CN110804265A - Preparation method of wheat straw and polyvinyl chloride based wood-plastic composite material - Google Patents
Preparation method of wheat straw and polyvinyl chloride based wood-plastic composite material Download PDFInfo
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- CN110804265A CN110804265A CN201911263169.5A CN201911263169A CN110804265A CN 110804265 A CN110804265 A CN 110804265A CN 201911263169 A CN201911263169 A CN 201911263169A CN 110804265 A CN110804265 A CN 110804265A
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- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
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Abstract
The invention discloses a preparation method of a wheat straw and polyvinyl chloride based wood-plastic composite material, which comprises the following steps: (1) crushing; (2) performing amination treatment on the wheat straw powder; (3) sequentially adding the aminated wheat straw powder, the resin microspheres and the polyvinyl chloride resin into an internal mixer for internal mixing treatment to obtain an internal mixed material; (4) mixing the banburying material obtained in the step (3) and triethyl citrate, adding into an injection molding machine, and performing injection molding to obtain the final product; the wood-plastic composite material prepared by the method has excellent tensile property and ageing resistance.
Description
Technical Field
The invention belongs to the technical field of wood-plastic composite materials, and particularly relates to a preparation method of a wheat straw and polyvinyl chloride based wood-plastic composite material.
Background
As a big agricultural country, the wheat straw resource yield of China is very rich, a large amount of wheat straws are generated every year, however, most of the existing measures for processing the large amount of wheat straws are to stack, bury or burn on the spot, not only a large amount of land resources are occupied, but also a large amount of carbon dioxide and dust generated by burning cause serious pollution to the ecological environment, and therefore, how to reasonably process the large amount of wheat straws is a technical problem to be solved at present.
The existing wood-plastic composite material has a large number of applications, particularly, the straw and polyvinyl chloride composite material has wide application, however, the existing straw and polyvinyl chloride composite material has relatively high aging speed, so that the service life of the composite material is short, and the application field of the composite material is greatly limited.
Disclosure of Invention
The invention is realized by the following technical scheme.
A preparation method of a wheat straw and polyvinyl chloride based wood-plastic composite material comprises the following steps:
(1) crushing: crushing wheat straws to obtain wheat straw powder;
(2) performing amination treatment on the wheat straw powder: carrying out oxidation treatment on the wheat straw powder obtained in the step (1) to obtain oxidized wheat straw powder, and then mixing the oxidized wheat straw powder with a solvent of 150-180 g: adding 400mL of the mixture into an ethylenediamine solution, adding a catalyst, heating to 80-85 ℃ in a water bath under the protection of inert atmosphere, preserving heat, stirring, reacting for 2 hours, filtering, washing to be neutral, and drying to constant weight to obtain aminated wheat straw powder;
(3) sequentially adding the aminated wheat straw powder obtained in the step (2), the resin microspheres and the polyvinyl chloride resin into an internal mixer according to the mass ratio of 30-35:4-6:55-60 for internal mixing treatment for 18-22min to obtain an internal mixed material;
(4) and (4) mixing the banburying material obtained in the step (3) and triethyl citrate according to the mass ratio of 20:1-1.5, adding into an injection molding machine, and performing injection molding at 178 ℃, thus obtaining the alloy.
The granularity of the wheat straw powder in the step (1) is 250 meshes.
The oxidation treatment in the step (2) comprises the following steps: mixing the wheat straw powder according to the mixing ratio of 100-110 g: adding 400mL of the mixture into hydrogen peroxide, heating to 60 ℃, stirring for reacting for 40min, filtering, naturally draining, and adding 50-60g of the mixture: adding 150mL of the solution into a sodium hypochlorite solution, heating to 55 ℃, stirring for reaction for 1 hour, then filtering, washing with clear water to be neutral, and drying to be constant weight.
The concentration of the hydrogen peroxide is 1.5 mol/L.
The concentration of the sodium hypochlorite solution is 1.0 mol/L.
The concentration of the ethylenediamine solution in the step (2) is 1.8 mol/L.
The catalyst in the step (2) is bis 2, 4-dichlorobenzoyl peroxide, and the addition amount of the cross-linking agent is 1.5% of the mass of the oxidized wheat straw powder.
And (3) the inert atmosphere in the step (2) is a nitrogen atmosphere.
The banburying temperature in the step (3) is 150-160 ℃.
The preparation method of the resin microsphere in the step (3) comprises the following steps: adding melamine and formaldehyde into a reaction kettle according to a molar ratio of 3:1, adding a formic acid solution with a mass fraction of 0.2 percent, which is 5 times of the mass of the melamine, heating to 100 ℃, keeping the temperature for reaction for 5 hours, then reducing the pressure, naturally cooling to room temperature to obtain a reaction product, washing the reaction product to be neutral by using clear water, and drying the reaction product to be constant weight.
According to the technical scheme, the beneficial effects of the invention are as follows:
the invention provides a preparation method of a wheat straw and polyvinyl chloride based wood-plastic composite material, the wood-plastic composite material prepared by the method has excellent tensile property and ageing resistance, the wheat straw powder is firstly oxidized, the surface activity of the wheat straw powder can be effectively improved, lignin can be oxidized, and the subsequent amination treatment can be better carried out, more amino groups are grafted on the surface of the wheat straw powder, the wheat straw powder subjected to the amination treatment can be combined with a macromolecular chain of polyvinyl chloride resin to form a stable chemical bond, so that the compatibility between the wheat straw and the polyvinyl chloride resin is greatly improved, the mechanical property of the wood-plastic composite material can be better improved, particularly, the surface chemical property of the wheat straw powder after the treatment tends to be more stable, the prepared wood-plastic composite material can better resist aging erosion and improve the aging resistance of the wood-plastic composite material, and the resin microspheres prepared by the invention can absorb ultraviolet energy in a certain wavelength range and convert the ultraviolet energy into heat energy, so that the absorption effect of polyvinyl chloride molecular chains on ultraviolet rays and the degradation reaction of polyvinyl chloride are weakened, and the aging resistance of the wood-plastic composite material is improved.
Drawings
FIG. 1 is a graph showing an aging test.
Detailed Description
The invention provides a preparation method of a wheat straw and polyvinyl chloride based wood-plastic composite material, and a person skilled in the art can use the content for reference and appropriately improve process parameters to realize the preparation method. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
A preparation method of a wheat straw and polyvinyl chloride based wood-plastic composite material comprises the following steps:
(1) crushing: crushing wheat straws to obtain wheat straw powder;
(2) performing amination treatment on the wheat straw powder: carrying out oxidation treatment on the wheat straw powder obtained in the step (1) to obtain oxidized wheat straw powder, and then mixing the oxidized wheat straw powder with a solvent of 150-180 g: 400mL of the amino group-containing ethylene diamine is added into an ethylene diamine solution, then a catalyst is added, under the protection of inert atmosphere, the mixture is heated in a water bath to 80-85 ℃, the mixture is subjected to heat preservation stirring reaction for 2 hours, then the reaction is carried out, the reaction is filtered, washed to be neutral and dried to constant weight, and the aminated wheat straw powder is obtained. Particularly, after treatment, the surface chemical property of the wheat straw powder tends to be more stable, so that the prepared wood-plastic composite material can better resist aging and erosion, and the aging resistance of the wood-plastic composite material is improved;
(3) sequentially adding the aminated wheat straw powder obtained in the step (2), the resin microspheres and the polyvinyl chloride resin into an internal mixer according to the mass ratio of 30-35:4-6:55-60 for internal mixing treatment for 18-22min to obtain an internal mixed material;
(4) and (4) mixing the banburying material obtained in the step (3) and triethyl citrate according to the mass ratio of 20:1-1.5, adding into an injection molding machine, and performing injection molding at 178 ℃, thus obtaining the alloy.
The granularity of the wheat straw powder in the step (1) is 250 meshes.
The oxidation treatment in the step (2) comprises the following steps: mixing the wheat straw powder according to the mixing ratio of 100-110 g: adding 400mL of the mixture into hydrogen peroxide, heating to 60 ℃, stirring for reacting for 40min, filtering, naturally draining, and adding 50-60g of the mixture: adding 150mL of the solution into a sodium hypochlorite solution, heating to 55 ℃, stirring for reaction for 1 hour, then filtering, washing with clear water to be neutral, and drying to be constant weight.
The concentration of the hydrogen peroxide is 1.5 mol/L.
The concentration of the sodium hypochlorite solution is 1.0 mol/L.
The concentration of the ethylenediamine solution in the step (2) is 1.8 mol/L.
The catalyst in the step (2) is bis 2, 4-dichlorobenzoyl peroxide, and the addition amount of the cross-linking agent is 1.5% of the mass of the oxidized wheat straw powder.
And (3) the inert atmosphere in the step (2) is a nitrogen atmosphere.
The banburying temperature in the step (3) is 150-160 ℃.
The preparation method of the resin microsphere in the step (3) comprises the following steps: adding melamine and formaldehyde into a reaction kettle according to a molar ratio of 3:1, adding a formic acid solution with a mass fraction of 0.2% and a mass which is 5 times of that of the melamine, heating to 100 ℃, carrying out heat preservation reaction for 5 hours, then carrying out depressurization, naturally cooling to room temperature to obtain a reaction product, washing to neutrality by using clear water, and drying to constant weight to obtain the resin microsphere.
For further understanding of the present application, the following embodiments are combined to specifically describe a method for preparing a wheat straw and polyvinyl chloride based wood-plastic composite material provided by the present application:
example 1
The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material comprises the following steps:
(1) crushing: crushing wheat straws, and sieving the crushed wheat straws with a 250-mesh sieve to obtain wheat straw powder;
(2) performing amination treatment on the wheat straw powder: carrying out oxidation treatment on the wheat straw powder obtained in the step (1) to obtain oxidized wheat straw powder, wherein the oxidation treatment comprises the following steps: mixing wheat straw powder according to the weight ratio of 100 g: adding 400mL of the mixture into hydrogen peroxide, heating to 60 ℃, stirring for reacting for 40min, filtering, naturally draining, and mixing according to the weight ratio of 50 g: adding 150mL of the solution into a sodium hypochlorite solution, heating to 55 ℃, stirring for reacting for 1 hour, filtering, washing with clear water to be neutral, drying to be constant weight, wherein the concentration of hydrogen peroxide is 1.5mol/L, the concentration of the sodium hypochlorite solution is 1.0mol/L, and then adding the oxidized wheat straw powder into the solution according to the weight ratio of 150 g: adding 400mL of the mixture into an ethylenediamine solution, wherein the concentration of the ethylenediamine solution is 1.8mol/L, adding a catalyst which is bis-2, 4-dichlorobenzoyl peroxide, and adding a cross-linking agent in an amount which is 1.5% of the mass of the oxidized wheat straw powder, heating the mixture in a water bath to 80 ℃ under the protection of nitrogen atmosphere, carrying out heat preservation stirring reaction for 2 hours, then carrying out filtration, washing to be neutral, and drying to constant weight to obtain aminated wheat straw powder;
(3) sequentially adding the aminated wheat straw powder obtained in the step (2), the resin microspheres and the polyvinyl chloride resin into an internal mixer according to the mass ratio of 30:4:55 for internal mixing for 18min at the internal mixing temperature of 150 ℃ to obtain an internal mixed material, wherein the preparation method of the resin microspheres comprises the following steps: adding melamine and formaldehyde into a reaction kettle according to a molar ratio of 3:1, adding a formic acid solution with a mass fraction of 0.2 percent, which is 5 times of the mass of the melamine, heating to 100 ℃, keeping the temperature for reaction for 5 hours, then reducing the pressure, naturally cooling to room temperature to obtain a reaction product, washing the reaction product to be neutral by using clear water, and drying the reaction product to be constant weight to obtain the melamine-formaldehyde resin;
(4) and (4) mixing the banburying material obtained in the step (3) and triethyl citrate according to a mass ratio of 20:1, adding into an injection molding machine, and performing injection molding at 178 ℃ to obtain the alloy.
Example 2
The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material comprises the following steps:
(1) crushing: crushing wheat straws, and sieving the crushed wheat straws with a 250-mesh sieve to obtain wheat straw powder;
(2) performing amination treatment on the wheat straw powder: carrying out oxidation treatment on the wheat straw powder obtained in the step (1) to obtain oxidized wheat straw powder, wherein the oxidation treatment comprises the following steps: mixing wheat straw powder according to the proportion of 110 g: adding 400mL of the mixture into hydrogen peroxide, heating to 60 ℃, stirring for reacting for 40min, filtering, naturally draining, and mixing according to the weight ratio of 60 g: adding 150mL of the solution into a sodium hypochlorite solution, heating to 55 ℃, stirring for reacting for 1 hour, filtering, washing with clear water to be neutral, drying to be constant weight, wherein the concentration of hydrogen peroxide is 1.5mol/L, the concentration of the sodium hypochlorite solution is 1.0mol/L, and then adding the oxidized wheat straw powder into the solution according to the ratio of 180 g: adding 400mL of the mixture into an ethylenediamine solution, wherein the concentration of the ethylenediamine solution is 1.8mol/L, adding a catalyst which is bis-2, 4-dichlorobenzoyl peroxide, and adding a cross-linking agent in an amount which is 1.5% of the mass of the oxidized wheat straw powder, heating the mixture in a water bath to 85 ℃ under the protection of nitrogen atmosphere, carrying out heat preservation stirring reaction for 2 hours, then carrying out filtration, washing to be neutral, and drying to constant weight to obtain aminated wheat straw powder;
(3) sequentially adding the aminated wheat straw powder obtained in the step (2), the resin microspheres and the polyvinyl chloride resin into an internal mixer according to the mass ratio of 35: 6: 60 for internal mixing for 22min at the internal mixing temperature of 160 ℃ to obtain an internal mixed material, wherein the preparation method of the resin microspheres comprises the following steps: adding melamine and formaldehyde into a reaction kettle according to a molar ratio of 3:1, adding a formic acid solution with a mass fraction of 0.2 percent, which is 5 times of the mass of the melamine, heating to 100 ℃, keeping the temperature for reaction for 5 hours, then reducing the pressure, naturally cooling to room temperature to obtain a reaction product, washing the reaction product to be neutral by using clear water, and drying the reaction product to be constant weight to obtain the melamine-formaldehyde resin;
(4) and (4) mixing the banburying material obtained in the step (3) and triethyl citrate according to the mass ratio of 20: 1.5, adding into an injection molding machine, and performing injection molding at 178 ℃ to obtain the alloy.
Example 3
The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material comprises the following steps:
(1) crushing: crushing wheat straws, and sieving the crushed wheat straws with a 250-mesh sieve to obtain wheat straw powder;
(2) performing amination treatment on the wheat straw powder: carrying out oxidation treatment on the wheat straw powder obtained in the step (1) to obtain oxidized wheat straw powder, wherein the oxidation treatment comprises the following steps: mixing wheat straw powder in a proportion of 105 g: adding 400mL of the mixture into hydrogen peroxide, heating to 60 ℃, stirring for reacting for 40min, filtering, naturally draining, and mixing according to the weight ratio of 56 g: adding 150mL of the solution into a sodium hypochlorite solution, heating to 55 ℃, stirring for reacting for 1 hour, filtering, washing with clear water to be neutral, drying to be constant weight, wherein the concentration of hydrogen peroxide is 1.5mol/L, the concentration of the sodium hypochlorite solution is 1.0mol/L, and then adding the oxidized wheat straw powder into the solution according to the weight ratio of 160 g: adding 400mL of the mixture into an ethylenediamine solution, wherein the concentration of the ethylenediamine solution is 1.8mol/L, adding a catalyst which is bis-2, 4-dichlorobenzoyl peroxide, and adding a cross-linking agent in an amount which is 1.5% of the mass of the oxidized wheat straw powder, heating the mixture in a water bath to 80-85 ℃ under the protection of nitrogen atmosphere, carrying out heat preservation stirring reaction for 2 hours, then carrying out filtration, washing to be neutral, and drying to constant weight to obtain the aminated wheat straw powder;
(3) sequentially adding the aminated wheat straw powder obtained in the step (2), the resin microspheres and the polyvinyl chloride resin into an internal mixer according to the mass ratio of 32:5:58 for internal mixing treatment for 20min, wherein the internal mixing temperature is 156 ℃, and the preparation method of the resin microspheres comprises the following steps: adding melamine and formaldehyde into a reaction kettle according to a molar ratio of 3:1, adding a formic acid solution with a mass fraction of 0.2 percent, which is 5 times of the mass of the melamine, heating to 100 ℃, keeping the temperature for reaction for 5 hours, then reducing the pressure, naturally cooling to room temperature to obtain a reaction product, washing the reaction product to be neutral by using clear water, and drying the reaction product to be constant weight to obtain the melamine-formaldehyde resin;
(4) and (4) mixing the banburying material obtained in the step (3) and triethyl citrate according to the mass ratio of 20:1.2, adding into an injection molding machine, and performing injection molding at 178 ℃ to obtain the alloy.
Tensile properties of specimens (100 mm. times.5 mm. times.20 mm) of the same specifications as in examples were examined (see ASTM D638-03);
TABLE 1
| Tensile strength/MPa | |
| Example 1 | 23.07 |
| Example 2 | 21.75 |
| Example 3 | 25.62 |
As can be seen from Table 1, the wood-plastic composite prepared by the method of the present invention has excellent tensile properties.
The sample of example 1 was subjected to aging test (according to GB/T164222-1999 standard, samples of examples and control groups were subjected to xenon lamp light source exposure test on a sample holder of a flash lamp aging resistant test chamber, the aging time was 25 days, and then the samples were taken out for testing, the test conditions were that a 6KW water-cooled xenon lamp was used, the working temperature was 50 + -1 deg.C, the blackboard temperature was 65 + -1 deg.C, the relative humidity of the working chamber was 60 + -2%, the rainfall cycle was 30min/100min (rainfall time/non-rainfall time), the light source radiation intensity was 600 + -10W/m:), as shown in FIG. 1;
the preparation method of the control group comprises the following steps:
(1) crushing: crushing wheat straws, and sieving the crushed wheat straws with a 250-mesh sieve to obtain wheat straw powder;
(2) sequentially adding wheat straw powder, resin microspheres and polyvinyl chloride resin into an internal mixer according to a mass ratio of 30:4:55 for internal mixing treatment for 18min, wherein the internal mixing temperature is 150 ℃, and the preparation method of the resin microspheres comprises the following steps: adding melamine and formaldehyde into a reaction kettle according to a molar ratio of 3:1, adding a formic acid solution with a mass fraction of 0.2 percent, which is 5 times of the mass of the melamine, heating to 100 ℃, keeping the temperature for reaction for 5 hours, then reducing the pressure, naturally cooling to room temperature to obtain a reaction product, washing the reaction product to be neutral by using clear water, and drying the reaction product to be constant weight to obtain the melamine-formaldehyde resin;
(3) and (3) mixing the banburying material obtained in the step (2) and triethyl citrate according to a mass ratio of 20:1, adding into an injection molding machine, and performing injection molding at 178 ℃ to obtain the alloy.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art should understand that they can make various changes, modifications, additions and substitutions within the spirit and scope of the present invention.
Claims (10)
1. A preparation method of a wheat straw and polyvinyl chloride based wood-plastic composite material is characterized by comprising the following steps:
(1) crushing: crushing wheat straws to obtain wheat straw powder;
(2) performing amination treatment on the wheat straw powder: carrying out oxidation treatment on the wheat straw powder obtained in the step (1) to obtain oxidized wheat straw powder, and then mixing the oxidized wheat straw powder with a solvent of 150-180 g: adding 400mL of the mixture into an ethylenediamine solution, adding a catalyst, heating to 80-85 ℃ in a water bath under the protection of inert atmosphere, preserving heat, stirring, reacting for 2 hours, filtering, washing to be neutral, and drying to constant weight to obtain aminated wheat straw powder;
(3) sequentially adding the aminated wheat straw powder obtained in the step (2), the resin microspheres and the polyvinyl chloride resin into an internal mixer according to the mass ratio of 30-35:4-6:55-60 for internal mixing treatment for 18-22min to obtain an internal mixed material;
(4) and (4) mixing the banburying material obtained in the step (3) and triethyl citrate according to the mass ratio of 20:1-1.5, adding into an injection molding machine, and performing injection molding to obtain the alloy.
2. The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material according to claim 1, wherein the particle size of the wheat straw powder in the step (1) is 250 meshes.
3. The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material according to claim 1, wherein the oxidation treatment in the step (2) is: mixing the wheat straw powder according to the mixing ratio of 100-110 g: adding 400mL of the mixture into hydrogen peroxide, heating to 60 ℃, stirring for reacting for 40min, filtering, naturally draining, and adding 50-60g of the mixture: adding 150mL of the solution into a sodium hypochlorite solution, heating to 55 ℃, stirring for reaction for 1 hour, then filtering, washing with clear water to be neutral, and drying to be constant weight.
4. The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material as claimed in claim 3, wherein the concentration of hydrogen peroxide is 1.5 mol/L.
5. The preparation method of the wheat straw and polyvinyl chloride-based wood-plastic composite material according to claim 3, wherein the concentration of the sodium hypochlorite solution is 1.0 mol/L.
6. The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material according to claim 1, wherein the concentration of the ethylenediamine solution in the step (2) is 1.8 mol/L.
7. The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material according to claim 1, wherein the catalyst in the step (2) is bis 2, 4-dichlorobenzoyl peroxide, and the addition amount of the cross-linking agent is 1.5% of the mass of the oxidized wheat straw powder.
8. The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material according to claim 1, wherein the inert atmosphere in the step (2) is a nitrogen atmosphere.
9. The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material as claimed in claim 1, wherein the banburying temperature in step (3) is 150-160 ℃.
10. The preparation method of the wheat straw and polyvinyl chloride based wood-plastic composite material according to claim 1, wherein the preparation method of the resin microspheres in the step (3) is as follows: adding melamine and formaldehyde into a reaction kettle according to a molar ratio of 3:1, adding a formic acid solution with a mass fraction of 0.2 percent, which is 5 times of the mass of the melamine, heating to 100 ℃, keeping the temperature for reaction for 5 hours, then reducing the pressure, naturally cooling to room temperature to obtain a reaction product, washing the reaction product to be neutral by using clear water, and drying the reaction product to be constant weight.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113429584A (en) * | 2021-06-24 | 2021-09-24 | 西北民族大学 | Wear-resistant wheat straw composite board and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113429584A (en) * | 2021-06-24 | 2021-09-24 | 西北民族大学 | Wear-resistant wheat straw composite board and preparation method thereof |
| CN113429584B (en) * | 2021-06-24 | 2022-07-05 | 西北民族大学 | Wear-resistant wheat straw composite board and preparation method thereof |
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Application publication date: 20200218 |