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Polyvinyl alcohol macromonomer based method for preparing functional microsphere

A macromonomer and functional technology, applied in the field of functional polymer microsphere preparation, can solve the problems of limiting the application field of PVA microspheres, toxic glutaraldehyde residue, etc.

Inactive Publication Date: 2014-03-05
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, the traditional preparation method of PVA microspheres is to use glutaraldehyde to prepare PVA microspheres through acetal reaction. This method has the problem of residual toxic glutaraldehyde, which greatly limits the application field of PVA microspheres.

Method used

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  • Polyvinyl alcohol macromonomer based method for preparing functional microsphere

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) Synthesis of PVA macromonomer: Take 1.05g of amino acetal dimethyl acetal and 1.01g of triethylamine in a 100mL three-necked flask by mass, dilute with dichloromethane, and slowly add 0.905g dropwise at 0°C Acryloyl chloride, then reacted for 3 hours, the product was washed with saturated brine, separated, and the organic phase was rotary evaporated to obtain N-(2,2-dimethoxyethyl)acrylamide; then PVA178810g was taken by mass, dissolved in Hot water at 90°C was prepared into a solution with a mass fraction of 10%. After cooling to room temperature, pour it into a 250mL three-neck flask, add 0.5g of N-(2,2-dimethoxyethyl)acrylamide, stir well, and Add 3mL of concentrated hydrochloric acid dropwise to the separatory funnel, react at room temperature for 24h, and obtain the PVA macromer through dialysis and freeze-drying;

[0014] (2) Preparation of functional microspheres: get the PVA macromer synthesized by 5g step (1), 0.5gAMPS, take potassium persulfate as initiato...

Embodiment 2

[0016] (1) Synthesis of PVA macromonomer: Take 1.05g of amino acetal dimethyl acetal and 1.01g of triethylamine in a 100mL three-necked flask by mass, dilute with dichloromethane, and slowly add 0.905g dropwise at 0°C Acryloyl chloride, then reacted for 3 hours, the product was washed with saturated brine, separated, and the organic phase was rotary evaporated to obtain N-(2,2-dimethoxyethyl)acrylamide; then PVA178810g was taken by mass, dissolved in Hot water at 90°C was prepared into a solution with a mass fraction of 10%. After cooling to room temperature, pour it into a 250mL three-neck flask, add 0.5g of N-(2,2-dimethoxyethyl)acrylamide, stir well, and Add 3mL of concentrated hydrochloric acid dropwise to the separatory funnel, react at room temperature for 24h, and obtain the PVA macromer through dialysis and freeze-drying;

[0017] (2) Preparation of functional microspheres: get the PVA macromer synthesized by 5g step (1), 1.0gAMPS, take potassium persulfate as initiato...

Embodiment 3

[0019] (1) Synthesis of PVA macromonomer: Take 1.05g of amino acetal dimethyl acetal and 1.01g of triethylamine in a 100mL three-necked flask by mass, dilute with dichloromethane, and slowly add 0.905g dropwise at 0°C Acryloyl chloride, then reacted for 3 hours, the product was washed with saturated brine, separated, and the organic phase was rotary evaporated to obtain N-(2,2-dimethoxyethyl)acrylamide; then PVA178810g was taken by mass, dissolved in Hot water at 90°C was prepared into a solution with a mass fraction of 10%. After cooling to room temperature, pour it into a 250mL three-neck flask, add 0.5g of N-(2,2-dimethoxyethyl)acrylamide, stir well, and Add 3mL of concentrated hydrochloric acid dropwise to the separatory funnel, react at room temperature for 24h, and obtain the PVA macromer through dialysis and freeze-drying;

[0020] (2) Preparation of functional microspheres: get the PVA macromer synthesized by 5g step (1), 1.5gAMPS, take potassium persulfate as initiato...

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Abstract

A polyvinyl alcohol (PVA) macromonomer based method for preparing functional microspheres belongs to the technical field of functional polymer microsphere preparation. The invention firstly uses amino acetal and propylene acyl chloride to synthesize an intermediate N-(2,2-dimethoxy ethyl) acrylamide; the intermediate and PVA are subjected to acetal exchange reaction to prepare PVA macromonomers; then the PVA macromonomers, functional monomers and an initiator as raw materials are subjected to reversed phase suspension polymerization to prepare polymer microspheres with the particle size of 10-400 mum. The preparation process has mild reaction conditions and simple and practicable method; and the prepared microspheres do not have the problem of residual toxic glutaraldehyde, which exists in the microspheres prepared from glutaraldehyde crosslinking, and can be used in the fields of biological medicine carrier, controlled release carrier and sewage treatment.

Description

technical field [0001] The invention discloses a preparation method of a PVA macromonomer and functional PVA microspheres, and belongs to the technical field of preparation of functional polymer microspheres. Background technique [0002] PVA is obtained by alcoholysis of polyvinyl acetate. It has excellent properties such as biocompatibility, hydrophilicity and biodegradability. It is widely used in drug carriers and biosensors through physical or chemical cross-linking to form microspheres. And super absorbent materials and other fields. [0003] However, the traditional preparation method of PVA microspheres is to use glutaraldehyde to prepare PVA microspheres through acetal reaction. This method has the problem of residual toxic glutaraldehyde, which greatly limits the application field of PVA microspheres. . However, there are a large number of hydroxyl groups on the PVA chain, which can undergo substitution reactions with acetal, isocyanate, urethane, etc., making it...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F290/12C08F2/32C08F16/06C08F8/30A61K47/32
Inventor 倪忠斌郑广通陈明清钟汶贵何嘉健
Owner JIANGNAN UNIV