CN102205142B - Water-soluble hemostatic material and preparation method thereof - Google Patents
Water-soluble hemostatic material and preparation method thereof Download PDFInfo
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- CN102205142B CN102205142B CN201110129217.9A CN201110129217A CN102205142B CN 102205142 B CN102205142 B CN 102205142B CN 201110129217 A CN201110129217 A CN 201110129217A CN 102205142 B CN102205142 B CN 102205142B
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Abstract
The invention provides a water-soluble hemostatic material and a preparation method thereof and relates to a hemostatic material and a preparation method thereof, wherein the water-soluble hemostatic material and the preparation method thereof can be used for overcoming the problems that the existing oxidized regenerated cellulose materials are not water-soluble, have poor biological absorbability and slow hemostatic speed. The water-soluble hemostatic material is prepared from oxidized regenerated cellulose carboxylic sodium fabrics and hydrochloric acid. The preparation method comprises the following steps: winding the oxidized regenerated cellulose carboxylic sodium fabrics on a glass porous core of an acidification rotary reactor; adding the hydrochloric acid for close acidification; decompressing, filtering and washing with absolute ethanol; and freezing and drying to obtain the water-soluble hemostatic material. The water-soluble hemostatic material can be used as a hemostatic material.
Description
Technical field
The present invention relates to a kind of hemostatic material and preparation method thereof.
Background technology
Oxidized regenerated cellulose (ORC) is known and extensive use by people at medical field as hemostatic material.Oxidized regenerated cellulose is to take regenerated cellulose fabric as raw material, adopt applicable oxidation system (as nitrogen dioxide class or TEMPO system) to carry out selective oxidation to it, make the oxidized regenerated cellulose fabrics of carboxyl-content between 3.56～5.33mmol/g, and then make clinical medical oxidized regenerated cellulose hemostasia products through processes such as washing, dry, encapsulation and sterilizations.
Oxidized regenerated cellulose can activate the platelet at wound place and accelerate hemostasis.And along with some composition in blood is adsorbed onto oxidized regenerated cellulose surface, oxidized regenerated cellulose can slowly expand, and then the vascular compression broken ends of fractured bone and stopping blooding, but it is little to be only applicable to wound, the situation that amount of bleeding is low, and also anthemorrhagic speed is slow.
Because oxidized regenerated cellulose is non-water-soluble hemostatic material, its pH value is about 3.5, can only be dissolved in the alkaline solution of pH value in 10～14 scopes.So oxidized regenerated cellulose Bioabsorbable is in vivo poor, and the acidity of oxidized regenerated cellulose is stronger, causes it to some nervous system, may cause damage, and then has limited the application of oxidized regenerated cellulose at sensitive parts such as brains.The acidity of simultaneous oxidation regenerated cellulose hemostatic material also can cause number acid sensitive medicaments and lose efficacy, as thrombin etc.
In oxidized regenerated cellulose acid carboxyl structure can with Fe in hemoglobin
3+in conjunction with playing certain anastalsis, but in clinical use procedure because the carboxyl in oxidized regenerated cellulose can neutralize by the very fast buffer substance by blood, so this haemostatic effect is of short duration and not remarkable.
Oxidized regenerated cellulose as the study on the modification of hemostatic material always in constantly making great efforts to carry out.The people such as Doub disclose the method that adopts the aqueous solution of sodium bicarbonate or calcium acetate to neutralize oxidized regenerated cellulose, and the oxidized regenerated cellulose with the neutralization of thrombin dipping sodium bicarbonate, then the fabric after dipping is freezed to process and be dried under this state, made a kind of efficient oxidized cellulose class surgical operation hemostatic material.In United States Patent (USP), the people such as Saferstein has narrated the alcohol-water solution that uses salt of weak acid, as sodium acetate, oxidized regenerated cellulose is neutralized to pH value between 5～8, this method not only makes oxidized regenerated cellulose store by ambient-temp-stable, and the sour sensitive materials of similar thrombin on can load, and then improve the anthemorrhagic performance of oxidized regenerated cellulose material.They also find simultaneously, the people such as Doub adopt the method for sodium bicarbonate neutralization can cause the gel of oxidized regenerated cellulose fabrics part, distortion, and cause the hot strength of oxidation regeneration fabric of final neutralization too low and cannot be applied in actual hemostasis.And although the oxidized regenerated cellulose of the calcium acetate that the people such as Doub mention in patent neutralization has guaranteed original form of fabric, but because material calcium content after neutralization is too high, in use can produce zest to the mammal skin of contact position and other somatic cells, and in use location, form the large granulation lump turning white, hinder the bio-absorbable of material.Said method utilizes modification can improve the anthemorrhagic performance of oxidized regenerated cellulose, but its Bioabsorbable significantly reduces.In another part of United States Patent (USP), the people such as Stilwell adopts the method for neutralization to prepare a kind of regenerated oxycellulose as styptic material of calcium modification of good results, when they find that calcium content in oxidized cellulose is between 0.4～5.0, the anthemorrhagic performance of the oxidized cellulose of calcium modification is better than the oxidized regenerated cellulose of unmodified oxidized regenerated cellulose and sodium or potassium modification, and is not too large on the Bioabsorbable impact of material.When adopting calcium and sodium or potassium mixed and modified, the modified oxidized regenerated cellulose of gained has higher pH value and meets the condition with acid-sensitive sense substances compatible, the while calcium containing wherein both can be realized enhancing haemostatic effect, was unlikely to again to cause biological tissue stimulation reaction.
Because oxidized regenerated cellulose can be dissolved in pH value completely, it is 10～14 alkaline solution, and cause intensity greatly to reduce even can not keeping oxidized regenerated cellulose fabrics shape, so, in patent in the past and research, all adopt in salt of weak acid system and modified oxidized cellulose.Although, above-mentioned research is to weakening the acidity of regenerated oxycellulose as styptic material with modification in regenerated oxycellulose as styptic material, but adopt the product after salt of weak acid neutralizes oxidized regenerated cellulose all to belong to non-water-soluble, it is very little again that the degree of polymerization reduces amplitude, even do not degrade, therefore still exist Bioabsorbable poor, cannot improve the defect of its anthemorrhagic speed.
Summary of the invention
The present invention is non-water-soluble in order to solve existing oxidized regenerated cellulose material, Bioabsorbable is poor, the problem that anthemorrhagic speed is slow, and employing is different from the water-soluble regenerated oxycellulose as styptic material of having prepared a kind of new functional group concentration's distribution gradient in existing oxidized regenerated cellulose with the angle of modification.
Water-soluble hemostatic material is made by oxidized regenerated cellulose carboxylic acid sodium fabric and hydrochloric acid, and in water-soluble hemostatic material, carboxyl-functional mass contg is 0.10～5.21mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, the acescency of carboxylic acid sodium is 3%～98%; Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.30～4.77mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, in carboxylic acid sodium and hydrochloric acid, hydrionic mol ratio is (100: 1)～(1: 20).
Above-mentioned water-soluble hemostatic material is prepared according to the following steps:
Oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center of acidify rotary reactor, add again the airtight acidify 0.5～72h of hydrochloric acid, souring temperature is 10～30 ℃, then with dehydrated alcohol decompress filter, rinse 3～5 times, be placed in again-10～-80 ℃ of environment lyophilization 24～120h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.30～4.77mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, in carboxylic acid sodium and hydrochloric acid, hydrionic mol ratio is (100: 1)～(1: 20); The rotating speed of acidify rotary reactor is 100～400r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
The present invention carries out controlled acidify with hydrochloric acid to oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium structure division in oxidized regenerated cellulose carboxylic acid sodium fabric is converted into carboxylic acid structure, owing to there is no (in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxyl-functional mass contg is 0) of carboxyl in the oxidized regenerated cellulose carboxylic acid sodium fabric construction adopting, therefore in acidization, the carboxylic acid functional concentration of acidify presents Gradient distribution, and still can keep original shape; Due to the hydrochloric acid that adds acidify rotary reactor in the situation that acidify rotary reactor does not start not with oxidized regenerated cellulose carboxylic acid sodium clothing in contact, so oxidized regenerated cellulose carboxylic acid sodium fabric does not dissolve, its intensity meets clinical hemostasis requirement.
In water-soluble hemostatic material of the present invention except the carboxylic acid functional being formed by acidify, also have the carboxylic acid sodium functional group of part to exist, so the acidity of water-soluble hemostatic material is weaker than oxidized regenerated cellulose material, can reduce, even eliminate the probability that causes nerve system of human body damage, and then expanded the range of application of hemostatic material, and the faintly acid of water-soluble hemostatic material make water-soluble hemostatic material of the present invention can with the responsive hemostatic material of number acid or medicine compound use, be expected to further produce hemostasia products more fast.
Carboxylic acid functional concentration in water-soluble hemostatic material of the present invention presents Gradient distribution, and the content of carboxylic acid sodium functional group from outward appearance to inner essence raises gradually, and the content of carboxylic acid functional from outward appearance to inner essence reduces gradually.The hemostatic mechanism that functional group concentration's Gradient distribution that water-soluble hemostatic material of the present invention has can be sent out different at hemostasis different times, the hemorrhage process of the wound of more fitting; Water-soluble hemostatic material of the present invention contacts the initial stage with blood, and its blood flow volume adsorbing is less, mainly relies on Fe in the carboxylic acid functional of surface distributed and hemoglobin
3+in conjunction with playing anastalsis, increase along with water-soluble hemostatic material absorption blood flow volume, blood penetration is inner to water-soluble hemostatic material, carboxylic acid sodium functional group in water-soluble hemostatic material possesses water solublity, under the effect of carboxylic acid sodium functional group, water-soluble hemostatic material forms rapidly gel, fills up wound surface space, compressing and artery-clogging end and stops blooding.Water-soluble hemostatic material of the present invention is met the formation gel of can degrading rapidly at short notice after water or saline solution, therefore, the biology hemostasis of water-soluble hemostatic material of the present invention and the double-hemostasis function mechanism of physics hemostasis all play a role at short notice, and greatly shorten bleeding stopping period, improve haemostatic effect.And water-soluble hemostatic material of the present invention can also activate the platelet at wound place and accelerate hemostasis.
Because the carboxylic acid sodium functional group in water-soluble hemostatic material of the present invention possesses water solublity, so water-soluble hemostatic material of the present invention has the water solublity more more excellent than oxidized regenerated cellulose, degradability, can by metabolism faster, be absorbed in vivo.
In the preparation process of water-soluble hemostatic material of the present invention, do not occur to decompose or degraded, and preparation method is simple, reaction condition is easy to operate and control.In the preparation process of water-soluble hemostatic material of the present invention, dehydrated alcohol is only as rinsing use, and consumption is few, can save great amount of cost.
Accompanying drawing explanation
Fig. 1 is the structural representation of acidify rotary reactor, and direction of rotation is the direction of arrow in Fig. 1.Fig. 2 is the profile of acidify rotary reactor.Fig. 3 is the cross section of acidify rotary reactor.Fig. 4 is placed in the observation figure after the 60s of wound surface top by regenerated oxycellulose as styptic material.Fig. 5 is placed in the observation figure after the 60s of wound surface top by the water-soluble hemostatic material of the specific embodiment 28 preparations.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises the combination in any between each specific embodiment.
The specific embodiment one: present embodiment water-soluble hemostatic material is made by oxidized regenerated cellulose carboxylic acid sodium fabric and hydrochloric acid, in water-soluble hemostatic material, carboxyl-functional mass contg is 0.10～5.2lmmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, the acescency of carboxylic acid sodium is 3%～98%; Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.30～4.77mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, in carboxylic acid sodium and hydrochloric acid, hydrionic mol ratio is (100: 1)～(1: 20).
In present embodiment, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxyl-functional mass contg is 0.
Oxidized regenerated cellulose carboxylic acid sodium fabric is that to utilize oxidation system be 2,2,6,6-tetramethyl piperidine oxide free radical TEMPO-NaBr-NaClO reacts oxidation and makes with regenerated cellulose fabric, wherein TEMPO (2,2,6,6-tetramethyl piperidine oxide) quality is 0.1%～8.0% of regenerated cellulose fabric quality, the quality of NaBr is 5.0%～80.0% of regenerated cellulose fabric quality, the available chlorine content of NaClO solution is 5%～16%, NaClO liquor capacity is 30～80ml, and NaClO solution adopts and adds mode in batches, is 5～10ml at every turn; Oxidizing reaction temperature is 0～15 ℃, and the pH value of oxidation system is between 9.0～11.0, and mixing speed is 200～400 turn/min.Oxidized regenerated cellulose carboxylic acid sodium fabric preparation method instantiation: the cotton-shaped viscose fiber fabric of 2g, TEMPO 100mg, NaBr 0.96g, NaClO solution 60ml, at 8 ℃, react, with 0.4mol/L NaOH solution, keep the pH of reactant liquor in 10.0 left and right, divide and add NaClO solution 4 times, while consuming 31ml NaOH, cessation reaction, pours into reactant liquor in excessive ethanol (300ml), and precipitate is oxidized regenerated cellulose carboxylic acid sodium fabric.
The specific embodiment two: the difference of present embodiment and the specific embodiment one is: the concentration of hydrochloric acid is 0.01～2.00mol/L.Other is identical with embodiment one.
The specific embodiment three: the difference of present embodiment and the specific embodiment one is: the concentration of hydrochloric acid is 0.10～1.50mol/L.Other is identical with embodiment one.
The specific embodiment four: the difference of one of present embodiment and specific embodiment one to three is: in water-soluble hemostatic material, carboxyl-functional mass contg is 0.17～2.25mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, the acescency of carboxylic acid sodium is 5%～45%.Other is identical with one of embodiment one to three.
The specific embodiment five: the difference of one of present embodiment and specific embodiment one to five is: in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.40～4.14mmol/g.Other is identical with one of embodiment one to four.
The specific embodiment six: the difference of one of present embodiment and specific embodiment one to five is: in oxidized regenerated cellulose carboxylic acid sodium fabric, in carboxylic acid sodium and hydrochloric acid, hydrionic mol ratio is (4: 1)～(1: 10).Other is identical with one of embodiment one to four.
The specific embodiment seven: present embodiment water-soluble hemostatic material is prepared according to the following steps:
Oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center of acidify rotary reactor, add again the airtight acidify 0.5～72h of hydrochloric acid, souring temperature is 10～30 ℃, then with dehydrated alcohol decompress filter, rinse 3～5 times, be placed in again-10～-80 ℃ of environment lyophilization 24～120h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.30～4.77mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, in carboxylic acid sodium and hydrochloric acid, hydrionic mol ratio is (100: 1)～(1: 20); The rotating speed of acidify rotary reactor is 100～400r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
Oxidized regenerated cellulose carboxylic acid sodium fabric is that to utilize oxidation system be 2,2,6,6-tetramethyl piperidine oxide free radical TEMPO-NaBr-NaClO reacts oxidation and makes with regenerated cellulose fabric, wherein TEMPO (2,2,6,6-tetramethyl piperidine oxide) quality is 0.1%～8.0% of regenerated cellulose fabric quality, the quality of NaBr is 5.0%～80.0% of regenerated cellulose fabric quality, the available chlorine content of NaClO solution is 5%～16%, NaClO liquor capacity is 30～80ml, and NaClO solution adopts and adds mode in batches, is 5～10ml at every turn; Oxidizing reaction temperature is 0～15 ℃, and the pH value of oxidation system is between 9.0～11.0, and mixing speed is 200～400 turn/min.Oxidized regenerated cellulose carboxylic acid sodium fabric preparation method instantiation: the cotton-shaped viscose fiber fabric of 2g, TEMPO 100mg, NaBr 0.96g, NaClO solution 60ml, at 8 ℃, react, with 0.4mol/L NaOH solution, keep the pH of reactant liquor in 10.0 left and right, divide and add NaClO solution 4 times, while consuming 31ml NaOH, cessation reaction, pours into reactant liquor in excessive ethanol (300ml), and precipitate is oxidized regenerated cellulose carboxylic acid sodium fabric.
In present embodiment water-soluble hemostatic material, carboxyl-functional mass contg is 0.10～5.21mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, the acescency of carboxylic acid sodium is 3%～98%.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In present embodiment acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The specific embodiment eight: the difference of present embodiment and the specific embodiment seven is: the concentration of hydrochloric acid is 0.01～2.00mol/L.Other step and parameter are identical with embodiment seven.
The specific embodiment nine: the difference of present embodiment and the specific embodiment seven is: the concentration of hydrochloric acid is 0.10～1.50mol/L.Other step and parameter are identical with embodiment seven.
The specific embodiment ten: the difference of one of present embodiment and specific embodiment seven to nine is: in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.40～4.14mmol/g.Other step and parameter are identical with one of embodiment seven to nine.
The specific embodiment 11: the difference of one of present embodiment and specific embodiment seven to ten is: in oxidized regenerated cellulose carboxylic acid sodium fabric, in carboxylic acid sodium and hydrochloric acid, hydrionic mol ratio is (4: 1)～(1: 10).Other step and parameter are identical with one of embodiment seven to ten.
The specific embodiment 12: the difference of one of present embodiment and specific embodiment seven to 11 is: acidificatoin time is 8～48h, and souring temperature is 20～25 ℃.Other step and parameter are identical with one of embodiment seven to 11.
Present embodiment can regulate the acescency of water-soluble hemostatic material, gives the applicable intensity of present embodiment water-soluble hemostatic material and haemostatic effect.
The specific embodiment 13: the difference of one of present embodiment and specific embodiment seven to 12 is: lyophilization temperature is that-20～-65 ℃, sublimation drying are 48～72h.Other step and parameter are identical with one of embodiment seven to 12.
The specific embodiment 14: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 55.77ml, concentration are 0.01mol/L, airtight acidify 24h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 48h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.38mmol/g; The rotating speed of acidify rotary reactor is 100r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 0.11mmol/g, shows that acescency is 3.10%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 10s.
The specific embodiment 15: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 135.20ml, concentration are 0.01mol/L, airtight acidify 24h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 48h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.38mmol/g; The rotating speed of acidify rotary reactor is 150r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 0.27mmol/g, shows that acescency is 7.93%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 10s.
The specific embodiment 16: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 1690.00ml, concentration are 0.01mol/L, airtight acidify 24h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 48h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.38mmol/g; The rotating speed of acidify rotary reactor is 200r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 3.51mmol/g, shows that acescency is 96.37%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 120s.
The specific embodiment 17: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 11.83ml, concentration are 0.50mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.38mmol/g; The rotating speed of acidify rotary reactor is 250r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 1.19mmol/g, shows that acescency is 34.22%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 60s.
The specific embodiment 18: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 6.65ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 250r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 0.25mmol/g, shows that acescency is 6.64%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 10s.
The specific embodiment 19: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 14.25ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 300r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 0.56mmol/g, shows that acescency is 14.50%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 30s.
The specific embodiment 20: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 28.5ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 350r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 1.12mmol/g, shows that acescency is 28.87%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 60s.
The specific embodiment 21: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 38.00ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 400r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 1.47mmol/g, shows that acescency is 37.52%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 60s.
The specific embodiment 22: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 61.75ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 200r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 2.49mmol/g, shows that acescency is 62.17%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 60s.
The specific embodiment 23: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 78.89ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 300r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 3.39mmol/g, shows that acescency is 83.04%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 120s.
The specific embodiment 24: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 95.00ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 200r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 3.98mmol/g, shows that acescency is 96.33%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 120s.
The specific embodiment 25: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 95.00ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 300r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 3.98mmol/g, shows that acescency is 96.33%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 120s.
The specific embodiment 26: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 190.00ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 200r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 3.99mmol/g, shows that acescency is 96.58%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 120s.
The specific embodiment 27: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 190.00ml, concentration are 0.20mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 120r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 3.99mmol/g, shows that acescency is 96.58%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 120s.
The specific embodiment 28: present embodiment water-soluble hemostatic material is prepared according to the following steps:
5.00g oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center 1 of acidify rotary reactor, add again the hydrochloric acid that 95.00ml, concentration are 2.00mol/L, airtight acidify 48h, souring temperature is 25 ℃, then with dehydrated alcohol decompress filter, rinse 5 times, be placed in again-50 ℃ of environment lyophilization 72h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.80mmol/g; The rotating speed of acidify rotary reactor is 180r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
As shown in Figure 1, as shown in Figure 2, as shown in Figure 3, glass multi-hole center 1 is positioned at the axle core of acidify rotary reactor to the cross section of acidify rotary reactor to the profile of acidify rotary reactor to the structural representation of acidify rotary reactor, and direction of rotation as shown in Figure 1.
In acidization, hydrochloric acid brings to acidify rotary reactor inner tip by the projection stupefied 2 of acidify rotary reactor inside, then is fallen and the oxidized regenerated cellulose carboxylic acid sodium clothing in contact being wound on the glass multi-hole center 1 of acidify rotary reactor by gravity.
The carboxyl-functional mass contg of titration present embodiment water-soluble hemostatic material is 3.96mmol/g, shows that acescency is 95.76%.
Present embodiment water-soluble hemostatic material can form rapidly gel after meeting water or saline solution in 120s.
Anthemorrhagic performance contrast experiment:
Select 20 of body weight 3.0Kg New Zealand white rabbit, be divided at random 4 groups every group 5; Corresponding test material is respectively: the water-soluble hemostatic material (carboxyl-functional mass contg is 1.47mmol/g) of common antiseptic gauze (blank group), oxidized regenerated cellulose (positive controls), the specific embodiment 21 preparations and the water-soluble hemostatic material (carboxyl-functional mass contg is 0.11mmol/g) of the specific embodiment 14 preparations.New zealand white rabbit is fixed on dissecting table, after auricular vein sterilization, slowly injects 1ml 2.5% pentobarbital sodium solution, after rabbit anesthesia, successively open abdomen, with sterile gauze, blot tissue fluid and the blood on abdominal cavity, stomach wall, expose liver.On lobe of the liver, with scalpel, make the wound surface of 1.0cm * 1.0cm * 0.3cm.In wound surface forming process, oozing of blood first absorbs with the hospital gauze after sterilizing, then the above-mentioned hemostatic material of 1.5cm * 1.5cm is applied and is pressed on wound surface, applies while pressing and take sterilizing hospital gauze as auxiliary, observe haemostatic effect, and with manual time-keeping, observe haemostatic effect, after stopping blooding completely, record bleeding stopping period; Every kind of material repeats respectively 5 tests, records respectively complete bleeding stopping period, and result is as table 1.
Table 1
| Test material | Average bleeding stopping period (min) |
| Common antiseptic gauze | ＞15 |
| Oxidized regenerated cellulose | 3.6 |
| The water-soluble hemostatic material of the specific embodiment 21 preparations | 2.7 |
| The water-soluble hemostatic material of the specific embodiment 14 preparations | 2.2 |
Experimental result explanation water-soluble hemostatic material has anthemorrhagic speed faster.
Regenerated oxycellulose as styptic material is placed in to wound surface top, observes regenerated oxycellulose as styptic material and be still positioned at wound top after 60s, bleeding does not take a turn for the better (as shown in Figure 4).Water-soluble hemostatic material prepared by present embodiment is placed in wound surface top, after 60s, observing water-soluble hemostatic material prepared by present embodiment merges mutually with the liver of New Zealand white rabbit, become transparent gel-form (as shown in Figure 5), and by wound sealing, reach haemostatic effect.
Biodegradability contrast experiment:
Select 18 of body weight 3.0Kg New Zealand white rabbit, be divided at random 3 groups every group 6, corresponding test material is respectively: the water-soluble hemostatic material (carboxyl-functional mass contg is 1.47mmol/g) of oxidized regenerated cellulose (matched group), the specific embodiment 21 preparations and the water-soluble hemostatic material (carboxyl-functional mass contg is 0.11mmol/g) of the specific embodiment 14 preparations.New zealand white rabbit is fixed on dissecting table, and after auricular vein sterilization, slowly injection 1ml 2.5% pentobarbital sodium solution makes rabbit anesthesia.Respectively at spinal column both sides otch, heeling-in test material in muscle, scantling is 2.0cm * 0.5cm, then sews up.Within 1 day after surgery, 3 days, 7 days, 10 days, 14 days, 21 days, take out muscular tissue and the embedded material at heeling-in position respectively, and make pathology section examination, sum up the time that embedded material is absorbed by organism completely, experimental result is in Table 2.
Table 2
| Test material | Complete soak time (my god) |
| Oxidized regenerated cellulose | 14～21 |
| The water-soluble hemostatic material of the specific embodiment 21 preparations | 7～10 |
| The water-soluble hemostatic material of the specific embodiment 14 preparations | 5～7 |
Experimental result explanation water-soluble hemostatic material Bioabsorbable is good.
Claims (10)
1. water-soluble hemostatic material, it is characterized in that water-soluble hemostatic material made by oxidized regenerated cellulose carboxylic acid sodium fabric and hydrochloric acid, in water-soluble hemostatic material, carboxyl-functional mass contg is 0.10～5.21mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, the acescency of carboxylic acid sodium is 3%～98%; Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.30～4.77mmol/g, in oxidized regenerated cellulose carboxylic acid sodium fabric, in carboxylic acid sodium and hydrochloric acid, hydrionic mol ratio is (100: 1)～(1: 20), carboxylic acid functional concentration in wherein said water-soluble hemostatic material presents Gradient distribution, the content of carboxylic acid sodium functional group from outward appearance to inner essence raises gradually, and the content of carboxylic acid functional from outward appearance to inner essence reduces gradually.
2. water-soluble hemostatic material according to claim 1, is characterized in that in water-soluble hemostatic material, carboxyl-functional mass contg is 0.17～2.25mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, the acescency of carboxylic acid sodium is 5%～45%.
3. water-soluble hemostatic material according to claim 1, is characterized in that in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.40～4.14mmol/g.
4. water-soluble hemostatic material according to claim 1, is characterized in that in oxidized regenerated cellulose carboxylic acid sodium fabric in carboxylic acid sodium and hydrochloric acid that hydrionic mol ratio is for (4:1)～(1:10).
5. the preparation method of water-soluble hemostatic material as claimed in claim 1, is characterized in that water-soluble hemostatic material prepared according to the following steps:
Oxidized regenerated cellulose carboxylic acid sodium fabric is wound on the glass multi-hole center of acidify rotary reactor, add again the airtight acidify 0.5～72h of hydrochloric acid, souring temperature is 10～30 ℃, then with dehydrated alcohol decompress filter, rinse 3～5 times, be placed in again-10～-80 ℃ of environment lyophilization 24～120h, obtain water-soluble hemostatic material;
Wherein, in oxidized regenerated cellulose carboxylic acid sodium fabric, carboxylic acid sodium functional group content is 3.30～4.77mmol/g, and in oxidized regenerated cellulose carboxylic acid sodium fabric, in carboxylic acid sodium and hydrochloric acid, hydrionic mol ratio is (100: 1)～(1: 20); The rotating speed of acidify rotary reactor is 100～400r/min, and adds hydrochloric acid not direct and oxidized regenerated cellulose carboxylic acid sodium clothing in contact in the situation that acidify rotary reactor does not start of acidify rotary reactor.
6. the preparation method of water-soluble hemostatic material according to claim 5, the concentration that it is characterized in that hydrochloric acid is 0.01～2.00mol/L.
7. the preparation method of water-soluble hemostatic material according to claim 6, is characterized in that oxidized regenerated cellulose carboxylic
In acid sodium fabric, carboxylic acid sodium functional group content is 3.40～4.14mmol/g.
8. the preparation method of water-soluble hemostatic material according to claim 7, is characterized in that oxidized regenerated cellulose carboxylic
In acid sodium fabric, in carboxylic acid sodium and hydrochloric acid, hydrionic mol ratio is (4: 1)～(1: 10).
9. the preparation method of water-soluble hemostatic material according to claim 8, is characterized in that acidificatoin time is 8～48h, and souring temperature is 20～25 ℃.
10. the preparation method of water-soluble hemostatic material according to claim 8, is characterized in that lyophilization temperature is that-20～-65 ℃, sublimation drying are 48～72h.
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