CN110791047B - Nontoxic harmless high-strength high-heat-resistance hemicellulose foam composite material and preparation method thereof - Google Patents
Nontoxic harmless high-strength high-heat-resistance hemicellulose foam composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a non-toxic harmless hemicellulose foam composite material and a preparation method thereof. The method comprises the following steps: (1) dissolving hemicellulose in water, heating and stirring until the hemicellulose is dissolved to obtain a hemicellulose solution, and dissolving a cross-linking agent and citric acid in the hemicellulose solution 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 foam composite material. The foam composite material is easy to process, has excellent mechanical property, good restorability and higher heat resistance, and has wide application prospect in the aspect of functional materials taking foam porous materials as substrates, such as anti-seismic and anti-compression materials and the like. In addition, the foam material has no toxic and harmful substance residue, so that the foam material has great application potential in the aspects of materials related to human health, such as 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-heat-resistance hemicellulose foam composite material and a preparation method thereof.
Background
The foam is a polymer with a three-dimensional high molecular structure, has a uniform interconnected network structure with high porosity, has high similarity with soft tissues in a human body, and therefore has rationality and practicability when being applied to the aspect of soft tissue engineering. Foams have also found great application in tissue engineering, for example, soft tissue growth, cartilage replacement, nucleus replacement, wound healing, bone regeneration, vascular replacement, and the like.
Natural polymers and artificially synthesized polymers having biocompatibility are the main biological raw materials currently used in soft tissue engineering for preparing foams. In recent years, with the global interest in environment and sustainable development, natural polymers, such as natural polysaccharides, have become increasingly important for tissue engineering applications due to their properties of being renewable, environmentally friendly, remarkably biocompatible, non-toxic, etc. Hemicellulose in plants is used as a new biomass material, has wide sources and abundant reserves, and in addition, the reproducibility, the adjustable functionality and the biocompatibility of xylan cause that the xylan receives great attention in biomass refining and biological materials in nearly ten years.
Most of the cross-linking agents used in the currently reported foam composite materials are boric acid, glutaraldehyde, formaldehyde and the like, the cross-linking agents are toxic and have certain harm to human bodies, and the prepared foam composite materials are not suitable for human soft tissue engineering. In addition, the poor mechanical strength of the biomass foam composites reported so far severely limits their development in human soft tissue engineering. At present, no report is found about the method for applying the xylan hemicellulose prepared foam composite material to soft tissue engineering.
Disclosure of Invention
Aiming at the defects of the mechanical property and stability of the current foam composite material, the invention provides a non-toxic, harmless, high-strength and high-heat-resistance hemicellulose foam composite material and a preparation method thereof.
The above object of the present invention can be achieved by at least one of the following technical means.
The non-toxic harmless high-strength high-heat-resistance hemicellulose foam composite material is prepared by crosslinking sodium trimetaphosphate, and is characterized by comprising the following steps of:
(1) mixing hemicellulose, citric acid and a cross-linking agent, adding into deionized water, heating and stirring until the mixture is dissolved to obtain a mixed solution;
(2) adding polyvinyl alcohol into deionized water, and stirring and dissolving under a heating condition to obtain a polyvinyl alcohol solution;
(3) and (3) mixing and stirring the mixed solution in the step (1) and the polyvinyl alcohol solution in the step (2) to obtain a cross-linked product, cooling, forming, washing and drying to obtain the non-toxic, harmless, high-strength and high-heat-resistance hemicellulose foam composite material.
Preferably, in the step (1), the hemicellulose is xylan, and the cross-linking agent is sodium trimetaphosphate.
Preferably, in the step (1), the heating temperature is 70-90 ℃, and the stirring time is 3-5 hours.
Preferably, the concentration of hemicellulose in the mixed solution in the step (1) is 1-7 wt%.
Preferably, in the step (1), the mass ratio of the cross-linking agent to the citric acid to the hemicellulose is 10: 5: (1-7).
Preferably, the mass ratio of the hemicellulose to the polyvinyl alcohol in the cross-linked product of the step (3) is (1-7): 5.
Preferably, in the step (2), the heating temperature is 70-90 ℃, and the stirring time is 1-2 hours.
Preferably, in the step (3), the stirring speed is 500-700 r/min, and the stirring time is 30-50 s.
Preferably, in the step (3), the washing method is to wash the surface of the foam with deionized water for 3-5 times, and the drying method is to dry naturally for 3-5 days at room temperature.
The non-toxic harmless high-strength high-heat-resistance hemicellulose foam composite material prepared by the preparation method.
The hemicellulose foam composite material is prepared by taking xylan hemicellulose rich in natural content and polyvinyl alcohol with high biocompatibility as substrates, taking non-toxic and harmless sodium trimetaphosphate as a cross-linking agent, and cross-linking the xylan hemicellulose mixed with the polyvinyl alcohol and the sodium trimetaphosphate, and has high mechanical property and stability. 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 has the characteristics of easy control of reaction conditions, simple operation and the like;
(2) 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 uses non-toxic and harmless sodium trimetaphosphate as a cross-linking agent, which are beneficial to environmental protection and development of application of biomass;
(3) according to the invention, citric acid is used as a plasticizer, and the mechanical strength of the prepared hemicellulose foam composite material is increased through the esterification reaction of the citric acid and hemicellulose;
(4) the hemicellulose foam composite material prepared by the invention is nontoxic and harmless, and does not react with human tissues, so that the hemicellulose foam composite material has great 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 good mechanical property, good heat resistance, excellent mechanical property and good restorability, and does not reduce the mechanical strength because of the increase of the use times, so the foam composite material has wide application prospect in the aspect of functional materials taking foam porous materials as substrates, such as anti-seismic and anti-compression materials and the like.
Drawings
FIG. 1 is a flow chart of the preparation of the non-toxic, harmless, high-strength and high-heat-resistance hemicellulose foam composite material.
Detailed Description
The following further illustrates the invention by reference to specific examples, which should not be construed as limiting the invention. It is within the scope of the present invention to make simple modifications or substitutions of materials, methods, steps or conditions involved in the present invention without departing from the spirit and substance of the present invention; unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated. Unless otherwise indicated, reagents and materials used in the present invention are commercially available.
Example 1
A method for preparing nontoxic, harmless, high-strength and high-heat-resistance hemicellulose foam composite material (see figure 1) comprises the following steps:
(1) adding 1.0g of xylan hemicellulose, 5g of citric acid 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 1 wt%;
(2) adding 5.0g of polyvinyl alcohol into deionized water, stirring and dissolving for 1h at 90 ℃ to obtain a polyvinyl alcohol solution;
(3) and (3) 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 mold, cooling and molding, washing the surface of the foam for 5 times by using deionized water, and drying at room temperature for 5 days to obtain the high-strength high-heat-resistance hemicellulose foam.
Soaking the obtained hemicellulose foam in deionized water at 37 ℃ for 24h, and performing cyclic compression by using a tensile compression material testing machine INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%.
The compressive stress of the hemicellulose foam composite material prepared in example 1 is detected to be 3.6 MPa.
Example 2
The preparation of non-toxic harmless high-strength high-heat-resistance hemicellulose foam composite material comprises the following steps:
(1) adding 2.0g of xylan hemicellulose, 5g of citric acid 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 deionized water, stirring and dissolving for 1.5 hours at 80 ℃ to obtain a polyvinyl alcohol solution;
(3) and (3) 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 600 r/min, pouring the obtained cross-linked product into a mould, cooling and forming, washing the surface of the foam for 4 times by using deionized water, and drying at room temperature for 4 days to obtain the high-strength high-heat-resistance hemicellulose foam.
Soaking the obtained hemicellulose foam in deionized water at 37 ℃ for 24h, and performing cyclic compression by using a tensile compression material testing machine INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%.
The compressive stress of the hemicellulose foam composite material prepared in example 2 is detected to be 4.4 MPa.
Example 3
The preparation of non-toxic harmless high-strength high-heat-resistance hemicellulose foam composite material comprises the following steps:
(1) adding 3.0g of xylan hemicellulose, 5g of citric acid and 10g of sodium trimetaphosphate into deionized water, stirring and dissolving at 70 ℃ for 3 hours to obtain a mixed solution with the xylan hemicellulose concentration of 3 wt%;
(2) adding 5.0g of polyvinyl alcohol into deionized water, and stirring and dissolving the polyvinyl alcohol for 2 hours at 70 ℃ to obtain a polyvinyl alcohol solution;
(3) and (3) 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 500 r/min, pouring the obtained cross-linked product into a mold, cooling and molding, washing the surface of the foam for 3 times by using deionized water, and drying at room temperature for 3 days to obtain the high-strength high-heat-resistance hemicellulose foam.
Soaking the obtained hemicellulose foam in deionized water at 37 ℃ for 24h, and performing cyclic compression by using a tensile compression material testing machine INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%.
The compressive stress of the hemicellulose foam composite material prepared in example 3 is detected to be 5.2 MPa.
Example 4
The preparation of non-toxic harmless high-strength high-heat-resistance hemicellulose foam composite material comprises the following steps:
(1) adding 4.0g of xylan hemicellulose, 5g of citric acid 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 deionized water, and stirring and dissolving the polyvinyl alcohol for 1 hour at 90 ℃ to obtain a polyvinyl alcohol solution;
(3) and (3) 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 mold, cooling and molding, washing the surface of the foam for 3 times by using deionized water, and drying at room temperature for 4 days to obtain the high-strength high-heat-resistance hemicellulose foam.
Soaking the obtained hemicellulose foam in deionized water at 37 ℃ for 24h, and performing cyclic compression by using a tensile compression material testing machine INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%.
The compressive stress of the hemicellulose foam composite material prepared in example 4 is detected to be 5.3 MPa.
Example 5
The preparation of non-toxic harmless high-strength high-heat-resistance hemicellulose foam composite material comprises the following steps:
(1) adding 5.0g of xylan hemicellulose, 5g of citric acid 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 deionized water, and stirring and dissolving the polyvinyl alcohol for 1 hour at 90 ℃ to obtain a polyvinyl alcohol solution;
(3) and (3) 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 mold, cooling and molding, washing the surface of the foam for 3 times by using deionized water, and drying at room temperature for 4 days to obtain the high-strength high-heat-resistance hemicellulose foam.
Soaking the obtained hemicellulose foam in deionized water at 37 ℃ for 24h, and performing cyclic compression by using a tensile compression material testing machine INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%.
The compressive stress of the hemicellulose foam composite material prepared in example 5 is detected to be 7.4 MPa.
Example 6
The preparation of non-toxic harmless high-strength high-heat-resistance hemicellulose foam composite material comprises the following steps:
(1) adding 6.0g of xylan hemicellulose, 5g of citric acid 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%;
(2) adding 5.0g of polyvinyl alcohol into deionized water, and stirring and dissolving the polyvinyl alcohol for 1 hour at 90 ℃ to obtain a polyvinyl alcohol solution;
(3) and (3) 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 700r/min, pouring the obtained cross-linked product into a mold, cooling and molding, washing the surface of the foam for 3 times by using deionized water, and drying at room temperature for 4 days to obtain the high-strength high-heat-resistance hemicellulose foam.
Soaking the obtained hemicellulose foam in deionized water at 37 ℃ for 24h, and performing cyclic compression by using a tensile compression material testing machine INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%.
The compressive stress of the hemicellulose foam composite material prepared in example 6 is detected to be 4.3 MPa.
Example 7
The preparation of non-toxic harmless high-strength high-heat-resistance hemicellulose foam composite material comprises the following steps:
(1) adding 7.0g of xylan hemicellulose, 5g of citric acid 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 7 wt%;
(2) adding 5.0g of polyvinyl alcohol into deionized water, and stirring and dissolving the polyvinyl alcohol for 1 hour at 90 ℃ to obtain a polyvinyl alcohol solution;
(3) and (3) 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 mold, cooling and molding, washing the surface of the foam for 3 times by using deionized water, and drying at room temperature for 4 days to obtain the high-strength high-heat-resistance hemicellulose foam.
Soaking the obtained hemicellulose foam in deionized water at 37 ℃ for 24h, and performing cyclic compression by using a tensile compression material testing machine INSTRON 5565, wherein the compression rate is 1.5mm/min, and the compression strain is 70%.
The compressive stress of the hemicellulose foam composite material prepared in example 7 is detected to be 4.0 MPa.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any equivalent alterations, modifications or improvements made by those skilled in the art to the above-described embodiments using the technical solutions of the present invention are still within the scope of the technical solutions of the present invention.
Claims (5)
1. A preparation method of a non-toxic harmless high-strength high-heat-resistance hemicellulose foam composite material is characterized by comprising the following steps of:
(1) mixing hemicellulose, citric acid and a cross-linking agent, adding into deionized water, heating and stirring until the mixture is dissolved to obtain a mixed solution;
(2) adding polyvinyl alcohol into deionized water, and stirring and dissolving under a heating condition to obtain a polyvinyl alcohol solution;
(3) mixing and stirring the mixed solution in the step (1) and the polyvinyl alcohol solution in the step (2) to obtain a cross-linked product, cooling, forming, washing and drying to obtain the non-toxic, harmless, high-strength and high-heat-resistance hemicellulose foam composite material;
in the step (1), the hemicellulose is xylan, and the cross-linking agent is sodium trimetaphosphate;
in the step (1), the concentration of hemicellulose in the mixed solution is 1-7 wt%;
in the step (1), the mass ratio of the cross-linking agent to the citric acid to the hemicellulose is 10: 5: (1-7);
the mass ratio of the hemicellulose to the polyvinyl alcohol in the cross-linked product obtained in the step (3) is (1-7): 5;
in the step (3), the stirring speed is 500-700 r/min, and the stirring time is 30-50 s.
2. The preparation method according to claim 1, wherein in the step (1), the heating temperature is 70-90 ℃ and the stirring time is 3-5 h.
3. The preparation method according to claim 1, wherein in the step (2), the heating temperature is 70-90 ℃ and the stirring time is 1-2 h.
4. The preparation method according to claim 1, wherein in the step (3), the washing method is to wash the foam surface with deionized water 3-5 times, and the drying method is to dry naturally at room temperature for 3-5 days.
5. The non-toxic, harmless, high-strength, high-heat-resistant hemicellulose foam composite material prepared by the preparation method according to any one of claims 1-4.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| Cross-linked polyvinyl alcohol (PVA) foams reinforced with cellulose nanocrystals (CNCs);Kristiina Oksman 等;《Cellulose》;20160630;第23卷(第3期);第1925-1938页 * |
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