CN1068158A - The method for making of absorbable hemostatic dressing - Google Patents

The method for making of absorbable hemostatic dressing Download PDF

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Publication number
CN1068158A
CN1068158A CN92105622A CN92105622A CN1068158A CN 1068158 A CN1068158 A CN 1068158A CN 92105622 A CN92105622 A CN 92105622A CN 92105622 A CN92105622 A CN 92105622A CN 1068158 A CN1068158 A CN 1068158A
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alginate
calcium chloride
weight
sodium
making
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CN1030339C (en
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孙玉山
李振华
卢森
王玥
骆强
王小龙
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TEXTILE SCIENTIFIC RESEARCH ACADEMY MINISTRY OF TEXTILE INDUSTRY
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TEXTILE SCIENTIFIC RESEARCH ACADEMY MINISTRY OF TEXTILE INDUSTRY
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Abstract

The present invention relates to the method for making of absorbable hemostatic medical dressing.It is that raw material is made into spinning solution that the present invention adopts Sodium Alginate, the aqueous solution that employing contains coagulating agent calcium chloride is coagulation system, spinning moulding on the conventional 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 Calcium Alginate-sodium complex salt of reduction jet stretch, drawing-off in air dielectric, obtain the alginate fiber that intensity reaches 3g/d, drying, cut-out and dry method do not have spinning process and obtain wanting medical dressing.Technology of the present invention is simple, and production cost is low, and products obtained therefrom has quick-acting haemostatic powder, high-absorbable.

Description

The method for making of absorbable hemostatic dressing
The present invention relates to the method for making in chemical the aspect field, particularly absorbable hemostatic dressing of medical dressing.
Make hemostatic gauze (" trial-production of hemostatic algin gauze and animal, clinical testing " from alginate fiber, the Institute of Oceanology of the Chinese Academy of Sciences, the Qingdao Chemical Fiber Plant technology is summed up, and is stated from the survey report B of the Institute of Oceanology of the Chinese Academy of Sciences No. 7, and trial-produce successfully in April, 1974).This institute adopts 200CPS raw material control degradation; Make coagulating agent with high calcium chloride content, high shower nozzle wire drawing is carried out post processing after being made into gauze again, so that the Sodium ratio in the control alginic acid acid Sodium complex salt.Its shortcoming is that technology is complicated, is difficult to form suitability for industrialized production, and fibre strength is low, and the product result of use is not obvious.
Also made nonwoven fabric (film shape) (EPU 0072680A and WO80/02300) with alginate fiber, they adopt clorox control oxidative degradation, make protective agent with sodium sulfite, hot aqueous medium's drawing-off, wet method laying net (aqueous suspension dispersion).Its technical disadvantages is: the adding ingredient in the stoste influences purity, stability and rheological property, and wet nonwoven fabrics is comparatively stiff, lacks bulk soft feeling, thereby influences haemostatic effect.
Also have at Medical Textiles, Vol.6.No.1 is loaded with the alginate fabric nonwoven cloth on p.2, and this article is undeclared to be to adopt dry method or wet method to make nonwoven fabric, but adopt hot draft process, prevent the processing method of fibre damage in the loose and nonwoven fabric process of fiber.Its shortcoming is that the fiber degree of hot draft process is lower.
Also having a kind of is glycerine medium drawing-off [Golovach, N.S, Illarionova, E.L., Kalinina, T.N.(VSSR), Deposited Dec.1981 SPSIL 331 Khp-D81,6pp(Russian)], it is the drawing-off medium that this author adopts the mixture of glycerine-water, and the intensity of gained alginate fiber can reach 21.8CN/tex(2.5g/d), but the cost height, glycerine reclaims difficulty, and fibre strength is not as good as air draft medium height.
The object of the invention is: a kind of method for making of bleeding-stopping dressing is provided, simplifies technological process in the method, enhance product performance, make the 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 after 1.5~2.5 times of the drawing-offs intensity reaches the alginate fiber of 3g/d, 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 → γShe Xianmiejun → 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 1.5~2.5 times of the drawing-offs, 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 the aqueous solution of the Sodium Alginate of best 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 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 former protein acid sodium of molecular weight, then it is this raw material of powder, solubility is low, the molecular weight distribution broad, the institute join the stoste rheological property and spinnability poor, must be by artificial control degradation, for example the Institute of Oceanology of the Chinese Academy of Sciences in 85~87 ℃ of 20 hours (see before and state document) of degrading, thereby has increased one procedure with the baking oven for heating method more; Then use peroxide degradation in WD 80/02300 patent application, operation is complicated.
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 seconds, 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.
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.
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 is with 10~30% jet stretches, and 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 γShe Xianmiejun, 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 weekly 1~2 time, until healing entirely, therefore, this dressing also is the desirable material that treats patients with decubitus.

Claims (4)

1, the method for making of absorbable hemostatic dressing is a raw material with the Sodium Alginate, as coagulating agent, makes dressing from spinning technique, drawing process and nonwoven fabric manufacturing technique with calcium chloride water, it is characterized in that:
A) used Sodium Alginate raw material specification is 20~200CPS, and solvent for use is a water, and the former protein acid sodium solid content that is made into stoste is 3~10 (weight) %;
B) adopt contain calcium chloride be the solid system of calcium chloride-water-setting of 1~6 (weight) % as coagulating bath, setting time is 10~50 seconds, thus the calcium/sodium ratio in control gained Calcium Alginate-sodium salt is: 4.5/5.5~7.5/2.5;
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 55~65 millimeters.
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 4.5~5.5(weight) %.
3, according to the said dressing method for making of claim 1, it is characterized in that: b) adopt in the operation to contain calcium chloride 1~2(weight) the solid system of calcium chloride-water-setting of % does coagulating bath.
4, 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%.
CN92105622A 1992-07-18 1992-07-18 Method for making absorbable hemostatic dressing Expired - Fee Related CN1030339C (en)

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CN1030339C CN1030339C (en) 1995-11-22

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Cited By (5)

* Cited by examiner, † Cited by third party
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
CN102051751A (en) * 2010-11-22 2011-05-11 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

Cited By (6)

* Cited by examiner, † Cited by third party
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
CN102051751A (en) * 2010-11-22 2011-05-11 浙江帕达斯医疗科技有限公司 Preparation method of bamboo cellulose oily gauze dedicated for external wound
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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