CN104587517A - Preparation process of regenerated cellulose fiber absorbable hemostatic material - Google Patents
Preparation process of regenerated cellulose fiber absorbable hemostatic material Download PDFInfo
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- CN104587517A CN104587517A CN201410848483.0A CN201410848483A CN104587517A CN 104587517 A CN104587517 A CN 104587517A CN 201410848483 A CN201410848483 A CN 201410848483A CN 104587517 A CN104587517 A CN 104587517A
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- hemostatic material
- absorbable hemostatic
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Abstract
The invention provides a preparation process of a regenerated cellulose fiber absorbable hemostatic material, wherein the preparation process satisfies the using demand of clinical operation and is convenient to operate, the oxidation process of the existing regenerated cellulose fiber absorbable hemostatic material is improved, and the problem that the process cost is high, the pollution is great and the materials are severely wasted. The preparation process comprises the following steps: packing cyclohexane in a memory and introducing nitrogen dioxide gas after sealing to dissolve cyclohexane; preparing a regenerated cellulose fiber layer by using a blowing-carding unit and placing in a reaction kettle after cutting; introducing cyclohexane in the memory into the reactor to react, and after reaction, discharging cyclohexane to the memory for later use; cleaning an oxidative product in the reaction kettle by using alcohol and then dehydrating the product by using anhydrous ethanol; and blowing the dehydrated product and drying the product in vacuum to remove alcohol to obtain the absorbable hemostatic material. The production efficiency of the preparation process provided by the invention is close to that of the conventional process, and the product is easily decomposed and used in clinical use; and moreover, the production cost is lowered, the discharge of environmental pollutants is reduced, the reaction is uniform and controllable, and the preparation process is suitable for industrial production.
Description
Technical field
The present invention relates to preparation and the oxidation technology of regenerated cellulose.
Background technology
Regenerated cellulose of the present invention refers to viscose rayon, and it forms by native cellulose is refining, and from structure, it and native cellulose are all made up of glucose monomer, but it is purer than native cellulose, more homogeneous.Common regenerated cellulose is difficult to be degraded and absorbed in human body, but the regenerated cellulose after nitrogen dioxide oxidation, because the hydroxyl on its 6 is oxidized to carboxyl, become the carboxycellulose be easily absorbed by the body, simultaneously because the homogeneity of regenerated cellulose is better, the time that the carboxycellulose of preparation is absorbed by the body is also more homogeneous, thus becomes the excellent selection preparing Absorbable hemostatic material.
The oxidation technology of regenerated cellulose has been studied for many years, and be oxidized mainly through the nitrogen dioxide be dissolved in inert fluid at present, inert fluid is generally carbon tetrachloride, freon etc.Be generally textile cloth with the product of this explained hereafter, its fiber is comparatively thick, generally between 5D-150D, therefore the concentration of oxidant needs higher, the concentration of general nitrogen dioxide is selected more than 10%, and will reach this concentration, needs reactor to make pressure vessel dissolved under pressure.The nitrogen dioxide oxidation reaction of high concentration is relatively more violent and difficultly control, and is easily even ruptured by regenerated cellulose over oxidation.
The cleaning such as regenerated cellulose ethanol, isopropyl alcohol after oxidation, then dry.There is the impurity such as ethanol, isopropyl alcohol, water in regenerated celulose fibre, because regenerated cellulose poor heat conduction, general vacuum drying is difficult to the removing such as water, ethanol, and usually adopt lyophilization, energy consumption and efficiency are all lower.
Summary of the invention
The object of the invention is the non-woven fabrics moulding process problem for existing regenerated cellulose Absorbable hemostatic material, a kind of preparation technology of regenerated celulose fibre Absorbable hemostatic material is provided, can reaction cost be reduced, reduce production process to the impact of environment.For this reason, the present invention is by the following technical solutions:
A preparation technology for regenerated celulose fibre Absorbable hemostatic material, is characterized in that it carries out according to the following steps:
(1), in storage capsule load cyclohexane extraction, pass into nitrogen dioxide gas after sealing, make it be dissolved in cyclohexane extraction and form oxidation solution, in oxidation solution, the mass percent concentration of nitrogen dioxide is 1%-3%;
(2), regenerated celulose fibre be carded to block non-woven fabrics, non-woven fabrics is put into reactor, sealed reactor, pass into oxidation solution in step (1), in 10-35 DEG C of reaction, obtain oxidation product, the fiber number of regenerated cellulose is 1.0-3.0 danier;
(3), oxidation product is cleaned
(4), by the drying in 30-50 DEG C of forced air drying of the oxidation product after cleaning, removing volatile liquid, and then dewater in 50-80 DEG C of vacuum drying, obtain described Absorbable hemostatic material.
On the basis adopting technique scheme, the present invention has gone back and has adopted following further technical scheme:
In step (2), the length of regenerated cellulose is 30-40mm.
Block non-woven fabrics density in step (2) is 100g/ ㎡-300g/ ㎡.
In step (2), the mass ratio of regenerated cellulose and nitrogen dioxide is 0.05-3:1.
In 10-35 DEG C of response time 20-48h in step (2).
Step (3) middle volumetric concentration is flushing oxidation product 4-6 time of the ethanol water of 90%-95%, and then with soaked in absolute ethyl alcohol oxidation product 15-60min.
In step (4), oxidation product is at 30-50 DEG C of forced air drying 1-5h, and then at 50-80 DEG C of vacuum drying 1-10h.
First the present invention employs the viscose rayon of 1.0-3.0 danier as raw material, regenerated cellulose non-woven fabrics is prepared into by the method for combing, then react, now because viscose rayon diameter attenuates, surface area increases, the nitrogen dioxide of low concentration just can be oxidized, and reaction uniformity, controllability all promote, and also there is suitable shortening the simultaneous reactions time.
The inertia solution dissolving nitrogen dioxide gas in the present invention is cyclohexane extraction, and common inertia solution is carbon tetrachloride, freon etc.Cyclohexane extraction is used to solve freon, carbon tetrachloride etc. to environment, climatic influences.
Hemostasia products prepared by the present invention is non-woven fabrics, and during use, it can be larger than common gauze with the contact area of wound, simultaneously also faster by human body degraded and absorbed speed after hemostasis.By the contrast of like product, Non-woven fabrics product anthemorrhagic speed is than the anthemorrhagic speed fast about 33% of common gauze series products.
In the present invention, in inertia solution, content of nitrogen dioxide is very low, and the equipment therefore dissolving nitrogen dioxide does not need to be prepared into pressure vessel, thus has saved equipment cost and social resources.
The mode adopting forced air drying to be combined with vacuum drying when the present invention is dry, first removes the volatile gas such as ethanol, isopropyl alcohol with forced air drying, then removes moisture with vacuum drying.Avoid cryodesiccated use, saved equipment cost and social resources, also improved production efficiency.
Accompanying drawing explanation
Fig. 1 is the infrared absorption pattern of regenerated cellulose absorbable hemostatic product prepared by the embodiment of the present invention 6, and its abscissa is wavelength, and vertical coordinate is light transmittance.
Fig. 2 is the infrared absorption pattern of the regenerated cellulose absorbable hemostatic product of certain leading company commercially available.
Fig. 3 is the product structure schematic diagram prepared after utilizing Blowing carding conjunction technology.
Fig. 4 is Product Rendering prepared by the present invention.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited detailed description of the invention, also comprises the combination in any between each detailed description of the invention.
Embodiment 1:
The preparation method of present embodiment regenerated cellulose Absorbable hemostatic material, carry out according to the following steps: (1), in bin, load cyclohexane extraction, nitrogen dioxide gas is passed into after sealing, make it be dissolved in cyclohexane extraction and form oxidation solution, in oxidation solution, the mass percent concentration of nitrogen dioxide is 1%-3%; (2), on blowing-carding-drawing unit regenerated celulose fibre is carded to block non-woven fabrics, non-woven fabrics is put into reactor, sealed reactor, pass into oxidation solution in step (1), in 10-35 DEG C of response time 20-48h, obtain oxidation product; (3), by volumetric concentration be that the ethanol water of 90%-95% rinses oxidation product 4-6 time, then use soaked in absolute ethyl alcohol oxidation product 15-60min; (4), by the drying in 30-50 DEG C of forced air drying of the oxidation product after soaked in absolute ethyl alcohol, drying time is 1-5h, and then dry in 50-80 DEG C of vacuum drying, drying time is 1-10h, obtains Absorbable hemostatic material.
Above-mentioned cyclohexane extraction can be recycled.
Embodiment 2:
The present embodiment is as different from Example 1: in step (2), the fiber number of regenerated cellulose is 1.0-3.0 danier, length is 38mm.Other are identical with detailed description of the invention (1).
Embodiment 3:
The present embodiment is as different from Example 2: in step (2), the fiber number density of non-woven fabrics is 100-300g/ ㎡.Other are identical with embodiment 2.
Embodiment 4:
The present embodiment is as different from Example 3: in step (2), the mass ratio of regenerated cellulose and nitrogen dioxide is 0.05-3:1.Other are identical with embodiment 3.
Embodiment 5:
(1), in bin, load 4L cyclohexane extraction, pass into 32g nitrogen dioxide gas after sealing, make it be dissolved in cyclohexane extraction and form oxidation solution, now in oxidation solution, the mass percent concentration of nitrogen dioxide is 1%; (2), on blowing-carding-drawing unit, the regenerated cellulose short fiber of 1.5 daniers, 38mm length is carded to the block non-woven fabrics that density is 180g/ ㎡, get 16g non-woven fabrics and put into reactor, sealed reactor, pass into oxidation solution in step (1), in 25 DEG C of response time 48h, obtain oxidation product; (3), by volumetric concentration be 95% ethanol water rinse oxidation product 4 times, then use 500ml soaked in absolute ethyl alcohol oxidation product 15min; (4), by the drying in 30 DEG C of forced air dryings of the oxidation product after soaked in absolute ethyl alcohol, drying time is 1h, and then dry in 50 DEG C of vacuum dryings, drying time is 6h, obtains Absorbable hemostatic material.
Embodiment 6:
(1) in bin, load 40 cyclohexane extraction, pass into 64g nitrogen dioxide gas after sealing, make it be dissolved in cyclohexane extraction and form oxidation solution, now in oxidation solution, the mass percent concentration of nitrogen dioxide is 2%; (2), on blowing-carding-drawing unit, the regenerated cellulose short fiber of 1.5 daniers, 38mm length is carded to the block non-woven fabrics that density is 180g/ ㎡, get 32g non-woven fabrics and put into reactor, sealed reactor, pass into oxidation solution in step (1), in 25 DEG C of response time 24h, obtain oxidation product; (3), by volumetric concentration be 95% ethanol water rinse oxidation product 4 times, then use 500ml soaked in absolute ethyl alcohol oxidation product 15min; (4), by the drying in 30 DEG C of forced air dryings of the oxidation product after soaked in absolute ethyl alcohol, drying time is 1h, and then dry in 50 DEG C of vacuum dryings, drying time is 6h, obtains Absorbable hemostatic material.
The commercially available hemostasia products of this class adopts line density 5D ~ 150D(danier usually, line density unit, reactor product thickness) regenerated cellulose filaments be raw material, by weaving make hemostatic gauze.Because raw material line is comparatively thick, need could be oxidized with the nitrogen dioxide of high concentration, oxidizing process is wayward, and easy selective oxidation is excessive, and simultaneous reactions process need pressurizes, and consersion unit need make pressure vessel.The INFRARED ABSORPTION figure of its composition is shown in Fig. 2.
The present invention adopts nonwoven raw material regenerated cellulose short fiber, and line density is only 1.5D, and close technique by Blowing carding and be made into nonwoven cloth, its structural representation is shown in Fig. 3.Because raw material is comparatively thin, the nitrogen dioxide of available low concentration is oxidized, and whole course of reaction is gentleer, and controllability improves greatly, and simultaneous reactions carries out at normal temperatures and pressures, and process is safer.The INFRARED ABSORPTION figure of product of the present invention is shown in Fig. 1, from the contrast of Fig. 1, Fig. 2, both absworption peak position consistency, can prove that the chemical constitution of both products, composition are consistent, but the method applied in the present invention are safer, condition is more gentle, technical process is more easy to control.
Product utilization Blowing carding of the present invention closes technology and makes, and final form is non-woven fabrics, and available hands is divided into multilamellar, and Fig. 4 is shown in by effect schematic diagram.Can according to hemorrhage wound surface size when Clinical practice, the non-woven fabrics tearing off the suitable number of plies stops blooding, and because its fibril is short and small, fine and closely woven, can closely be applied on wound surface, by the lifting of this contact area, haemostatic effect exceedes 30% of textile hemostatic material.
Claims (6)
1. a preparation technology for regenerated celulose fibre Absorbable hemostatic material, is characterized in that it carries out according to the following steps:
(1), in storage capsule load cyclohexane extraction, pass into nitrogen dioxide gas after sealing, make it be dissolved in cyclohexane extraction and form oxidation solution, in oxidation solution, the mass percent concentration of nitrogen dioxide is 1%-3%;
(2), regenerated celulose fibre be carded to block non-woven fabrics, non-woven fabrics is put into reactor, sealed reactor, pass into oxidation solution in step (1), in 10-35 DEG C of reaction, obtain oxidation product, the fiber number of regenerated cellulose is 1.0-3.0 danier;
(3), oxidation product is cleaned
(4), by the drying in 30-50 DEG C of forced air drying of the oxidation product after cleaning, removing volatile liquid, and then dewater in 50-80 DEG C of vacuum drying, obtain described Absorbable hemostatic material.
2. the preparation technology of a kind of regenerated celulose fibre Absorbable hemostatic material according to claim 1, is characterized in that the block non-woven fabrics density in step (2) is 100g/ ㎡-300g/ ㎡.
3. the preparation technology of a kind of regenerated celulose fibre Absorbable hemostatic material according to claim 1, is characterized in that the mass ratio of regenerated cellulose and nitrogen dioxide in step (2) is 0.05-3:1.
4. the preparation technology of a kind of regenerated celulose fibre Absorbable hemostatic material according to claim 1, is characterized in that in step (2) in 10-35 DEG C of response time 20-48h.
5. the preparation technology of a kind of regenerated celulose fibre Absorbable hemostatic material according to claim 1, it is characterized in that step (3) middle volumetric concentration is flushing oxidation product 4-6 time of the ethanol water of 90%-95%, and then with soaked in absolute ethyl alcohol oxidation product 15-60min.
6. the preparation technology of a kind of regenerated celulose fibre Absorbable hemostatic material according to claim 1, is characterized in that in step (4), oxidation product is at 30-50 DEG C of forced air drying 1-5h, and then at 50-80 DEG C of vacuum drying 1-10 h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109295551A (en) * | 2018-08-30 | 2019-02-01 | 浙江科技学院 | A kind of novel processing step of oxidized regenerated cellulose product |
| CN114010834A (en) * | 2021-10-29 | 2022-02-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Acetyl-containing oxidized regenerated cellulose hemostatic dressing |
| CN114748499A (en) * | 2021-12-30 | 2022-07-15 | 杭州协合医疗用品有限公司 | Medical chitosan for articular cavity injection and preparation method thereof |
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| CN102018990A (en) * | 2010-12-16 | 2011-04-20 | 浙江科技学院 | Preparing method of oxidation cellulose hemostatic product |
| CN102558368A (en) * | 2011-12-16 | 2012-07-11 | 威高集团有限公司 | Preparation method of oxidized regenerated cellulose (ORC) absorbable hemostasis material |
| CN102908651A (en) * | 2012-10-30 | 2013-02-06 | 威高集团有限公司 | Preparation method of oxidized regenerated cellulose hemostatic material with micro-nano composite structure |
| CN102912622A (en) * | 2012-10-30 | 2013-02-06 | 威高集团有限公司 | Preparation method for oxidized regenerated cellulose hemostatic material with surface nanostructure |
| CN103643480A (en) * | 2013-12-11 | 2014-03-19 | 威高集团有限公司 | Preparation method of degradable composite oxidized microcrystalline cellulose haemostatic material |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4615880A (en) * | 1980-07-30 | 1986-10-07 | Ceskoslovenska Akademie Ved Of Prague | Dressing for wounds and the method for manufacturing thereof |
| CN102018990A (en) * | 2010-12-16 | 2011-04-20 | 浙江科技学院 | Preparing method of oxidation cellulose hemostatic product |
| CN102558368A (en) * | 2011-12-16 | 2012-07-11 | 威高集团有限公司 | Preparation method of oxidized regenerated cellulose (ORC) absorbable hemostasis material |
| CN102908651A (en) * | 2012-10-30 | 2013-02-06 | 威高集团有限公司 | Preparation method of oxidized regenerated cellulose hemostatic material with micro-nano composite structure |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109295551A (en) * | 2018-08-30 | 2019-02-01 | 浙江科技学院 | A kind of novel processing step of oxidized regenerated cellulose product |
| CN109295551B (en) * | 2018-08-30 | 2021-03-05 | 浙江科技学院 | Novel preparation method of oxidized regenerated cellulose product |
| CN114010834A (en) * | 2021-10-29 | 2022-02-08 | 上海纳米技术及应用国家工程研究中心有限公司 | Acetyl-containing oxidized regenerated cellulose hemostatic dressing |
| CN114748499A (en) * | 2021-12-30 | 2022-07-15 | 杭州协合医疗用品有限公司 | Medical chitosan for articular cavity injection and preparation method thereof |
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