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CN109401338A - A kind of preparation method of gelatine-chitosan-carboxymethyl cellulose biomaterial - Google Patents

A kind of preparation method of gelatine-chitosan-carboxymethyl cellulose biomaterial Download PDF

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Publication number
CN109401338A
CN109401338A CN201811176606.5A CN201811176606A CN109401338A CN 109401338 A CN109401338 A CN 109401338A CN 201811176606 A CN201811176606 A CN 201811176606A CN 109401338 A CN109401338 A CN 109401338A
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China
Prior art keywords
chitosan
carboxymethyl cellulose
gelatine
solution
mass fraction
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CN201811176606.5A
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Chinese (zh)
Inventor
蒋旭
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Jiangsu Ginkgo Lake Biotechnology Co Ltd
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Jiangsu Ginkgo Lake Biotechnology Co Ltd
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Priority to CN201811176606.5A priority Critical patent/CN109401338A/en
Publication of CN109401338A publication Critical patent/CN109401338A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2201/00Foams characterised by the foaming process
    • C08J2201/04Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
    • C08J2201/052Inducing phase separation by thermal treatment, e.g. cooling a solution
    • C08J2201/0524Inducing phase separation by thermal treatment, e.g. cooling a solution the liquid phase being aqueous
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2389/00Characterised by the use of proteins; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/08Cellulose derivatives
    • C08J2401/26Cellulose ethers
    • C08J2401/28Alkyl ethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/08Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Medicinal Preparation (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention discloses a kind of gelatine-chitosan-carboxymethyl cellulose biomaterial preparation methods, it include: that chitosan is dissolved in the acetum that mass fraction is 2~4% by (1), stir 30~40min, the carboxymethyl cellulose aqueous solution that mass fraction is 1~3% is slowly added dropwise again, the pH value for adjusting solution is 5~6, it is stirred to react 5~10h under the revolving speed of 800~1200r/min, obtains chitosan-carboxymethyl cellulose mixing suspension;(2) in deionized water by a certain amount of Gelatin, 1~3h of ultrasonic disperse, at room temperature place 12~be swollen it sufficiently for 24 hours, obtain mass fraction be 1~10% gelatin solution;(3) chitosan-carboxymethyl cellulose mixing suspension is uniformly mixed with institute gelatine solution, gained mixed liquor is dry under vacuum condition, remove solvent, it pours into bracket mould again, freeze forming, the low temperature drying 12~demould for 24 hours under the conditions of 0~5 DEG C washs, obtains gelatine-chitosan-carboxymethyl cellulose biomaterial.Material porosity height in the present invention, mechanical property are good.

Description

A kind of preparation method of gelatine-chitosan-carboxymethyl cellulose biomaterial
Technical field
The present invention relates to field of material technology, more particularly to a kind of gelatine-chitosan-carboxymethyl cellulose biomaterial Preparation method.
Background technique
Material for tissue engineering bracket mainly has natural macromolecular material and synthesis high molecular material, the former generally has There is preferable cellular affinity, but cause properties of product to be difficult to reappear due to the source of material difference, processing method difference etc., The controllable range of its conventional physico-chemical properties is very limited, and opereating specification is relatively narrow in process also limits it in special-shaped material Application;Synthesis high molecular material has good processing performance and can be by the composition and synthesis process of adjusting product Technological parameter, and its physicochemical property is enable to regulate and control.But due to such material surface lacks cell recognition site etc., influence The adherency and growth of cell on the surface thereof.Therefore, biomedical material is modified affine to improve the cell of material Property, machinability and mechanical property research just become life science and the common research hotspot of material science.And function admirable The successful exploitation of tissue engineering rack material wound and plastic surgery will be made to enter a brand-new field.
Chitosan is unique a kind of positively charged alkaline polysaccharide present in nature, nontoxic, non-stimulated, is had good Biocompatibility, biodegradability.Cartilage cell's apposition growth on chitin fiber rack is rapid, and keeps it good Gene phenotype.Carboxymethyl cellulose is the water-soluble cellulose ether analog derivative of native cellulose after being chemically modified, belongs to poly- Anion superpolymer.Because carboxymethyl cellulose has unique adhesiveness, thickening property, film forming, suspension and water retentivity, Thus it is widely used in field of biomedicine.In order to make full use of the bioactivity of chitosan and the adhesiveness of carboxymethyl cellulose And the compound of chitosan and carboxymethyl cellulose has been made using different methods by machinability, people.But the prior art In chitosan-carboxymethyl cellulose bracket obtained mechanical property it is not ideal enough.
For this reason, it is necessary in view of the above-mentioned problems, propose a kind of system of gelatine-chitosan-carboxymethyl cellulose biomaterial Preparation Method is able to solve problems of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of gelatine-chitosan-carboxymethyl cellulose biomaterial preparation method, with Overcome deficiency in the prior art.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of gelatine-chitosan-carboxymethyl cellulose biomaterial, comprising:
(1) chitosan is dissolved in the acetum that mass fraction is 2~4%, stirs 30~40min, then be slowly added dropwise The carboxymethyl cellulose aqueous solution that mass fraction is 1~3%, the pH value for adjusting solution is 5~6,800~1200r/min's It is stirred to react 5~10h under revolving speed, obtains chitosan-carboxymethyl cellulose mixing suspension;
(2) in deionized water by a certain amount of Gelatin, 1~3h of ultrasonic disperse, at room temperature place 12~make for 24 hours It is sufficiently swollen, and obtains the gelatin solution that mass fraction is 1~10%;
(3) chitosan-carboxymethyl cellulose mixing suspension is uniformly mixed with institute gelatine solution, gained mixing Liquid is dry under vacuum condition, removes solvent, then pour into bracket mould, freeze forming, the low temperature drying under the conditions of 0~5 DEG C 12~demould for 24 hours, it washs, obtains gelatine-chitosan-carboxymethyl cellulose biomaterial.
Preferably, in step (1), 50~150g is contained in chitosan described in every 1L-carboxymethyl cellulose mixing suspension Chitosan.
Preferably, in step (1), the rate of addition of the carboxymethyl cellulose aqueous solution is 15~25 drops/min.
Preferably, in step (2), the mass fraction of institute's gelatine solution is 5%.
Preferably, in step (2), ultrasonic power is 500~1000W.
Preferably, in step (3), the body of the chitosan-carboxymethyl cellulose mixing suspension and institute's gelatine solution Product is than being 1:2~4.
Preferably, in step (3), dry temperature is 110~150 DEG C under the vacuum condition.
Compared with the prior art, the advantages of the present invention are as follows: the gelatine-chitosan-that the method in the present invention is prepared The porosity of carboxymethyl cellulose biomaterial is higher, mechanical property is good, has good biocompatibility.
Specific embodiment
The present invention is described further by the following example: according to following embodiments, the present invention may be better understood. However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described in embodiment are only used In illustrating the present invention, without the present invention described in detail in claims should will not be limited.
The present invention discloses a kind of preparation method of gelatine-chitosan-carboxymethyl cellulose biomaterial, comprising:
(1) chitosan is dissolved in the acetum that mass fraction is 2~4%, stirs 30~40min, then be slowly added dropwise The carboxymethyl cellulose aqueous solution that mass fraction is 1~3%, the pH value for adjusting solution is 5~6,800~1200r/min's It is stirred to react 5~10h under revolving speed, obtains chitosan-carboxymethyl cellulose mixing suspension;
(2) in deionized water by a certain amount of Gelatin, 1~3h of ultrasonic disperse, at room temperature place 12~make for 24 hours It is sufficiently swollen, and obtains the gelatin solution that mass fraction is 1~10%;
(3) chitosan-carboxymethyl cellulose mixing suspension is uniformly mixed with institute gelatine solution, gained mixing Liquid is dry under vacuum condition, removes solvent, then pour into bracket mould, freeze forming, the low temperature drying under the conditions of 0~5 DEG C 12~demould for 24 hours, it washs, obtains gelatine-chitosan-carboxymethyl cellulose biomaterial.
Wherein, in step (1), 50~150g shell is contained in chitosan described in every 1L-carboxymethyl cellulose mixing suspension Glycan, it is preferred that contain 100g chitosan in chitosan described in every 1L-carboxymethyl cellulose mixing suspension;The carboxymethyl The rate of addition of cellulose aqueous solution is 15~25 drops/min, it is preferred that the rate of addition of the carboxymethyl cellulose aqueous solution For 20 drops/min.
Wherein, in step (2), the mass fraction of institute's gelatine solution is 5%;Ultrasonic power is 500~1000W, preferably , ultrasonic power 800W.
Wherein, in step (3), the volume of the chitosan-carboxymethyl cellulose mixing suspension and institute's gelatine solution Than for 1:2~4, it is preferred that the chitosan-carboxymethyl cellulose mixing suspension and the volume ratio of institute's gelatine solution are 1: 3;Dry temperature is 110~150 DEG C under the vacuum condition, it is preferred that dry temperature is 120 under the vacuum condition ℃。
Gelatine-chitosan in the present invention-carboxymethyl cellulose biomaterial is illustrated with specific embodiment below Preparation method.
Embodiment 1
(1) chitosan is dissolved in the acetum that mass fraction is 2%, stirs 30min, with 15 drops/min dropwise addition speed The carboxymethyl cellulose aqueous solution that mass fraction is 1% is slowly added dropwise in degree, and the pH value for adjusting solution is 5, in turning for 800r/min It is stirred to react 5h under speed, obtains chitosan-carboxymethyl cellulose mixing suspension, wherein chitosan described in every 1L-carboxymethyl is fine It ties up in plain mixing suspension and contains 50g chitosan;
(2) in deionized water by a certain amount of Gelatin, ultrasonic disperse 1h, placing 12h at room temperature makes it sufficiently Swelling obtains the gelatin solution that mass fraction is 1%;
(3) chitosan-carboxymethyl cellulose mixing suspension is mixed with institute's gelatine solution according to volume ratio for 1:2 It closing uniformly, gained mixed liquor is dry under 110 DEG C of vacuum condition, solvent is removed, then pour into bracket mould, freeze forming, Low temperature drying 12h is demoulded under the conditions of 0 DEG C, and washing obtains gelatine-chitosan-carboxymethyl cellulose biomaterial.
Embodiment 2
(1) chitosan is dissolved in the acetum that mass fraction is 3%, stirs 35min, with 20 drops/min dropwise addition speed The carboxymethyl cellulose aqueous solution that mass fraction is 2% is slowly added dropwise in degree, and the pH value for adjusting solution is 5.5,1000r/min's It is stirred to react 8h under revolving speed, obtains chitosan-carboxymethyl cellulose mixing suspension, wherein chitosan-carboxymethyl described in every 1L Contain 100g chitosan in cellulose mixing suspension;
(2) in deionized water by a certain amount of Gelatin, ultrasonic disperse 2h, placing 18h at room temperature makes it sufficiently Swelling obtains the gelatin solution that mass fraction is 5%;
(3) chitosan-carboxymethyl cellulose mixing suspension is mixed with institute's gelatine solution according to volume ratio for 1:3 It closing uniformly, gained mixed liquor is dry under 120 DEG C of vacuum condition, solvent is removed, then pour into bracket mould, freeze forming, Low temperature drying 18h is demoulded under the conditions of 2 DEG C, and washing obtains gelatine-chitosan-carboxymethyl cellulose biomaterial.
Embodiment 3
(1) chitosan is dissolved in the acetum that mass fraction is 4%, stirs 40min, with 25 drops/min dropwise addition speed The carboxymethyl cellulose aqueous solution that mass fraction is 3% is slowly added dropwise in degree, and the pH value for adjusting solution is 6, in turning for 1200r/min It is stirred to react 10h under speed, obtains chitosan-carboxymethyl cellulose mixing suspension, wherein chitosan-carboxymethyl described in every 1L Contain 150g chitosan in cellulose mixing suspension;
(2) in deionized water by a certain amount of Gelatin, ultrasonic disperse 3h, placing at room temperature for 24 hours makes it sufficiently Swelling obtains the gelatin solution that mass fraction is 10%;
(3) chitosan-carboxymethyl cellulose mixing suspension is mixed with institute's gelatine solution according to volume ratio for 1:4 It closing uniformly, gained mixed liquor is dry under 150 DEG C of vacuum condition, solvent is removed, then pour into bracket mould, freeze forming, Low temperature drying demoulds for 24 hours under the conditions of 5 DEG C, and washing obtains gelatine-chitosan-carboxymethyl cellulose biomaterial.
In the gelatine-chitosan that method in the present invention is prepared-carboxymethyl cellulose biomaterial, chitosan and carboxylic Methylcellulose is capable of forming fenestral fabric, so that the composite material has biggish porosity;Meanwhile by the way that gelatin is added So that respectively at the Adhesion enhancement between branch, so as to enhance the mechanical property of the biomaterial.It is omnipotent using PT-1036PC Material experiment-machine tests the compression strength of biomaterial in the present invention, the results showed that, the compression strength of the biomaterial It can reach 58.6MPa.Biomaterial in the present invention can be used for preparing biological support, with good application prospect.
Finally, it is to be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive Property include so that include a series of elements process, method, article or equipment not only include those elements, but also Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic Element.

Claims (7)

1. a kind of gelatine-chitosan-carboxymethyl cellulose biomaterial preparation method characterized by comprising
(1) chitosan is dissolved in the acetum that mass fraction is 2~4%, stirs 30~40min, then quality is slowly added dropwise The carboxymethyl cellulose aqueous solution that score is 1~3%, the pH value for adjusting solution is 5~6, in the revolving speed of 800~1200r/min Under be stirred to react 5~10h, obtain chitosan-carboxymethyl cellulose mixing suspension;
(2) in deionized water by a certain amount of Gelatin, 1~3h of ultrasonic disperse, at room temperature place 12~fill it for 24 hours Divide swelling, obtains the gelatin solution that mass fraction is 1~10%;
(3) chitosan-carboxymethyl cellulose mixing suspension is uniformly mixed with institute gelatine solution, gained mixed liquor in It is dry under vacuum condition, remove solvent, then pour into bracket mould, freeze forming, under the conditions of 0~5 DEG C low temperature drying 12~ It demoulds for 24 hours, washs, obtain gelatine-chitosan-carboxymethyl cellulose biomaterial.
2. gelatine-chitosan according to claim 1-carboxymethyl cellulose biomaterial preparation method, feature exist In, in step (1), in chitosan described in every 1L-carboxymethyl cellulose mixing suspension contain 50~150g chitosan.
3. gelatine-chitosan according to claim 1-carboxymethyl cellulose biomaterial preparation method, feature exist In in step (1), the rate of addition of the carboxymethyl cellulose aqueous solution is 15~25 drops/min.
4. gelatine-chitosan according to claim 1-carboxymethyl cellulose biomaterial preparation method, feature exist In in step (2), the mass fraction of institute's gelatine solution is 5%.
5. gelatine-chitosan according to claim 1-carboxymethyl cellulose biomaterial preparation method, feature exist In in step (2), ultrasonic power is 500~1000W.
6. gelatine-chitosan according to claim 1-carboxymethyl cellulose biomaterial preparation method, feature exist In in step (3), the volume ratio of the chitosan-carboxymethyl cellulose mixing suspension and institute's gelatine solution is 1:2~4.
7. gelatine-chitosan according to claim 1-carboxymethyl cellulose biomaterial preparation method, feature exist In in step (3), dry temperature is 110~150 DEG C under the vacuum condition.
CN201811176606.5A 2018-10-10 2018-10-10 A kind of preparation method of gelatine-chitosan-carboxymethyl cellulose biomaterial Pending CN109401338A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116003842A (en) * 2022-12-21 2023-04-25 广东石油化工学院 A kind of preparation method of carboxymethyl cellulose/chitosan shape memory film

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CN101181642A (en) * 2007-11-09 2008-05-21 华南理工大学 A kind of preparation method of asymmetric composite sponge
CN104524620A (en) * 2014-11-25 2015-04-22 苏州市贝克生物科技有限公司 Modified composite sponge dressing and preparation method thereof
CN105860099A (en) * 2016-04-25 2016-08-17 宁波工程学院 Preparation method of gelatin-based hydrogel in microwave-ultrasonic coupling field

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116003842A (en) * 2022-12-21 2023-04-25 广东石油化工学院 A kind of preparation method of carboxymethyl cellulose/chitosan shape memory film

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Application publication date: 20190301