CN102886066A - Preparation method of calcium-containing soluble hemostatic material - Google Patents
Preparation method of calcium-containing soluble hemostatic material Download PDFInfo
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- CN102886066A CN102886066A CN2012103984802A CN201210398480A CN102886066A CN 102886066 A CN102886066 A CN 102886066A CN 2012103984802 A CN2012103984802 A CN 2012103984802A CN 201210398480 A CN201210398480 A CN 201210398480A CN 102886066 A CN102886066 A CN 102886066A
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Abstract
The invention discloses a preparation method of calcium-containing soluble hemostatic material. The calcium-containing soluble hemostatic material takes polysaccharide fiber as a raw material and is prepared by alkalization, etherification, calcification, alcohol washing and the like. The preparation method is mild in preparation conditions and short in production period which is about 2-3hours. The calcium-containing soluble hemostatic material has rapid hemostatic effect and adopts low-concentration alcoholic solution for washing; and compared with the prior art, the calcium-containing soluble hemostatic material saves 40-50% of alcohol and uses the low-concentration alcohol, thus production technology is simple and suitable for large-scale production.
Description
Technical field
The present invention relates to a kind of preparation method of medical dressing, particularly a kind of calcic soluble hemostyptic material preparation method.
Background technology
At present, medical dressing generally all be disinfect with degreasing cotton gauze rear for medical department, sucking blood of this medical dressing is relatively poor with hemostatic capability, particularly process chronic wound with the pus and blood exudate, after wound fluid is absorbed by dressing, mainly be absorbed in the capillary space between fiber and the fiber, liquid can be along the structure diffusion of fabric, pus and blood is taken to the healthy skin of wound perimeter from wound surface, cause the dipping of edge of wound, wound surface is enlarged; Easy adhesion when gauze is changed or removed destroy new tissue of growing, and it is not perishable to become garbage after using.Therefore, since the forties in 20th century, novel hemostatic material in medical use is just explored and study in the medical institutions of countries in the world constantly.Come out one after another such as hemostatic materials such as styptic powder, gelfoam, solvable hemostatic gauzes.Solvable hemostatic gauze has stronger affinity to water and saline, and fiber expands after moisture absorption, and on the one hand, a large amount of liquid are fixed on fibrous inside, has improved the total moisture pick-up properties of product; On the other hand, fiber makes the capillary space in the fabric stop up after expansion, thereby stops the horizontal proliferation of liquid, avoids the wound perimeter healthy skin to be flooded.After the fiber that has absorbed liquid is converted to hydrogel, wound surface is remained in the moistening environment, be conducive to gushing of cell and move and breed, can effectively promote the healing of wound.Quick moisture and dissolving in absorbing blood when solvable hemostatic gauze runs into blood, it is terminal that the colloid of formation stops up blood capillary, and impel blood concentrated, and viscosity increases, the blood flow that slows down, thus reach the purpose of sucking blood, stopping blooding.Solvable hemostatic gauze is compared with other hemostasis mode, and it is easier to operate, and can arbitrarily fold, twine, and sticks closely with wound surface, and haemostatic effect is good.20 century 70 America and Europes begin one's study and develop solvable hemostatic gauze, and be applied to clinical the eighties.China in 20th century the mid-80 begin to use clinically solvable hemostatic gauze, but most from import.The enterprise of existing several the solvable hemostatic gauzes of research and production of recent year, and Patents is arranged.But still because of complex technical process, the response time is long, and production cost is too high, and haemostatic effect is bad, uses the shortcomings such as raw material is safe not still can not large-scale production and be widely used.As the response time in Chinese patent CN1232236C, the CN1047976 production process more than 10h, adopt the alcoholic solution washing 80% or more in the washing process, consume a large amount of ethanol, the production cost height is not suitable for large-scale production.Patent CN186490 discloses a kind of hydroxyethyl modified cotton fiber fabric and preparation method thereof, use aborning oxirane, this raw material chemical property is active, very violent with the cotton fabric reaction, produce easily blast, reaction must slowly be carried out under vacuum condition, has certain potential safety hazard in the production process, response time needs 20～24h, and production efficiency is low.
Summary of the invention
Problem for prior art exists the invention provides a kind of calcic soluble hemostyptic material preparation method.
Its technical solution is:
A kind of calcic soluble hemostyptic material preparation method may further comprise the steps:
(1) alkalization: choosing the polysaccharide fiber is raw material, and itself and the alcohol-water solution of sodium hydroxide are reacted;
(2) etherificate: after step (1) is finished, in mentioned solution, add monoxone, at 40～90 ℃ of lower reaction 0.2～3h;
(3) calcification: the polysaccharide fiber after step (2) is processed is placed the alcohol-water solution of calcium chloride solution or calcium chloride, carry out ion-exchange reactions;
(4) alcohol wash: the employing percent by volume is 30%～50% the polysaccharide fiber of alcoholic solution washing after step (3) is processed, and drying gets calcic soluble hemostyptic material.
In the step (1): the alcohol of selecting in the alcohol-water solution of described sodium hydroxide is ethanol, isopropyl alcohol or both mixture.
In the step (1): the content of sodium hydroxide is preferably 50～100g/L in the alcohol-water solution of described sodium hydroxide; The quaternization time is preferably 0.5～2h.
In the step (2): etherification reaction temperature is preferably 60～70 ℃, and the response time is preferably 1～2h.
In the step (3): the ion-exchange reactions time is preferably 10～20min.
In the step (4): the calcium content of preferred described calcic soluble hemostyptic material 〉=0.1%(w/w).
In the step (4): preferably adopt alcoholic solution washing 2～4 times.
Compared with prior art, the present invention has the following advantages:
(1) the calcic soluble hemostyptic material of the present invention's preparation has stronger affinity to water and saline, a large amount of moisture can be introduced the inside of fiber, and behind liquid-absorbing, still can keep its fibrous structure, when absorbing a large amount of wound fluid, can peel off from wound on full wafer ground.Can carry out ion exchange with sodium ion in the blood after running into blood, because the formation of clot in the blood capillary end has been accelerated in the release of calcium ion, rapidly hemostasis.Simultaneously, it is terminal that lysigenous colloid stops up blood capillary, and impel blood concentrated, and viscosity increases, and the blood flow that slows down reaches the purpose of sucking blood, stopping blooding.In addition, because this product dissolving is rear with a large amount of anion, can activate Hageman factor, start intrinsic coagulation system, impel the generation of thrombin, under the effect of thrombin, Fibrinogen is hydrolyzed then, reinforce formation insoluble fibrin polymer through fibrin stabilizing factor, playing hemostasis and protecting the effect of wound.
(2) cost of material of the present invention's use is cheap, safety, and the process conditions such as alkalization in the production, etherificate, calcification, alcohol wash are gentle, and are with short production cycle, need approximately 2～3h; In the alcohol wash step, because the existence of calcium ion causes fiber water dissolubility variation, can use the low concentration alcoholic solution during washing, to compare with existing patent and can save 40～50% alcohol, and use the alcohol of low concentration, production technology is safer, suitable for mass production.
The present invention adopts alkalization and the principle of etherificate treatment step to be:
It is raw material that the present invention chooses the polysaccharide fiber, because the polysaccharide fiber is the polyhydroxy glucose polymer, hydroxyl can form hydrogen bond with water, therefore has certain water absorption, but its degree of crystallinity is high, and moisture is difficult for infiltrating through crystal region, the liquid that absorbs mainly is maintained in the capillary space between fiber and the fiber, so its water absorption and retentiveness are relatively poor.After using alkali treatment, the degree of crystallinity of fiber descends, and is conducive to the infiltration of reactant liquor, and the hydroxyl of fiber can with alkali reaction, generate the fiber sodium salt, the nucleophilie nucleus ability grow of hydroxyl group anion is conducive to the etherification reaction in later stage.
Etherification reaction mechanism as shown in the formula:
Etherification reaction is nucleophilic substitution, and reaction is easy to carry out under alkali condition, and the cellulose hydroxyl after the alkalization becomes negative oxygen ion, and its nucleophilicity grow is conducive to and chloroacetate reaction.
The specific embodiment
The invention will be further described below in conjunction with specific embodiment:
Embodiment 1
(1) be wrapped in from level to level the polysaccharide fiber of choosing on the instrument, immerse in the ethanol water of sodium hydroxide, the content of sodium hydroxide is 60g/L in the ethanol water of sodium hydroxide, the volume ratio of ethanol and water is 80%; bath raio (mass ratio of the ethanol water of polysaccharide fiber and sodium hydroxide) is 1:20; reactant liquor constantly flows in the control instrument, alkalization 1h.
(2) adding monoxone after alkalization is finished, 60 ℃ of etherificate 1h.
(3) roll except the solution on the polysaccharide fiber after etherificate is finished, put into the alcohol-water solution of calcium chloride, the mass percent concentration of calcium chloride is 0.5% in the alcohol-water solution of calcium chloride, and alcohol is 30% with the volume ratio of water, ion-exchange reactions 20min.
(4) after step (3) is finished, be the polysaccharide fiber of 40% alcoholic solution washing after calcification processing 2～3 times with percent by volume, after the salt that the eccysis reaction generates, hot air drying makes calcic soluble hemostyptic material.
The calcium content of prepared calcic soluble hemostyptic material reaches 0.1%(w/w) more than, the alcohol wash step is compared with existing patent can save 40～50% ethanol.
Embodiment 2
(1) roll except the solution on the polysaccharide fiber after etherificate is finished, put into the alcohol-water solution of calcium chloride, the mass percent concentration of calcium chloride is 1% in the alcohol-water solution of calcium chloride, and alcohol is 30% with the volume ratio of water, ion-exchange reactions 20min.
(2) be 30% washing with alcohol 2～3 times with percent by volume, after the salt that the eccysis reaction generates, hot air drying.
(3) all the other operations are identical with embodiment 1.
The calcium content of prepared calcic soluble hemostyptic material reaches 0.1%(w/w) more than, the alcohol wash step is compared with existing patent can save 40～50% ethanol.
Embodiment 3
(1) roll except the solution on the polysaccharide fiber after etherificate is finished, put into the alcohol-water solution of calcium chloride, the mass percent concentration of calcium chloride is 2% in the alcohol-water solution of calcium chloride, and alcohol is 30% with the volume ratio of water, ion-exchange reactions 10min.
(2) be 30% washing with alcohol 2～3 times with percent by volume, after the salt that the eccysis reaction generates, hot air drying.
(3) all the other operations are identical with embodiment 1.
The calcium content of prepared calcic soluble hemostyptic material reaches 0.1%(w/w) more than, the alcohol wash step is compared with existing patent can save 40～50% ethanol.
The preferred linen-cotton class of the polysaccharide fiber that adopts in above-described embodiment, chitosan etc., prepared calcic soluble hemostyptic material can utilize conventional method to make the medical dressing of the forms such as gauze, powder, film.
Claims (7)
1. calcic soluble hemostyptic material preparation method is characterized in that may further comprise the steps:
(1) alkalization: choosing the polysaccharide fiber is raw material, and itself and the alcohol-water solution of sodium hydroxide are reacted;
(2) etherificate: after step (1) is finished, in mentioned solution, add monoxone, at 40～90 ℃ of lower reaction 0.2～3h;
(3) calcification: the polysaccharide fiber after step (2) is processed is placed the alcohol-water solution of calcium chloride solution or calcium chloride, carry out ion-exchange reactions;
(4) alcohol wash: the employing percent by volume is 30%～50% the polysaccharide fiber of alcoholic solution washing after step (3) is processed, and drying gets calcic soluble hemostyptic material.
2. a kind of calcic soluble hemostyptic material preparation method according to claim 1 is characterized in that, in the step (1): the alcohol of selecting in the alcohol-water solution of described sodium hydroxide is ethanol, isopropyl alcohol or both mixture.
3. a kind of calcic soluble hemostyptic material preparation method according to claim 1 is characterized in that in the step (1): the content of sodium hydroxide is 50～100g/L in the alcohol-water solution of described sodium hydroxide; Response time is 0.5～2h.
4. a kind of calcic soluble hemostyptic material preparation method according to claim 1 is characterized in that in the step (2): reaction temperature is 60～70 ℃, and the response time is 1～2h.
5. a kind of calcic soluble hemostyptic material preparation method according to claim 1 is characterized in that in the step (3): the ion-exchange reactions time is 10～20min.
6. a kind of calcic soluble hemostyptic material preparation method according to claim 1 is characterized in that, in the step (4): the calcium content of described calcic soluble hemostyptic material 〉=0.1%.
7. a kind of calcic soluble hemostyptic material preparation method according to claim 1 is characterized in that, in the step (4): adopt alcoholic solution washing 2～4 times.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106265718A (en) * | 2016-08-17 | 2017-01-04 | 贵州金玖生物技术有限公司 | Surgical irrigating fluid and preparation method thereof |
| CN106474525A (en) * | 2016-11-16 | 2017-03-08 | 广东泰宝医疗科技股份有限公司 | A kind of novel antibacterial hemostatic gauze and preparation method thereof |
| CN106638092A (en) * | 2016-09-14 | 2017-05-10 | 青岛大学 | Flame-retardant paper pulp and preparation method for flame-retardant paper |
| CN108379649A (en) * | 2018-03-20 | 2018-08-10 | 张博 | A kind of biological polyoses Hemostatic Oral Liquid and preparation method thereof |
| CN109125794A (en) * | 2018-09-07 | 2019-01-04 | 广州迈普再生医学科技股份有限公司 | A kind of degradable high water-absorbing styptic powder and its preparation method and application |
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| US5470576A (en) * | 1992-06-08 | 1995-11-28 | The Kendall Company | Process for preparing the alginate-containing wound dressing |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106265718A (en) * | 2016-08-17 | 2017-01-04 | 贵州金玖生物技术有限公司 | Surgical irrigating fluid and preparation method thereof |
| CN106638092A (en) * | 2016-09-14 | 2017-05-10 | 青岛大学 | Flame-retardant paper pulp and preparation method for flame-retardant paper |
| CN106474525A (en) * | 2016-11-16 | 2017-03-08 | 广东泰宝医疗科技股份有限公司 | A kind of novel antibacterial hemostatic gauze and preparation method thereof |
| CN108379649A (en) * | 2018-03-20 | 2018-08-10 | 张博 | A kind of biological polyoses Hemostatic Oral Liquid and preparation method thereof |
| CN109125794A (en) * | 2018-09-07 | 2019-01-04 | 广州迈普再生医学科技股份有限公司 | A kind of degradable high water-absorbing styptic powder and its preparation method and application |
| CN109125794B (en) * | 2018-09-07 | 2021-08-31 | 广州迈普再生医学科技股份有限公司 | Degradable high-water-absorptivity hemostatic powder and preparation method and application thereof |
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