CN110903579B - Nontoxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material and preparation method thereof - Google Patents
Nontoxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material and preparation method thereof Download PDFInfo
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- C08J9/28—Working-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
- C08J9/286—Working-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 the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
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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
- C08J2305/14—Hemicellulose; Derivatives thereof
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- 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
- C08J2405/14—Hemicellulose; Derivatives thereof
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- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
Abstract
The invention discloses a non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material and a preparation method thereof. The method comprises the following steps: (1) adding hemicellulose and a cross-linking agent into deionized water, heating and stirring until the hemicellulose and the cross-linking agent are dissolved to obtain a mixed solution; (2) dissolving PVA in water, heating, stirring and dissolving to obtain a PVA solution; (3) and mixing and stirring the mixed solution and the PVA solution to obtain a cross-linked product, cooling, forming, washing and drying to obtain the non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material. The foam composite material is easy to process, non-toxic and harmless, has high mechanical strength and high elasticity, and has great application potential in the aspects of anti-seismic and anti-compression materials, elastic response materials, soft tissue engineering materials, biomedical materials and the like.
Description
Technical Field
The invention belongs to the technical field of biomass materials, and particularly relates to a non-toxic harmless high-strength high-elasticity hemicellulose foam composite material and a preparation method thereof.
Background
Foam is an artificial, low density, highly porous material. They have some superior physical properties such as large specific surface area, high impact energy absorption and excellent strength to weight ratio, compared to the bulk of the same product. Depending on their properties, foams are useful in absorbent materials, packaging applications, and soft tissue engineering.
Due to the growing environmental concerns and the ready availability of xylans in downstream products, xylans are receiving increasing attention from researchers. In addition, the xylan has wide sources, abundant reserves, renewability, adjustable functionality and biocompatibility, so that the xylan has wide application potential in the aspects of biomass refining and biological materials. Researchers are actively researching that xylan sugar natural biomass materials can gradually replace petroleum-based products.
The hemicellulose foam composite material reported at present has poor mechanical strength and cycle recovery, and has great limitation in application in many aspects. In addition, most of the reported cross-linking agents used for the foam composite materials are toxic reagents such as boric acid, glutaraldehyde, formaldehyde and the like, so that the cross-linking agents have certain harm to human bodies and have great limitation on the application of the cross-linking agents. At present, the foam composite material with high mechanical strength and high elasticity prepared by taking hemicellulose as a base material is not reported.
Disclosure of Invention
The invention provides a non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material and a preparation method thereof, aiming at the defects of the current hemicellulose foam composite material in the aspects of mechanical property and rebound resilience and considering the problem of environmental protection. The hemicellulose foam composite material prepared by the invention has good mechanical property and elasticity, is nontoxic and harmless to human bodies, and has great application potential in the aspects of anti-seismic and anti-compression materials, elastic response materials, soft tissue engineering materials, biomedical materials and the like.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention prepares the non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material by crosslinking sodium trimetaphosphate.
The invention provides a preparation method of a non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material, which comprises the following steps of:
(1) adding hemicellulose and a cross-linking agent into deionized water, and heating and dissolving under a stirring state to obtain a mixed solution;
(2) adding polyvinyl alcohol into water, and heating and dissolving under a stirring state to obtain a polyvinyl alcohol solution;
(3) and (3) mixing the mixed solution obtained in the step (1) with the polyvinyl alcohol solution obtained in the step (2), stirring to obtain a cross-linked product, pouring the cross-linked product into a mold, cooling and molding at room temperature to obtain a foamed material, washing, and drying to obtain the non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material.
Further, the hemicellulose in the step (1) is xylan, and the cross-linking agent is sodium trimetaphosphate; the mass ratio of the cross-linking agent to the hemicellulose is 10: 1-7.
Further, the temperature of the heating and dissolving treatment in the step (1) is 70-90 ℃, and the time of the heating and dissolving treatment is 3-5 h.
Further, in the mixed solution of the step (1), the concentration of hemicellulose is 1-7 wt%.
Further, the mass ratio of the hemicellulose in the step (1) to the polyvinyl alcohol in the step (2) is 1-7: 5.
further, the temperature of the heating and dissolving treatment in the step (2) is 70-90 ℃, and the time of the heating and dissolving treatment is 1-2 h.
Further, the concentration of the polyvinyl alcohol solution in the step (2) is 10-20 wt%.
Further, the rotation speed of the stirring treatment in the step (3) is 500-.
Further, the washing in the step (3) is to wash the surface of the foam material with deionized water for 3-5 times; the drying is natural drying for 3-5 days at room temperature.
The invention provides a non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material prepared by the preparation method.
According to the invention, xylan hemicellulose with rich content in nature and polyvinyl alcohol with high biocompatibility are taken as substrates, non-toxic and harmless sodium trimetaphosphate is taken as a cross-linking agent, and the xylan hemicellulose mixed with the polyvinyl alcohol and the sodium trimetaphosphate is cross-linked to prepare the hemicellulose foam composite material which has excellent mechanical properties and high elasticity. The method has important significance for researching that the foam material is applied to soft tissue engineering and utilizing the biomass material to gradually supplement and replace non-renewable resources such as petroleum and the like.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the preparation method provided by the invention has the characteristics of easy control of reaction conditions, simple operation and the like;
(2) the preparation method provided by the invention adopts xylan hemicellulose with the characteristics of regeneration, environmental protection, no toxicity, outstanding biocompatibility, adjustable functionality and the like and polyvinyl alcohol with higher biocompatibility as raw materials, and adopts non-toxic and harmless sodium trimetaphosphate as a cross-linking agent, which are beneficial to environmental protection and development of application of biomass;
(3) the non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material prepared by the method is non-toxic and harmless, so that the composite material has a large application potential in the aspects of materials related to human health, such as tissue engineering materials, biomedical materials and the like; the foam composite material has excellent mechanical properties which are close to the mechanical property requirements of human cartilage, has high elasticity and can still recover to be close to the initial height after multiple compression tests; therefore, the foam material has wide application prospect in the aspects of anti-seismic and anti-compression materials, elastic response materials and the like.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
A preparation method of a non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material comprises the following steps:
(1) adding 1.0g of xylan hemicellulose and 10g of sodium trimetaphosphate into deionized water, stirring and dissolving for 3 hours at 90 ℃ to obtain a mixed solution with the xylan hemicellulose concentration of 1 wt%;
(2) adding 5.0g of polyvinyl alcohol into 20g of deionized water, and stirring and dissolving at 90 ℃ for 1h to obtain a polyvinyl alcohol solution;
(3) and (2) mixing the mixed solution obtained in the step (1) with the polyvinyl alcohol solution obtained in the step (2), stirring for 50s at a stirring speed of 500 r/min, pouring the obtained cross-linked product into a mold, cooling and molding to obtain a foam composite material, washing the surface of the foam composite material for 5 times by using deionized water, and drying at room temperature for 5 days to obtain the non-toxic, harmless, high-mechanical-strength and high-elasticity hemicellulose foam composite material.
The obtained non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material is soaked in deionized water at 37 ℃ for 24 hours, and is circularly compressed by using a tensile compression material tester INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%. Further, 1000 cycles of compression were conducted under the condition that the compression strain became 30%.
The hemicellulose foam composite material prepared in example 1 was tested to have a compressive stress of 4.59MPa and a height recovery of 96.54% after 1000 compression cycles.
Example 2
The preparation of non-toxic harmless high-mechanical strength high-elasticity hemicellulose foam composite material comprises the following steps:
(1) adding 2.0g of xylan hemicellulose and 10g of sodium trimetaphosphate into deionized water, stirring and dissolving for 4 hours at 80 ℃ to obtain a mixed solution with the xylan hemicellulose concentration of 2 wt%;
(2) adding 5.0g of polyvinyl alcohol into 28.5g of deionized water, stirring and dissolving for 1.5h at 80 ℃ to obtain a polyvinyl alcohol solution;
(3) and (2) mixing the mixed solution obtained in the step (1) and the polyvinyl alcohol solution obtained in the step (2) and stirring for 40s at the stirring speed of 600 r/min, pouring the obtained cross-linked product into a mould, cooling and forming to obtain a foam composite material, washing the surface of the foam composite material for 4 times by using deionized water, and drying at room temperature for 4 days to obtain the non-toxic, harmless, high-mechanical-strength and high-elasticity hemicellulose foam composite material.
The obtained non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material is soaked in deionized water at 37 ℃ for 24 hours, and is circularly compressed by using a tensile compression material tester INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%. Further, 1000 cycles of compression were conducted under the condition that the compression strain became 30%.
The hemicellulose foam composite prepared in example 2 was tested to have a compressive stress of 5.76MPa and a height recovery of 96.32% after 1000 compression cycles.
Example 3
The preparation of non-toxic harmless high-mechanical strength high-elasticity hemicellulose foam composite material comprises the following steps:
(1) adding 3.0g of xylan hemicellulose and 10g of sodium trimetaphosphate into deionized water, stirring and dissolving for 5 hours at 70 ℃ to obtain a mixed solution with the xylan hemicellulose concentration of 3 wt%;
(2) adding 5.0g of polyvinyl alcohol into 45g of deionized water, and stirring and dissolving for 2 hours at 70 ℃ to obtain a polyvinyl alcohol solution;
(3) and (2) mixing the mixed solution obtained in the step (1) and the polyvinyl alcohol solution obtained in the step (2) and stirring for 30s at the stirring speed of 700r/min, pouring the obtained cross-linked product into a mould, cooling and forming to obtain a foam composite material, washing the surface of the foam composite material for 3 times by using deionized water, and drying at room temperature for 3 days to obtain the non-toxic, harmless, high-mechanical-strength and high-elasticity hemicellulose foam composite material.
The obtained non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material is soaked in deionized water at 37 ℃ for 24 hours, and is circularly compressed by using a tensile compression material tester INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%. Further, 1000 cycles of compression were conducted under the condition that the compression strain became 30%.
The hemicellulose foam composite material prepared in example 3 has a compressive stress of 6.92MPa and a height recovery of 97.44% after 1000 compression cycles.
Example 4
The preparation of non-toxic harmless high-mechanical strength high-elasticity hemicellulose foam composite material comprises the following steps:
(1) adding 4.0g of xylan hemicellulose and 10g of sodium trimetaphosphate into deionized water, stirring and dissolving for 5 hours at 90 ℃ to obtain a mixed solution with the xylan hemicellulose concentration of 4 wt%;
(2) adding 5.0g of polyvinyl alcohol into 20g of deionized water, and stirring and dissolving for 2 hours at 90 ℃ to obtain a polyvinyl alcohol solution;
(3) and (2) mixing the mixed solution obtained in the step (1) and the polyvinyl alcohol solution obtained in the step (2) and stirring for 50s at the stirring speed of 700r/min, pouring the obtained cross-linked product into a mould, cooling and forming to obtain a foam composite material, washing the surface of the foam composite material for 5 times by using deionized water, and drying at room temperature for 5 days to obtain the non-toxic, harmless, high-mechanical-strength and high-elasticity hemicellulose foam composite material.
The obtained non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material is soaked in deionized water at 37 ℃ for 24 hours, and is circularly compressed by using a tensile compression material tester INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%. Further, 1000 cycles of compression were conducted under the condition that the compression strain became 30%.
The hemicellulose foam composite material prepared in example 1 was tested to have a compressive stress of 7.72MPa and a height recovery of 97.89% after 1000 compression cycles.
Example 5
The preparation of non-toxic harmless high-mechanical strength high-elasticity hemicellulose foam composite material comprises the following steps:
(1) adding 5.0g of xylan hemicellulose and 10g of sodium trimetaphosphate into deionized water, stirring and dissolving for 5 hours at 90 ℃ to obtain a mixed solution with the xylan hemicellulose concentration of 5 wt%;
(2) adding 5.0g of polyvinyl alcohol into 20g of deionized water, and stirring and dissolving for 2 hours at 90 ℃ to obtain a polyvinyl alcohol solution;
(3) and (2) mixing the mixed solution obtained in the step (1) and the polyvinyl alcohol solution obtained in the step (2) and stirring for 50s at the stirring speed of 700r/min, pouring the obtained cross-linked product into a mould, cooling and forming to obtain a foam composite material, washing the surface of the foam composite material for 5 times by using deionized water, and drying at room temperature for 5 days to obtain the non-toxic, harmless, high-mechanical-strength and high-elasticity hemicellulose foam composite material.
The obtained non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material is soaked in deionized water at 37 ℃ for 24 hours, and is circularly compressed by using a tensile compression material tester INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%. Further, 1000 cycles of compression were conducted under the condition that the compression strain became 30%.
The hemicellulose foam composite prepared in example 5 was tested to have a compressive stress of 10.61MPa and a height recovery of 98.57% after 1000 compression cycles.
Example 6
The preparation of non-toxic harmless high-mechanical strength high-elasticity hemicellulose foam composite material comprises the following steps:
(4) adding 6.0g of xylan hemicellulose and 10g of sodium trimetaphosphate into deionized water, stirring and dissolving for 5 hours at 90 ℃ to obtain a mixed solution with the xylan hemicellulose concentration of 6 wt%;
(5) adding 5.0g of polyvinyl alcohol into 20g of deionized water, and stirring and dissolving for 2 hours at 90 ℃ to obtain a polyvinyl alcohol solution;
(6) and (2) mixing the mixed solution obtained in the step (1) and the polyvinyl alcohol solution obtained in the step (2) and stirring for 50s at the stirring speed of 700r/min, pouring the obtained cross-linked product into a mould, cooling and forming to obtain a foam composite material, washing the surface of the foam composite material for 5 times by using deionized water, and drying at room temperature for 5 days to obtain the non-toxic, harmless, high-mechanical-strength and high-elasticity hemicellulose foam composite material.
The obtained non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material is soaked in deionized water at 37 ℃ for 24 hours, and is circularly compressed by using a tensile compression material tester INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%. Further, 1000 cycles of compression were conducted under the condition that the compression strain became 30%.
The hemicellulose foam composite material prepared in example 6 was tested to have a compressive stress of 10.24MPa and a height recovery of 99.21% after 1000 compression cycles.
Example 7
The preparation of non-toxic harmless high-mechanical strength high-elasticity hemicellulose foam composite material comprises the following steps:
(7) adding 7.0g of xylan hemicellulose and 10g of sodium trimetaphosphate into deionized water, stirring and dissolving for 3 hours at 90 ℃ to obtain a mixed solution with the xylan hemicellulose concentration of 7 wt%;
(8) adding 5.0g of polyvinyl alcohol into 20g of deionized water, and stirring and dissolving for 2 hours at 90 ℃ to obtain a polyvinyl alcohol solution;
(9) and (2) mixing the mixed solution obtained in the step (1) and the polyvinyl alcohol solution obtained in the step (2) and stirring for 50s at the stirring speed of 700r/min, pouring the obtained cross-linked product into a mould, cooling and forming to obtain a foam composite material, washing the surface of the foam composite material for 5 times by using deionized water, and drying at room temperature for 5 days to obtain the non-toxic, harmless, high-mechanical-strength and high-elasticity hemicellulose foam composite material.
The obtained non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material is soaked in deionized water at 37 ℃ for 24 hours, and is circularly compressed by using a tensile compression material tester INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%. Further, 1000 cycles of compression were conducted under the condition that the compression strain became 30%.
The hemicellulose foam composite prepared in example 7 was tested to have a compressive stress of 7.68MPa and a height recovery of 98.52% after 1000 compression cycles.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (5)
1. The preparation method of the non-toxic harmless high-mechanical-strength high-elasticity hemicellulose foam composite material is characterized by comprising the following steps of:
(1) adding hemicellulose and a cross-linking agent into water, and heating and dissolving under a stirring state to obtain a mixed solution;
(2) adding polyvinyl alcohol into water, and heating and dissolving under a stirring state to obtain a polyvinyl alcohol solution;
(3) mixing the mixed solution obtained in the step (1) with the polyvinyl alcohol solution obtained in the step (2), stirring to obtain a cross-linked product, pouring the cross-linked product into a mold, cooling and molding at room temperature to obtain a foamed material, washing, and drying to obtain the non-toxic, harmless, high-mechanical-strength and high-elasticity hemicellulose foamed composite material;
the hemicellulose in the step (1) is xylan, and the cross-linking agent is sodium trimetaphosphate; the mass ratio of the cross-linking agent to the hemicellulose is 10: 1 to 7;
in the mixed solution in the step (1), the concentration of hemicellulose is 1-7 wt%;
the mass ratio of the hemicellulose obtained in the step (1) to the polyvinyl alcohol obtained in the step (2) is 1-7: 5;
the concentration of the polyvinyl alcohol solution in the step (2) is 10-20 wt%;
the rotation speed of the stirring treatment in the step (3) is 500-700r/min, and the stirring treatment time is 30-50 s.
2. The method for preparing a non-toxic, harmless, high mechanical strength, high elasticity hemicellulose foam composite material according to claim 1, wherein the temperature of the heating dissolution treatment in step (1) is 70-90 ℃ and the time of the heating dissolution treatment is 3-5 h.
3. The method for preparing a non-toxic, harmless, high mechanical strength, high elasticity hemicellulose foam composite material according to claim 1, wherein the temperature of the heating dissolution treatment in the step (2) is 70-90 ℃, and the time of the heating dissolution treatment is 1-2 h.
4. The method for preparing a non-toxic, harmless, high mechanical strength, high elasticity hemicellulose foam composite material as claimed in claim 1, wherein the washing in step (3) is to wash the surface of the foam material with deionized water 3-5 times; the drying is natural drying for 3-5 days at room temperature.
5. A non-toxic, harmless, high mechanical strength, high resilience hemicellulose foam composite produced by the method of any one of claims 1-4.
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| CN102775525A (en) * | 2012-07-16 | 2012-11-14 | 华南理工大学 | Preparation method and application of cross-linking type hemicellulose |
| CN103073738A (en) * | 2013-01-22 | 2013-05-01 | 华南理工大学 | Polyvinyl alcohol/xylan biodegradable composite membrane and preparation method and application thereof |
| CN106012654A (en) * | 2016-06-11 | 2016-10-12 | 苏州思创源博电子科技有限公司 | Preparation method for high-quality paper pulp |
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