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Preparation method of ion-exchange polyvinyl alcohol micro-spheres

A technology of polyvinyl alcohol microspheres and ion exchange, which is applied in the field of medical devices, can solve the problems of harming health, the inability to prepare large particle size microspheres, and changing the shape of microspheres, so as to improve production efficiency, shorten synthesis time, and achieve good results. spherical effect

Pending Publication Date: 2018-11-06
杭州艾力康医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Spray drying and phase separation methods cannot prepare large particle size microspheres. The shape of microspheres will be changed by crushing in the freeze drying method. Toxic substances such as glutaraldehyde are usually used in the emulsification dispersion method, which endangers people's health.

Method used

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  • Preparation method of ion-exchange polyvinyl alcohol micro-spheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Weigh 10g of polyvinyl alcohol with a viscosity of 15-25mPa*s, add it to 110g of water, heat to 85°C, stir for 2 hours to dissolve, and cool it for later use; weigh 80g of sodium acrylate, add 100g of water to dissolve, add potassium persulfate 0.7g, N, N-methylenebisacrylamide 0.5g, after stirring evenly, add the prepared polyvinyl alcohol solution, stir to make a mixed solution, and ultrasonically eliminate the bubbles of the solution;

[0040] (2) Measure 500g of soybean oil, add 1g of Span 80, stir evenly at 120r / min, preheat to 45°C, keep warm for 30 minutes, then add the mixture obtained in step (1), stir at 100r / min for 20 Minutes, finally add 4g of catalyst dimethylethylenediamine to initiate high-temperature polymerization reaction, the number of revolutions is 120r / min, react for 4 hours, wash with water several times after the reaction, collect, and obtain ion-exchange polyvinyl alcohol microspheres .

[0041] Ion-exchange polyvinyl alcohol microspheres,...

Embodiment 2

[0052] Weigh 10g of polyvinyl alcohol with a viscosity of 25-35mPa*s, add it to 120g of water, heat to 85°C, stir for 2 hours to dissolve, cool and set aside. Weigh 70g of acrylic acid, add 120ml of 8mol / L NaOH solution, add 0.5g of potassium persulfate, 1g of N, N-methylenebisacrylamide, stir well, then add polyvinyl alcohol solution, stir to form a mixed solution, and ultrasonically eliminate solution bubbles;

[0053] Measure 500g of n-heptane, add 1.5g of Span 80, stir evenly at 130r / min, preheat to 50°C, keep warm for 30 minutes, then add the above mixture, stir at 130r / min for 30 minutes, and finally add the catalyst 5 g of dimethylethylenediamine was used to initiate a high-temperature polymerization reaction, and the reaction was carried out for 4 hours at the same number of rotations. After the reaction was completed, it was washed with water several times, and after collection, ion-exchange polyvinyl alcohol microspheres were obtained.

[0054] The obtained microsph...

Embodiment 3

[0065] Weigh 8g of polyvinyl alcohol with a viscosity of 25-35mPa*s, add it to 100g of water, heat to 85°C, stir for 2 hours to dissolve, cool down and set aside. Weigh 80g of sodium acrylate, add 100g of water to dissolve, add 1g of potassium persulfate, 2g of N, N-methylene bisacrylamide, stir well, then add polyvinyl alcohol solution, stir to form a mixed solution, and ultrasonically eliminate bubbles in the solution;

[0066] Measure 500g of liquid paraffin, add Tween 60 1g, stir evenly at 150r / min, preheat to 60°C, keep warm for 30 minutes, then add the above mixed solution, stir at 150r / min for 30 minutes, and finally add catalyst tetramethyl 5 g of ethylenediamine was used to initiate a high-temperature polymerization reaction, and the reaction was carried out for 5 hours at the same number of rotations. After the reaction, it was washed with water several times, and after collection, ion-exchange polyvinyl alcohol microspheres were obtained.

[0067] The obtained micro...

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Abstract

The invention discloses a preparation method of ion-exchange polyvinyl alcohol micro-spheres. The method comprises the steps that a water-soluble functional monomer is dissolved in water, and an initiator, a cross-linking agent and a polyvinyl alcohol aqueous solution with the mass fraction of 5%-15% are added for even mixing to obtain mixed liquid; an oil phase containing an emulsifying agent isprepared, stirred and heated to 40-80 DEG C, then the obtained mixed liquid is added into the oil phase, stirring is conducted for 10-60 minutes, then a catalyst is added for reaction for 3-6 hours, and after reaction is completed, an obtained product is washed to obtain the ion-exchange polyvinyl alcohol micro-spheres. According to the method, the technology is simple and convenient to operate, reaction heat is fully used, energy consumption is relatively low, synthesis time is short, the reaction temperature is reduced, and the production efficiency in industrialized production is improved;the prepared polyvinyl alcohol micro-spheres have good deformability and elasticity, are smooth in sphere surface, even in dispersion and high in drug loading capability and have good biocompatibilityand stability at the same time.

Description

technical field [0001] The invention relates to the preparation of embolic agents in the field of medical devices, in particular to a preparation method of ion-exchange polyvinyl alcohol microspheres. Background technique [0002] Interventional therapy refers to the use of puncture needles, catheters and other interventional equipment to insert specific instruments through natural channels or tiny wounds under the guidance and monitoring of digital subtraction angiography (DSA), CT, ultrasound or MRI and other imaging equipment. A general term for a series of technologies that are introduced into human diseased parts for minimally invasive treatment. Among them, transcatheter vascular embolization (TACE) is a very important category. It mainly injects embolic agents into the supply vessels of the diseased target organs through arterial or intravenous catheters to occlude the vessels and interrupt the blood supply. Purpose. [0003] The performance and application of vascu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61L24/06A61L24/00A61K9/52A61K47/32A61K47/22A61K31/704A61P35/00C08F220/06C08F222/38
CPCA61K9/5015A61K9/5026A61K31/704A61L24/00A61L24/001A61L24/06A61L2300/416A61L2300/602A61P35/00C08F220/06C08L29/04C08F222/385
Inventor 吴健骆晨涛王鹏飞张林杰
Owner 杭州艾力康医药科技有限公司
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