1) synthesizing monomer ethyleneimine, reacting ethanolamine with concentrated sulfuric acid or hydrogen chloride, and treating with strong base to obtain monomer ethyleneimine and an inorganic salt byproduct; and (2) synthesizing polyethyleneimine, namely directly polymerizing the monomer ethyleneimine obtained in the step (1) under the conditions of an acid catalyst and a polyhaloalkane catalyst without separation treatment to generate polyethyleneimine. According to the one-step synthesis method, on one hand, the use and storage risk and harm caused by high reactivity, corrosivity, toxicity, flammability and explosiveness of the ethyleneimine are avoided; on the other hand, special treatment for removing residual ethyleneimine in the monomer separation process is also avoided. According to the method disclosed by the invention, an intermediate separation step is not needed, so that the possible risks of poisoning, combustion and explosion to operators are greatly reduced, and the pressure of environmental protection is also greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of polyethyleneimine preparation, and specifically relates to a one-step synthesis method of polyethyleneimine. Background technique [0002] Polyethyleneimine (referred to as PEI) is a water-soluble high molecular polymer. The primary amine, secondary amine, tertiary amine and other groups contained in its molecular structure have high chemical reactivity. The densest cationic organic polymer. The difference in the performance of PEI is mainly due to the different proportions of different amino groups in the PEI structure. The unique structure leads to the unique performance of PEI, which makes it have special applications in the fields of heavy metal ion adsorption, gas adsorption, and oil field applications. In particular, PEI can absorb a large amount of carbon dioxide in the air at room temperature, and the separation process is also very convenient. It can be used for the adsorption of carbon dioxide ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/02
CPCC08G73/0206C08G73/0213Y02C20/40
Inventor 曹华斌
Owner 上海氟聚化学产品股份有限公司
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