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Preparation and application of 1,8-diamino-p-methane hyperbranched polyether amine and its hybrid hydrogel

A hyperbranched polyetheramine, hydrogel technology, applied in the directions of alkali metal oxides/hydroxides, inorganic chemistry, water pollutants, etc. The post-processing process is simple and the effect of improving the degree of branching

Inactive Publication Date: 2017-02-15
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The amine monomers used in the previous literature reports on the functional modification of hyperbranched polyetheramines are all N-ethylethylenediamine, and the hyperbranched polyetheramines prepared by 1,8-p-mentediamine and their functions have not been seen yet. reports on modification

Method used

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  • Preparation and application of 1,8-diamino-p-methane hyperbranched polyether amine and its hybrid hydrogel
  • Preparation and application of 1,8-diamino-p-methane hyperbranched polyether amine and its hybrid hydrogel
  • Preparation and application of 1,8-diamino-p-methane hyperbranched polyether amine and its hybrid hydrogel

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Weigh 3.4g (0.02mol) of 1,8-p-mendiamine, add 8.5mL of absolute ethanol, stir magnetically, and pass nitrogen gas for half an hour. Weigh 20g (0.04mmol) of polyethylene glycol diglycidyl ether (Mn=500) and dissolve it in 50mL of ethanol, slowly drop it into the reaction solution, after the dropwise addition, stir for 24h, then raise the temperature to 85°C and react for 24h to obtain The reaction solution was distilled under reduced pressure to remove ethanol under the condition of vacuum degree of 0.086MPa, then settled with petroleum ether for many times, discarded the upper layer liquid, and the lower layer paste was vacuum-dried under the condition of vacuum degree of 0.09MPa for 6h to obtain the overrun Polyetheramines. as attached figure 2 As shown, the product is measured by GPC, and the GPC retention time RT of the obtained hyperbranched polyetheramine is 10.9min, its number average molecular mass Mn is 3.8K, and the weight average molecular mass Mn is 3.8K. ...

Embodiment 2

[0049] Weigh 3.4g (0.02mol) of 1,8-p-mendiamine, add 8.5mL of absolute ethanol, stir magnetically, and pass nitrogen gas for half an hour. Weigh 38.4g (0.06mol) of polypropylene alcohol diglycidyl ether (Mn=640) and dissolve it in 64mL of ethanol, and slowly drop it into the reaction solution. After the dropwise addition, stir for 24h, then raise the temperature to 80°C for 30h, and the obtained reaction The liquid was distilled under reduced pressure to remove ethanol under the condition of vacuum degree of 0.09MPa, and then settled with n-hexane several times, the upper layer liquid was discarded, and the lower layer paste was vacuum-dried under the condition of vacuum degree of 0.09MPa for 6h to obtain hyperbranched Polyetheramine.

Embodiment 3

[0051] Weigh 1.7g (0.01mol) of 1,8-p-mentediamine, add 10mL of absolute ethanol, stir magnetically, and pass nitrogen gas for half an hour. Weigh 6.4g (0.01mol) of polypropylene alcohol diglycidyl ether (Mn=640) and 5g (0.01mol) of polyethylene glycol diglycidyl ether (Mn=500) and dissolve them in 60mL of ethanol, slowly drop them into the reaction solution, After the dropwise addition, stir for 24 hours, then raise the temperature to 85°C and react for 24 hours. The obtained reaction liquid is distilled under reduced pressure to remove ethanol under the condition of vacuum degree of 0.09 MPa, and then settle with n-hexane for many times. The upper layer is discarded, and the lower layer is paste-like The product was vacuum-dried for 4 hours under the condition of vacuum degree of 0.09MPa to obtain hyperbranched polyetheramine.

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Abstract

The invention discloses preparation and application of 1,8-diamino-p-methane hyperbranched polyether amine and its hybrid hydrogel; the hyperbranched polyether amine is prepared from 1,8-diamino-p-methane via one-pot method; terminal amino groups of the 1,8-diamino-p-methane hyperbranched polyether amine are functionally modified with double bonds introduced, the double bonds and 3-mercaptopropyltrimethoxysilane are then subjected to 'click chemical' reaction to introduce organic silicon groups, and the 1,8-diamino-p-methane hyperbranched polyether amine hybrid hydrogel is prepared by crosslinking of silicon-oxygen bonds in water. The A2B4 type hyperbranched polyether amine is prepared through one-pot method, the method is simple, expensive equipment and complex operations are not required, the product contains mass hydroxyl radicals, facilitating further functional modification and application; the prepared hydrogel is applicable to the adsorption of water-soluble dyes and modification of polyacrylamide hydrogels; reaction conditions are simple, operating is simple, additional catalysts are not required, and post-treatment is simple.

Description

[0001] Technical field: [0002] The present invention designs a hyperbranched high molecular polymer and a method for synthesizing the polymer, specifically a synthesis method of 1,8-p-mentediamine hyperbranched polyetheramine and 1,8-p-mentediamine hyperbranched Preparation and Application of Polyetheramine Hybrid Hydrogel Background technique [0003] 1,8-p-mentediamine is a cycloaliphatic dibasic primary amine with tetrafunctionality, and it is an important derivative of pinene, a monoterpenoid compound. The two amine groups of 1,8-p-mendiamine are respectively connected to two tertiary carbon atoms, and the structure is shown below. [0004] [0005] Due to its special six-membered ring structure, its reactivity is slightly lower than that of straight-chain dibasic primary amines, so its reaction is easy to control. 1,8-p-mentediamine was synthesized and industrialized in the middle of the 20th century, Feng Zhiyong et al. ,25(S1):168-170.) reviewed the properties a...

Claims

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Application Information

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IPC IPC(8): C08G73/02C08J3/24C08J3/075C08L79/02B01J20/26B01J20/28B01J20/30C02F1/28C02F1/58C08L33/26
CPCC08G73/024B01J20/267B01J20/28047C02F1/285C02F2101/308C08J3/075C08J3/24C08J2333/26C08J2379/02C08J2479/02C08L33/26C08L79/02
Inventor 赵振东衣晓庆朱守记徐士超陈玉湘毕良武王婧卢言菊
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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