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Improvement on method for preparing complex of polyvinylpyrrolidone grafted with natural polymer or water-soluble derivate thereof and iodine derivate

A technology of vinylpyrrolidone and natural polymer is applied in the field of preparation improvement of natural polymer or its water-soluble derivative grafted polyvinylpyrrolidone complexed iodine derivative, and can solve the problem of high energy consumption, uneconomical and long drying time. And other issues

Active Publication Date: 2014-05-28
陈煜
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] (2) The stability of the complexed iodine under the preparation conditions of the patent CN101073325A has certain improvement compared with povidone iodine and povidone iodine, and the loss of iodine 2 When compounded with other materials and used as an antibacterial agent in solid materials such as diaphragms and sponges, it is required to have a longer shelf life (> 1 year) and stability of iodine content. Therefore, CMCTS-g-(PAAMe-co-PVP )-I 2 The complex stability of iodine needs to be further improved
But for CMCTS-g-(PAAMe-co-PVP)-I 2 In the process of forming powder by freeze-drying after the solution is concentrated, since the water content in the concentrated solution usually accounts for about 40% to 60%, the freeze-drying efficiency is low, the drying time is long, the energy consumption is large, and it is uneconomical. Improve work efficiency during freeze-drying

Method used

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  • Improvement on method for preparing complex of polyvinylpyrrolidone grafted with natural polymer or water-soluble derivate thereof and iodine derivate
  • Improvement on method for preparing complex of polyvinylpyrrolidone grafted with natural polymer or water-soluble derivate thereof and iodine derivate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Example 1: Preparation of CMCTS-g-(PAANa-co-PVP)

[0061] After fully dissolving 1.5 parts of carboxymethyl chitosan in distilled water, control the temperature of the system at 60° C., add azobisisobutyronitrile with a total mass of acrylate and N-vinylpyrrolidone of 2.5 wt % under nitrogen protection, and react After 30 minutes, add the unsaturated vinyl monomer mixture that is 10:1 with carboxymethyl chitosan mass ratio, the massfraction of the acrylic acid neutralized with sodium hydroxide in this mixture is 70%, the N-vinylpyrrolidone The mass fraction is 30%, and the cross-linking agent N,N'-methylenebisacrylamide of 2wt% monomer is added at the same time, the total water in the control system and the monomer mass ratio are 15:1, and the reaction is carried out at 60°C for 8 hours After the reaction is stopped, the product is precipitated with ethanol with a mass ratio of 12:1 to the monomer, and then the precipitate is broken up by high-speed stirring at 2500 rp...

Embodiment 2

[0063] Dissolve CMCTS-g-(PAANa-co-PVP) powder in distilled water 10 times its mass, neutralize the solution to pH=6.0 through 5% dilute acetic acid solution, add CMCTS-g-(PAANa-co- PVP) long-chain anionic surfactant sodium dodecylsulfonate with a mass fraction of 10%, stirred evenly at 50°C. In addition, it is 15% iodine elemental powder and the potassium iodide powder that is 1.1: 1 with the molar ratio of the iodine elemental substance to add the tert-butyl alcohol / butanol / In the water mixed solution (tert-butanol accounts for 50%, water accounts for 50%), stir at 50°C to dissolve the iodine evenly, then slowly add the solution to the CMCTS-g-(PAANa-co-PVP) aqueous solution , kept warm in a water bath, stirred and reacted for 5 hours, and then the product was concentrated by distillation under reduced pressure, and excess uncomplexed iodine was removed. The product is fully soaked in n-heptane until the supernatant is colorless and transparent, the supernatant is poured ou...

Embodiment 3

[0065]Dissolve CMCTS-g-(PAANa-co-PVP) powder in distilled water 10 times its mass, neutralize the solution to pH=5.3 by 5% dilute acetic acid solution, and take another 25% of the mass fraction of the graft copolymer % iodine elemental powder and the potassium iodide powder that the molar ratio of iodine elemental substance is 1.1: 1 joins together in the DMSO / water mixed solution that the mass ratio of graft copolymer is 2: 1 (DMSO accounts for 30%, water accounts for 70%) %), after stirring at 55°C to make the iodine dissolve evenly, slowly add the solution into the CMCTS-g-(PAANa-co-PVP) aqueous solution, and keep stirring in a water bath at 55°C for 30 minutes, Add the long-chain nonionic surfactant lauryl alcohol polyoxyethylene ether that accounts for CMCTS-g-(PAANa-co-PVP) massfraction 15%, continue stirring reaction in the water bath of this temperature for 5 hours and pass decompression Distillation concentrates the product and removes excess uncomplexed iodine. The ...

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Abstract

The invention provides improvement on a method for preparing complex of a polyvinylpyrrolidone copolymer grafted with a natural polymer or a water-soluble derivate thereof and an iodine derivate. The effective iodine content in the complex of the graft copolymer of the natural polymer or the water-soluble derivate thereof and iodine, the stability of the complex iodine and the freezing and drying working efficiency of the concentrate of the complex or the compounds thereof are improved by improved means of compounding a long-chain alkyl anion surfactant or a long-chain alkyl nonionic surfactant and the polyvinyl-containing natural polymer or the water-soluble derivate-grafted polyvinylpyrrolidone chain segment, compounding iodide and iodine, and replacing ethanol with an organic solvent with a high freezing point, high volatility and capability of dissolving in water and dissolving the iodine to a certain degree to improve the freezing and drying speed of the concentrate the complex of the graft copolymer and the iodine or compounds thereof, and the like.

Description

technical field [0001] The invention relates to a method for preparing a complex compound of a natural polymer or its water-soluble derivatives grafted with a copolymer containing polyvinylpyrrolidone segments and iodine, especially the preparation of natural polymers or their water-soluble derivatives by complexing It is a complex compound of polyvinylpyrrolidone-containing copolymer and iodine. Background technique [0002] The applicant disclosed in the patent application "a povidone-iodine antibacterial material and its preparation method" (CN101073325A) a new type of povidone-iodine antibacterial material-carboxymethyl chitosan immobilized by carboxymethyl chitosan Graft (polyacrylate-co-N-vinylpyrrolidone)-iodine complex (CMCTS-g-(PAAMe-co-PVP)-I 2 , where Me=Na or K), and specifically discloses the preparation method of the complex. The preparation of the complex in this application adopts the solution method to make the iodine molecule grafted with carboxymethyl ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F251/00C08F251/02C08F289/00C08F253/00C08F8/18A61K31/79A61P31/00A01N59/12A01P1/00
Inventor 陈煜
Owner 陈煜
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