CN103113492A - Method for preparing iodine chitosan - Google Patents
Method for preparing iodine chitosan Download PDFInfo
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- CN103113492A CN103113492A CN2012105560299A CN201210556029A CN103113492A CN 103113492 A CN103113492 A CN 103113492A CN 2012105560299 A CN2012105560299 A CN 2012105560299A CN 201210556029 A CN201210556029 A CN 201210556029A CN 103113492 A CN103113492 A CN 103113492A
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Abstract
The invention discloses a method for preparing iodine chitosan. The method comprises the following steps of: (1) adding 1-6 parts of chitosan and 1 part of iodine into a solid phase reactor according to a mass ratio, and covering tightly; rotating the reactor for 10-30minutes slowly and uniformly mixing; (2) slowing heating to 60-90 DEG C and then maintaining at a constant temperature for 8-16 hours, wherein in the process, the reactor rotates positively and negatively in an alternating manner at an interval of 30-60minutes till the reaction is finished; and (3) after reaction, stopping rotation of the reactor; after the materials are cooled to room temperature, discharging and sieving to obtain an iodine chitosan product, wherein the chitosan is water-insoluble chitosan. According to the solid phase reaction method for preparing chitosan provided by the invention, no catalysts are used, and iodine chitosan stable in quality and high in output is produced, so that a novel preparation method of iodine chitosan is explored. The iodine chitosan used as a raw material can be used to prepare various dosage forms, medical materials and disinfectors for cavities and external use.
Description
Technical field
The present invention relates to medical material, particularly chitosan iodine, also relate to its preparation method.
Background technology
Chitosan is a kind of macromolecular compound of biological property excellence, and after absorption iodine, the thermostability of iodine improves greatly, and chitosan iodine can discharge elemental iodine, thereby has strong sterilization.Bibliographical information there be the sterilising effect of chitosan iodine (see " experimental observation of chitosan iodine liquid sterilization effect ", be stated from Hengyang Medical College's journal (medicine) 05 phase in 2000).
Chitosan iodine is a kind of efficient, wide spectrum, nontoxic polymer medical disinfecting sterilization material.It can progressively discharge iodine and bring into play anti-microbial effect, and its mechanism of action is to make bacterium protein sex change, death, and is all effective to bacterium, fungi, virus, is characterized in little to tissue irritation.At present, the method for making of chitosan iodine has solid reaction process and liquid phase reaction method, and the chitosan of use is water-soluble chitosan normally.The liquid phase reaction method is produced chitosan iodine generally can produce purer product, but cost is higher.It is simple and easy to do that solid reaction process is produced chitosan iodine, is suitable for scale operation, but the shortcoming incomplete, unstable product quality that responds.Adopt solid reaction process to produce chitosan iodine, when chitosan and Iod R, traditional method is to adopt to produce I
3 -The catalyzer accelerated reaction, make the reaction carry out more fully.Commonly used have hydrogen iodide (HI), a sodium iodide (NaI) etc., and catalyzer makes iodide ion (I
-) at first with iodine molecule (I
2) generation I
3 -, then be combined generating chitosan iodine with chitosan.Adopt this method technique wayward, the unstable product quality of producing.
In Chinese patent database, the patent application that relates to chitosan iodine only has No. 94107473.0 " preparation of chitosan iodine wound and burns dressing ", No. 200410052654 " preparation method of chitosan quaternary ammonium salt ", No. 201010149420 " a kind of broad-spectrum contact type hemostatic medical fungicide and preparation method thereof ".These technical schemes are not that solid reaction process is produced chitosan iodine.
Summary of the invention
The purpose of this invention is to provide a kind of method that steady quality, solid phase that cost is low prepare chitosan iodine, use water-insoluble chitosan to be raw material, to overcome the defective of prior art.
The method for preparing chitosan iodine that the contriver provides comprises the following steps:
The first step, adds in solid phase reactor 1 part of 1～6 part of chitosan and iodine according to mass ratio, tightly adds a cover; Reactor slow circumvolve 10～30min makes mixing of materials even;
Second step then slowly is heated to 60 ℃～90 ℃, afterwards constant temperature 8～16h; In process, reactor is done rotatablely moving of positive and negative alternate every 30～60min, until reaction is completed;
After three-step reaction finishes, the rotation of stopped reaction device, after material was cooled to room temperature, discharging was sieved, and the particulate that obtains is the chitosan iodine product;
Wherein said chitosan is water-insoluble chitosan.
In above-mentioned chitosan class raw material, the viscosity of chitosan is 0.02～0.10Pas.
In the above-mentioned the first step and second step, the speed of rotation of reactor is controlled at below 100r/min.
In above-mentioned the 3rd step, the described order number that sieves is more than 60 orders.
The contriver points out: reactor seals, and is because iodine and chitosan iodine all have volatility, reacts in airtight environment, can reduce volatilization and scatter and disappear.
The principle of the inventive method is iodine energy oxidation chitosan molecule end-RH group (chitosan itself contains a small amount of water):
-RH＋I
2＋H
20→?-ROH＋2I
-＋3H
+
Can generate a large amount of I
-, with I
2Be combined into I
3 -, further with H
+Be combined into HI
3, last and chitosan complex forms chitosan iodine.
The present invention adopts solid reaction process to prepare chitosan iodine, does not use any catalyzer, produces steady quality, chitosan iodine that output is high, for chitosan iodine has been opened up a kind of new preparation method.This chitosan iodine can be prepared into as raw material and be applicable to cavity use, the various pharmaceutical dosage forms of external application, medical material, sterilizing agent.
Embodiment
The following example describes the specific embodiment of the invention in detail, but is not limited to following examples:
EXAMPLE lTake chitosan 10kg, iodine l0kg adds in solid phase reactor, seals, reactor makes mixing of materials even with the speed of 50r/min rotation 10min; Slowly be heated to 60 ℃, keep constant temperature 8h; In reaction process, reactor is constantly done rotatablely moving of positive and negative alternate every 30min, makes material reaction complete; Reaction is shut down after finishing, and after material was cooling, the opening discharging was crossed 65 mesh sieves and namely got chitosan iodine 19.8kg.
Embodiment 2Take chitosan 20kg, iodine l0kg adds in solid phase reactor, seals, reactor makes mixing of materials even with the speed of 60r/min rotation 20min; Slowly be heated to 80 ℃, keep constant temperature 8h; In reaction process, reactor is constantly done rotatablely moving of positive and negative alternate every 30min, makes material reaction complete; Reaction is shut down after finishing, and after material was cooling, the opening discharging was crossed 65 mesh sieves and namely got chitosan iodine 29.7kg.
Embodiment 3Take chitosan 30kg, iodine l0kg adds in solid phase reactor, seals, reactor makes mixing of materials even with the speed of 70r/min rotation 30min; Slowly be heated to 90 ℃, keep constant temperature 12h; In reaction process, reactor is constantly done rotatablely moving of positive and negative alternate every the 50min clock, makes material reaction complete; Reaction is shut down after finishing, and after material was cooling, the opening discharging was crossed 80 mesh sieves and namely got chitosan iodine 39.6kg.
Embodiment 4Take chitosan 40kg, iodine l0kg adds in solid phase reactor, seals, reactor makes mixing of materials even with the speed of 80r/min rotation 10min; Slowly be heated to 70 ℃, keep constant temperature 14h; In reaction process, reactor is constantly done rotatablely moving of positive and negative alternate every 60min, makes material reaction complete; Reaction is shut down after finishing, and after material was cooling, the opening discharging was crossed 65 mesh sieves and namely got chitosan iodine 49.5kg.
Embodiment 5Take chitosan 50kg, iodine l0kg adds in solid phase reactor, seals, reactor makes mixing of materials even with the speed of 90r/min rotation 20min; Slowly be heated to 80 ℃, when keeping constant temperature 16h; In reaction process, reactor is constantly done rotatablely moving of positive and negative alternate every 50min, makes material reaction complete; Reaction is shut down after finishing, and after material was cooling, the opening discharging was crossed 65 mesh sieves and namely got chitosan iodine 59.4kg.
Embodiment 6Take chitosan 60kg, iodine l0kg adds in solid phase reactor, seals, reactor makes mixing of materials even with the speed of 100r/min rotation 30min; Slowly be heated to 90 ℃, keep constant temperature 14h; In reaction process, reactor is constantly done rotatablely moving of positive and negative alternate every 40min, makes material reaction complete; Reaction is shut down after finishing, and after material was cooling, the opening discharging was crossed 80 mesh sieves and namely got chitosan iodine 69.3kg.
Accelerated stability test measurement result such as the following table of available iodine content in the chitosan iodine of making:
Available iodine content measurement result unit (%) in chitosan iodine
Claims (4)
1. method for preparing chitosan iodine, its feature comprises the following steps:
The first step, adds in solid phase reactor 1 part of 1～6 part of chitosan and iodine according to mass ratio, tightly adds a cover; Reactor slow circumvolve 10～30min makes mixing of materials even;
Second step then slowly is heated to 60 ℃～90 ℃, afterwards constant temperature 8～16h; In process, reactor is done rotatablely moving of positive and negative alternate every 30～60min, until reaction is completed;
After three-step reaction finishes, the rotation of stopped reaction device, after material was cooled to room temperature, discharging was sieved, and the particulate that obtains is the chitosan iodine product;
Wherein said chitosan is water-insoluble chitosan.
2. the method for claim 1, the viscosity that it is characterized in that described chitosan is 0.02～0.10Pas.
3. the method for claim 1, is characterized in that in the described the first step and second step, the speed of rotation of reactor is controlled at below 100r/min.
4. the method for claim 1, is characterized in that in described the 3rd step, the described order number that sieves is more than 60 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105560299A CN103113492A (en) | 2012-12-20 | 2012-12-20 | Method for preparing iodine chitosan |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105560299A CN103113492A (en) | 2012-12-20 | 2012-12-20 | Method for preparing iodine chitosan |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103113492A true CN103113492A (en) | 2013-05-22 |
Family
ID=48411915
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012105560299A Pending CN103113492A (en) | 2012-12-20 | 2012-12-20 | Method for preparing iodine chitosan |
Country Status (1)
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| CN (1) | CN103113492A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107281473A (en) * | 2017-05-08 | 2017-10-24 | 阮伟 | A kind of composition of maintenance uterine cavity mucous membrane and preparation method thereof |
| CN109125792A (en) * | 2018-07-16 | 2019-01-04 | 广西民族大学 | A kind of cassava porous-starch hemostatic material and its preparation method and application |
| RU2795219C1 (en) * | 2022-07-21 | 2023-05-02 | Федеральное государственное бюджетное учреждение науки Иркутский институт химии им. А.Е. Фаворского Сибирского отделения Российской академии наук (ИрИХ СО РАН) | Method for obtaining iodine-containing arabinogalactan composites with antimicrobial and antifungal properties |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994026788A1 (en) * | 1993-05-07 | 1994-11-24 | Development Biotechnological Processes S.N.C. Di Pelliccia Maria Teresa | Process for the preparation of iodinated biopolymers having disinfectant and cicatrizing activity, and the iodinated biopolymers obtainable thereby |
-
2012
- 2012-12-20 CN CN2012105560299A patent/CN103113492A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994026788A1 (en) * | 1993-05-07 | 1994-11-24 | Development Biotechnological Processes S.N.C. Di Pelliccia Maria Teresa | Process for the preparation of iodinated biopolymers having disinfectant and cicatrizing activity, and the iodinated biopolymers obtainable thereby |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107281473A (en) * | 2017-05-08 | 2017-10-24 | 阮伟 | A kind of composition of maintenance uterine cavity mucous membrane and preparation method thereof |
| CN109125792A (en) * | 2018-07-16 | 2019-01-04 | 广西民族大学 | A kind of cassava porous-starch hemostatic material and its preparation method and application |
| RU2795219C1 (en) * | 2022-07-21 | 2023-05-02 | Федеральное государственное бюджетное учреждение науки Иркутский институт химии им. А.Е. Фаворского Сибирского отделения Российской академии наук (ИрИХ СО РАН) | Method for obtaining iodine-containing arabinogalactan composites with antimicrobial and antifungal properties |
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Application publication date: 20130522 |