CN109370133B - Method for reinforcing polymethyl methacrylate by cellulose - Google Patents
Method for reinforcing polymethyl methacrylate by cellulose Download PDFInfo
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- CN109370133B CN109370133B CN201811175300.8A CN201811175300A CN109370133B CN 109370133 B CN109370133 B CN 109370133B CN 201811175300 A CN201811175300 A CN 201811175300A CN 109370133 B CN109370133 B CN 109370133B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
- C08L33/12—Homopolymers or copolymers of methyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses a method for reinforcing polymethyl methacrylate by cellulose, belonging to the technical field of cellulose reinforced materials. The method comprises the following steps: s01, smashing the wood blocks into wood particles; s02, preparing a delignification solution, placing wood particles in the delignification solution, continuously boiling for more than 4 hours, and then washing with distilled water to remove impurities to obtain wood particles I; s03, placing the wood particles I in H with the mass fraction of 30%2O2Boiling while neutralizing, wherein the quality of wood particles I is not higher than H2O230% of the mass. The invention aims to improve the mechanical strength of polymethyl methacrylate, the modified wood fiber and the prepolymerization MMA solution are utilized to prepare the PMMA transparent composite material with any size and high optical transmittance, the wood fiber raw material has wide sources, even sawdust processing waste materials (such as sawdust, branches and the like) can be adopted, the cost is low, the resources are saved, and the preparation efficiency is high.
Description
Technical Field
The invention relates to a method for reinforcing polymethyl methacrylate by cellulose, belonging to the technical field of cellulose reinforced materials.
Background
In order to maintain energy resources of the world and reduce environmental burdens, the manufacture of green buildings has become a problem that needs to be rapidly dealt with. Harmless and sustainable materials become priorities in world interest lists, and organic glass made of Methyl Methacrylate (MMA) is gradually replacing the application of traditional inorganic glass in life, such as baby feeding bottles, children's kettles and the like, due to the advantages of light weight, safety, no toxicity, good breakage resistance and the like. However, the product produced by only adopting single MMA has single functionality and limited applicable places, and the application range can be further improved by adopting the addition of functional materials.
As one of the most abundant biomass materials, wood has been widely used as tools, fuels, and building materials. Cellulose in wood, which is high in strength and good in elasticity, has been used for energy saving windows due to its excellent optical transmittance and excellent heat insulation. By adding the index-matched cellulose to the polymethyl methacrylate (PMMA), the original high permeability can be maintained, and the mechanical properties of the window are improved. However, in the current research, the added wood sample has small size and thin thickness, because the preparation of the existing transparent composite material needs complete wood as a substrate, and lignin is a key substance for connecting wood cells, the large-sized substrate is very easy to break during the delignification, and the glass size in practical application is difficult to achieve. And the larger the thickness of the wood is, the difficulty of impregnating the wood by using the MMA solution is increased, and the gap between the MMA and the wood is increased due to incomplete impregnation, so that the internal refractive index of the prepared transparent composite material is inconsistent, and the light attenuation phenomenon is caused. Therefore, in the prior art, the production of thick and large-sized transparent composite materials is very suitable for practical application. Therefore, in the existing method for reinforcing the polymethyl methacrylate by the cellulose, the cellulose raw material is a complete wood template, and the problems of high manufacturing cost, low preparation efficiency, size limitation of the produced PMMA transparent composite material and the like exist.
Disclosure of Invention
The invention aims to provide a method for enhancing polymethyl methacrylate (PMMA) by cellulose, aiming at improving the mechanical strength of PMMA, preparing a PMMA transparent composite material with any size and high optical transmittance by utilizing modified wood fibers and a prepolymerization MMA solution, and ensuring that wood fiber raw materials have wide sources, even wood chips can be used for processing waste materials (such as sawdust, branches and the like), the cost is low, resources are saved, and the preparation efficiency is high.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method of cellulose reinforced polymethylmethacrylate comprising the steps of:
s01, smashing the wood blocks into wood particles;
s02, preparing a delignification solution, placing wood particles in the delignification solution, continuously boiling for more than 4 hours, and then washing with distilled water to remove impurities to obtain wood particles I;
s03, placing the wood particles I in H with the mass fraction of 30%2O2Boiling while neutralizing, wherein the quality of wood particles I is not higher than H2O230% of the mass, when all the wood particles I are white, stirring the wood particles I into fibers, and performing suction filtration for at least three times by using distilled water to prepare delignified wood fibers;
s04, soaking the delignified wood fibers in the pre-polymerized MMA solution, and permeating the pre-polymerized MMA solution for at least 10 minutes under vacuum pressure to fully impregnate the delignified wood fibers;
s05, placing the fully impregnated wood fibers in glass molds with different specifications and sizes, and heating for more than 6 hours at 50-70 ℃ to prepare the PMMA transparent composite material.
The diameter of the crushed wood particles in S01 is 3-5 mm.
The preparation method of the delignification solution in the S02 comprises the following steps: NaOH 10% by weight, Na2SO3The mass fraction of the active component is 5 percent, and the active component is prepared by dissolving the active component in distilled water.
In S02, the mass of the wood particles is not higher than 30% of the mass of the delignifying solution.
In S04, the mass of the delignified wood fibers is less than 30% of the mass of the prepolymerized MMA solution.
The prepolymerized MMA solution in S04 contains an initiator.
The initiator is azobisisobutyronitrile, and the addition amount of the azobisisobutyronitrile is 0.3-0.5% of the mass of the prepolymerization MMA solution.
And (3) prepolymerizing the MMA solution for prepolymerization at 70-80 ℃ under the action of azobisisobutyronitrile until the solution is in a glycerol state, and after the prepolymerization is finished, quickly transferring the prepolymerized solution into an ice water bath to cool to room temperature to terminate the reaction.
The refractive index of the PMMA transparent composite material is matched with that of the cellulose.
The dimensions of the glass mold used in the present invention include, but are not limited to, the following dimensions: 80 mm. times.25 mm. times.1 mm, 80 mm. times.25 mm. times.5 mm and 300 mm. times.300 mm. times.10 mm.
In the invention, firstly, the crushed wood particles are delignified, dried at the temperature of 105 +/-3 ℃, and dried wood particle samples are put into NaOH and Na2SO3And (2) keeping the sample boiling in a delignification solution prepared by distilled water, then washing the delignification solution by deionized water, treating the sample by using 30 mass percent of hydrogen peroxide, stirring the sample into fibers when all particles are white, carrying out suction filtration for at least three times by using the distilled water (namely extraction and then washing by the deionized water) to prepare delignified wood fibers, fully soaking the wood fibers in a prepolymerization MMA (methyl methacrylate) solution, infiltrating a nano cellulose fiber web on a cavity and a cell wall of the wood fibers, and transferring the wood fibers to a glass mold to prepare the PMMA transparent composite material.
The refractive index of lignin is 1.61, while the refractive index of cellulose (refractive index 1.53) and hemicellulose (refractive index approximately equal to 1.53) is lower, after lignin is removed, the refractive index of cell wall components can be considered as 1.53, the refractive index of the wood fiber after lignin is removed is close to that of PMMA, so that the optical interface is adjusted, and the addition of the wood fiber can enable the PMMA transparent composite material to have certain haze.
The MMA in the invention can generate synergistic effect with the cellulose directionally arranged on the cell wall, so that after the wood fiber is added, the PMMA transparent composite material has better mechanical properties (high strength and elastic modulus) than single PMMA organic glass, has light weight and low cost, is more suitable for large-scale commercial production and application, and has very wide prospect.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention improves the mechanical strength of the organic glass produced by using MMA;
(2) the preparation method of the transparent composite material is simple in process and high in preparation efficiency, and the prepared transparent composite material is not limited by size;
(3) the transparent composite material prepared by the invention is not limited by raw materials, can adopt wood processing waste, agricultural wastes and the like, has low cost, saves resources and protects the environment;
(4) the transparent composite material produced by the invention has good transmittance and high haze, and can be used in places requiring privacy protection.
The method prepares the PMMA transparent composite material with any size by mixing the prepolymerized MMA solution with the delignified wood fiber and fully soaking the MMA solution into the wood fiber. The PMMA transparent composite material prepared by the method not only keeps the high permeability of the organic glass, but also improves the mechanical strength of the organic glass, and has certain haze so as to be used in occasions needing privacy protection. The wood fiber raw material has wide sources, even can adopt sawdust to process waste materials (such as sawdust, branches and the like), has low cost and saves resources. And the method can produce the PMMA transparent composite material without size limitation, and compared with the method for preparing the transparent composite material by using a complete wood template, the preparation efficiency is improved by about three times, so that the PMMA transparent composite material prepared by the method is more suitable for large-scale commercial production and application, and has a very wide prospect.
Detailed Description
The present invention will be further described below.
Example 1
A method for reinforcing polymethyl methacrylate by cellulose comprises the following steps:
(1) the density is 0.386g/cm3The poplar wood is smashed into wood particles with the diameter of about 3-5 mm;
(2) NaOH with the mass fraction of 10 percent and Na with the mass fraction of 5 percent are used2SO3Preparing a delignification solution in distilled water, putting wood particles which are 30% of the mass of the delignification solution into the delignification solution and boiling for more than 4 hours continuously, and then removing impurities by using distilled water to obtain wood particles I;
(3) placing the wood particles I in H with the mass fraction of 30%2O2Neutralizing and keeping boiling; when all the particles become white, stirring the wood particles I into fibers, and performing suction filtration for three times by using distilled water to prepare delignified wood fibers;
(4) prepolymerization of MMA solution 2,2' -Azobis (2-methyl propionitril) (i.e., azobisisobutyronitrile) was used as an initiator, and prepolymerization was carried out at 80 ℃ for 15 minutes under the action of the initiator; the addition amount of azobisisobutyronitrile is 0.3 percent of the mass of the prepolymerization MMA solution;
(5) quickly cooling the prepolymerized MMA solution to room temperature in an ice water bath to terminate the reaction;
(6) soaking the delignified wood fibers in a pre-polymerized MMA solution, and permeating for 10 minutes under vacuum pressure to fully impregnate the wood fibers with the pre-polymerized MMA solution; the added amount of delignified wood fibres corresponds to 10% of the mass of the prepolymerised MMA solution;
(7) the treated wood fibers were placed in a glass mold having the dimensions of 80mm × 25mm × 1mm, and heated at 60 ℃ for 8 hours to prepare a PMMA transparent composite.
Tests prove that the light transmittance of the PMMA transparent composite material prepared by the embodiment reaches 92 percent, and is close to that of PMMA (the light transmittance of PMMA is 95 percent); haze 56%; the elastic modulus is 2.2 GPa (the elastic modulus of PMMA is 1.8 GPa); the tensile strength was 46.8 MPa (PMMA tensile strength was 41.4 MPa).
Example 2
This example differs from example 1 only in that: in step (7), the treated wood fibers were placed in a glass mold having dimensions of 80mm × 25mm × 5 mm.
Through tests, the light transmittance of the PMMA transparent composite material prepared by the embodiment reaches 83%; haze 72%; the elastic modulus is 2.2 GPa; the tensile strength was 46.8 MPa.
Example 3
This example differs from example 1 only in that: in step (7), the treated wood fibers were placed in a glass mold having dimensions of 300mm × 300mm × 10 mm.
Through tests, the light transmittance of the PMMA transparent composite material prepared by the embodiment reaches 68 percent; haze 76%; the elastic modulus is 2.2 GPa; the tensile strength was 46.8 MPa.
In summary, the method for reinforcing the polymethyl methacrylate by using the cellulose has good transmittance and certain haze, can be used in specific places needing privacy protection, simultaneously improves the mechanical strength of the organic glass produced by using MMA as a raw material, has important significance for the preparation of large-size PMMA transparent composite materials, and the produced PMMA transparent composite materials are not limited by size.
Example 4
A method of cellulose reinforced polymethylmethacrylate comprising the steps of:
s01, smashing the wood blocks into wood particles; the diameter of the crushed wood particles is about 3-5 mm;
s02, wherein the mass fraction of NaOH is 10 percent and Na is2SO3The mass fraction of the wood particles is 5 percent, the wood particles are dissolved in distilled water to prepare delignification solution, the wood particles are placed in the delignification solution and continuously boiled for 10 hours, the mass of the wood particles is 30 percent of that of the delignification solution, and then the wood particles are washed by distilled water to remove impurities, so that wood particles I are obtained;
s03, placing the wood particles I in H with the mass fraction of 30%2O2Heating to boil, wherein the wood particles I have a mass of H2O2When all the wood particles I are white, stirring the wood particles I into fibers, and performing suction filtration for four times by using distilled water to prepare delignified wood fibers;
s04, prepolymerizing MMA solution by using azobisisobutyronitrile as an initiator at 70 ℃ until the solution is in a glycerol state; the addition amount of azobisisobutyronitrile is 0.5 percent of the mass of the prepolymerization MMA solution; after the prepolymerization is finished, quickly transferring the prepolymerization solution into an ice water bath to cool to room temperature to terminate the reaction; soaking the delignified wood fibers in a pre-polymerized MMA solution, and permeating for 12 minutes under vacuum pressure to fully impregnate the delignified wood fibers with the pre-polymerized MMA solution;
s05, placing the fully impregnated wood fiber in a glass mold of any size, and heating at 50 ℃ for 15h to prepare the PMMA transparent composite material.
In the embodiment, lignin with poor mechanical strength and light transmittance in wood is removed, cellulose with good mechanical strength is kept to be mixed with MMA to prepare the polymethyl methacrylate (PMMA) transparent composite material, when the MMA is used for preparing organic glass, the original transmittance is maintained, meanwhile, the cellulose has certain haze in the prepared glass, the composite material is suitable for occasions where privacy is protected, and the high elasticity of the cellulose also plays a role in enhancing the mechanical strength of the glass.
Example 5
A method of cellulose reinforced polymethylmethacrylate comprising the steps of:
s01, smashing the wood blocks into wood particles; the diameter of the crushed wood particles is about 3-5 mm;
s02, wherein the mass fraction of NaOH is 10 percent and Na is2SO3The mass fraction of the wood particles is 5 percent, the wood particles are dissolved in distilled water to prepare delignification solution, the wood particles are placed in the delignification solution and continuously boiled for 6 hours, the mass of the wood particles is 20 percent of that of the delignification solution, and then the wood particles are washed by distilled water to remove impurities, so that wood particles I are obtained;
s03, placing the wood particles I in H with the mass fraction of 30%2O2Heating to boil, wherein the wood particles I have a mass of H2O2When all the wood particles I are white, stirring the wood particles I into fibers, and performing suction filtration for four times by using distilled water to prepare delignified wood fibers;
s04, prepolymerizing MMA solution by using azobisisobutyronitrile as an initiator at 75 ℃ until the solution is in a glycerol state; the addition amount of azobisisobutyronitrile is 0.4 percent of the mass of the prepolymerization MMA solution; after the prepolymerization is finished, quickly transferring the prepolymerization solution into an ice water bath to cool to room temperature to terminate the reaction; soaking the delignified wood fibers in a prepolymerization MMA solution, and permeating for 15 minutes under vacuum pressure to ensure that the delignified wood fibers are fully impregnated by the prepolymerization MMA solution;
s05, placing the fully impregnated wood fiber in a glass mold of any size, and heating at 70 ℃ for 6h to prepare the PMMA transparent composite material.
In the embodiment, lignin with poor mechanical strength and light transmittance in wood is removed, cellulose with good mechanical strength is kept to be mixed with MMA to prepare the polymethyl methacrylate (PMMA) transparent composite material, when the MMA is used for preparing organic glass, the original transmittance is maintained, meanwhile, the cellulose has certain haze in the prepared glass, the composite material is suitable for occasions where privacy is protected, and the high elasticity of the cellulose also plays a role in enhancing the mechanical strength of the glass.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (8)
1. A method of cellulose reinforced polymethylmethacrylate, characterized by: the method comprises the following steps:
s01, smashing the wood blocks into wood particles;
s02, preparing a delignification solution, placing wood particles in the delignification solution, continuously boiling for more than 4 hours, and then washing with distilled water to remove impurities to obtain wood particles I;
s03, placing the wood particles I in H with the mass fraction of 30%2O2Boiling while neutralizing, wherein the quality of wood particles I is not higher than H2O230% of the mass, when all the wood particles I are white, stirring the wood particles I into fibers, and performing suction filtration for at least three times by using distilled water to prepare delignified wood fibers;
s04, soaking the delignified wood fibers in the pre-polymerized MMA solution, and permeating the pre-polymerized MMA solution for at least 10 minutes under vacuum pressure to fully impregnate the delignified wood fibers;
s05, placing the fully impregnated wood fibers in glass molds with different specifications and sizes, and heating for more than 6 hours at 50-70 ℃ to prepare the PMMA transparent composite material;
the preparation method of the delignification solution in the S02 comprises the following steps: NaOH 10% by weight, Na2SO3The mass fraction of the active component is 5 percent, and the active component is prepared by dissolving the active component in distilled water.
2. The method of claim 1, wherein the cellulose-reinforced polymethylmethacrylate comprises: the diameter of the crushed wood particles in S01 is 3-5 mm.
3. The method of claim 1, wherein the cellulose-reinforced polymethylmethacrylate comprises: in S02, the mass of the wood particles is not higher than 30% of the mass of the delignifying solution.
4. The method of claim 1, wherein the cellulose-reinforced polymethylmethacrylate comprises: in S04, the mass of the delignified wood fibers is less than 30% of the mass of the prepolymerized MMA solution.
5. The method of claim 1, wherein the cellulose-reinforced polymethylmethacrylate comprises: the prepolymerized MMA solution in S04 contains an initiator.
6. The method of claim 5, wherein the cellulose-reinforced polymethylmethacrylate comprises: the initiator is azobisisobutyronitrile, and the addition amount of the azobisisobutyronitrile is 0.3-0.5% of the mass of the prepolymerization MMA solution.
7. The method of claim 6, wherein the cellulose-reinforced polymethylmethacrylate comprises: and (3) prepolymerizing the MMA solution for prepolymerization at 70-80 ℃ under the action of azobisisobutyronitrile until the solution is in a glycerol state, and after the prepolymerization is finished, quickly transferring the prepolymerized solution into an ice water bath to cool to room temperature to terminate the reaction.
8. The method of claim 1, wherein the cellulose-reinforced polymethylmethacrylate comprises: the refractive index of the PMMA transparent composite material is matched with that of the cellulose.
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| CN111300583A (en) * | 2020-02-28 | 2020-06-19 | 南通大学 | Method for manufacturing wooden light-emitting lampshade |
| CN112078217A (en) * | 2020-09-02 | 2020-12-15 | 中国林业科学研究院林业新技术研究所 | Preparation method of wood reinforced thermoplastic resin-based environment-friendly formaldehyde-free composite material |
| CN112080109B (en) * | 2020-09-02 | 2022-11-01 | 中国林业科学研究院林业新技术研究所 | Preparation method of multidimensional special-shaped high-transparency high-scattering environment-friendly formaldehyde-free wood-based composite material |
| CN112574577B (en) * | 2020-12-14 | 2022-05-20 | 湖南福森竹木科技有限公司 | Nano-material wood veneer |
| CN114685976B (en) * | 2022-04-27 | 2023-10-24 | 苏州博利迈新材料科技有限公司 | High-toughness conductive nylon material and preparation method thereof |
| CN115075042B (en) * | 2022-07-12 | 2023-08-15 | 大湾区大学(筹) | Lignocellulose-based transparent plastic substitute product, manufacturing method and production system thereof |
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| CN106243391A (en) * | 2016-08-05 | 2016-12-21 | 南京林业大学 | The preparation method of transparent timber |
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| WO1999024174A1 (en) * | 1997-11-10 | 1999-05-20 | Katoot Mohammad W | Method for modifying the surface of an object |
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