CN101724078A - Method for preparing oxidized cellulose - Google Patents
Method for preparing oxidized cellulose Download PDFInfo
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- CN101724078A CN101724078A CN200910310491A CN200910310491A CN101724078A CN 101724078 A CN101724078 A CN 101724078A CN 200910310491 A CN200910310491 A CN 200910310491A CN 200910310491 A CN200910310491 A CN 200910310491A CN 101724078 A CN101724078 A CN 101724078A
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Abstract
The invention discloses a method for preparing oxidized cellulose. The preparation method comprises the following steps: a, putting an oxidized cellulose material into inert solution; b, adding an oxidant into the inert solution, sealing the solution, stirring the solution for 10 to 12 hours by using a magnetic stirrer at the temperature of between 20 and 60 DEG C; c, taking the oxidized cellulose material out, and washing the oxidized cellulose material with purified water; d, drying the oxidized cellulose material by using a centrifugal machine, and then washing the oxidized cellulose material by cleaning solution; and e, drying the oxidized cellulose material to obtain a finished product. Because the inert solution is used as a reaction solvent, the oxidization reaction can be performed under the controllable conditions, the reaction is even, and the manufactured oxidized cellulose and oxidized regenerated cellulose products are stable and easy to store; and the reaction solvent and the oxidant can be reclaimed for recycle, so the method is economic and environment-friendly, and the production cost is greatly reduced.
Description
Technical field
The present invention relates to the particularly preparation method of SURGICEL of a kind of hemostatic material in medical use.
Background technology
At present, the preparation of SURGICEL is to be added in the aqueous solution by oxygenant to react, because of the polarity of water is very big, and the SURGICEL of the being produced fracture of easily shrinking, and the product structure instability, be difficult for preserving.Directly with under the oxynitride gaseous state condition Mierocrystalline cellulose being carried out oxidation, temperature of reaction is difficult to control, and reaction product instability, and want cryopreservation, and the costing an arm and a leg of oxynitride are difficult to recovery, and production cost is high.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of new preparation process of SURGICEL.This method adopts inert liq as action solvent, and oxidizing reaction is carried out under controlled condition, reaction evenly, product is stable to be preserved easily, and action solvent and oxygenant can recycle and reuse not only economy but also environmental protection.
For solving the problems of the technologies described above technical scheme of the present invention: the preparation method of SURGICEL.This method comprises the steps;
A, get the oxidized fibre cellulosic material, put into inertia solution;
B, in inertia solution, add oxygenant, airtight; Stirred 10-12 hour with magnetic stirrer, temperature is 20-60 ℃;
C, taking-up oxidized fibre cellulosic material are with purified water washing 2-3 time;
D, dry, wash with scavenging solution again with whizzer;
E, temperature 80-90 ℃ dry 1-3 hour down.
Among the preparation method of above-mentioned SURGICEL, described inertia solution can be HCFC-141b, tetracol phenixin, cyanogen fluorine ether and derivative thereof or fluoridize liquid and derivative.
Among the preparation method of aforesaid SURGICEL, described oxygenant is oxynitrides, perchloric acid and its esters, Periodic acid and its esters or nitric acid and nitrous acid and its esters.
Among the preparation method of aforesaid SURGICEL, described scavenging solution is alcohols and mixed solution thereof.
Among the preparation method of aforesaid SURGICEL, described oxidized fibre cellulosic material is cotton, purified cotton, absorbent cotton, degreasing cotton gauze and is other textiless of raw material with the cotton, or be the single of raw material or be mixed and made into regenerated fibre, viscose fiber, and be other textiless of raw material with regenerated fibre, viscose fiber with cotton or wood pulp.
Beneficial effect of the present invention: compared with prior art, the present invention adopts inert liq as action solvent, oxidizing reaction is carried out under controlled condition, reaction evenly, SURGICEL of making and oxidized regenerated cellulose product are stable to be preserved easily, and action solvent and oxygenant can recycle and reuse, not only economy but also environmental protection, and production cost reduces greatly.
The present invention is further illustrated below in conjunction with embodiment.
Embodiment
Embodiment 1.Add nitric acid and nitrite in the inertia solution.
Get purified cotton 50g, put into the 5000ml flask, add HCFC-141b solution 2000ml, add 8% nitric acid 500ml, add Sodium Nitrite 50g again, airtight; Stirred 12 hours temperature 20-30 ℃ with magnetic stirrer; Take out the each 2000ml of using purified water washing three times, after drying with whizzer, with anhydrous isopropyl alcohol 2000ml washing once, took out 90 ℃ of dryings 2 hours again, recording carboxyl-content is 8%.
Embodiment 2.Add nitric acid and nitrite in the inertia solution.
Extracting degreasing cotton gauze 50g puts into the 5000ml flask, adds HCFC-141b solution 2000ml, adds 8% nitric acid 500ml, adds Sodium Nitrite 50g again, and is airtight; Stirred 12 hours with magnetic stirrer, temperature 20-30 ℃, take out the each 2000ml of using purified water washing three times, after drying with whizzer, with anhydrous isopropyl alcohol 2000ml washing once, took out 90 ℃ of dryings 2 hours again, recording carboxyl-content is 7%.
Embodiment 3.Add nitric acid and nitrite in the inertia solution.
Get regenerated fibre silk goods 50g, put into the 5000ml flask, add cyanogen fluorine ethereal solution 2000ml, add 8% nitric acid 500ml, add Sodium Nitrite 50g again, airtight; Stirred 12 hours with magnetic stirrer, temperature 20-60 ℃, take out the each 2000ml of using purified water washing three times, after drying with whizzer, with anhydrous isopropyl alcohol 2000ml washing once, took out 90 ℃ of dryings 2 hours again, recording carboxyl-content is 10%.
Embodiment 4.Add nitrogen peroxide in the inertia solution
Get purified cotton 50g, put into the 5000ml flask, add HCFC-141b solution 2000ml, add nitrogen peroxide 60g, airtight; Stirred 12 hours with magnetic stirrer, temperature 20-30 ℃, take out the each 2000ml of using purified water washing three times, after drying with whizzer, with anhydrous isopropyl alcohol 2000ml washing once, took out 90 ℃ of dryings 2 hours again, recording carboxyl-content is 9%.
Embodiment 5.Add nitrogen peroxide in the inertia solution.
Extracting degreasing cotton gauze 50g puts into the 5000ml flask, adds cyanogen fluorine ethereal solution 2000ml, adds nitrogen peroxide 70g, and is airtight; Stirred 12 hours with magnetic stirrer, temperature 20-60 ℃, take out each 50% washed with isopropyl alcohol with 2000ml three times, after drying with whizzer, with anhydrous isopropyl alcohol 2000ml washing once, took out 90 ℃ of dryings 2 hours again, recording carboxyl-content is 10%.
Embodiment 6.Add nitrogen peroxide in the inertia solution.
Get regenerated fibre silk goods 50g, put into the 5000ml flask, add and fluoridize liquor 2000ml, add nitrogen peroxide 75g, airtight; Stirred 12 hours with magnetic stirrer, temperature 20-30 ℃, take out each 60% methanol wash with 2000ml three times, after drying with whizzer, with anhydrous isopropyl alcohol 2000ml washing once, took out 90 ℃ of dryings 2 hours again, recording carboxyl-content is 12%.
Embodiments of the present invention are not limited to the foregoing description, and the various variations of making under the prerequisite that does not break away from aim of the present invention all belong within protection scope of the present invention.
Claims (5)
1. the preparation method of a SURGICEL is characterized in that: comprise the steps;
A, get the oxidized fibre cellulosic material, put into inertia solution;
B, in inertia solution, add oxygenant, airtight; Stirred 10-12 hour with magnetic stirrer, temperature is 20-60 ℃;
C, taking-up oxidized fibre cellulosic material are with purified water washing 2-3 time;
D, dry, wash with scavenging solution again with whizzer;
E, temperature 80-90 ℃ dry 1-3 hour down.
2. the preparation method of SURGICEL according to claim 1, it is characterized in that: described inertia solution is HCFC-141b, tetracol phenixin, cyanogen fluorine ether and derivative thereof or fluoridizes liquid and derivative.
3. the preparation method of SURGICEL according to claim 1, it is characterized in that: described oxygenant is oxynitrides, perchloric acid and its esters, Periodic acid and its esters or nitric acid and nitrous acid and its esters.
4. the preparation method of SURGICEL according to claim 1, it is characterized in that: described scavenging solution is alcohols and mixed solution thereof.
5. the preparation method of SURGICEL according to claim 1, it is characterized in that: described oxidized fibre cellulosic material is other textiless of raw material for cotton, purified cotton, absorbent cotton, degreasing cotton gauze and with the cotton, or be the single of raw material or be mixed and made into regenerated fibre, viscose fiber, and be other textiless of raw material with regenerated fibre, viscose fiber with cotton or wood pulp.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103104919A CN101724078B (en) | 2009-11-26 | 2009-11-26 | Method for preparing oxidized cellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103104919A CN101724078B (en) | 2009-11-26 | 2009-11-26 | Method for preparing oxidized cellulose |
Publications (2)
| Publication Number | Publication Date |
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| CN101724078A true CN101724078A (en) | 2010-06-09 |
| CN101724078B CN101724078B (en) | 2011-09-14 |
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| CN2009103104919A Active CN101724078B (en) | 2009-11-26 | 2009-11-26 | Method for preparing oxidized cellulose |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102018990A (en) * | 2010-12-16 | 2011-04-20 | 浙江科技学院 | Preparing method of oxidation cellulose hemostatic product |
| CN105131130A (en) * | 2015-09-24 | 2015-12-09 | 江苏蓝湾生物科技有限公司 | Synthetic method of oxidized cellulose |
| CN105131131A (en) * | 2015-09-24 | 2015-12-09 | 江苏蓝湾生物科技有限公司 | Synthesis method of high-carboxylation-degree oxidized cellulose |
| CN108383916A (en) * | 2018-04-14 | 2018-08-10 | 青岛科技大学 | II crystal form Cellulose nanocrystal of one kind and preparation method thereof |
| CN108727507A (en) * | 2017-04-21 | 2018-11-02 | 中国农业大学 | Oxycellulose is prepared and its in the application for washing and carrying prescription face |
| CN109338722A (en) * | 2018-10-23 | 2019-02-15 | 河南祥禾卫材有限公司 | A kind of preparation process of absorabable hemostatic gauze |
-
2009
- 2009-11-26 CN CN2009103104919A patent/CN101724078B/en active Active
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102018990A (en) * | 2010-12-16 | 2011-04-20 | 浙江科技学院 | Preparing method of oxidation cellulose hemostatic product |
| CN102018990B (en) * | 2010-12-16 | 2013-05-08 | 浙江科技学院 | Preparing method of oxidation cellulose hemostatic product |
| CN105131130A (en) * | 2015-09-24 | 2015-12-09 | 江苏蓝湾生物科技有限公司 | Synthetic method of oxidized cellulose |
| CN105131131A (en) * | 2015-09-24 | 2015-12-09 | 江苏蓝湾生物科技有限公司 | Synthesis method of high-carboxylation-degree oxidized cellulose |
| CN108727507A (en) * | 2017-04-21 | 2018-11-02 | 中国农业大学 | Oxycellulose is prepared and its in the application for washing and carrying prescription face |
| CN108727507B (en) * | 2017-04-21 | 2022-09-30 | 中国农业大学 | Preparation of oxidized cellulose and application thereof in washing and medicine loading |
| CN108383916A (en) * | 2018-04-14 | 2018-08-10 | 青岛科技大学 | II crystal form Cellulose nanocrystal of one kind and preparation method thereof |
| CN108383916B (en) * | 2018-04-14 | 2020-12-22 | 青岛科技大学 | II-crystal-form cellulose nanocrystal and preparation method thereof |
| CN109338722A (en) * | 2018-10-23 | 2019-02-15 | 河南祥禾卫材有限公司 | A kind of preparation process of absorabable hemostatic gauze |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101724078B (en) | 2011-09-14 |
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