CN115160814A - Preparation method of wood-plastic composite material based on mechanochemical modified wood powder - Google Patents
Preparation method of wood-plastic composite material based on mechanochemical modified wood powder Download PDFInfo
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- CN115160814A CN115160814A CN202210949991.2A CN202210949991A CN115160814A CN 115160814 A CN115160814 A CN 115160814A CN 202210949991 A CN202210949991 A CN 202210949991A CN 115160814 A CN115160814 A CN 115160814A
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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
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H8/00—Macromolecular compounds derived from lignocellulosic 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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/20—Recycled plastic
Abstract
The invention discloses a preparation method of a wood-plastic composite material based on mechanochemical modified wood powder, which comprises the following steps: s1, preparing watered wood flour: mixing the weighed wood powder with water to obtain water-added wood powder with a certain water content; s2, preparing mechanochemical modified wood powder: adding the weighed wood flour with water and the active compound into a mixing device for mixing, and placing the mixture into a mechanochemical device for mechanochemical grafting modification to obtain mechanochemical modified wood flour; s3, preparing the wood-plastic composite material: weighing the mechanochemical modified wood powder, the regenerated thermoplastic plastic, the lubricant and the antioxidant, sequentially adding the weighed materials into a mixing device for premixing, plasticizing and granulating the obtained premix by using a double-screw extruder to obtain a wood-plastic composite material, and then processing and molding the composite material to obtain the wood-plastic composite product. The invention has the advantages that the interfacial compatibility of the wood-plastic composite material can be improved, so that the wood powder is more uniformly dispersed in the plastic matrix, and the mechanical property of the composite material is improved.
Description
Technical Field
The invention relates to the technical field of resource utilization of wastes, in particular to a preparation method of a wood-plastic composite material based on mechanochemical modified wood powder.
Background
The wood-plastic composite material is an environment-friendly composite material which is prepared by mixing thermoplastic plastics such as polyethylene, polypropylene, polyvinyl chloride and the like with more than 50% of wood flour, adding a certain amount of processing aids, and carrying out processes such as high-temperature extrusion or injection molding, compression molding and the like. The wood flour is a strong-polarity hydrophilic material, the interface compatibility with non-polar plastics is poor, a large amount of free water and bound water are contained in the wood flour, the wood flour is easy to absorb moisture from the environment, and the compatibility between the polar wood flour and the non-polar plastics can be further reduced by too high moisture in the wood flour, so that the mechanical property of the composite material is influenced. Meanwhile, too high water content in the wood powder affects the processing flowability of the material, so that the processing technology is difficult to control, and even foaming, performance deterioration and the like of the product are caused. Therefore, in the traditional wood-plastic composite material processing, wood powder needs to be dried firstly, and the drying equipment is expensive and has high energy consumption. Meanwhile, the wood powder and the plastic must be subjected to interface modification so as to improve the mechanical property of the wood-plastic composite material. Therefore, improving the interfacial compatibility of the wood-plastic composite material is a key step for preparing the wood-plastic composite material.
Disclosure of Invention
The invention aims to provide a preparation method of a wood-plastic composite material based on mechanochemical modified wood powder, which improves the interface compatibility of the wood-plastic composite material, so that the wood powder is more uniformly dispersed in a plastic matrix, and the mechanical property of the composite material is improved.
The technical purpose of the invention is realized by the following technical scheme:
a preparation method of wood-plastic composite material based on mechanochemical modified wood powder is characterized by comprising the following steps:
s1, preparing watered wood flour: weighing 90-100 parts of wood powder and 0-10 parts of water in parts by mass, and adding the weighed wood powder and the water into a closed container for mixing to obtain watered wood powder with a certain water content;
s2, preparing mechanochemical modified wood powder: weighing 90-98 parts of water-added wood powder and 2-10 parts of active compound reacting with hydroxyl according to the mass parts, adding the weighed water-added wood powder and the active compound into mixing equipment for mixing, putting the mixture into a mechanochemical device such as a millstone type mechanochemical reactor or a ball mill for mechanochemical grafting modification, and reacting for 0.5-4 hours to obtain mechanochemical modified wood powder;
s3, preparing the wood-plastic composite material: weighing 45-60 parts of mechanochemical modified wood powder, 35-50 parts of regenerated thermoplastic plastic, 1-5 parts of lubricant and 0.5-1 part of antioxidant according to the mass parts, wherein the total mass parts of the mechanochemical modified wood powder, the regenerated thermoplastic plastic, the lubricant and the antioxidant are 100 parts, sequentially adding the weighed mechanochemical modified wood powder, the weighed regenerated thermoplastic plastic, the lubricant and the antioxidant into mixing equipment for premixing to obtain a premix, plasticizing and granulating the premix by using a double-screw extruder to obtain a wood-plastic composite material, and then processing and molding the composite material to obtain the wood-plastic composite product.
Preferably, the wood flour in the S1 is one of poplar flour, camphor wood flour, wheat straw powder, rice straw powder and corn straw powder.
Preferably, in S1, the mixing temperature of the wood powder and the water is 20-80 ℃, and the mixing time is 1-10h.
Preferably, the compound having reactivity with hydroxyl in S2 is one of amide wax, maleic anhydride and ethylene oxide.
Preferably, the mixing temperature of the water-added wood flour and the active compound in the S2 is normal temperature, the mixing rotation speed is 500-3000 r/min, and the mixing time is 3-8 min.
Preferably, the recycled thermoplastic in S3 is one or more of recycled polyethylene, recycled polypropylene and recycled polyvinyl chloride.
Preferably, the lubricant in S3 is one or both of stearic acid and paraffin.
Preferably, the antioxidant in S3 is one or two of antioxidant 1010, antioxidant 1076 and antioxidant 168.
Preferably, in the S3, the premixing temperature of the mixing equipment is 20 to 90 ℃, the premixing rotating speed is 500 to 3000r/min, and the premixing time is 3 to 8min.
Preferably, in S3, the parameters of plasticizing and granulating the premix by using a twin-screw extruder are as follows: the temperature of the first area to the sixth area is 160 to 220 ℃, the head temperature is 160 to 180 ℃, the screw rotation speed is 15 to 45r/min, and the feeding speed is 5 to 15r/min.
In conclusion, the invention has the following beneficial effects:
1. according to the invention, the wood powder used in the method does not need to be dried, trace moisture is added, the moisture content in the wood powder is controlled, the wood powder with certain moisture content is obtained, the wood powder and an active compound which reacts with hydroxyl are subjected to mechanochemical grafting modification, the mechanochemical modified wood powder is obtained, finally, the mechanochemical modified wood powder is mixed with the regenerated thermoplastic, and the wood-plastic product is obtained through processes such as extrusion, mould pressing or injection molding.
2. After the wood flour is grafted and modified by the active compound, the active compound can serve as a bridge between the wood flour and the plastic, the interface bonding property of the wood flour and the plastic is improved, the wood flour is more uniformly dispersed in a plastic matrix, and the mechanical property of the composite material is improved. Compared with the unmodified wood-plastic composite material, the bending strength and the impact strength of the composite material are improved by more than 30% after the mechanochemical modified wood powder is added, and meanwhile, the wood-plastic composite material has good processing fluidity.
3. The wood-plastic composite material prepared by the invention has the advantages of low cost, simple process and excellent performance, and can be used in industries such as building materials, furniture, logistics packaging and the like.
Drawings
FIG. 1 is a structural formula of cellulose in wood flour;
FIG. 2 is an FTIR spectrum of mechanochemical modified wood flour and amide wax prepared in example 1 of the present invention.
Detailed Description
The following description will further describe the embodiments of the present invention with reference to the accompanying drawings, which are not intended to limit the present invention.
Example 1
S1, preparing the poplar wood powder
Weighing 99.5 parts of poplar powder and 0.5 part of water according to the mass parts, and hermetically mixing for 10 hours at 60 ℃ to obtain the poplar powder with water.
S2, preparing mechanochemical modified poplar powder
Weighing 95 parts of poplar powder added with water and 5 parts of amide wax according to the mass parts, adding the weighed poplar powder and the amide wax into a mixing device, and mixing for 3min at normal temperature at the rotating speed of 1000r/min; and (3) putting the mixture into a ball mill for mechanochemical grafting modification to obtain mechanochemical modified poplar powder, wherein the rotating speed of the ball mill is 350r/min, and the ball milling time is 1h.
S3, preparing the wood-plastic composite material
Weighing 55 parts of mechanochemical modified poplar powder, 40 parts of regenerated high-density polyethylene rHDPE,4.5 parts of stearic acid and 0.5 part of antioxidant 1010 in parts by mass, sequentially adding the weighed mechanochemical modified poplar powder, the weighed regenerated high-density polyethylene rHDPE, the weighed stearic acid and the antioxidant 1010 into a mixing device for premixing to obtain a premix, wherein the premixing parameters are as follows: plasticizing and granulating the premix by using a double-screw extruder at the normal temperature of 2000r/min for 5min to obtain a wood-plastic composite material, and then carrying out injection molding on the composite material to obtain a wood-plastic composite product, wherein the extrusion parameters are as follows: the temperature of the first zone is 180 ℃, the temperature of the second zone is 190 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 205 ℃, the temperature of the fifth zone is 190 ℃, the temperature of the sixth zone is 180 ℃, the temperature of the machine head is 170 ℃, the rotating speed of the screw is 25r/min, and the feeding speed is 5r/min; injection molding parameters: the temperature of a charging barrel is 180-210 ℃, the temperature of a nozzle is 205 ℃, the temperature of a die is 30 ℃, and the pressure maintaining and cooling time is 45s.
Example 2
S1, preparing water-added camphor wood powder
Weighing 99.5 parts of camphorwood powder and 0.5 part of water in parts by mass, and hermetically mixing for 5 hours at 60 ℃ to obtain the camphorwood powder added with water.
S2, preparing mechanochemical modified camphor wood powder
Weighing 95 parts of water-added camphor wood powder and 5 parts of maleic anhydride in parts by mass, and adding the weighed camphor wood powder and maleic anhydride into a mixing device to mix for 3min at normal temperature at the rotation speed of 1000r/min; and (3) putting the mixture into a millstone type mechanochemical reactor for mechanochemical grafting modification to obtain mechanochemical modified camphor wood powder, wherein the rotational speed of a millstone is 100r/min, and the milling time is 10min.
S3, preparing the wood-plastic composite material
Weighing 57 parts of mechanochemical modified camphorwood powder, 40 parts of regenerated polypropylene rPP,2.5 parts of stearic acid and 0.5 part of antioxidant 1010 in parts by mass, sequentially adding the weighed mechanochemical modified camphorwood powder, regenerated polypropylene rPP, stearic acid and antioxidant 1010 into a mixing device for premixing to obtain premix, wherein the premixing parameters are as follows: at normal temperature, the rotating speed is 1000r/min, the time is 5min, the premix is plasticized and granulated by a double-screw extruder to obtain a wood-plastic composite material, then the composite material is subjected to compression molding to obtain a wood-plastic composite product, and the extrusion parameters are as follows: the temperature of a first area is 180 ℃, the temperature of a second area is 190 ℃, the temperature of a third area is 200 ℃, the temperature of a fourth area is 205 ℃, the temperature of a fifth area is 190 ℃, the temperature of a sixth area is 180 ℃, the temperature of a machine head is 170 ℃, the rotating speed of a screw is 25r/min, and the feeding speed is 5r/min; molding parameters: hot pressing temperature is 180 to 210 ℃, pressure is 20MPa, hot pressing time is 10min, cold pressing temperature is 20 ℃, pressure is 10MPa, and cold pressing time is 10min.
Example 3
S1, preparing water-added rice straw powder
Weighing 98 parts of rice straw powder and 2 parts of water according to the mass parts, and hermetically mixing for 24 hours at 60 ℃ to obtain the added rice straw powder.
S2, preparing mechanochemical modified rice straw powder
Weighing 96 parts by mass of rice straw powder and 4 parts by mass of maleic anhydride, adding the weighed rice straw powder and maleic anhydride into a mixing device, and mixing for 3min at normal temperature and at the rotating speed of 1000r/min; and (3) putting the mixture into a ball mill for mechanochemical grafting modification to obtain mechanochemical modified rice straw powder, wherein the rotating speed of the ball mill is 350r/min, and the ball milling time is 1h.
S3, preparing the wood-plastic composite material
Weighing 55 parts of mechanochemical modified rice straw powder, 20 parts of regenerated polypropylene rPP,20 parts of regenerated polyethylene rPE,4.5 parts of paraffin and 0.5 part of antioxidant 1010 in parts by mass, and sequentially adding the weighed mechanochemical modified rice straw powder, the weighed regenerated polypropylene rPP, the weighed regenerated polyethylene rPE, the weighed paraffin and the weighed antioxidant 1010 into a mixing device for premixing to obtain the premix. Premixing parameters: plasticizing and granulating the premix by using a double-screw extruder at normal temperature at a rotating speed of 3000r/min for 5min to obtain a wood-plastic composite material, and then performing injection molding on the composite material to obtain a wood-plastic composite product, wherein the extrusion parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 180 ℃, the temperature of the third zone is 195 ℃, the temperature of the fourth zone is 195 ℃, the temperature of the fifth zone is 190 ℃, the temperature of the sixth zone is 190 ℃, the temperature of the machine head is 180 ℃, the rotating speed of the screw is 30r/min, and the feeding speed is 10r/min; injection molding parameters: the temperature of a charging barrel is 190 to 205 ℃, the temperature of a nozzle is 200 ℃, the temperature of a die is 30 ℃, and the pressure maintaining and cooling time is 60s.
Example 4
S1, preparing water-added wheat straw powder
Weighing 96 parts of wheat straw powder and 4 parts of water according to the mass parts, and hermetically mixing for 24 hours at the temperature of 60 ℃ to obtain the wheat straw powder added with water.
S2, preparing the mechanochemical modified wheat straw powder
Weighing 95 parts by mass of wheat straw powder and 5 parts by mass of ethylene oxide, and mixing the weighed wheat straw powder and ethylene oxide in a mixing device at normal temperature for 3min at the rotating speed of 1000r/min; and (3) putting the mixture into a ball mill for mechanochemical grafting modification to obtain mechanochemical modified wheat straw powder, wherein the rotating speed of the ball mill is 500r/min, and the ball milling time is 2 hours.
3. Preparing wood-plastic composite material
Weighing 60 parts of mechanochemical modified wheat straw powder, 20 parts of regenerated polyvinyl chloride rPVC,10 parts of regenerated polypropylene rPP,10 parts of regenerated polyethylene rPE,4.5 parts of stearic acid, 3 parts of paraffin and 0.5 part of antioxidant 1010, sequentially adding the weighed mechanochemical modified wheat straw powder, the regenerated polyvinyl chloride rPVC, the regenerated polypropylene rPP, the regenerated polyethylene rPE, dioctyl phthalate, tribasic lead, stearic acid, paraffin and the antioxidant 1010 into a mixing device for premixing to obtain a premix, wherein premixing parameters are as follows: the temperature is 80 ℃, the rotating speed is 2000r/min, the time is 8min, the premix is plasticized and granulated by a double-screw extruder to obtain a wood-plastic composite material, then the composite material is subjected to injection molding to obtain a wood-plastic composite product, and the extrusion parameters are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 165 ℃, the temperature of the third zone is 170 ℃, the temperature of the fourth zone is 175 ℃, the temperature of the fifth zone is 170 ℃, the temperature of the sixth zone is 165 ℃, the temperature of the machine head is 160 ℃, the rotating speed of the screw is 25r/min, and the feeding speed is 10r/min; injection molding parameters: the temperature of a charging barrel is 160 to 180 ℃, the temperature of a nozzle is 175 ℃, the temperature of a die is 30 ℃, and the pressure maintaining and cooling time is 50s.
Comparative example 1
Comparative example 1 differs from example 1 only in that the poplar powder and amide wax blend was not placed in a ball mill for mechanochemical graft modification.
Comparative example 2
Comparative example 2 is different from example 2 only in that the camphorwood flour and maleic anhydride mixture are not put into a millstone type mechanochemical reactor for mechanochemical grafting modification.
Comparative example 3
Comparative example 3 differs from example 3 only in that the rice straw powder and maleic anhydride mixture was not put into a ball mill for mechanochemical grafting modification.
Comparative example 4
Comparative example 4 differs from example 4 only in that the wheat straw powder and ethylene oxide mixture were not placed in a ball mill for mechanochemical graft modification.
The mechanical properties of the samples prepared in the above examples and comparative examples were compared to obtain the test data shown in table 1 below.
TABLE 1
| Sample(s) | Flexural Strength (MPa) | Impact strength of simple beam gap (kJ/square meter) |
| Example 1 | 32.1 | 3.2 |
| Comparative example 1 | 21.0 | 1.44 |
| Increased amplitude after modification | 53% | 122% |
| Example 2 | 35.1 | 2.5 |
| Comparative example 2 | 25.0 | 1.7 |
| Increased amplitude after modification | 40% | 47% |
| Example 3 | 52.3 | 3.5 |
| Comparative example 3 | 23.2 | 1.3 |
| Increased amplitude after modification | 125% | 169% |
| Example 4 | 37.5 | 2.8 |
| Comparative example 4 | 21.2 | 1.4 |
| Increased amplitude after modification | 77% | 100% |
According to the invention, a hydration layer can be formed on the surface of cellulose by mainly utilizing added trace moisture to regulate and control the moisture content in wood powder, the hydration layer can be used as a nano medium to destroy hydrogen bonds, shield secondary hydroxyl (C2 and C3) with low reaction activity on the cellulose, selectively expose primary hydroxyl (C6) with high reaction activity, further promote the grafting chemical reaction of the secondary hydroxyl and an active compound, improve the selective grafting modification activity of the wood powder, reduce energy consumption and save cost.
FIG. 2 is an FTIR spectrum of mechanochemical modified wood flour prepared in example 1 of the present invention, together with wood flour and amide wax, FTIR analysis showed that wood flour after mechanochemical modification was 3300cm -1 The peak of stretching vibration of the N-H appears, 1562cm -1 The bending vibration peak of N-H is shown, and the amide wax is provedThe amide wax can be used as a bridge between wood powder and plastic to improve the interfacial bonding property of the wood powder and the plastic, so that the wood powder is more uniformly dispersed in a plastic matrix, and the mechanical property of the composite material is improved. As can be seen from Table 1, compared with the unmodified wood-plastic composite material, the bending strength and the impact strength of the composite material are at least improved by more than 30% after the mechanochemical modified wood powder is added, and meanwhile, the wood-plastic composite material has good processing flowability.
While the invention has been described with reference to certain preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention.
Claims (10)
1. A preparation method of wood-plastic composite material based on mechanochemical modified wood powder is characterized by comprising the following steps:
s1, preparing watered wood flour: weighing 90-100 parts of wood powder and 0-10 parts of water according to the mass parts, adding the weighed wood powder and the water into a closed container, and mixing to obtain watered wood powder with a certain water content;
s2, preparing mechanochemical modified wood powder: weighing 90-98 parts of water-added wood powder and 2-10 parts of active compound reacting with hydroxyl according to the mass parts, adding the weighed water-added wood powder and the active compound into mixing equipment for mixing, putting the mixture into a mechanochemical device such as a millstone type mechanochemical reactor or a ball mill for mechanochemical grafting modification, and reacting for 0.5-4 hours to obtain mechanochemical modified wood powder;
s3, preparing the wood-plastic composite material: weighing 45 to 60 parts by mass of mechanochemical modified wood powder, 35 to 50 parts by mass of regenerated thermoplastic, 1 to 5 parts by mass of lubricant and 0.5 to 1 part by mass of antioxidant, wherein the total parts by mass of the weighed mechanochemical modified wood powder, the weighed regenerated thermoplastic, the lubricant and the antioxidant are 100 parts, sequentially adding the weighed mechanochemical modified wood powder, the weighed regenerated thermoplastic, the lubricant and the antioxidant into mixing equipment for premixing to obtain a premix, plasticizing and granulating the premix by using a double-screw extruder to obtain a wood-plastic composite material, and then processing and molding the composite material to obtain the wood-plastic composite product.
2. The preparation method of the wood-plastic composite material based on the mechanochemical modified wood flour as claimed in claim 1, characterized in that: the wood powder in the S1 is one of poplar powder, camphor wood powder, wheat straw powder, rice straw powder and corn straw powder.
3. The preparation method of the wood-plastic composite material based on mechanochemical modified wood powder according to claim 1, characterized in that: in the S1, the mixing temperature of the wood powder and the water is 20-80 ℃, and the mixing time is 1-10h.
4. The preparation method of the wood-plastic composite material based on the mechanochemical modified wood flour as claimed in claim 1, characterized in that: the compound which has reactivity with hydroxyl in S2 is one of amide wax, maleic anhydride and ethylene oxide.
5. The preparation method of the wood-plastic composite material based on the mechanochemical modified wood flour as claimed in claim 1, characterized in that: the mixing temperature of the water added wood flour and the active compound in the S2 is normal temperature, the mixing rotating speed is 500-3000 r/min, and the mixing time is 3-8 min.
6. The preparation method of the wood-plastic composite material based on the mechanochemical modified wood flour as claimed in claim 1, characterized in that: the regenerated thermoplastic plastic in S3 is one or more of regenerated polyethylene, regenerated polypropylene and regenerated polyvinyl chloride.
7. The preparation method of the wood-plastic composite material based on the mechanochemical modified wood flour as claimed in claim 1, characterized in that: and the lubricant in the S3 is one or two of stearic acid and paraffin.
8. The preparation method of the wood-plastic composite material based on the mechanochemical modified wood flour as claimed in claim 1, characterized in that: and the antioxidant in S3 is one or two of an antioxidant 1010, an antioxidant 1076 and an antioxidant 168.
9. The preparation method of the wood-plastic composite material based on the mechanochemical modified wood flour as claimed in claim 1, characterized in that: and in the S3, the premixing temperature of the mixing equipment is 20 to 90 ℃, the premixing rotating speed is 500 to 3000r/min, and the premixing time is 3 to 8min.
10. The preparation method of the wood-plastic composite material based on mechanochemical modified wood powder according to claim 1, characterized in that: in the S3, the parameters of plasticizing and granulating the premix by using a double-screw extruder are as follows: the temperature of the first area to the sixth area is 160 to 220 ℃, the head temperature is 160 to 180 ℃, the screw rotation speed is 15 to 45r/min, and the feeding speed is 5 to 15r/min.
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