CN108841011A - A kind of nano-cellulose self-healing material and preparation method thereof - Google Patents
A kind of nano-cellulose self-healing material and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
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- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/04—Alginic acid; Derivatives thereof
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
- C08J2401/04—Oxycellulose; Hydrocellulose
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- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/12—Agar-agar; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
Abstract
The invention belongs to natural macromolecular material fields, and in particular to a kind of nano-cellulose self-healing material and preparation method thereof.The preparation method includes the following steps：（1）The preparation of aldehyde radical nano-cellulose；（2）By step（1）The aldehyde radical nano-cellulose of preparation is dissolved in deionized water, and compound concentration is the solution of 1wt%-7wt%, and amino-containing natural polymer then is added into aldehyde radical nano-cellulose solution, is uniformly mixed at room temperature, forms self-healing material.Prepared nano-cellulose self-healing material has excellent self-healing capability, and self-healing is high-efficient, speed is fast, and intensity is high, and biodegradability is good, while the preparation process is easy to operate, and the reaction time is short, mild condition, is applicable to produce in batches.
Description
Technical field
The invention belongs to natural macromolecular material fields, and in particular to a kind of nano-cellulose self-healing material and its preparation
Method.
Background technique
Self-healing（Self-healing）Material is to refer to automatic identification, partly or entirely repair breakage, has perception
It is one of the emphasis of polymer science field development with the intellectual material of response function（Bekas et al., 2016）.Self-healing
The importance of condensation material is that the service life of material can be extended, and can play the role of repairing in the use process of material, especially
It is that have self-healing capability with greater need for material for adverse circumstances such as stimulation, burn into radiation.The development of self-healing material
Cheng Zhong, the dynamics covalent bonds such as disulfide bond, acylhydrazone key, boric acid ester bond, Diels-Alder reaction have played important function.But base
The outside stimulus such as light, heat, electricity, which are usually required, in the self-healing material that these dynamic covalent bonds are constructed just is able to achieve self-healing, and
The processes such as Diels-Alder reaction are complicated, it usually needs use toxic chemical reagent, these all seriously limit self-healing material
The application range of material.Imine linkage is a kind of dynamic covalent bond by the formation that interacts between aldehyde radical and amino, do not need by
The stimulations such as external power, heat, light, pH can realize the separation and healing of key automatically.Therefore, based on aldehyde in imine linkage forming process
Base and the mutual dynamic equilibrium of amino, can assign the self-healing capability of material brilliance.
Mainly from artificial synthesized macromolecule, preparation process is related to complicated chemical synthesis for the preparation of self-healing material at present
The use of step and a large amount of organic reagents, brings a negative impact to environment, while these synthesis usual biological degradabilities of macromolecule
And poor biocompatibility, self-healing material is limited in the application in the fields such as biological medicine, organizational project, cell culture.
Cellulose is natural polymer the most abundant on the earth, the nanometer with nanoscale extracted by cellulose
Cellulose not only remains the good biodegradability of native cellulose and biocompatibility, and has nanoparticle
The characteristics such as high intensity, high transparency, high elastic modulus, be remarkably improved the performances such as intensity, light, electricity, the magnetic of material
（Kaushik & Moores, 2016）, in pharmaceutical carrier, photoelectric device, food, cosmetics, composite material, intellectual material etc.
Field has huge potential using value.Vicinal hydroxyl groups in the nano-cellulose structure quilt under the oxidation of potassium metaperiodate
It is oxidized to aldehyde radical, using the stronger reactivity of aldehyde radical, can react to form dynamic imines with amino-containing natural polymer
Key can prepare nano-cellulose self-healing material by the invertibity of imine linkage.Therefore, using nano-cellulose as carrier, benefit
With its intensity is high, reactivity is strong and the property of polyhydroxy, Surface Oxidation Modification is carried out to it, nanofiber can not only be improved
Interface compatibility between element and macromolecule, and high molecular material intelligent response and self-healing capability can be assigned, it improves
The mechanical property of self-healing material.Based on nano-cellulose and the good biocompatibility of amino-containing natural polymer and biology
Degradability can assign the self-healing material of preparation with excellent biocompatibility and degradability, expand it in biology and carry medicine, group
Knit the application of the biomedicine fields such as reparation, wound healing.At present to constructed using natural polymer can with good biological
The research of self-healing material of degradability, biocompatibility is rarely reported.
Summary of the invention
Present invention aim to address existing self-healing material performance and the deficiencies of technology of preparing, provide a kind of nanofiber
Plain self-healing material and preparation method thereof.Prepared nano-cellulose self-healing material has excellent self-healing capability, from
Healing efficiency is high, speed is fast, and intensity is high, and biodegradability is good, while the preparation process is easy to operate, and the reaction time is short, item
Part is mild, is applicable to produce in batches.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of preparation method of nano-cellulose self-healing material, includes the following steps：
（1）The preparation of aldehyde radical nano-cellulose；
（2）By step（1）The aldehyde radical nano-cellulose of preparation is dissolved in deionized water, and compound concentration is the solution of 1wt%-7wt%,
Then amino-containing natural polymer is added into aldehyde radical nano-cellulose solution, is uniformly mixed at room temperature, form self-healing material
Material；Aldehyde radical is formed in conjunction with imine linkage with amino, the dynamic reversibility based on imine linkage, which is at room temperature
Rapid self-healing can occur, without applying other stimulations.
Step（1）Specially：Oxidant potassium metaperiodate is added to the nano-cellulose that solid content is 0.2wt%-1.5wt%
In water slurry, 60 DEG C are protected from light 4h, obtain the aldehyde radical nano-cellulose that aldehyde group content is 5-9.5mmol/g.
The nano-cellulose is acid system nano-cellulose, physical method nano-cellulose, enzyme process nano-cellulose, bacterium
One of cellulose.
The mass ratio of potassium metaperiodate and nano-cellulose is：0.5:1-2:1.
Step（2）Described in amino-containing natural polymer be gelatin, chitosan, carboxymethyl chitosan, N- succinyl
Chitosan, chitin, amino cellulose, aminated alginic acid sodium, amination starch, amination hyaluronic acid, amination fine jade
One of rouge.
Step（2）Described in aldehyde radical nano-cellulose and amino-containing natural polymer mass ratio be 1:0.1-1:
1.5。
Nano-cellulose self-healing material made from a kind of preparation method as claimed in any one of claims 1 to 6.
Remarkable advantage of the invention：
（1）Self-healing material prepared by the present invention forms imines through peroxidating and amino-containing natural polymer by nano-cellulose
Bond is closed, and rapid self-healing, nothing can occur at room temperature for the dynamic reversibility based on imine linkage, the natural macromolecular material
Other stimulations need to be applied；
（2）Self-healing material prepared by the present invention is made of natural polymer completely, without any artificial synthesized high molecular addition,
It is good biocompatibility, biodegradable, nontoxic and pollution-free, environmentally friendly；
（3）The method of the present invention is easy to operate, the reaction time is short, reaction condition is mild, high-efficient, can be used for mass production；
（4）Nano-cellulose self-healing material self-healing capability prepared by the present invention is strong, healing efficiency is high, speed is fast, intensity is high,
There is potential application prospect in fields such as organizational project, medicament slow release, medical dressing.
Detailed description of the invention
Fig. 1 is the self-healing process photo of self-healing material produced by the present invention；In figure, a is self-healing material, and b is certainly
Healing material is cut open, and c is the material after self-healing 20s；
Fig. 2 is the scanning electron microscope (SEM) photograph on self-healing material surface.
Specific embodiment
The present invention is further illustrated by the following examples, but protection scope of the present invention is not limited to following reality
Apply example.
Embodiment 1
The oxidant potassium metaperiodate for weighing 3g is added to the sulfuric acid process nano-cellulose aqueous suspension that 500mL solid content is 0.3wt%
In liquid, 60 DEG C are protected from light 4h, obtain the aldehyde radical nano-cellulose that aldehyde group content is 6mmol/g；The aldehyde radical Nanowire that will be obtained
Dimension element is dissolved in deionized water, is configured to the solution that concentration is 2wt%, is added gelatin into the solution, aldehyde radical nano-cellulose with
The mass ratio of gelatin is 1:1, it is uniformly mixed at room temperature, forms self-healing material.
Nano-cellulose self-healing material obtained in this example, which is destroyed in rear 30s, can be achieved self-healing, material after healing
The intensity of material can be restored to original 90%.
Embodiment 2
By the oxidant potassium metaperiodate of 4g, it is added to the phosphotungstic acid method nano-cellulose aqueous suspension that 600mL solid content is 0.7wt%
In liquid, 60 DEG C are protected from light 4h, obtain the aldehyde radical nano-cellulose that aldehyde group content is 5mmol/g.The aldehyde radical Nanowire that will be obtained
Dimension element is dissolved in deionized water, is configured to the solution that concentration is 3wt%, carboxymethyl chitosan is added into the solution, wherein aldehyde
The mass ratio of based nano-fiber element and carboxymethyl chitosan is 1:0.3, it is uniformly mixed at room temperature, forms self-healing material.
Nano-cellulose self-healing material obtained in this example, which is destroyed in rear 60s, can be achieved self-healing, material after healing
The intensity of material can be restored to original 80%.
Embodiment 3
The oxidant potassium metaperiodate for weighing 2g is added in the bacteria cellulose water slurry that 400mL solid content is 0.9wt%, 60
DEG C it is protected from light 4h, obtains the aldehyde radical nano-cellulose that aldehyde group content is 8.5mmol/g.Obtained aldehyde radical nano-cellulose is matched
The solution that concentration is 4wt% is made, the aminated alginic acid sodium to weigh, aldehyde radical nano-cellulose and aminated alginic acid is added
The mass ratio of sodium is 1:1.5, it is uniformly mixed at room temperature, forms self-healing material.
Nano-cellulose self-healing material obtained in this example, which is destroyed in rear 20s, can be achieved self-healing, material after healing
The intensity of material can be restored to original 95%.
Embodiment 4
The oxidant potassium metaperiodate of 3g is added in the enzyme process nano-cellulose water slurry that 450mL solid content is 1.4wt%,
60 DEG C are protected from light 4h, obtain the aldehyde radical nano-cellulose that aldehyde group content is 7mmol/g.Obtained aldehyde radical nano-cellulose is molten
In deionized water, it is configured to the solution that concentration is 6wt%, amination agar is added into aldehyde radical nano-cellulose solution,
The mass ratio of middle aldehyde radical nano-cellulose and amination agar is 1:0.8, it is uniformly mixed at room temperature, forms self-healing material.This
Nano-cellulose self-healing material obtained in example, which is destroyed in rear 80s, can be achieved self-healing, and the intensity of material can after healing
Restore to original 82%.
Embodiment 5
The oxidant potassium metaperiodate for weighing 1g is added to the high pressure homogenization method nano-cellulose water that 100mL solid content is 1.1wt%
In suspension, 60 DEG C are protected from light 4h, obtain the aldehyde radical nano-cellulose that aldehyde group content is 5.5mmol/g.The aldehyde radical that will be obtained
Nano-cellulose is dissolved in deionized water, is configured to the solution that concentration is 5wt%, and N- succinyl-chitosan is added to aldehyde radical nanometer
In cellulose solution, wherein the mass ratio of aldehyde radical nano-cellulose and N- succinyl-chitosan is 1:0.5, mixing is equal at room temperature
It is even, form self-healing material.Nano-cellulose self-healing material obtained in this example, which is destroyed in rear 50s, can be achieved self-healing
It closes, the intensity of material can be restored to original 93% after healing.
Embodiment 6
By the oxidant potassium metaperiodate of 2g, it is added to the p-methyl benzenesulfonic acid method nano-cellulose water that 200mL solid content is 0.5wt%
In suspension, 60 DEG C are protected from light 4h, obtain the aldehyde radical nano-cellulose that aldehyde group content is 9mmol/g.Obtained aldehyde radical is received
Rice cellulose is configured to the solution that concentration is 2.3wt%, and amino cellulose is added in the aldehyde radical nano-cellulose solution,
Wherein the mass ratio of aldehyde radical nano-cellulose and amino cellulose is 1:1.2, it is uniformly mixed at room temperature, forms self-healing material
Material.
Nano-cellulose self-healing material obtained in this example, which is destroyed in rear 10s, can be achieved self-healing, material after healing
The intensity of material can be restored to original 96%.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (7)
1. a kind of preparation method of nano-cellulose self-healing material, it is characterised in that：Include the following steps：
（1）The preparation of aldehyde radical nano-cellulose；
（2）By step（1）The aldehyde radical nano-cellulose of preparation is dissolved in deionized water, and compound concentration is the solution of 1wt%-7wt%,
Then amino-containing natural polymer is added into aldehyde radical nano-cellulose solution, is uniformly mixed at room temperature, form self-healing material
Material.
2. the preparation method of nano-cellulose self-healing material according to claim 1, it is characterised in that：Step（1）Tool
Body is：Oxidant potassium metaperiodate is added in the nano-cellulose water slurry that solid content is 0.2wt%-1.5wt%, 60 DEG C are kept away
Light reaction 4h obtains the aldehyde radical nano-cellulose that aldehyde group content is 5-9.5mmol/g.
3. the preparation method of nano-cellulose self-healing material according to claim 2, it is characterised in that：The nanometer
Cellulose is one of acid system nano-cellulose, physical method nano-cellulose, enzyme process nano-cellulose, bacteria cellulose.
4. the preparation method of nano-cellulose self-healing material according to claim 2, it is characterised in that：Potassium metaperiodate and
The mass ratio of nano-cellulose is：0.5:1-2:1.
5. the preparation method of nano-cellulose self-healing material according to claim 1, it is characterised in that：Step（2）In
The amino-containing natural polymer is gelatin, chitosan, carboxymethyl chitosan, N- succinyl-chitosan, chitin, amino
One of cellulose, aminated alginic acid sodium, amination starch, amination hyaluronic acid, amination agar.
6. the preparation method of nano-cellulose self-healing material according to claim 1, it is characterised in that：Step（2）In
The mass ratio of the aldehyde radical nano-cellulose and amino-containing natural polymer is 1:0.1-1:1.5.
7. nano-cellulose self-healing material made from a kind of preparation method as claimed in any one of claims 1 to 6.
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Cited By (6)
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| CN109912850A (en) * | 2019-03-11 | 2019-06-21 | 同济大学 | Contain the self-healing hydrogel and its preparation method and application of excretion body |
| CN112341299A (en) * | 2020-11-05 | 2021-02-09 | 南京理工大学 | Preparation of nano core-shell Al @ KIO by spray coprecipitation method4Thermite method |
| CN113045938A (en) * | 2021-02-19 | 2021-06-29 | 佛山职业技术学院 | Preparation method and application of nanocellulose-based oleophobic oil-resistant fluorine-free coating |
| CN113150319A (en) * | 2021-03-30 | 2021-07-23 | 武汉纺织大学 | Cellulose nanocrystal enhanced efficient self-healing hydrogel and preparation method thereof |
| CN114853952A (en) * | 2022-06-10 | 2022-08-05 | 闽江学院 | Super-stretching self-repairing nano cellulose gel and preparation method thereof |
| CN115844927A (en) * | 2023-03-02 | 2023-03-28 | 深圳汉盛汇融再生医学科技有限公司 | Application of stem cells in preparation of preparation for treating leukoencephalopathy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109912850A (en) * | 2019-03-11 | 2019-06-21 | 同济大学 | Contain the self-healing hydrogel and its preparation method and application of excretion body |
| CN109912850B (en) * | 2019-03-11 | 2021-03-02 | 同济大学 | Self-healing hydrogel entrapping exosomes and preparation method and application thereof |
| CN112341299A (en) * | 2020-11-05 | 2021-02-09 | 南京理工大学 | Preparation of nano core-shell Al @ KIO by spray coprecipitation method4Thermite method |
| CN113045938A (en) * | 2021-02-19 | 2021-06-29 | 佛山职业技术学院 | Preparation method and application of nanocellulose-based oleophobic oil-resistant fluorine-free coating |
| CN113150319A (en) * | 2021-03-30 | 2021-07-23 | 武汉纺织大学 | Cellulose nanocrystal enhanced efficient self-healing hydrogel and preparation method thereof |
| CN113150319B (en) * | 2021-03-30 | 2022-07-05 | 武汉纺织大学 | Cellulose nanocrystal reinforced efficient self-healing hydrogel and preparation method thereof |
| CN114853952A (en) * | 2022-06-10 | 2022-08-05 | 闽江学院 | Super-stretching self-repairing nano cellulose gel and preparation method thereof |
| CN114853952B (en) * | 2022-06-10 | 2024-03-08 | 闽江学院 | Super-stretching self-repairing nanocellulose gel and preparation method thereof |
| CN115844927A (en) * | 2023-03-02 | 2023-03-28 | 深圳汉盛汇融再生医学科技有限公司 | Application of stem cells in preparation of preparation for treating leukoencephalopathy |
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Application publication date: 20181120 |