CN111647172B - Modification method of rice hull powder, modified rice hull powder and composite material - Google Patents
Modification method of rice hull powder, modified rice hull powder and composite material Download PDFInfo
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Abstract
The invention discloses a rice hull powder modification method, modified rice hull powder and a composite material, wherein the rice hull powder modification method comprises the following steps: s1, preparing nano-silver modified rice hull powder; s2, preparing polydopamine-nano silver coated rice hull powder; s3, modifying the polydopamine-nano silver coated rice hull powder by using a modified epoxy emulsion to obtain modified rice hull powder. The composite material prepared by blending the modified rice hull powder and the melamine resin has excellent hydrophobic property and antibacterial property, good mechanical property, high appearance quality, good sanitation and strong durability, and is suitable for being widely applied to the field of tableware manufacturing.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a rice hull powder modification method, modified rice hull powder and a composite material.
Background
With more and more attention paid to ecological environment, the degradability and recyclability of materials become the key points of attention of people. The rice hull powder as a natural lignocellulose material has the advantages of light weight, high strength, degradability, environmental friendliness and the like, is a recyclable natural green material, and is widely applied to the manufacture of green environment-friendly tableware. These tableware are usually made by mixing rice hull powder as a filler with a raw material such as resin and molding. However, the rice hull powder has hydrophilicity and high water absorption rate, is easy to absorb water in the air to cause deformation and cracking, influences the durability of tableware, is also affected with damp to cause bacterial breeding, and seriously influences the sanitary performance of the tableware. Therefore, it is an important research topic to improve the hydrophobicity and antibacterial property of rice hull powder and keep the excellent mechanical property.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a rice hull powder modification method, modified rice hull powder and a composite material.
The invention provides a method for modifying rice hull powder, which comprises the following steps:
s1, preparing nano-silver modified rice hull powder;
s2, preparing polydopamine-nano silver coated rice hull powder;
s3, modifying the polydopamine-nano silver coated rice hull powder by using a modified epoxy emulsion to obtain modified rice hull powder.
Preferably, the method for modifying rice hull powder comprises the following steps:
s1, adding the rice hull powder into a silver nitrate solution, uniformly mixing, then slowly dropwise adding an ascorbic acid solution, stirring for reaction, filtering, washing and drying to obtain nano-silver modified rice hull powder;
s2, dipping the nano-silver modified rice hull powder obtained in the step S1 in a dopamine hydrochloride solution, washing and drying to obtain poly-dopamine-nano-silver coated rice hull powder;
s3, uniformly spraying the modified epoxy emulsion into the polydopamine-nano silver coated rice hull powder, and drying to obtain the modified rice hull powder, wherein the modified epoxy emulsion is obtained by mixing water-based epoxy emulsion, nano silicon dioxide and nano titanium dioxide.
Preferably, the weight ratio of the rice hull powder to the silver nitrate solution is (0.05-0.1): 1, the concentration of the silver nitrate solution is 1.5-2.5mmol/L, the concentration of the ascorbic acid solution is 10-15mmol/L, and the volume ratio of the silver nitrate solution to the ascorbic acid solution is (0.8-1.2): 1.
preferably, in the step S1, the reaction temperature is 25-45 ℃ and the reaction time is 6-12 h.
Preferably, the concentration of the dopamine hydrochloride solution is 2-5g/L, and the dopamine hydrochloride solution is preferably prepared by dissolving dopamine hydrochloride in a Tris-HCl solution with the pH of 8.5.
Preferably, the weight ratio of the nano-silver modified rice hull powder to the dopamine hydrochloride solution is (0.1-0.2): 1.
preferably, in the step S2, the temperature of the dipping treatment is 25-30 ℃ and the time is 12-24 h.
Preferably, the weight ratio of the modified epoxy emulsion to the polydopamine-nano silver coated rice hull powder is (0.05-0.1): 1, in the modified epoxy emulsion, the weight ratio of the water-based epoxy emulsion to the nano silicon dioxide to the nano titanium dioxide is 1: (0.01-0.02): (0.01-0.03), the solid content of the aqueous epoxy emulsion is 10-30%, the particle size of the nano-silica is 100-200nm, and the particle size of the nano-titania is 30-50 nm.
A modified rice hull powder is prepared by the modification method of the rice hull powder.
A composite material containing modified rice hull powder comprises the following raw materials in parts by weight:
70-90 parts of melamine formaldehyde resin, 70-90 parts of modified rice hull powder, 0.1-1 part of curing agent and 0-2 parts of auxiliary agent.
A preparation method of a composite material containing modified rice hull powder comprises the following steps:
s1, weighing the raw materials according to the weight, mixing and stirring the melamine formaldehyde resin, the modified rice hull powder and the auxiliary agent uniformly, and then drying until the water content is less than or equal to 10%;
s2, mixing the material obtained in the step S1 with a curing agent, and then ball-milling for 6-10h to obtain the material.
Preferably, the curing agent is ethanolamine sulfate.
Preferably, the auxiliary agent comprises the following raw materials in parts by weight: 0.2-0.5 part of antioxidant, 0.2-0.5 part of coupling agent and 0.2-1 part of colorant.
Preferably, the antioxidant is one or a mixture of several of antioxidant 168, antioxidant 1076 and antioxidant DLTP; the coupling agent is one or a mixture of more of silane coupling agents KH550, KH560 and KH 570.
Preferably, the preparation method of the melamine formaldehyde resin comprises the following steps:
adding 100-120 parts by weight of formaldehyde solution with the concentration of 37% into a reactor, adjusting the pH to 9.3-9.5 by using NaOH solution, then heating to 35 ℃, stirring for 0.5-1h until the pH is stable, and then adding 30-40 parts by weight of melamine to react for 2-3h at 90-95 ℃ to obtain the melamine formaldehyde-formaldehyde resin.
The invention has the following beneficial effects:
the method comprises the steps of firstly using silver nitrate as a precursor, using ascorbic acid as a reducing agent, preparing rice hull powder with nano-silver loaded on the surface by an in-situ reduction method, then soaking the rice hull powder in a dopamine hydrochloride solution, forming a poly-dopamine crosslinking layer on the surface of the rice hull powder by utilizing the self-polymerization-crosslinking reaction of dopamine in water to obtain poly-dopamine-nano-silver coated rice hull powder, finally spraying aqueous epoxy emulsion modified by nano-silica and nano-titanium dioxide on the surface of the poly-dopamine-nano-silver coated rice hull powder, and utilizing the affinity of the poly-dopamine to epoxy resin to firmly attach the epoxy resin to the surface of the poly-dopamine-nano-silver coated rice hull powder to form a nano-silica-nano-titanium dioxide-epoxy composite layer. According to the modification method, on one hand, composite layers formed by nano silicon dioxide, nano titanium dioxide and epoxy resin with different particle sizes have certain roughness and water resistance, and the nano silver coating layer is combined, so that the coating layer on the surface of the rice hull powder has good density and certain roughness, a better hydrophobic effect is achieved, and the water resistance of the modified rice hull powder is greatly improved. The modified rice hull powder prepared by the invention is used as a filler, has excellent antibacterial property and water resistance, can introduce an epoxy group on the surface, greatly improves the compatibility with melamine resin, and a composite material prepared by blending the modified rice hull powder with the melamine resin has excellent hydrophobic property and antibacterial property, has good mechanical property, high appearance quality, good sanitation and strong durability, and is suitable for being widely applied to the field of tableware manufacturing.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A method for modifying rice hull powder comprises the following steps:
s1, adding the rice hull powder into a silver nitrate solution with the concentration of 1.5mmol/L, uniformly mixing, then slowly dropwise adding an ascorbic acid solution with the concentration of 10mmol/L, stirring and reacting for 6 hours at 25 ℃, filtering, washing and drying to obtain the nano-silver modified rice hull powder, wherein the weight ratio of the rice hull powder to the silver nitrate solution is 0.05: 1, the volume ratio of the silver nitrate solution to the ascorbic acid solution is 0.8: 1;
s2, dipping the nano-silver modified rice hull powder obtained in the step S1 in a dopamine hydrochloride solution with the concentration of 2g/L at 25 ℃ for 12 hours, washing and drying to obtain poly-dopamine-nano-silver coated rice hull powder, wherein the weight ratio of the nano-silver modified rice hull powder to the dopamine hydrochloride solution is 0.1: 1;
s3, uniformly spraying the modified epoxy emulsion into the polydopamine-nano silver coated rice hull powder, and drying to obtain the modified rice hull powder, wherein the modified epoxy emulsion comprises 10% of water-based epoxy emulsion, 100-200nm of nano-silica and 30-50nm of nano-titanium dioxide according to the weight ratio of 1: 0.01: 0.01, wherein the weight ratio of the modified epoxy emulsion to the polydopamine-nano silver coated rice hull powder is 0.05: 1.
a composite material containing modified rice hull powder comprises the following raw materials in parts by weight:
70 parts of melamine formaldehyde resin, 90 parts of modified rice hull powder, 0.1 part of ethanolamine sulfate, 1680.2 parts of antioxidant, KH 5500.2 parts of silane coupling agent and 0.2 part of colorant.
The preparation method of the composite material containing the modified rice hull powder comprises the following steps:
s1, weighing the raw materials according to the weight, mixing and stirring the melamine formaldehyde resin, the modified rice hull powder, the antioxidant 168, the silane coupling agent KH550 and the colorant uniformly, and then drying until the water content is less than or equal to 10%;
s2, mixing the material obtained in the step S1 with ethanolamine sulfate, and then ball-milling for 6 hours to obtain the product.
Example 2
A method for modifying rice hull powder comprises the following steps:
s1, adding the rice hull powder into a silver nitrate solution with the concentration of 2.5mmol/L, uniformly mixing, then slowly dropwise adding an ascorbic acid solution with the concentration of 15mmol/L, stirring and reacting at 45 ℃ for 12 hours, filtering, washing and drying to obtain the nano-silver modified rice hull powder, wherein the weight ratio of the rice hull powder to the silver nitrate solution is 0.1: 1, the volume ratio of the silver nitrate solution to the ascorbic acid solution is 1.2: 1;
s2, dipping the nano-silver modified rice hull powder obtained in the step S1 in a dopamine hydrochloride solution with the concentration of 5g/L for 24 hours at 30 ℃, washing and drying to obtain poly-dopamine-nano-silver coated rice hull powder, wherein the weight ratio of the nano-silver modified rice hull powder to the dopamine hydrochloride solution is 0.2: 1;
s3, uniformly spraying the modified epoxy emulsion into the polydopamine-nano silver coated rice hull powder, and drying to obtain the modified rice hull powder, wherein the modified epoxy emulsion comprises 30% of water-based epoxy emulsion, 100-200nm nano-silica and 30-50nm nano-titania in a weight ratio of 1: 0.02: 0.03, wherein the weight ratio of the modified epoxy emulsion to the polydopamine-nano silver coated rice hull powder is 0.1: 1.
a composite material containing modified rice hull powder comprises the following raw materials in parts by weight:
90 parts of melamine formaldehyde resin, 70 parts of modified rice hull powder and 1 part of ethanolamine sulfate.
The preparation method of the composite material containing the modified rice hull powder comprises the following steps:
s1, weighing the raw materials according to the weight, mixing and stirring the melamine formaldehyde resin and the modified rice hull powder uniformly, and then drying until the water content is less than or equal to 10%;
s2, mixing the material obtained in the step S1 with ethanolamine sulfate, and then ball-milling for 10 hours to obtain the product.
Example 3
A method for modifying rice hull powder comprises the following steps:
s1, adding the rice hull powder into a silver nitrate solution with the concentration of 2mmol/L, uniformly mixing, then slowly dropwise adding an ascorbic acid solution with the concentration of 12mmol/L, stirring and reacting at 30 ℃ for 10 hours, filtering, washing and drying to obtain the nano-silver modified rice hull powder, wherein the weight ratio of the rice hull powder to the silver nitrate solution is 0.08: 1, the volume ratio of the silver nitrate solution to the ascorbic acid solution is 1: 1;
s2, dipping the nano-silver modified rice hull powder obtained in the step S1 in a dopamine hydrochloride solution with the concentration of 3g/L at 28 ℃ for 20 hours, washing and drying to obtain poly-dopamine-nano-silver coated rice hull powder, wherein the weight ratio of the nano-silver modified rice hull powder to the dopamine hydrochloride solution is 0.15: 1;
s3, uniformly spraying the modified epoxy emulsion into the polydopamine-nano silver coated rice hull powder, and drying to obtain the modified rice hull powder, wherein the modified epoxy emulsion comprises 20% of water-based epoxy emulsion, 100-200nm nano-silica and 30-50nm nano-titania in a weight ratio of 1: 0.015: 0.025, and the weight ratio of the modified epoxy emulsion to the polydopamine-nano silver coated rice hull powder is 0.08: 1.
a composite material containing modified rice hull powder comprises the following raw materials in parts by weight:
80 parts of melamine formaldehyde resin, 80 parts of modified rice hull powder, 0.5 part of ethanolamine sulfate, 1680.2 parts of antioxidant, 10760.1 parts of antioxidant, KH 5700.3 parts of silane coupling agent and 0.5 part of colorant.
The preparation method of the composite material containing the modified rice hull powder comprises the following steps:
s1, weighing the raw materials according to the weight, mixing and stirring the melamine formaldehyde resin, the modified rice hull powder, the antioxidant 168, the antioxidant 1076, the silane coupling agent KH570 and the colorant uniformly, and then drying until the water content is less than or equal to 10%;
s2, mixing the material obtained in the step S1 with ethanolamine sulfate, and then ball-milling for 8 hours to obtain the product.
Comparative example 1
A method for modifying rice hull powder comprises the following steps:
s1, dipping the rice hull powder in a dopamine hydrochloride solution with the concentration of 3g/L for 20h at 28 ℃, washing and drying to obtain polydopamine-coated rice hull powder, wherein the weight ratio of the rice hull powder to the dopamine hydrochloride solution is 0.15: 1;
s2, uniformly spraying the modified epoxy emulsion into the polydopamine-coated rice hull powder, and drying to obtain the modified rice hull powder, wherein the modified epoxy emulsion comprises 20% of water-based epoxy emulsion, 100-200nm nano-silica and 30-50nm nano-titania in a weight ratio of 1: 0.015: 0.025, wherein the weight ratio of the modified epoxy emulsion to the polydopamine-coated rice hull powder is 0.08: 1.
a composite material containing modified rice hull powder comprises the following raw materials in parts by weight:
80 parts of melamine formaldehyde resin, 80 parts of modified rice hull powder, 0.5 part of ethanolamine sulfate, 1680.2 parts of antioxidant, 10760.1 parts of antioxidant, KH 5700.3 parts of silane coupling agent and 0.5 part of colorant.
The preparation method of the composite material containing the modified rice hull powder comprises the following steps:
s1, weighing the raw materials according to the weight, mixing and stirring the melamine formaldehyde resin, the modified rice hull powder, the antioxidant 168, the antioxidant 1076, the silane coupling agent KH570 and the colorant uniformly, and then drying until the water content is less than or equal to 10%;
s2, mixing the material obtained in the step S1 with ethanolamine sulfate, and then ball-milling for 8 hours to obtain the product.
Comparative example 2
A method for modifying rice hull powder comprises the following steps:
s1, adding the rice hull powder into a silver nitrate solution with the concentration of 2mmol/L, uniformly mixing, then slowly dropwise adding an ascorbic acid solution with the concentration of 12mmol/L, stirring and reacting at 30 ℃ for 10 hours, filtering, washing and drying to obtain the nano-silver modified rice hull powder, wherein the weight ratio of the rice hull powder to the silver nitrate solution is 0.08: 1, the volume ratio of the silver nitrate solution to the ascorbic acid solution is 1: 1;
s2, uniformly spraying the modified epoxy emulsion into the nano-silver modified rice hull powder, and drying to obtain the modified rice hull powder, wherein the modified epoxy emulsion comprises 20% of water-based epoxy emulsion, 100-200nm of nano-silica and 30-50nm of nano-titania according to the weight ratio of 1: 0.015: 0.025, and the weight ratio of the modified epoxy emulsion to the nano-silver modified rice hull powder is 0.08: 1.
a composite material containing modified rice hull powder comprises the following raw materials in parts by weight:
80 parts of melamine formaldehyde resin, 80 parts of modified rice hull powder, 0.5 part of ethanolamine sulfate, 1680.2 parts of antioxidant, 10760.1 parts of antioxidant, KH 5700.3 parts of silane coupling agent and 0.5 part of colorant.
The preparation method of the composite material containing the modified rice hull powder comprises the following steps:
s1, weighing the raw materials according to the weight, mixing and stirring the melamine formaldehyde resin, the modified rice hull powder, the antioxidant 168, the antioxidant 1076, the silane coupling agent KH570 and the colorant uniformly, and then drying until the water content is less than or equal to 10%;
s2, mixing the material obtained in the step S1 with ethanolamine sulfate, and then ball-milling for 8 hours to obtain the product.
Comparative example 3
A method for modifying rice hull powder comprises the following steps:
s1, adding the rice hull powder into a silver nitrate solution with the concentration of 2mmol/L, uniformly mixing, then slowly dropwise adding an ascorbic acid solution with the concentration of 12mmol/L, stirring and reacting at 30 ℃ for 10 hours, filtering, washing and drying to obtain the nano-silver modified rice hull powder, wherein the weight ratio of the rice hull powder to the silver nitrate solution is 0.08: 1, the volume ratio of the silver nitrate solution to the ascorbic acid solution is 1: 1;
s2, dipping the nano-silver modified rice hull powder obtained in the step S1 in a dopamine hydrochloride solution with the concentration of 3g/L at 28 ℃ for 20 hours, washing and drying to obtain the modified rice hull powder, wherein the weight ratio of the nano-silver modified rice hull powder to the dopamine hydrochloride solution is 0.15: 1.
a composite material containing modified rice hull powder comprises the following raw materials in parts by weight:
80 parts of melamine formaldehyde resin, 80 parts of modified rice hull powder, 0.5 part of ethanolamine sulfate, 1680.2 parts of antioxidant, 10760.1 parts of antioxidant, KH 5700.3 parts of silane coupling agent and 0.5 part of colorant.
The composite material containing the modified rice hull powder comprises the following steps:
s1, weighing the raw materials according to the weight, mixing and stirring the melamine formaldehyde resin, the modified rice hull powder, the antioxidant 168, the antioxidant 1076, the silane coupling agent KH570 and the colorant uniformly, and then drying until the water content is less than or equal to 10%;
s2, mixing the material obtained in the step S1 with ethanolamine sulfate, and then ball-milling for 8 hours to obtain the product.
Test examples
The composite materials containing the modified rice hull powder obtained in examples 1 to 3 and comparative examples 1 to 3 were compression molded by a flat plate molding press, wherein the mold temperature was 160 ℃, the molding pressure was 35MPa, and the time was 100 seconds, and test specimens were prepared for performance testing. Wherein the test standard of bending performance is GB/T9341-5CFU/mL. The results are shown in table 1:
TABLE 1 results of Performance test of each sample
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A method for modifying rice hull powder is characterized by comprising the following steps:
s1, preparing nano-silver modified rice hull powder, which comprises the specific steps of adding the rice hull powder into a silver nitrate solution, uniformly mixing, then slowly dropwise adding an ascorbic acid solution, stirring for reaction, filtering, washing and drying to obtain the nano-silver modified rice hull powder;
s2, preparing poly-dopamine-nano-silver-coated rice hull powder, and specifically comprises the steps of dipping the nano-silver modified rice hull powder obtained in the step S1 in a dopamine hydrochloride solution, washing and drying to obtain the poly-dopamine-nano-silver-coated rice hull powder;
s3, carrying out modification treatment on the polydopamine-nano silver coated rice hull powder by using a modified epoxy emulsion to obtain the modified rice hull powder, wherein the specific steps are uniformly spraying the modified epoxy emulsion into the polydopamine-nano silver coated rice hull powder, and drying to obtain the modified rice hull powder, wherein the modified epoxy emulsion is obtained by mixing a water-based epoxy emulsion, nano silicon dioxide and nano titanium dioxide.
2. A method for modifying rice hull powder according to claim 1, characterized in that the weight ratio of said rice hull powder to silver nitrate solution is (0.05-0.1): 1, the concentration of the silver nitrate solution is 1.5-2.5mmol/L, the concentration of the ascorbic acid solution is 10-15mmol/L, and the volume ratio of the silver nitrate solution to the ascorbic acid solution is (0.8-1.2): 1.
3. a method for modifying rice hull powder according to claim 1, wherein in said step S1, the reaction temperature is 25-45 ℃ and the reaction time is 6-12 hours.
4. A method for modifying rice hull powder according to claim 1, wherein said dopamine hydrochloride solution has a concentration of 2-5g/L, and the weight ratio of said nano-silver modified rice hull powder to dopamine hydrochloride solution is (0.1-0.2): 1.
5. a method for modifying rice hull powder according to claim 1, wherein in said step S2, the temperature of the dipping treatment is 25 to 30 ℃ and the time is 12 to 24 hours.
6. A method for modifying rice hull powder according to claim 1, characterized in that the weight ratio of said modified epoxy emulsion to poly-dopamine-nanosilver-coated rice hull powder is (0.05-0.1): 1, in the modified epoxy emulsion, the weight ratio of the water-based epoxy emulsion to the nano silicon dioxide to the nano titanium dioxide is 1: (0.01-0.02): (0.01-0.03), the solid content of the aqueous epoxy emulsion is 10-30%, the particle size of the nano-silica is 100-200nm, and the particle size of the nano-titania is 30-50 nm.
7. A modified rice husk powder characterized by being obtained by the method for modifying rice husk powder according to any one of claims 1 to 6.
8. The composite material containing the modified rice hull powder is characterized by comprising the following raw materials in parts by weight:
70-90 parts of melamine formaldehyde resin, 70-90 parts of modified rice hull powder as claimed in claim 7, 0.1-1 part of curing agent and 0-2 parts of auxiliary agent.
9. A method for producing a composite material containing modified rice husk powder according to claim 8, comprising the steps of:
s1, weighing the raw materials according to the weight, mixing and stirring the melamine formaldehyde resin, the modified rice hull powder and the auxiliary agent uniformly, and then drying until the water content is less than or equal to 10%;
s2, mixing the material obtained in the step S1 with a curing agent, and then ball-milling for 6-10h to obtain the material.
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