CN102886066B - Preparation method of calcium-containing soluble hemostatic material - Google Patents
Preparation method of calcium-containing soluble hemostatic material Download PDFInfo
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- CN102886066B CN102886066B CN201210398480.2A CN201210398480A CN102886066B CN 102886066 B CN102886066 B CN 102886066B CN 201210398480 A CN201210398480 A CN 201210398480A CN 102886066 B CN102886066 B CN 102886066B
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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 preparation method of calcic soluble hemostyptic material.
Background technology
At present, medical dressing be all generally disinfect with degreasing cotton gauze rear for medical department, sucking blood of this medical dressing is poor with hemostatic capability, particularly process the chronic wound with pus and blood exudate, after wound fluid is absorbed by dressing, be mainly absorbed in the capillary space between fiber and 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, when serious, can make wound surface expand; Easy adhesion when gauze is changed or removed, destroy new tissue of growing, and it is not perishable after using, to become garbage.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.As the hemostatic materials such as styptic powder, gelfoam, solvable hemostatic gauze are come out one after another.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 fabric stop up after expansion, thereby stops the horizontal proliferation of liquid, avoids wound perimeter healthy skin to be flooded.The fiber that has absorbed liquid is converted to after hydrogel, can make wound surface remain in a moistening environment, is conducive to gushing of cell and moves and breed, and can effectively promote the healing of wound.Quick moisture and dissolving in absorbing blood when solvable hemostatic gauze runs into blood, the colloid of formation stops up blood capillary end, and impels blood concentrated, and viscosity increases, the blood flow that slows down, thus reach the object of sucking blood, stopping blooding.Solvable hemostatic gauze, compared with other hemostasis mode, it is easier to operate, and can arbitrarily fold, be wound around, 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 start to apply 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 have Patents.But still because of complex technical process, the response time is long, 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.If the response time in Chinese patent CN1232236C, CN1047976 production process is more than 10h, in washing process, adopt more than 80% alcoholic solution washing, consume a large amount of ethanol, production cost is high, 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, react very violent with cotton fabric, easily produce blast, reaction must slowly be carried out under vacuum condition, has certain potential safety hazard in production process, response time needs 20～24h, and production efficiency is low.
Summary of the invention
For the problem of prior art existence, the invention provides a kind of preparation method of calcic soluble hemostyptic material.
Its technical solution is:
A preparation method for calcic soluble hemostyptic material, comprises the following steps:
(1) alkalization: choosing polysaccharide fiber is raw material, and it is reacted with the alcohol-water solution of sodium hydroxide;
(2) etherificate: after step (1) completes, add monoxone in above-mentioned solution, react 0.2～3h at 40～90 ℃;
(3) calcification: will be placed in through step (2) polysaccharide fiber after treatment the alcohol-water solution of calcium chloride solution or calcium chloride, and carry out ion-exchange reactions;
(4) alcohol wash: adopt the alcoholic solution that percent by volume is 30%～50% to wash through step (3) polysaccharide fiber after treatment, dry, obtain calcic soluble hemostyptic material.
In step (1): the alcohol of selecting in the alcohol-water solution of described sodium hydroxide is ethanol, isopropyl alcohol or both mixture.
In step (1): in the alcohol-water solution of described sodium hydroxide, the content of sodium hydroxide is preferably 50～100g/L; The quaternization time is preferably 0.5～2h.
In step (2): etherification reaction temperature is preferably 60～70 ℃, and the response time is preferably 1～2h.
In step (3): the ion-exchange reactions time is preferably 10～20min.
In step (4): the calcium content >=0.1%(w/w of preferred described calcic soluble hemostyptic material).
In 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 that prepared by the present invention has stronger affinity to water and saline, a large amount of moisture can be introduced to the inside of fiber, and after absorption liquid, still can keep its fibrous structure, in the time absorbing a large amount of wound fluid, can peel off from wound full wafer.After running into blood, can carry out ion exchange with sodium ion in blood, due to the release of calcium ion, accelerate the formation of clot in blood capillary end, rapidly hemostasis.Meanwhile, lysigenous colloid stops up blood capillary end, and impels blood concentrated, and viscosity increases, and the blood flow that slows down, reaches the object of sucking blood, stopping blooding.In addition, due to this product dissolve after 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 and form insoluble fibrin polymer through fibrin stabilizing factor, play hemostasis and protect the effect of wound.
(2) cost of material that the present invention uses is cheap, safety, and the process conditions gentlenesses such as alkalization in production, etherificate, calcification, alcohol wash, with short production cycle, approximately need 2～3h; In alcohol wash step, due to the existence of calcium ion, cause fiber water dissolubility variation, when washing, can use low concentration alcoholic solution, can save 40～50% alcohol compared with existing patent, 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 polysaccharide fiber, because polysaccharide fiber is polyhydroxy glucose polymer, hydroxyl can form hydrogen bond with water, therefore there is certain water absorption, but its degree of crystallinity is high, moisture is difficult for infiltrating through crystal region, the liquid absorbing is mainly maintained in the capillary space between fiber and fiber, and therefore its water absorption and retentiveness are poor.Use after alkali treatment, the degree of crystallinity of fiber declines, and is conducive to the infiltration of reactant liquor, and the hydroxyl of fiber can with alkali reaction, generate 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 alkalization becomes negative oxygen ion, and its nucleophilicity grow, is conducive to and chloroacetate reaction.
The specific embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1
(1) the polysaccharide fiber of choosing is wrapped on instrument from level to level, immerse in the ethanol water of sodium hydroxide, in the ethanol water of sodium hydroxide, the content of sodium hydroxide is 60g/L, 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; in control instrument, reactant liquor constantly flows, alkalization 1h.
(2) add monoxone, 60 ℃ of etherificate 1h after having alkalized.
(3) etherificate is rolled except the solution on polysaccharide fiber after completing, and puts into the alcohol-water solution of calcium chloride, and in the alcohol-water solution of calcium chloride, the mass percent concentration of calcium chloride is 0.5%, and the volume ratio of alcohol and water is 30%, ion-exchange reactions 20min.
(4) after step (3) completes, the alcoholic solution that is 40% by percent by volume washs polysaccharide fiber after calcification processing 2～3 times, and after the salt that 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, alcohol wash step can be saved 40～50% ethanol compared with existing patent.
Embodiment 2
(1) etherificate is rolled except the solution on polysaccharide fiber after completing, and puts into the alcohol-water solution of calcium chloride, and in the alcohol-water solution of calcium chloride, the mass percent concentration of calcium chloride is 1%, and the volume ratio of alcohol and water is 30%, ion-exchange reactions 20min.
(2) washing with alcohol that is 30% by percent by volume 2～3 times, after the salt that 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, alcohol wash step can be saved 40～50% ethanol compared with existing patent.
Embodiment 3
(1) etherificate is rolled except the solution on polysaccharide fiber after completing, and puts into the alcohol-water solution of calcium chloride, and in the alcohol-water solution of calcium chloride, the mass percent concentration of calcium chloride is 2%, and the volume ratio of alcohol and water is 30%, ion-exchange reactions 10min.
(2) washing with alcohol that is 30% by percent by volume 2～3 times, after the salt that 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, alcohol wash step can be saved 40～50% ethanol compared with existing patent.
The preferred linen-cotton class of polysaccharide fiber, the chitosan etc. that in above-described embodiment, adopt, prepared calcic soluble hemostyptic material can utilize conventional method to make the medical dressing of the forms such as gauze, powder, film.
Claims (3)
1. a preparation method for calcic soluble hemostyptic material, is characterized in that comprising the following steps:
(1) alkalization: choosing polysaccharide fiber is raw material, and it is reacted with the alcohol-water solution of sodium hydroxide;
(2) etherificate: after step (1) completes, add monoxone in above-mentioned solution, react 0.2～3h at 40～90 ℃;
(3) calcification: will be placed in through step (2) polysaccharide fiber after treatment the alcohol-water solution of calcium chloride solution or calcium chloride, and carry out ion-exchange reactions;
(4) alcohol wash: adopt the alcoholic solution that percent by volume is 30%～50% to wash through step (3) polysaccharide fiber after treatment, dry, obtain calcic soluble hemostyptic material;
In step (1): the alcohol of selecting in the alcohol-water solution of described sodium hydroxide is ethanol, isopropyl alcohol or both mixture; In the alcohol-water solution of described sodium hydroxide, the content of sodium hydroxide is 50～100g/L; Response time is 0.5～2h;
In step (3): the ion-exchange reactions time is 10～20min;
Calcium content >=0.1% of described calcic soluble hemostyptic material.
2. the preparation method of a kind of calcic soluble hemostyptic material according to claim 1, is characterized in that, in step (2): reaction temperature is 60～70 ℃, the response time is 1～2h.
3. the preparation method of a kind of calcic soluble hemostyptic material according to claim 1, is characterized in that, in step (4): adopt alcoholic solution washing 2～4 times.
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| 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 |
| 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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| CN1047976A (en) * | 1989-06-12 | 1990-12-26 | 湖南省衡阳卫生材料厂 | A kind of improvement of hemostatic gauze production method |
| US5470576A (en) * | 1992-06-08 | 1995-11-28 | The Kendall Company | Process for preparing the alginate-containing wound dressing |
| CN1109708C (en) * | 2000-03-24 | 2003-05-28 | 大连永兴医用材料有限公司 | Solable adhesion-preventing material preparing process with cellulose material and product |
| WO2002087643A1 (en) * | 2001-04-30 | 2002-11-07 | Beijing Textile Research Institute | Water soluble cellulose etherified derivates styptic materials |
| CN101703519A (en) * | 2009-11-10 | 2010-05-12 | 浙江大学 | Method for improving hemostatic effect of external-use zeolite hemostat by calcium ion modification |
| CN102526794B (en) * | 2012-01-19 | 2014-08-13 | 华东理工大学 | Calcium-complex starch-based microporous haemostatic material, and preparation method and application thereof |
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