CN1030339C - Method for making absorbable hemostatic dressing - Google Patents
Method for making absorbable hemostatic dressing Download PDFInfo
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- CN1030339C CN1030339C CN92105622A CN92105622A CN1030339C CN 1030339 C CN1030339 C CN 1030339C CN 92105622 A CN92105622 A CN 92105622A CN 92105622 A CN92105622 A CN 92105622A CN 1030339 C CN1030339 C CN 1030339C
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- alginate
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Abstract
The present invention relates to a method for preparing absorbable hemostatic medical dressing. Sodium alginate is used as a raw material, and is prepared into spinning raw liquid. Water solution containing solidified calcium chloride is used as a solidification system, and is spun and formed on a spinning machine by a conventional method. The calcium content and the spun filament morphological structure in the calcium alginate-sodium compound salt are controlled by a method of properly decreasing the coagulant content in a coagulating bath, prolonging the coagulating time and decreasing the jet stretch. The spun filament is stretched in an air medium, the alginate fiber with the intensity of 3 g/d can be prepared, the alginate fiber is dried, cut and dried by a nonwoven fabric technology, and thus, the required medical dressing is prepared. The present invention has the advantages of simple technology and low production cost, and the prepared product has the characteristics of quick hemostasis and high absorbability.
Description
The present invention relates to the method for making in chemical the aspect field, particularly absorbable hemostatic dressing of medical dressing.
Spy in the open people's communique of Japan's special permission opens the method for making of having announced a kind of calcium phosphate fibre among the clear 63-145418.Its objective is that manufacturing is used as the choke material that the damaged hole of bone is gone up in medical treatment with phosphate fiber substituted apatite particle.Be in the method with the solution of Sodium Alginate and sodium phosphate calcium ions solidification liquid in be shaped the treated again hydration apatite fiber that obtains.Because sodium phosphate is a lower-molecular substance, thereby the spinning solution that can not form thickness soluble in water can not be spun into fiber,, removes algae depickling sodium and obtain the apatite fiber through processing at last so adopt Sodium Alginate solution as carrier.This fiber is without drawing orientation, and intensity is low, can not process by nonwoven fabric, only is made for choke material and uses.At as-spun fibre after Ageing Treatment, calcium content height in the fiber, and be the apatite composition, therefore, sintering makes the fiber before the alginic acid carbonization can not be used as medical absorbable hemostatic dressing purposes.
Spy in the open communique of Japan's special permission opens and has announced a kind of adsorbent fibers goods that contain the active carbon adsorption composition among the flat 1-52821, utilizes the carrier of Calcium Alginate fiber as activated carbon constituents.In the spinning technique of this application, do not comprise the operation that spinning solution is extruded from spinneret orifice, more can't draw orientation its fiber, fibrous because its product only is, but not fineness and length is than the fiber of homogeneous, its length is the 2-6 millimeter only.Therefore, the gained fibre strength is low, can not process by nonwoven fabric again, only limits to use for sorbing material.Calcium content height in fiber closes activated carbon 80%, and outward appearance is black, can not be used for medical absorbable hemostatic dressing purposes.
WO89/12471 has announced a kind of alginate series fiber nonwoven fabric with certain calcium/sodium ratio, is used for medical hemostatic dressing.Its manufacture method be with treated Sodium Alginate solution by viscose glue type spinning head be extruded into contain solidifying of calcium chloride molten in, again with fiber drawing-off in the steam heat case.Prepared thus fiber is the Calcium Alginate fiber, regulates calcium/sodium than the Calcium Alginate that obtains being suitable for medical hemostatic dressing purposes/sodium salt fiber, wherein Ca/Na=30: 70-70 through post processing again: 30.In this patent, having added clorox in spinning solution is the oxidative degradation agent; Sodium sulfite is the reduction protection agent, add cetylpyridinium chloride as preventing that fiber from gluing the And agent in molten solidifying, these compositions are unfavorable for the preparation of pure alginate, so the unit that makes of gained fiber spins that cloth only limits to body surface bleeding-stopping dressing purposes and can not use as absorbing bleeding-stopping dressing in the body; Secondly, this patent adopts the steam heat case in traction technology, this method is unsuitable for the draw orientation of alginate fiber, make fiber in the high-temperature water vapor medium, become fragile on the contrary and be unable to undergo high drafting, particularly even more serious to the influence of Calcium Alginate/sodium complex salt fiber, be unfavorable for the macromolecular orientation in the fibre structure and the raising of intensity; Three, this patent is the Calcium Alginate fiber by wet spinning technology gained fiber, its calcium content is near saturation value, need to regulate calcium/sodium ratio by complicated aftertreatment technology, so that obtain being suitable for Calcium Alginate/sodium salt fiber that medical hemostatic dressing is used, do that like this cost is increased greatly, and contaminated environment.
The object of the invention is: a kind of method for making of absorbable hemostatic dressing is provided, simplifies technological process in the method, enhance product performance, make the pure and bulk softness of product, gas permeability and moisture retention are good, thereby improve haemostatic effect.
The present invention seeks to reach like this: the employing Sodium Alginate is a raw material, omitted stoste degradation technique of the prior art, hot draft process, aftertreatment technology, spinning technique on conventional wet method frame, by coagulating agent content in the suitable reduction coagulating bath, prolong setting time, calcium content and spun filament morphosis in the method control alginate of reduction jet stretch, in air dielectric, get the alginate fiber that intensity reaches 3g/d after drawing-off 1.5-2.5 times, be made as the absorbable hemostatic dressing of nonwoven fabric subsequently by dry method nonwoven fabric prior art, thereby the object of the invention has just reached fully.
The present invention is described in detail below in conjunction with embodiment.
Technological process of the present invention is:
Sodium Alginate+water → dissolving → spinning solution → vacuum defoamation → extrusion metering → spray orifice extrudes → solidified forming and jet stretch → spun filament air dielectric drawing-off → alginate fiber → washing → drying → cut-out → combing in calcium chloride water, lapping, acupuncture → nonwoven fabric → section, packing → r ray sterilizing → absorbable hemostatic dressing.
From above-mentioned flow process as can be known: it is raw material that the present invention adopts Sodium Alginate, stoste degradation technique of the prior art, hot draft process, aftertreatment technology have been omitted, spinning technique on conventional wet method frame, by coagulating agent content in the suitable reduction coagulating bath, prolong setting time, reduce the method for jet stretch and control calcium content and spun filament morphosis in the alginate, in air dielectric, obtain the alginate fiber that intensity reaches 3g/d after drawing-off 1.5-2.5 times, make nonwoven fabric with the dry method non-woven technology.
The used spinning solution employing of the inventive method specification is that the Sodium Alginate of 95-105CPS is made preparation of raw material, preferably is solvent with the deionized water with pure water.Because molecular weight is moderate, does not need artificial control degradation, also need not oxidizer and reductant in solvent, this Sodium Alginate aqueous solution is made spinning solution stability, rheological characteristic and good spinnability.
One of characteristics of the present invention are exactly with 20-200CPS, and preferably the aqueous solution of the Sodium Alginate of 95-105CPS is as spinning solution, and solvent for use is a preferably deionized water of water; The Sodium Alginate solid content that is made into stoste is a 3-10(weight) %, preferably 4.5-5.5(weight) %.If with low excessively molecular weight stoste then coagulation ability is poor, the gained fiber crisp and a little less than; As using the too high Sodium Alginate of molecular weight; then it is a powder stock; solubility is low; the molecular weight distribution broad, institute join the stoste rheological property and spinnability poor, must be by artificial control degradation; for example just to add clorox in spinning solution be the oxidative degradation agent to WO89/12471; add sodium sulfite as the reduction protection agent, its operation is complicated, and influences the purity of product.
Two of characteristics of the present invention are to adopt to contain the moderate aqueous solution of calcium chloride and do coagulating bath and setting-time control: use calcium chloride to be coagulating agent, calcium chloride belongs to prior art as coagulating agent.When running into inorganic acid or the metal ion more than the divalence such as Ca, Cu, Fe, Al etc., water-soluble Sodium Alginate then generates corresponding water-insoluble alginic acid or its esters gel.The main points of this one procedure are to make calcium in Calcium Alginate-sodium salt-sodium ion ratio moderate, the effect of sodium ion is to increase the hydrophily of fiber, the effect of calcium ion is and disengages after blood contacts, become the calcium activated clotting factor, the ratio of calcium-sodium ion determines the comprehensive anastalsis mechanism of fibrin ferment gel layer of this bleeding-stopping dressing thus.Prior art also adopts the compound of Ca such as calcium chloride as coagulating agent, but its shortcoming is: the Ca-Na ratio is not suitable in alginate; Perhaps hydrophily is bad, and perhaps calcium has been released quantity not sufficient when contacting with blood.The inventive method contains calcium chloride 1-6(weight) %, best 1-2(weight) aqueous solution of %, the present invention adopts the aqueous solution of low calcium chloride content as coagulating bath, can make the Ca/Na ratio in the alginate moderate, setting time is 10-50 second, and then the Ca ratio is excessive for overlong time, and the time reaches weak point, it is little then to contain the Ca ratio, all can not meet the demands.Calcium/sodium ratio in such technology controlling and process gained Calcium Alginate-sodium salt is: 4.5/5.5-7.5/2.5.
In the WO89/12471 patent, also use calcium chloride to make coagulating agent, in embodiment, use 1% calcium chloride to make coagulating agent, and the calcium in gained Calcium Alginate-sodium salt/sodium content ratio is 30: 70-70: 30.So Calcium Alginate/sodium complex salt that also can obtain to meet the requirements.But in calcium chloride solution, add cetylpyridinium chloride (a kind of quaternary ammonium salt wetting agent) as preventing that fiber from gluing the And agent.This processing is influential to the purity of made Calcium Alginate fiber, thereby influences the range of application of bleeding-stopping dressing.
Three of main points of the present invention are that jet stretch is controlled to be 10-30% in the wet spinning process, are preferably 18-22%.By the Sodium Alginate aqueous solution as spinning solution, through vacuum defoamation, press water amount, spray orifice is extruded, clamp-on in the coagulating bath that contains calcium chloride, owing to the curing that is shaped of the solvent generation double diffusion effect in coagulating agent and the stoste, coagulation bath content is 10-45(weight in the spun filament in the wet spinning process after the jet stretch) %, be preferably 20-25(weight) %, spun filament air draft medium drawing-off after jet stretch, draw ratio is 1.5-2.5.
And in draft process, adopt wet method steam heat case in the WO89/12471 patent, this processing is unfavorable for the macromolecular orientation of fibre structure and the raising of intensity.
Be controlled to be 10-30% with jet stretch among the present invention, be preferably 18-22%, lower than prior art.As the jet stretch height, then easily make fiber form cortex-core structure, influence the overall orientation degree and the intensity of fiber.The present invention's 10-30% jet stretch, the overall orientation degree and the intensity of fiber are better.
Spun filament air draft medium drawing-off, method is easy, and is effective.The inventive method is with low jet stretch, high spun filament coagulating agent content, and the high jet stretch of air dielectric draw ratio, low spun filament coagulating agent content can improve about fibre strength 1g/d with the method for high moist steam or other medium drawing-off, and reduce cost.
Four of feature of the present invention is to adopt dry state alginate fiber to make nonwoven fabric by combing, lapping, needling process, the length of alginate fiber is chosen as 55-65mm, better in the uniformity of lapping under this fibre length and the nonwoven fabric intensity after the acupuncture, gas permeability is strong, and bulk softness.
The present invention relates to the method for making of absorbable hemostatic dressing, the employing alginate is a raw material, and technological process is brief, solidify and the jet stretch process in the ratio of calcium and sodium ion in the control alginate, thereby make product have bulk flexibility, and then improve the absorption haemostatic effect; The present invention is also by control process parameters and the drawing-off of employing air dielectric, thereby the raising fibre strength is improved serviceability; Production cost of the present invention is low, can carry out industrial production; Products obtained therefrom dressing has quick-acting haemostatic powder, high-hydroscopicity, biocompatibility and biodegradation absorbability concurrently, is wound medical field new type ideal material.
Embodiment 1:
With specification is that the Sodium Alginate of 50CPS is dissolved in and is made into 9% the Sodium Alginate aqueous solution in the distilled water, air pressure with 4.5 crust after vacuum defoamation is pressed out to gear pump metering and conveying, after extruding, 0.06 mm dia spray orifice containing solidified forming in the calcium chloride-water coagulating bath of 6% calcium chloride, setting time is 10 seconds, and jet stretch is 30%.Nascent tow is derived 2.0 times of first break draft with 10 meters/minute speed, getting filament number is 2d, intensity is the alginate fiber of 1.35g/d, and fiber is fully washed, cut into 55 millimeters short fibers after the drying, is processed into nonwoven fabric through combing-lapping-needling process then on the nonwoven fabric machine.
Embodiment 2:
With specification is that the Sodium Alginate of 100CPS is dissolved in and is made into 5% the Sodium Alginate aqueous solution in the distilled water, air pressure with 4.5bar after vacuum defoamation is pressed out to gear pump metering and conveying, after extruding, 0.08 mm dia spray orifice containing solidified forming in the calcium chloride-water coagulating bath of 1.5% calcium chloride, setting time is 25 seconds, and jet stretch is 20%.Nascent tow is derived 2.2 times of first break draft with 10 meters/minute speed, gets filament number 1.5d, the alginate fiber of intensity 3.03g/d.Fiber cuts into 60 millimeters short fibers through fully washing after the drying, then with method addition nonwoven fabric similarly to Example 1.
Embodiment 3:
With specification is that the Sodium Alginate of 190CPS is dissolved in and is made into 3% the Sodium Alginate aqueous solution in the distilled water, air pressure with 4.5bar after vacuum defoamation is pressed out to gear pump metering and conveying, after extruding, 0.12 mm dia spray orifice containing solidified forming in the calcium chloride-water coagulating bath of 1% calcium chloride, setting time is 45 seconds, jet stretch is 10%, nascent tow is derived 1.4 times of first break draft with 6 meters/minute speed, gets filament number 3d, the alginate fiber of intensity 1.9g/d.Fiber cuts into 65 millimeters short fibers through fully washing after the drying, be processed into nonwoven fabric with method similarly to Example 1 then.
Embodiment 4:
With alginate fiber/chitin fiber is wet nonwoven fabrics (paper shape) the parcel alginate fiber that 50/50 ratio makes, be rolled into short column behind the bag bar, behind ray sterilizing, after exodontia, carry out gum and go out blood test, the result shows its haemostatic effect rapidly, definitely, and has analgesia, receipts creation to use.When take out hemostasis back can with tooth nest natural separation, to patient's no pain, so this dressing is desirable dentistry hemostatic material.
Embodiment 5:
The absorbable hemostatic dressing that method described in the embodiment 1 the is made test that is used to treat patients with decubitus is applied this dressing to pathogenic site ulcer place and is given 2 grades of parcels.According to what of diffusate, originally every day or every other day more change dressings once, with the healing gradually of wound and the slow disappearance of diffusate are changed 1-2 time weekly, until healing entirely, therefore, this dressing also is the desirable material that treats patients with decubitus.
Claims (3)
1, the method for making of absorbable hemostatic dressing, with the Sodium Alginate is raw material, with calcium chloride water as coagulating agent, containing calcium chloride in solidification liquid is 1%, calcium in prepared Calcium Alginate-sodium salt/sodium equivalent proportion is 4.5/5.5-7.5/2.5, make absorbable hemostatic dressing through spinning to form shape, drawing process and do not have the gauze manufacturing technique, it is characterized in that:
A) used Sodium Alginate raw material specification is 20-200CPS, and solvent for use is a water, and the Sodium Alginate solid content that is made into stoste is 3-10 (weight) %;
B) system is as coagulating bath admittedly with calcium chloride-water-setting, and setting time is 10-50 second, thereby controls the calcium/sodium ratio in above-mentioned required Calcium Alginate-sodium salt;
C) jet stretch is controlled to be 10-30% in the wet spinning process, and coagulation bath content is 10-45 (weight) % in the spun filament, and spun filament adopts the drawing-off of air draft medium, and draw ratio is 1.5-2.5;
D) adopt dry state alginate fiber to make nonwoven fabric by combing, lapping, needling process, the length of used alginate fiber is selected the 55-65 millimeter.
2, according to the said dressing method for making of claim 1, it is characterized in that: the Sodium Alginate solid content that is made in this stoste with deionized water in operation a) is a 4.5-5.5(weight) %.
3, according to the said dressing method for making of claim 1, it is characterized in that: c) in the operation in the spun filament of jet stretch in the wet spinning process coagulation bath content be 20-25(weight) %, jet stretch is controlled to be 18-22%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92105622A CN1030339C (en) | 1992-07-18 | 1992-07-18 | Method for making absorbable hemostatic dressing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92105622A CN1030339C (en) | 1992-07-18 | 1992-07-18 | Method for making absorbable hemostatic dressing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1068158A CN1068158A (en) | 1993-01-20 |
| CN1030339C true CN1030339C (en) | 1995-11-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN92105622A Expired - Fee Related CN1030339C (en) | 1992-07-18 | 1992-07-18 | Method for making absorbable hemostatic dressing |
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| Country | Link |
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| CN (1) | CN1030339C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1065138C (en) * | 1996-10-21 | 2001-05-02 | 杭州仁德医药有限公司 | Method for manufacture seaweed acid calcium medicated plaster and seaweed acid calcium fibre nonwoven fabrics |
| CN1333126C (en) * | 2004-04-28 | 2007-08-22 | 王小建 | Method for preparing hemostatic fiber non-woven cloth |
| CN100457990C (en) * | 2007-04-16 | 2009-02-04 | 青岛大学 | Producing method and use for common and functional calcium alginate fiber |
| CN102051751B (en) * | 2010-11-22 | 2012-10-03 | 浙江帕达斯医疗科技有限公司 | Preparation method of bamboo cellulose oily gauze dedicated for external wound |
| CN104947245A (en) * | 2015-07-13 | 2015-09-30 | 苏州华良化纤纺织有限公司 | Fabricating technique of alginate fiber cloth |
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1992
- 1992-07-18 CN CN92105622A patent/CN1030339C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1068158A (en) | 1993-01-20 |
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