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Preparation method of amino-terminated hyper-branched polymer grafted chitosan microsphere formaldehyde adsorbent

A technology of amino-terminated hyperbranched and hyperbranched polymers, applied in alkali metal compounds, chemical instruments and methods, separation methods, etc., can solve the problems that limit the wide application of chitosan, chitosan anti-swelling, poor solubility, etc. , to achieve the effect of large enrichment factor, good reproducibility and good stability

Inactive Publication Date: 2019-01-25
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are a large number of hydrogen bonds in chitosan molecules, resulting in chitosan anti-swelling, poor solubility, and can only be dissolved in dilute acids and special halogen-containing organic solvents, which greatly limits the wide application of chitosan

Method used

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  • Preparation method of amino-terminated hyper-branched polymer grafted chitosan microsphere formaldehyde adsorbent
  • Preparation method of amino-terminated hyper-branched polymer grafted chitosan microsphere formaldehyde adsorbent
  • Preparation method of amino-terminated hyper-branched polymer grafted chitosan microsphere formaldehyde adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Synthetic tetracarboxylic acid ester: 15.2ml of diethyl malonate of 0.1mol, petroleum ether 50ml, tetrabutylammonium bromide 1.5g, K 2 CO 3 2.76g, 0.25mol methyl acrylate was added dropwise. Control the temperature at 64°C-66°C for 4h to obtain a white solid.

[0026] (2) Synthesis of amino-terminated hyperbranched polymers: 13.66 g of tetravalent carboxylate, 40 ml of methanol, 15 mL of diethylenetriamine was added dropwise, reacted at room temperature for 2 h under nitrogen protection, removed methanol under reduced pressure, and continued to heat up to 80 °C under reduced pressure. ℃, reacted for 3 hours, a light yellow viscous product was generated, and the hyperbranched polymer was obtained.

[0027] (3) chitosan grafted succinic anhydride: in the step 2, the acid anhydride compound adopts succinic anhydride, and 1g chitosan is dissolved in 1-allyl-3-methylimidazolium chloride salt ionic liquid earlier , dissolved for 60 min, then added 1.5 g of succinic anh...

Embodiment 2

[0031] (1) synthetic tetravalent carboxylic acid ester: dimethyl malonate 16ml of 0.1mol, ethyl acetate 50ml, benzyltriethylammonium chloride 1.5g, K 2 CO 3 2.83g, 0.25mol butyl acrylate was added dropwise. After reflux for 4 hours, the temperature was controlled between 64°C and 66°C, and a white solid was generated.

[0032] (2) Synthesis of amino-terminated hyperbranched polymers: 15.12 g of tetravalent carboxylate, 50 ml of n-butanol, 15 mL of ethylenediamine was added dropwise, reacted at room temperature for 2 h under nitrogen protection, removed methanol under reduced pressure, and continued to heat up to 80°C, reacted for 3 hours, a light yellow viscous product was generated, and the hyperbranched polymer was obtained.

[0033] (3) chitosan grafted succinic anhydride: in described step 2, acid anhydride compound adopts succinic anhydride, first 1g chitosan is dissolved in 1-butyl-3-methylimidazolium chloride salt ionic liquid, Dissolved for 60 minutes, then added 1....

Embodiment 3

[0037] (1) Synthetic tetracarboxylic acid ester: 14.72ml of diethyl malonate of 0.1mol, 50ml of cyclohexane, 1.5g of tetrabutylammonium chloride, K 2 CO 32.69g, 0.25mol of ethyl acrylate was added dropwise. After reflux for 4 hours, the temperature was controlled between 64°C and 66°C, and a white solid was generated.

[0038] (2) Synthesis of amino-terminated hyperbranched polymers: 14.12 g of tetravalent carboxylate, 40 ml of ethanol, 15 mL of triethylenetetramine was added dropwise, reacted at room temperature for 2 h under nitrogen protection, removed methanol under reduced pressure, and continued to heat up to 80 °C under reduced pressure. ℃, reacted for 3 hours, a light yellow viscous product was generated, and the hyperbranched polymer was obtained.

[0039] (3) Chitosan grafted succinic anhydride: in the step 2, the acid anhydride compound adopts succinic anhydride, and 1g chitosan is dissolved into 1-ethoxycarbonylmethyl-3-methylimidazole acetate Dissolve in the io...

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Abstract

The invention discloses a preparation method of an amino-terminated hyper-branched polymer grafted chitosan microsphere adsorbent (the simple formula is represented by figure I), and belongs to the field of preparation processes of adsorbing materials. According to the present invention, a hyper-branched polymer is cross-linked in a chitosan structure through succinic anhydride by using the rich nitrogen-containing groups (primary amino group, amide group and secondary amino group) in the hyper-branched polymer based on the highly-reactive amino group in the molecular structure of chitosan toprepare the amino-terminated hyper-branched polymer grafted chitosan solid-phase adsorbing material having a specific structure, wherein the adsorbing material is used for formaldehyde adsorption; a large amount of the nitrogen-containing groups are introduced on the chitosan so as to increase the content of the active groups, such that the formaldehyde adsorption capacity can be significantly improved; and by using the ionic liquid as the reaction medium for cross-linking the hyper-branched polymer and the chitosan, the reaction rate can be significantly increased, the cross-linking proportion can be increased, and the ionic liquid can be recycled so as to achieve the environmental protection.

Description

technical field [0001] The invention belongs to the field of adsorption material preparation technology, and in particular relates to a preparation method of an amino-terminated hyperbranched polymer grafted chitosan microsphere formaldehyde adsorbent. Background technique [0002] Formaldehyde is a major culprit of pollution and cancer, and has become an environmental problem faced by human beings. As a formaldehyde treatment method, the adsorption method has been widely used due to its advantages of low cost, high efficiency, simple operation, short time consumption, and the ability to complement each other with other environmental treatment technologies. However, relatively little research has been done on sorbents for non-degradable pollutants. Therefore, in order to solve the problem of dealing with such pollutants, research and preparation of new efficient and cheap adsorption materials has become a research direction that has attracted much attention. [0003] Chito...

Claims

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Application Information

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IPC IPC(8): B01J20/24B01J20/28B01J20/30B01D53/02
CPCB01D53/02B01J20/24B01J20/28021B01D2257/7022
Inventor 王国伟徐小青庄玲华厉巧萍
Owner NANJING UNIV OF TECH
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