CN106478825A - A kind of method for preparing hemostasis oxycellulose in ramie oxidation scouring processes - Google Patents
A kind of method for preparing hemostasis oxycellulose in ramie oxidation scouring processes Download PDFInfo
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- CN106478825A CN106478825A CN201610912568.XA CN201610912568A CN106478825A CN 106478825 A CN106478825 A CN 106478825A CN 201610912568 A CN201610912568 A CN 201610912568A CN 106478825 A CN106478825 A CN 106478825A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
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- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/04—Surgical adhesives or cements; Adhesives for colostomy devices containing macromolecular materials
- A61L24/08—Polysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
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- A61L2400/04—Materials for stopping bleeding
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Abstract
The invention provides raw ramie, with ramie raw ramie as raw material, is first ground into chopped fiber by a kind of method for preparing hemostasis oxycellulose in ramie oxidation scouring processes, it is swelling that immersion makes which fully soak；Then pretreated raw ramie chopped fiber is mixed with scouring solution, is incubated after intensification, fully removes the colloid in raw ramie using the oxidisability of specific oxidant, while the cellulose oxidation with active hydroxyl groups is become the oxycellulose containing a large amount of carboxyls；Fiber after oxidation processes is soaked with aqueous solutions of organic solvent, removes unreacted oxidant；Finally oxycellulose is separated from water, and dried process, finally give the hemostasis oxycellulose of powder state.The method flow that the present invention is provided is simple, and original two procedures are combined into a procedure, shortens total reaction time, saves medicine and cost, and efficiency is greatly improved.Products obtained therefrom anthemorrhagic speed is fast, and hemostasis efficiency is high, and effect stability is widely portable to the quick-acting haemostatic powder of the situations such as war wound, wound.
Description
Technical field
The present invention relates to a kind of method for preparing hemostasis oxycellulose in ramie oxidation scouring processes, belongs to weaving neck
The natural fiber in domain prepares the technical field with hemostasis with oxycellulose application.
Background technology
Medical absorbable hemostatic material causes the great attention of various countries' medical circle and industrial circle in recent years, with to hemostasis
The raising of material performance requirement, exploitation haemostatic effect more preferably, green, environmental protection, degradable, nontoxic, have no side effect, nonirritant,
Medical absorbable hemostatic material with good biocompatibility is imperative.Hemostatic material in medical use mainly has fibrin at present
The types such as glue, gelfoam, oxycellulose, microfibrillar collagen, shitosan and Sorbsan.Find from nature excellent
Biological material be processed improve, preparation method is simple, with low cost, the preferably new absorbable hemostatic material of haemostatic effect
Material, becomes a kind of and preferably selects.
The cellulose base hemostatic material extracted from cotton, flaxen fiber and various natural cellulosic materials is extensive by people's
Favor.Oxycellulose (Oxidized Cellulose, also referred to as 6- carboxycellulose) is the derivative of cellulose, with many
The big characteristic of hole and specific surface area, has good biocompatibility, biodegradability and nontoxic, can be answered as hemostatic material
Used in medical field.Ca after the hospital gauze that oxycellulose is made implants, in its carboxyl and blood plasma2+Hand over
Connection, is caused oxycellulose to be reacted with hemoglobin, forms artificial clot, so as to play anastalsis.Clinically it is used as at present
The oxycellulose commercial product of hemostatic gauze is " speed is yarn " (SURGICEL) of Johnson Co., but the existing shape of its product
State is unfavorable for being combined with other products, and production technology is more complicated, high cost, expensive, oxidation solution wave in production process
Take serious, it would be highly desirable to develop more preferable substitute products, probe into more excellent medical hemostatic oxycellulose preparation technology be one urgent
Proposition.
Ramie is a kind of native cellulose fibre of excellent performance, its tenacity fiber, is rich in gloss, and with corrosion resistant, no
Easily mouldy characteristic.The main component of ramie raw ramie is cellulose, additionally contains lignin, pectin, the non-fibre such as hemicellulose
The plain composition of dimension, is referred to as colloid.Before utilization, it is necessary to which winding colloid on cellulose is removed.Ramie aoxidizes degumming
From specific oxidant, the colloid molecule in ramee is cut off, oxidative degradation becomes small molecule, while retain cellulose becoming
The Degumming method for dividing.Oxidation degumming has the reaction time soon, and low cost is easy to operate, pollutes little, the advantage of less energy consumption, is current
The study hotspot of natural fiber preparation field.But, the oxidisability of some oxidants is stronger, with the intensification of degree of oxidation,
Also easily the C6 position primary hydroxy group on cellulose macromolecule chain glucose basic ring is become carboxyl, generates oxycellulose (i.e. 6-
Carboxycellulose), possess certain absorption property.Therefore, during ramie oxidation degumming prepares fiber, reasonable selection oxygen
Change system and modulation process condition, can achieve many things at one stroke, and can both remove gum components, also can be leniently the hydroxyl on cellulose
Base is oxidized to carboxyl, generates the oxycellulose with absorption property, realizes natural fiber and extracts and hemostatic material in medical use preparation
Double goal, so as to reach minimizing flow time, save medicine and cost, put forward efficient purpose.
Content of the invention
The technical problem to be solved in the present invention is to provide in a kind of ramie oxidation scouring processes to prepare hemostasis oxidized fibre
The method of element, by studying the relation between oxidation degumming and oxycellulose generation, rationally controls reaction process, allows ramie to take off
Glue is carried out with bath simultaneously with the generation of adsorptivity oxycellulose, obtains optimum degumming effect, and preparation is suitable for hemostasis
Cellulose-based Adsorbents, improve the added value of cellulose derivative.
In order to above-mentioned technical problem is solved, the technical scheme is that and prepare in a kind of ramie oxidation scouring processes of offer
The method of hemostasis oxycellulose, it is characterised in that：The method is made up of following 3 steps：
Step 1：Raw ramie fiber is pre-processed
Ramie raw ramie is ground into chopped fiber, chopped fiber is put into equilibrium water conten in closed container, determine returning for chopped fiber
Damp rate；Chopped fiber quality is weighed, its fiber dry weight is calculated according to regain；Deionized water is added in chopped fiber, by soaking
Raw ramie cellulose is made fully to soak swelling；
Step 2：The oxidation processes of cellulose
Concentration expressed in percentage by weight is 2%～10% oxidant, 0.5%～5% cellulose protective agent, 0.5%～4% fiber
Swelling agent, 0.5%～3% surfactant, 0.5%～3% chelating agent and distilled water are made into degumming reactant liquor；By ramie raw ramie
Chopped fiber and degumming reactant liquor mix in the reactor, and the initial pH value for adjusting degumming liquid is 3.0～14.0, and reactor is put into
In thermostat water bath, mixture under the conditions of lucifuge in stirred reactor, water-bath is warmed up to 50～100 DEG C, insulation 40
～150min, fully removes the colloid in raw ramie using the oxidisability of oxidant, while the cellulose oxidation with hydroxyl is become
Oxycellulose containing a large amount of carboxyls；
Step 3：The washing of oxycellulose and stabilization processes
By reacted fiber organic solvent washing by soaking, unreacted oxidant is removed, then deionized water is filled
Divide cleaning and dipping；Obtained mixture carries out centrifugation layering, and supernatant liquor is transferred in another container, and remaining concentration is fine
The plain suspension of dimension is put in vacuum freeze drier, is molded using liquid-nitrogen freeze drying, and the oxycellulose absorption of powder state is obtained
Agent, is finally putting into refrigerating chamber storage.
Preferably, in the step 1, the chopped fiber fineness being ground into is 20～100 mesh, adds distilled water in chopped fiber
It is 1%～10% to make cellulose solids mass percent concentration in distilled water, and the distilled water immersion time is 12～48h.
Preferably, in the step 2, by ramie raw ramie chopped fiber and degumming reactant liquor in mass ratio for 1: 10 in reactor
Middle mixing；It is the NaOH solution of 0.1mol/L or the HCl solution of 0.1mol/L to adjust the solution used by degumming liquid initial pH value；Stir
Mixing the mixture in reactor is continuously stirred with the speed of 200rpm with magnetic stirring apparatus.
Preferably, in the step 2, oxidant is sodium bromate, sodium chlorate, sodium chlorite, tetramethyl piperidine oxides-secondary
Sodium chlorate-sodium bromide tri compound oxidation system, nitric acid-phosphoric acid-natrium nitrosum oxidation system, SODIUM PERCARBONATE, sodium metaperiodate is high
Potassiumiodate, sodium hypochlorite, potassium percarbonate, sodium chlorate, one or more in sodium bromate.
Preferably, in the step 2, cellulose protective agent is polyaerylic acid sodium, anthraquinone, magnesium hydroxide, polyvinyl alcohol, water
Glass, polyacrylamide, magnesium silicate, antifebrin, resorcinol, sodium citrate, one or more in Sodium Benzoate.
Preferably, in the step 2, filament expansion agent includes urea, ethylenediamine, liquefied ammonia, thiocarbamide, 4- methyl morpholine-N-
Oxide, cupri ethylene diamine, one or two in dimethyl sulfoxide (DMSO).
Preferably, in the step 2, surfactant is polyvinyl alcohol, neopelex, dodecyl sodium sulfonate
Sodium, lauryl sodium sulfate, AEO (JFC), one or two in peregal.
Preferably, in the step 2, metal ion chelation agent includes aminotriacetic acid, sodium ethylenediamine tetramethylenephosphonate,
Diethylene triamine pentamethylene phosphonic, the adjacent sodium of ethylenediamine two, 1-hydroxy ethylidene-1,1-diphosphonic acid and its sodium salt, Sodium Polyacrylate,
One or more in ethylene diamine tetra methylene phosphonic acid sodium.
Preferably, in the step 3, the organic solvent after soaking reaction used by fiber is glycerine, ethylene glycol, acetone,
One or two in 1,3-PD, concentration are 0.1mol/L, and the washing by soaking time is 0.5～2h.
Preferably, in the step 3, the time of the abundant cleaning and dipping of deionized water is 24h；Obtained mixture leads to
Crossing centrifuge carries out centrifugation layering, and centrifuge speed is 6000～12000rpm, and centrifugation number of times is 3～6 times；Freeze-drying is molded
Temperature be -40～-60 DEG C, freeze-drying shaping 10～60Pa of pressure, freeze-drying shaping time be 4～10h.
The absorption of novel oxidized cellulose family is developed and developed to the method that the present invention is provided with natural remie fiber as raw material
Agent.From specific oxidant, Reasonable Regulation And Control reaction process condition, while Resins of Original Hemp composition is removed, cellulose
C6 position primary hydroxyl selective oxidation on chain becomes carboxyl, changes the structure of cellulose, gives cellulose new function so as to become
Oxycellulose with hemostatic function, has expanded the application of cellulose.
The present invention provide method overcome existing ramie oxidation degumming and hemostasis oxycellulose technology of preparing not
Foot, flow process are simple, and original two procedures are combined into a procedure, shorten total reaction time, save medicine and cost, efficiency
Greatly improve.While preparation method process is simple, environmental friendliness, gently, equipment requirement is low, is easy to scale metaplasia for reaction condition
Produce.The residual gum content of products obtained therefrom is 2.0%～2.3%, and the degree of polymerization is 300～500, and carboxyl-content is 18%～22%, hemostasis
Speed is fast, and hemostasis efficiency is high, effect stability, with the body absorption time is short, broad-spectrum sterilization anti-inflammatory, promotes wound healing etc. excellent
Point, is not in addition affected by surface of a wound size and position.Compared with existing hemostasis medical material, the oxycellulose of the present invention has
Environmental friendliness, reaction condition are gentle, equipment requirement is low, good chemical stability, are widely portable to the shapes such as war wound, wound
The quick-acting haemostatic powder of condition.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the present invention.In addition, it is to be understood that after the content for having read present invention instruction, people in the art
Member can be made various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
A kind of method for preparing hemostasis oxycellulose in ramie oxidation scouring processes is as follows：
Ramie raw ramie pulverizer is ground into the chopped fiber that fineness is 40 mesh, is put in the container with sealing ring and balances
Moisture, the regain for determining chopped fiber are 9.2%.It is 21.10g to weigh chopped fiber quality, calculates its fiber according to regain and does
Weight is 19.16g.Add deionized water to make raw ramie cellulose mass concentration 6%, soak 48h so as to fully soak.By chloric acid
Sodium 0.4g, resorcinol 0.1g, 4- methyhnorpholine-N-oxide 0.1g, polyvinyl alcohol 0.1g, aminotriacetic acid 0.1g, plus
199.2g water is made into degumming liquid；Ramie raw ramie chopped fiber and degumming reactant liquor are 1: 10 mixing in mass ratio, with 1000mL palm fibre
Color conical flask is used as reactor.The pH value of scouring solution is adjusted to 8.0 with the NaOH solution of 0.1mol/L, use under the conditions of lucifuge
Magnetic stirring apparatus continuously stirs the mixture of ramie raw materials and scouring solution with the speed of 200rpm.Water-bath is warmed up to 100
DEG C, it is incubated 40min at this temperature, fully removes the colloid in ramie raw ramie using the oxidisability of oxidant, while C6 position
Primary hydroxy group become carboxyl, generate 6- carboxylic-oxidized cellulose.By the reacted fiber aqueous acetone solution of 0.1mol/L
2h is soaked, unreacted oxidant is removed, then abundant cleaning and dipping 24h of deionized water.Using rotating speed it is finally
The centrifuge of 11000rpm is washed 3 times, and supernatant liquor is transferred in another container, remaining concentration of fibre element suspension
It is put in vacuum freeze drier；Process is carried out at -60 DEG C of temperature and 50Pa pressure and 4h is dry, finally give the oxidation of powder state
Cellulose adsorbent, is finally putting into refrigerating chamber storage.
From 4 Adult New Zealand rabbit (male and female half and half, 2.5～3kg of body weight) as animal used as test, to experimental rabbit ear edge
Intravenous injection Nembutal sodium solution makes its general anesthesia, cuts its muscle of back layer, exposed area about 2cm × 2cm.To be obtained
Oxycellulose (area 1cm × 1cm) be laid in the surface of a wound, investigate its haemostatic effect.Sew up a wound, the 6th after the test
Wound was opened with the 9th day, observed absorbing state.
The residual gum content for boiling measure oxycellulose using the NaOH solution of 20g/L is 2.3%, using X-ray diffractometer
The degree of crystallinity 60.12% of oxycellulose is determined, using the degree of polymerization (DP) of cupri ethylene diamine viscosity method test oxycellulose is
300, it is 18.0% using the carboxyl-content of acid base neutralization titration method test oxycellulose.Rabbit muscle of back Implantation Test table
Bright, oxycellulose effectively stops blooding by being attached in animal wound surface 100 seconds.The oxycellulose Partial digestion at the 6th day,
Almost degradable when the 9th day.
As can be seen here, the side of hemostasis oxycellulose is prepared in a kind of ramie oxidation scouring processes that the present invention is provided
Method, obtained hemostasis are little with oxycellulose residual gum content, and degree of crystallinity and the degree of polymerization are moderate, and carboxyl-content is high, while anthemorrhagic speed
Hurry up, anthemorrhagic performance is stable, good absorbing effect.
Embodiment 2
A kind of method for preparing hemostasis oxycellulose in ramie oxidation scouring processes is as follows：
Ramie raw ramie pulverizer is ground into the chopped fiber that fineness is 20 mesh, is put in the container with sealing ring and balances
Moisture, the regain for determining chopped fiber are 9.2%.It is 21.20g to weigh chopped fiber quality, calculates its fiber according to regain and does
Weight is 19.25g.Add deionized water to make raw ramie cellulose mass concentration 1%, soak 24h so as to fully soak.By tetramethyl
Phenylpiperidines oxide-sodium hypochlorite-sodium bromide tri compound oxidation system 1g, Sodium Benzoate 0.5g, urea 0.4g, dodecyl
Sodium sulfonate 0.3g, Sodium Polyacrylate 0.3g, plus 197.5g water is made into degumming liquid；Ramie raw ramie chopped fiber and degumming reactant liquor are pressed
Mass ratio is 1: 10 mixing, using 1000mL brown conical flask as reactor.Scouring solution is adjusted with the HCl solution of 0.1mol/L
PH value to 3.0, ramie raw materials and scouring solution are continuously stirred with the speed of 200rpm with magnetic stirring apparatus under the conditions of lucifuge
Mixture.Water-bath is warmed up to 85 DEG C, is incubated 100min at this temperature, fully removes ramie using the oxidisability of oxidant
Colloid in numb raw ramie, while the primary hydroxy group of C6 position is become carboxyl, generates 6- carboxylic-oxidized cellulose.By reacted fibre
The glycerin solution of Wesy 0.1mol/L soaks 0.5h, removes unreacted oxidant, and then deionized water is fully cleaned
Soak 24h.Finally the centrifuge using rotating speed for 6000rpm is washed 4 times, and supernatant liquor is transferred in another container,
Remaining concentration of fibre element suspension is put in vacuum freeze drier；Carry out at -40 DEG C of temperature and 20Pa pressure processing and do
Dry 4h, finally gives the oxycellulose adsorbent of powder state, is finally putting into refrigerating chamber storage.
From 4 Adult New Zealand rabbit (male and female half and half, 2.5～3kg of body weight) as animal used as test, to experimental rabbit ear edge
Intravenous injection Nembutal sodium solution makes its general anesthesia, cuts its muscle of back layer, exposed area about 2cm × 2cm.To be obtained
Oxycellulose (area 1cm × 1cm) be laid in the surface of a wound, investigate its haemostatic effect.Sew up a wound, the 6th after the test
Wound was opened with the 9th day, observed absorbing state.
The residual gum content for boiling measure oxycellulose using the NaOH solution of 20g/L is 2.1%, using X-ray diffractometer
The degree of crystallinity 61.09% of oxycellulose is determined, using the degree of polymerization (DP) of cupri ethylene diamine viscosity method test oxycellulose is
500, it is 22.0% using the carboxyl-content of acid base neutralization titration method test oxycellulose.Rabbit muscle of back Implantation Test table
Bright, oxycellulose effectively stops blooding by being attached in animal wound surface 100 seconds.The oxycellulose Partial digestion at the 6th day,
Almost degradable when the 9th day.
As can be seen here, the side of hemostasis oxycellulose is prepared in a kind of ramie oxidation scouring processes that the present invention is provided
Method, obtained hemostasis are little with oxycellulose residual gum content, and degree of crystallinity and the degree of polymerization are moderate, and carboxyl-content is high, while anthemorrhagic speed
Hurry up, anthemorrhagic performance is stable, good absorbing effect.
Embodiment 3
A kind of method for preparing hemostasis oxycellulose in ramie oxidation scouring processes is as follows：
Ramie raw ramie pulverizer is ground into the chopped fiber that fineness is 60 mesh, is put in the container with sealing ring and balances
Moisture, the regain for determining chopped fiber are 8.9%.It is 22.02g to weigh chopped fiber quality, calculates its fiber according to regain and does
Weight is 20.06g.Add deionized water to make raw ramie cellulose mass concentration 3%, soak 36h so as to fully soak.By nitric acid-
Phosphoric acid-natrium nitrosum oxidation system 2.0g, waterglass 1.0g, thiocarbamide 0.8g, neopelex 0.6g, diethylenetriamine
Five methylenephosphonic acid 0.6g, plus 195.0g water is made into degumming liquid；Ramie raw ramie chopped fiber and degumming reactant liquor are 1 in mass ratio:
10 mixing, using 1000mL brown conical flask as reactor.With the NaOH solution of 0.1mol/L adjust the pH value of scouring solution to
14.0, continuously stir the mixing of ramie raw materials and scouring solution under the conditions of lucifuge with magnetic stirring apparatus with the speed of 200rpm
Thing.Water-bath is warmed up to 50 DEG C, is incubated 150min at this temperature, fully removes ramie raw ramie using the oxidisability of oxidant
In colloid, while the primary hydroxy group of C6 position is become carboxyl, generate 6- carboxylic-oxidized cellulose.Reacted fiber is used
The glycol water of 0.1mol/L soaks 1h, removes unreacted oxidant, then the abundant cleaning and dipping of deionized water
24h.Finally the centrifuge using rotating speed for 10000rpm is washed 6 times, and supernatant liquor is transferred in another container, remaining
Concentration of fibre element suspension be put in vacuum freeze drier；Process is carried out at -60 DEG C of temperature and 10Pa pressure and 6h is dry,
The oxycellulose adsorbent of powder state is finally given, is finally putting into refrigerating chamber storage.
From 4 Adult New Zealand rabbit (male and female half and half, 2.5～3kg of body weight) as animal used as test, to experimental rabbit ear edge
Intravenous injection Nembutal sodium solution makes its general anesthesia, cuts its muscle of back layer, exposed area about 2cm × 2cm.To be obtained
Oxycellulose (area 1cm × 1cm) be laid in the surface of a wound, investigate its haemostatic effect.Sew up a wound, the 6th after the test
Wound was opened with the 9th day, observed absorbing state.
The residual gum content for boiling measure oxycellulose using the NaOH solution of 20g/L is 2.0%, using X-ray diffractometer
The degree of crystallinity 59.82% of oxycellulose is determined, using the degree of polymerization (DP) of cupri ethylene diamine viscosity method test oxycellulose is
418, it is 20.14% using the carboxyl-content of acid base neutralization titration method test oxycellulose.Rabbit muscle of back Implantation Test
Show, oxycellulose effectively stops blooding by being attached in animal wound surface 100 seconds.The oxycellulose part drop at the 6th day
Solution, almost degradable when the 9th day.
As can be seen here, the side of hemostasis oxycellulose is prepared in a kind of ramie oxidation scouring processes that the present invention is provided
Method, obtained hemostasis are little with oxycellulose residual gum content, and degree of crystallinity and the degree of polymerization are moderate, and carboxyl-content is high, while anthemorrhagic speed
Hurry up, anthemorrhagic performance is stable, good absorbing effect.
Embodiment 4
A kind of method for preparing hemostasis oxycellulose in ramie oxidation scouring processes is as follows：
Ramie raw ramie pulverizer is ground into the chopped fiber that fineness is 100 mesh, is put in the container with sealing ring and puts down
Hengshui is divided, and the regain for determining chopped fiber is 9.0%.It is 21.35g to weigh chopped fiber quality, calculates its fiber according to regain
Dry weight is 19.43g.Add deionized water to make raw ramie cellulose mass concentration 10%, soak 12h so as to fully soak.By height
Sodium iodate 1.5g, anthraquinone 0.6g, urea 0.3g, peregal 0.2g, Sodium Polyacrylate 0.2g, plus 197.2g water is made into degumming liquid；
Ramie raw ramie chopped fiber and degumming reactant liquor are 1: 10 mixing in mass ratio, using 1000mL brown conical flask as reactor.
The pH value of scouring solution is adjusted to 5.0 with the HCl solution of 0.1mol/L, with magnetic stirring apparatus with 200rpm's under the conditions of lucifuge
Speed continuously stirs the mixture of ramie raw materials and scouring solution.Water-bath is warmed up to 90 DEG C, is incubated at this temperature
120min, fully removes the colloid in ramie raw ramie using the oxidisability of oxidant, while the primary hydroxy group of C6 position is become carboxylic
Base, generates 6- carboxylic-oxidized cellulose.Reacted fiber is soaked 1.5h with the aqueous acetone solution of 0.1mol/L, is removed not anti-
The oxidant that answers, then abundant cleaning and dipping 24h of deionized water.Finally the centrifuge using rotating speed for 12000rpm is washed
Wash 5 times, supernatant liquor is transferred in another container, remaining concentration of fibre element suspension is put in vacuum freeze drier；
Process is carried out at -50 DEG C of temperature and 60Pa pressure and 10h is dry, the oxycellulose adsorbent of powder state is finally given, is finally put
Enter refrigerating chamber storage.
From 4 Adult New Zealand rabbit (male and female half and half, 2.5～3kg of body weight) as animal used as test, to experimental rabbit ear edge
Intravenous injection Nembutal sodium solution makes its general anesthesia, cuts its muscle of back layer, exposed area about 2cm × 2cm.To be obtained
Oxycellulose (area 1cm × 1cm) be laid in the surface of a wound, investigate its haemostatic effect.Sew up a wound, the 6th after the test
Wound was opened with the 9th day, observed absorbing state.
The residual gum content for boiling measure oxycellulose using the NaOH solution of 20g/L is 2.1%, using X-ray diffractometer
The degree of crystallinity 62.10% of oxycellulose is determined, using the degree of polymerization (DP) of cupri ethylene diamine viscosity method test oxycellulose is
409, it is 19.0% using the carboxyl-content of acid base neutralization titration method test oxycellulose.Rabbit muscle of back Implantation Test table
Bright, oxycellulose effectively stops blooding by being attached in animal wound surface 100 seconds.The oxycellulose Partial digestion at the 6th day,
Almost degradable when the 9th day.
As can be seen here, the side of hemostasis oxycellulose is prepared in a kind of ramie oxidation scouring processes that the present invention is provided
Method, obtained hemostasis are little with oxycellulose residual gum content, and degree of crystallinity and the degree of polymerization are moderate, and carboxyl-content is high, while anthemorrhagic speed
Hurry up, anthemorrhagic performance is stable, good absorbing effect.
Claims (10)
1. a kind of method for preparing hemostasis oxycellulose in ramie oxidation scouring processes, it is characterised in that：The method by with
Lower 3 steps composition：
Step 1：Raw ramie fiber is pre-processed
Ramie raw ramie is ground into chopped fiber, chopped fiber is put into equilibrium water conten in closed container, determine the regain of chopped fiber；
Chopped fiber quality is weighed, its fiber dry weight is calculated according to regain；Deionized water is added in chopped fiber, makes raw ramie by soaking
Cellulose fully soaks swelling；
Step 2：The oxidation processes of cellulose
Concentration expressed in percentage by weight is 2%～10% oxidant, 0.5%～5% cellulose protective agent, 0.5%～4% filament expansion
Agent, 0.5%～3% surfactant, 0.5%～3% chelating agent and distilled water are made into degumming reactant liquor；By short for ramie raw ramie fibre
Peacekeeping degumming reactant liquor mixes in the reactor, and the initial pH value for adjusting degumming liquid is 3.0～14.0, and reactor is put into constant temperature
In water-bath, mixture under the conditions of lucifuge in stirred reactor, water-bath is warmed up to 50～100 DEG C, insulation 40～
150min, fully removes the colloid in raw ramie using the oxidisability of oxidant, while the cellulose oxidation with hydroxyl is become to contain
There is the oxycellulose of a large amount of carboxyls；
Step 3：The washing of oxycellulose and stabilization processes
By reacted fiber organic solvent washing by soaking, unreacted oxidant is removed, then deionized water is fully clear
Wash immersion；Obtained mixture carries out centrifugation layering, and supernatant liquor is transferred in another container, remaining concentration of fibre element
Suspension is put in vacuum freeze drier, is molded using liquid-nitrogen freeze drying, the oxycellulose adsorbent of powder state is obtained, most
After be put into refrigerating chamber storage.
2. a kind of method for preparing hemostasis oxycellulose as claimed in claim 1 in ramie oxidation scouring processes, which is special
Levy and be：In the step 1, the chopped fiber fineness being ground into is 20～100 mesh, adds distilled water to make cellulose in chopped fiber
Solid mass percent concentration in distilled water is 1%～10%, and the distilled water immersion time is 12～48h.
3. a kind of method for preparing hemostasis oxycellulose as claimed in claim 1 in ramie oxidation scouring processes, which is special
Levy and be：In the step 2, ramie raw ramie chopped fiber and degumming reactant liquor are mixed in the reactor for 1: 10 in mass ratio；
It is the NaOH solution of 0.1mol/L or the HCl solution of 0.1mol/L to adjust the solution used by degumming liquid initial pH value；Stirring reaction
Mixture in device is continuously stirred with the speed of 200rpm with magnetic stirring apparatus.
4. a kind of method for preparing hemostasis oxycellulose as claimed in claim 1 in ramie oxidation scouring processes, which is special
Levy and be：In the step 2, oxidant is sodium bromate, sodium chlorate, sodium chlorite, tetramethyl piperidine oxides-sodium hypochlorite-
Sodium bromide tri compound oxidation system, nitric acid-phosphoric acid-natrium nitrosum oxidation system, SODIUM PERCARBONATE, sodium metaperiodate, potassium metaperiodate,
Sodium hypochlorite, potassium percarbonate, sodium chlorate, one or more in sodium bromate.
5. a kind of method for preparing hemostasis oxycellulose as claimed in claim 1 in ramie oxidation scouring processes, which is special
Levy and be：In the step 2, cellulose protective agent is polyaerylic acid sodium, anthraquinone, magnesium hydroxide, polyvinyl alcohol, and waterglass gathers
Acrylamide, magnesium silicate, antifebrin, resorcinol, sodium citrate, one or more in Sodium Benzoate.
6. a kind of method for preparing hemostasis oxycellulose as claimed in claim 1 in ramie oxidation scouring processes, which is special
Levy and be：In the step 2, filament expansion agent includes urea, ethylenediamine, liquefied ammonia, thiocarbamide, 4- methyhnorpholine-N-oxide, copper
Ethylenediamine, one or two in dimethyl sulfoxide (DMSO).
7. its feature of method of hemostasis oxycellulose is prepared in a kind of ramie oxidation scouring processes as claimed in claim 1
It is：In the step 2, surfactant is polyvinyl alcohol, neopelex, dodecyl sodium sulfate, dodecane
Base sodium sulphate, AEO (JFC), one or two in peregal.
8. its feature of method of hemostasis oxycellulose is prepared in a kind of ramie oxidation scouring processes as claimed in claim 1
It is：In the step 2, metal ion chelation agent includes aminotriacetic acid, sodium ethylenediamine tetramethylenephosphonate, diethylenetriamine
Five methylenephosphonic acids, the adjacent sodium of ethylenediamine two, 1-hydroxy ethylidene-1,1-diphosphonic acid and its sodium salt, Sodium Polyacrylate, ethylenediamine tetramethyl
One or more in fork Alendronate.
9. its feature of method of hemostasis oxycellulose is prepared in a kind of ramie oxidation scouring processes as claimed in claim 1
It is：In the step 3, the organic solvent after soaking reaction used by fiber is glycerine, ethylene glycol, acetone, 1,3-PD
In one or two, concentration be 0.1mol/L, the washing by soaking time be 0.5～2h.
10. its spy of method of hemostasis oxycellulose is prepared in a kind of ramie oxidation scouring processes as claimed in claim 1
Levy and be：In the step 3, the time of the abundant cleaning and dipping of deionized water is 24h；Obtained mixture passes through centrifuge
Centrifugation layering is carried out, centrifuge speed is 6000～12000rpm, centrifugation number of times is 3～6 times；The temperature of freeze-drying shaping
For -40～-60 DEG C, the 10～60Pa of pressure of freeze-drying shaping, the time that freeze-drying is molded are 4～10h.
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Cited By (11)
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| CN106894097A (en) * | 2017-03-13 | 2017-06-27 | 东华大学 | A kind of method for preparing ramee using the oxide radical oxidation system of 2,2,6,6 tetramethyl piperidine 1 |
| CN107189116A (en) * | 2017-07-07 | 2017-09-22 | 广西师范学院 | The preparation method of high-fire resistance tapioca sisal fiber composite |
| CN107216490A (en) * | 2017-07-07 | 2017-09-29 | 广西师范学院 | The preparation method of hydrophobicity tapioca sisal fiber composite |
| CN107236152A (en) * | 2017-07-07 | 2017-10-10 | 广西师范学院 | High intensity sisal fiber strengthens the preparation method of tapioca composite |
| CN107353444A (en) * | 2017-07-07 | 2017-11-17 | 广西师范学院 | The preparation method of degradable tapioca sisal fiber composite |
| CN108485660A (en) * | 2018-03-12 | 2018-09-04 | 大连工业大学 | A kind of preparation method and application of cellulose base N doping fluorescent carbon quantum dot |
| CN112807477A (en) * | 2020-12-30 | 2021-05-18 | 广州迈普再生医学科技股份有限公司 | Composite hemostatic material and preparation method thereof |
| CN114000205A (en) * | 2021-12-06 | 2022-02-01 | 东华大学 | High-quality low-pollution selective oxidation ramie degumming method |
| CN114086262A (en) * | 2021-12-06 | 2022-02-25 | 东华大学 | Oxidation degumming method for ramie by using N-hydroxyphthalimide |
| CN115874440A (en) * | 2022-12-30 | 2023-03-31 | 贵州金玖生物技术有限公司 | Preparation method of water-soluble gauze, product and application thereof |
| CN116375893A (en) * | 2023-03-03 | 2023-07-04 | 贵州金玖生物技术有限公司 | Preparation method of absorbable hemostatic oxidized regenerated cellulose, product and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105061606A (en) * | 2015-09-01 | 2015-11-18 | 东华大学 | Method for preparing adsorbable oxycellulose through ramie oxidation degumming process |
-
2016
- 2016-10-20 CN CN201610912568.XA patent/CN106478825B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105061606A (en) * | 2015-09-01 | 2015-11-18 | 东华大学 | Method for preparing adsorbable oxycellulose through ramie oxidation degumming process |
Non-Patent Citations (1)
| Title |
|---|
| 游振辉: "《外科用药手册》", 30 August 2003, 福建科学技术出版社 * |
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| CN106894097B (en) * | 2017-03-13 | 2019-09-27 | 东华大学 | A method of ramee is prepared using 2,2,6,6- tetramethyl piperidine -1- oxide radical oxidation system |
| CN107236152A (en) * | 2017-07-07 | 2017-10-10 | 广西师范学院 | High intensity sisal fiber strengthens the preparation method of tapioca composite |
| CN107216490A (en) * | 2017-07-07 | 2017-09-29 | 广西师范学院 | The preparation method of hydrophobicity tapioca sisal fiber composite |
| CN107353444A (en) * | 2017-07-07 | 2017-11-17 | 广西师范学院 | The preparation method of degradable tapioca sisal fiber composite |
| CN107189116A (en) * | 2017-07-07 | 2017-09-22 | 广西师范学院 | The preparation method of high-fire resistance tapioca sisal fiber composite |
| CN108485660A (en) * | 2018-03-12 | 2018-09-04 | 大连工业大学 | A kind of preparation method and application of cellulose base N doping fluorescent carbon quantum dot |
| CN112807477A (en) * | 2020-12-30 | 2021-05-18 | 广州迈普再生医学科技股份有限公司 | Composite hemostatic material and preparation method thereof |
| CN114000205A (en) * | 2021-12-06 | 2022-02-01 | 东华大学 | High-quality low-pollution selective oxidation ramie degumming method |
| CN114086262A (en) * | 2021-12-06 | 2022-02-25 | 东华大学 | Oxidation degumming method for ramie by using N-hydroxyphthalimide |
| CN115874440A (en) * | 2022-12-30 | 2023-03-31 | 贵州金玖生物技术有限公司 | Preparation method of water-soluble gauze, product and application thereof |
| CN115874440B (en) * | 2022-12-30 | 2023-10-03 | 贵州金玖生物技术有限公司 | Preparation method of water-soluble gauze, product and application thereof |
| CN116375893A (en) * | 2023-03-03 | 2023-07-04 | 贵州金玖生物技术有限公司 | Preparation method of absorbable hemostatic oxidized regenerated cellulose, product and application thereof |
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