CN108619555A - A kind of preparation method of organic/inorganic compound hemostatic material - Google Patents
A kind of preparation method of organic/inorganic compound hemostatic material Download PDFInfo
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- CN108619555A CN108619555A CN201810626490.4A CN201810626490A CN108619555A CN 108619555 A CN108619555 A CN 108619555A CN 201810626490 A CN201810626490 A CN 201810626490A CN 108619555 A CN108619555 A CN 108619555A
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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
- A61L24/0047—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L24/0073—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material with a macromolecular matrix
- A61L24/0089—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material with a macromolecular matrix containing inorganic fillers not covered by groups A61L24/0078 or A61L24/0084
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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
- A61L24/0042—Materials resorbable by the body
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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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/04—Materials for stopping bleeding
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Abstract
The present invention relates to a kind of preparation methods of organic/inorganic compound hemostatic material, belong to medical material preparing technical field.The present invention using natural organic high-molecular material chitosan be raw material as kernel,Ethyl orthosilicate is as silicon source,Oxidation modification is carried out to cornstarch again,The chitosan that obtained dialdehyde starch and surface are deposited to Si-Al zeolite molecular sieve carries out schiff base reaction,Organic/inorganic compound hemostatic material is made in final note film,Present invention adds EDTA and citric acid with metal ion-chelant,So that molecular sieve surface part metals ion is chelated, agent removes,The high-specific surface area of zeolite molecular sieve and institute is positively charged can adsorb a large amount of plasma proteins induction fibrin polymerizations,Play hemoglutination,By material,Fibrin,The blood clotting fritter that haemocyte collectively constitutes,Reach hemostasis purpose,The generation of cross-linked structure and the introducing of inorganic molecule sieve,So that hemostatic material mechanical property is greatly improved,It has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of organic/inorganic compound hemostatic material, belong to medical material technology of preparing neck
Domain.
Background technology
Bleeding be in ophthalmic surgical and wound it is most common, one of be most difficult to the problem of control, the bleeding of especially central internal organs,
Such as the rupture haemorrhage of liver, spleen and kidney, the life of people is directly threatened, effective hemostasis is in surgical operation, trauma hemostasis
It is badly in need of the main problem solved.
Clinically common hemostatic material has hemostatic gauze, stanch fibre, tourniquet bandage, but they are in use
In the presence of：Bleeding stopping period is longer, easily with wound adhesion and be not easy dressing, the infection to wound and helpless etc., the Er Qie that suppurates
The hemostasis problem of sudden massive haemorrhage is also always clinical problem after operation neutralization operation.
Usually require have following characteristic as excellent hemostatic material in medical use：
（1）With biocompatibility, and to organism nontoxicity；
（2）The infection that wound cannot be increased, the reaction of inflammation can't be induced by being unable to contaminated wound；
（3）Bleeding stopping period is short, haemostatic effect is good；
（4）Mechanical property reaches the excellent performance of hemostatic material in medical use；
（5）It is good with the adhesiveness of tissue, it is good with the identical property in site where wound, the surface of a wound；
（6）No antigen is answered, degradation absorption in vivo can select degradable absorbing material or non-according to different hemostasis purposes
Degradability material；
（7）A large amount of heat is not generated while hemostasis, with prevent tissue, nerve burn；
（8）Manufacturing cost is cheap etc. as possible.
Hemostatic material is broadly divided into biological at present and chemically two classes, biological hemostatic material include mainly：Fiber
Protein adhesive and collagen etc..Chemically hemostatic material mainly has：Chitosan, more micropore class inorganic material etc., such as zeolite, can
Dissolubility hemostatic gauze, tissue glue etc..But respectively there is disadvantage, though as Fibrin Glue and collagen have good adhesiveness, by
It is unable to hemostasis by compression in it, big surface of a wound hemostasis can not be applied individually to any, it is originated from the blood of animal and human body to this external cause, easily causes
Quick and viral infection；The tissue adsorptions power of gelatin and collagen is poor, the hemostatic function of the two all rely on enough blood platelets and
Coagulation factor, and degradation in vivo absorbability is poor, substantially increases the risk of wound site infection, therefore applies and limited
System；The general dissolubility of chitosan material is poor, and mechanical strength is low, and acid adding dissolving is generally required in process, and holds after acid adding
Easily generate that side reaction such as surrounding tissue is congested, the red and swollen, reactions such as shed tears to human body；Porous zeolite is put during being primarily present use
Thermal burn surface texture；Soluble stanching gauze be primarily present bleeding stopping period it is long, to swift and violent person's anthemorrhagic performance difference of bleeding etc., and
And patient is quite painful during dressing.
Hemostasis plays sizable effect for the success of operation and the safety of patient, therefore, develops a kind of with biology
Safety, biocompatibility, and there is the novel hemostatic material of stronger hemostatic function to seem extremely important.
Invention content
Present invention mainly solves the technical issues of, mainly have macromolecule organic and inorganic for current quick-acting haemostatic powder product
Class, but all there is certain defect, organic mechanical strength is low, and haemostatic effect is unstable, and inorganic easily remains to be caused in vascular
The defect of thrombus provides a kind of preparation method of organic/inorganic compound hemostatic material.
In order to solve the above-mentioned technical problem, the technical problem to be solved by the present invention is to：
A kind of preparation method of organic/inorganic compound hemostatic material, it is characterised in that specifically preparation process is：
（1）It is put into sonic oscillation instrument after chitosan and water that deacetylation is 96% are mixed, sonic oscillation mixing is hanged
Supernatant liquid is packed into beaker after mixing sodium metaaluminate, sodium hydroxide and suspension and obtains mixed liquor；
（2）The above-mentioned beaker equipped with mixed liquor is moved into water-bath, 70~80 DEG C is heated to, continues to be added dropwise into beaker
Ethyl orthosilicate, insulated and stirred react 2~3h, obtain prefabricated solution, obtained prefabricated solution are moved into high pressure water heating kettle, in normal pressure
Lower pre-reaction, obtains pre-product；
（3）Continue that ethylenediamine tetra-acetic acid and citric acid solution, enclosed high pressure water heating kettle, high temperature and pressure are added into high pressure water heating kettle
Reaction waits for being separated by filtration to obtain reaction filter residue after reaction, spare；
（4）Will the sodium periodate solution of cornstarch and a concentration of 0.3mol/L mix after be fitted into conical flask, then by conical flask
It is put into microwave oscillation instrument, microwave oscillation reacts under the conditions of being protected from light；
（5）After waiting for above-mentioned oscillating reactions, isolated filtrate is filtered, the ethylene glycol of filtrate and a concentration of 0.1mol/L is molten
After liquid mixing, 30~50min is stood, the isometric acetone of filtrate is added, isolated filter is filtered after continuing 1~3h of standing
Slag obtains dialdehyde starch；
（6）It is packed into reaction after the acetic acid solution that spare reaction filter residue and above-mentioned dialdehyde starch and mass fraction are 2% is mixed
In kettle, it is stirred to react 2~3h under the conditions of being protected from light, after reaction injects reaction product in mold, then mold is put into baking
Case demoulds after 3~5h of dry solidification to get organic/inorganic compound hemostatic material at 60~70 DEG C.
Step（1）Described in chitosan and water mass ratio be 1:10, sonic oscillation mixing frequency be 25~
The time of 30kHz, sonic oscillation mixing are 15~20min, and the mass ratio of sodium metaaluminate, sodium hydroxide and suspension is 1:3:
70。
Step（2）Described in the dripping quantity of ethyl orthosilicate be the 30% of mixed liquor quality, the temperature of pre-reaction is 120
~150 DEG C, the time of pre-reaction is 30~40min.
Step（3）Described in ethylenediamine tetra-acetic acid addition be pre-product quality 5%, the addition of citric acid solution
Amount is the 10% of pre-product quality, a concentration of 0.5mol/L of citric acid solution, the pressure of high-temperature high-voltage reaction is 1.8~
2.0MPa, the temperature of high-temperature high-voltage reaction are 250~280 DEG C, time of high-temperature high-voltage reaction is 20~for 24 hours.
Step（4）Described in cornstarch and a concentration of 0.3mol/L sodium periodate solution mass ratio be 1:30,
The power of microwave oscillation reaction is 200~300W, and the time of microwave oscillation reaction is 1~2h.
Step（5）Described in filtrate and a concentration of 0.1mol/L ethylene glycol solution volume ratio be 5:1.
Step（6）Described in spare reaction filter residue and above-mentioned dialdehyde starch and mass fraction be 2% acetic acid solution
Mass ratio be 8:5:50, the size of mold is 5cm × 5cm × 2mm.
Beneficial effects of the present invention：
（1）The present invention is raw material as kernel using natural organic high-molecular material chitosan, then uses ethyl orthosilicate as silicon
Source, and silicon source is added in alkali and the mixed liquor of silicon source sodium metaaluminate and chitosan kernel, it is heavy using hydro-thermal method synthetic surface
The chitosan of product Si-Al zeolite molecular sieve, then oxidation modification is carried out to cornstarch, obtained dialdehyde starch and surface are deposited
The chitosan of Si-Al zeolite molecular sieve carries out schiff base reaction, and organic/inorganic compound hemostatic material, the present invention is made in final film of noting
Using chitosan as kernel, using its polyhydroxy characteristic, using activity hydroxy as active deposit site so that hydro-thermal reaction generates
Zeolite molecular sieve be deposited on chitosan surface, obtain chitosan, molecular screen composite, and the present invention is also in hydrothermal deposition point
EDTA and citric acid with metal ion-chelant are added in the backward hydrothermal reaction kettle of sub- sieve, in the work of high temperature and pressure
It is removed with the lower agent so that molecular sieve surface part metals ion is chelated, to generate metal cavity in composite surface, these
Metal cavity has and loses the positive charge of metal ion equivalent, so that composite material surface is positively charged, in composite material
When being contacted with wound, the high-specific surface area of zeolite molecular sieve and institute is positively charged can adsorb a large amount of plasma proteins induction fiber eggs
White polymerization, at the same institute is positively charged can be in conjunction with haemocyte cell membrane, to play hemoglutination, and kernel chitosan therein
Can be with the adherency of induced platelet and red blood cell, aggregation, the blood collectively constituted by material, fibrin, haemocyte to composition
Solidifying fritter, reaches hemostasis purpose, chitosan and zeolite molecular sieve collective effect play splendid haemostatic effect；
（2）The present invention is aoxidized cornstarch by sodium metaperiodate, obtains the modified starch with dialdehyde functional group, and pass through it
Self-crosslinking modified starch and the amino on chitosan surface are subjected to schiff base reaction, form three-dimensional network cross-linked structure,
The generation of cross-linked structure and the introducing of inorganic molecule sieve so that hemostatic material mechanical property is greatly improved, while network
The generation of cross-linked structure makes the connection between molecular sieve and chitosan more secured, can be to avoid inorganic hemostatic component residue arteries and veins
It the problem of causing thrombus in pipe, has broad application prospects.
Specific implementation mode
It is 1 in mass ratio:10 will be put into after the chitosan that deacetylation is 96% and water mixing in sonic oscillation instrument, with 25
Frequency ultrasound oscillation 15~20min of mixing of~30kHz, obtains suspension, sodium metaaluminate, sodium hydroxide and suspension is pressed matter
Amount is than being 1:3:It is packed into beaker after 70 mixing and obtains mixed liquor；The above-mentioned beaker equipped with mixed liquor is moved into water-bath, heating
70~80 DEG C are warming up to, the ethyl orthosilicate that mixed liquor quality 30% is added dropwise into beaker is continued, insulated and stirred is reacted 2~3h, obtained
To prefabricated solution, obtained prefabricated solution is moved into high pressure water heating kettle, is heated to 120~150 DEG C under normal pressure, pre-reaction 30
~40min, obtains pre-product；Continue ethylenediamine tetra-acetic acid and pre-product matter that pre-product quality 5% is added into high pressure water heating kettle
A concentration of 0.5mol/L citric acid solutions of amount 10%, enclosed high pressure water heating kettle increase reacting kettle inner pressure to 1.8~2.0MPa
And 250~280 DEG C are heated to, high-temperature high-voltage reaction 20~for 24 hours, it waits for being separated by filtration to obtain reaction filter residue after reaction,
It is spare；It is 1 in mass ratio:30 will be packed into conical flask after the mixing of the sodium periodate solution of cornstarch and a concentration of 0.3mol/L
In, then conical flask is put into microwave oscillation instrument, with 1~2h of power microwave oscillating reactions of 200~300W under the conditions of being protected from light；
After waiting for above-mentioned oscillating reactions, isolated filtrate is filtered, the ethylene glycol solution of filtrate and a concentration of 0.1mol/L is pressed into body
Product is than being 5:After 1 mixing, 30~50min is stood, the isometric acetone of filtrate is added, separation is filtered after continuing 1~3h of standing
Filter residue is obtained, dialdehyde starch is obtained；It is 8 in mass ratio:5:50 by spare reaction filter residue and above-mentioned dialdehyde starch and quality
It is fitted into reaction kettle after the acetic acid solution mixing that score is 2%, 2~3h is stirred to react under the conditions of being protected from light, it after reaction will be anti-
It answers in the mold that product injection size is 5cm × 5cm × 2mm, then mold is put into baking oven, the dry solidification 3 at 60~70 DEG C
Demoulding is to get organic/inorganic compound hemostatic material after~5h.
It is 1 in mass ratio:10 will be put into after the chitosan that deacetylation is 96% and water mixing in sonic oscillation instrument, with
The frequency ultrasound oscillation mixing 15min of 25kHz, obtains suspension, is in mass ratio by sodium metaaluminate, sodium hydroxide and suspension
1:3:It is packed into beaker after 70 mixing and obtains mixed liquor；The above-mentioned beaker equipped with mixed liquor is moved into water-bath, is heated to
70 DEG C, continuing the ethyl orthosilicate that mixed liquor quality 30% is added dropwise into beaker, insulated and stirred reacts 2h, obtains prefabricated solution, will
To prefabricated solution move into high pressure water heating kettle in, be heated to 120 DEG C under normal pressure, pre-reaction 30min obtains pre-product；After
Continue a concentration of 0.5mol/L of ethylenediamine tetra-acetic acid and pre-product quality 10% that pre-product quality 5% is added into high pressure water heating kettle
Citric acid solution, enclosed high pressure water heating kettle increase reacting kettle inner pressure and to 1.8MPa and are heated to 250 DEG C, high temperature and pressure
20h is reacted, waits for being separated by filtration to obtain reaction filter residue after reaction, it is spare；It is 1 in mass ratio:30 by cornstarch and concentration
To be fitted into conical flask after the sodium periodate solution mixing of 0.3mol/L, then conical flask is put into microwave oscillation instrument, is being protected from light
Under the conditions of with the power microwave oscillating reactions 1h of 200W；After waiting for above-mentioned oscillating reactions, isolated filtrate is filtered, by filtrate
Ethylene glycol solution with a concentration of 0.1mol/L is 5 by volume:After 1 mixing, 30min is stood, it is isometric to add filtrate
Acetone continues to filter isolated filter residue after standing 1h, obtains dialdehyde starch；It is 8 in mass ratio:5:50 filter spare reaction
It is fitted into reaction kettle after the acetic acid solution mixing that slag and above-mentioned dialdehyde starch and mass fraction are 2%, is stirred under the conditions of being protected from light
2h is reacted, is injected reaction product in the mold that size is 5cm × 5cm × 2mm after reaction, then mold is put into baking oven,
It is demoulded to get organic/inorganic compound hemostatic material after dry solidification 3h at 60 DEG C.
It is 1 in mass ratio:10 will be put into after the chitosan that deacetylation is 96% and water mixing in sonic oscillation instrument, with
The frequency ultrasound oscillation mixing 17min of 27kHz, obtains suspension, is in mass ratio by sodium metaaluminate, sodium hydroxide and suspension
1:3:It is packed into beaker after 70 mixing and obtains mixed liquor；The above-mentioned beaker equipped with mixed liquor is moved into water-bath, is heated to
75 DEG C, continuing the ethyl orthosilicate that mixed liquor quality 30% is added dropwise into beaker, insulated and stirred reacts 2h, obtains prefabricated solution, will
To prefabricated solution move into high pressure water heating kettle in, be heated to 135 DEG C under normal pressure, pre-reaction 35min obtains pre-product；After
Continue a concentration of 0.5mol/L of ethylenediamine tetra-acetic acid and pre-product quality 10% that pre-product quality 5% is added into high pressure water heating kettle
Citric acid solution, enclosed high pressure water heating kettle increase reacting kettle inner pressure and to 1.9MPa and are heated to 265 DEG C, high temperature and pressure
22h is reacted, waits for being separated by filtration to obtain reaction filter residue after reaction, it is spare；It is 1 in mass ratio:30 by cornstarch and concentration
To be fitted into conical flask after the sodium periodate solution mixing of 0.3mol/L, then conical flask is put into microwave oscillation instrument, is being protected from light
Under the conditions of with the power microwave oscillating reactions 1h of 250W；After waiting for above-mentioned oscillating reactions, isolated filtrate is filtered, by filtrate
Ethylene glycol solution with a concentration of 0.1mol/L is 5 by volume:After 1 mixing, 40min is stood, it is isometric to add filtrate
Acetone continues to filter isolated filter residue after standing 2h, obtains dialdehyde starch；It is 8 in mass ratio:5:50 filter spare reaction
It is fitted into reaction kettle after the acetic acid solution mixing that slag and above-mentioned dialdehyde starch and mass fraction are 2%, is stirred under the conditions of being protected from light
2h is reacted, is injected reaction product in the mold that size is 5cm × 5cm × 2mm after reaction, then mold is put into baking oven,
It is demoulded to get organic/inorganic compound hemostatic material after dry solidification 3h at 65 DEG C.
It is 1 in mass ratio:10 will be put into after the chitosan that deacetylation is 96% and water mixing in sonic oscillation instrument, with
The frequency ultrasound oscillation mixing 20min of 30kHz, obtains suspension, is in mass ratio by sodium metaaluminate, sodium hydroxide and suspension
1:3:It is packed into beaker after 70 mixing and obtains mixed liquor；The above-mentioned beaker equipped with mixed liquor is moved into water-bath, is heated to
80 DEG C, continuing the ethyl orthosilicate that mixed liquor quality 30% is added dropwise into beaker, insulated and stirred reacts 3h, obtains prefabricated solution, will
To prefabricated solution move into high pressure water heating kettle in, be heated to 150 DEG C under normal pressure, pre-reaction 40min obtains pre-product；After
Continue a concentration of 0.5mol/L of ethylenediamine tetra-acetic acid and pre-product quality 10% that pre-product quality 5% is added into high pressure water heating kettle
Citric acid solution, enclosed high pressure water heating kettle increase reacting kettle inner pressure and to 2.0MPa and are heated to 280 DEG C, high temperature and pressure
Reaction for 24 hours, waits for being separated by filtration to obtain reaction filter residue after reaction, spare；It is 1 in mass ratio:30 by cornstarch and concentration
To be fitted into conical flask after the sodium periodate solution mixing of 0.3mol/L, then conical flask is put into microwave oscillation instrument, is being protected from light
Under the conditions of with the power microwave oscillating reactions 2h of 300W；After waiting for above-mentioned oscillating reactions, isolated filtrate is filtered, by filtrate
Ethylene glycol solution with a concentration of 0.1mol/L is 5 by volume:After 1 mixing, 50min is stood, it is isometric to add filtrate
Acetone continues to filter isolated filter residue after standing 3h, obtains dialdehyde starch；It is 8 in mass ratio:5:50 filter spare reaction
It is fitted into reaction kettle after the acetic acid solution mixing that slag and above-mentioned dialdehyde starch and mass fraction are 2%, is stirred under the conditions of being protected from light
3h is reacted, is injected reaction product in the mold that size is 5cm × 5cm × 2mm after reaction, then mold is put into baking oven,
It is demoulded to get organic/inorganic compound hemostatic material after dry solidification 5h at 70 DEG C.
The hemostatic material that comparative example is produced with company of Suzhou City is as a comparison case
Hemostatic material in organic/inorganic compound hemostatic material produced by the present invention and comparative example is detected, testing result
As shown in table 1：
Mechanics Performance Testing device therefor is electronic universal material testing machine（Test condition：Tensile speed is 500mm/min, is surveyed
Testing bar size is 115mm × 6mm × 2mm）.
Bacteriostasis property testing experiment is using staphylococcus aureus as test object, and test method is with reference to GB15979-
2002《Disposable Sanitary Accessory sanitary standard》4 stripping property of middle appendix C is anti-（Suppression）Bacterium product bacteriostasis property test method, and
It is evaluated according to evaluation criterion Yi Jun Shuai≤50%~90%.
Skin irritation is tested according to standard GB/T16886.10-2016, and above-mentioned leaching liquor 0.2mL is taken to be injected in skin,
2h after observation injection, for 24 hours, the oedema of 72h recipient sites and red and swollen situation.
Cytotoxicity test is tested sample by method of agar medium cover specified in GB/T16886.5.
1 performance measurement result of table
From the data in table 1, it can be seen that organic/inorganic compound hemostatic material produced by the present invention, is expanding relative to traditional hemostatic material
Property, haemostatic effect, degradability, safety, patients ' life quality, art chamber residual and there is advantage in price.This product does not have
It is toxic, without anaphylaxis and rejection, patient comfort no pain, degradation is complete, without taking out.It can be used for surgery and emergency treatment
Medical product may be designed as the every-day medical articles for use of ordinary consumer, have wide prospect of the application.
Claims (7)
1. a kind of preparation method of organic/inorganic compound hemostatic material, it is characterised in that specifically preparation process is：
（1）It is put into sonic oscillation instrument after chitosan and water that deacetylation is 96% are mixed, sonic oscillation mixing is hanged
Supernatant liquid is packed into beaker after mixing sodium metaaluminate, sodium hydroxide and suspension and obtains mixed liquor；
（2）The above-mentioned beaker equipped with mixed liquor is moved into water-bath, 70~80 DEG C is heated to, continues to be added dropwise into beaker
Ethyl orthosilicate, insulated and stirred react 2~3h, obtain prefabricated solution, obtained prefabricated solution are moved into high pressure water heating kettle, in normal pressure
Lower pre-reaction, obtains pre-product；
（3）Continue that ethylenediamine tetra-acetic acid and citric acid solution are added into high pressure water heating kettle, enclosed high pressure water heating kettle, high temperature is high
Pressure reaction waits for being separated by filtration to obtain reaction filter residue after reaction, spare；
（4）Will the sodium periodate solution of cornstarch and a concentration of 0.3mol/L mix after be fitted into conical flask, then by conical flask
It is put into microwave oscillation instrument, microwave oscillation reacts under the conditions of being protected from light；
（5）After waiting for above-mentioned oscillating reactions, isolated filtrate is filtered, the ethylene glycol of filtrate and a concentration of 0.1mol/L is molten
After liquid mixing, 30~50min is stood, the isometric acetone of filtrate is added, isolated filter is filtered after continuing 1~3h of standing
Slag obtains dialdehyde starch；
（6）It is packed into reaction after the acetic acid solution that spare reaction filter residue and above-mentioned dialdehyde starch and mass fraction are 2% is mixed
In kettle, it is stirred to react 2~3h under the conditions of being protected from light, after reaction injects reaction product in mold, then mold is put into baking
Case demoulds after 3~5h of dry solidification to get organic/inorganic compound hemostatic material at 60~70 DEG C.
2. a kind of preparation method of organic/inorganic compound hemostatic material according to claim 1, it is characterised in that：Step
（1）Described in chitosan and water mass ratio be 1:10, the frequency of sonic oscillation mixing is 25~30kHz, and sonic oscillation is mixed
The time of conjunction is 15~20min, and the mass ratio of sodium metaaluminate, sodium hydroxide and suspension is 1:3:70.
3. a kind of preparation method of organic/inorganic compound hemostatic material according to claim 1, it is characterised in that：Step
（2）Described in the dripping quantity of ethyl orthosilicate be the 30% of mixed liquor quality, the temperature of pre-reaction is 120~150 DEG C, pre- anti-
The time answered is 30~40min.
4. a kind of preparation method of organic/inorganic compound hemostatic material according to claim 1, it is characterised in that：Step
（3）Described in the addition of ethylenediamine tetra-acetic acid be the 5% of pre-product quality, the addition of citric acid solution is pre-product matter
The pressure of the 10% of amount, a concentration of 0.5mol/L of citric acid solution, high-temperature high-voltage reaction is 1.8~2.0MPa, high temperature high pressure reverse
The temperature answered is 250~280 DEG C, time of high-temperature high-voltage reaction is 20~for 24 hours.
5. a kind of preparation method of organic/inorganic compound hemostatic material according to claim 1, it is characterised in that：Step
（4）Described in cornstarch and a concentration of 0.3mol/L sodium periodate solution mass ratio be 1:30, microwave oscillation reaction
Power be 200~300W, microwave oscillation reaction time be 1~2h.
6. a kind of preparation method of organic/inorganic compound hemostatic material according to claim 1, it is characterised in that：Step
（5）Described in filtrate and a concentration of 0.1mol/L ethylene glycol solution volume ratio be 5:1.
7. a kind of preparation method of organic/inorganic compound hemostatic material according to claim 1, it is characterised in that：Step
（6）Described in spare reaction filter residue and above-mentioned dialdehyde starch and mass fraction be 2% the mass ratio of acetic acid solution be 8:
5:50, the size of mold is 5cm × 5cm × 2mm.
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Cited By (1)
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| CN110586047A (en) * | 2019-10-08 | 2019-12-20 | 辽宁工业大学 | Preparation method of modified dialdehyde starch for adsorbing lead ions |
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