CN112852177B - Solvent corrosion resistant sweet sorghum residue composite material and preparation method thereof - Google Patents

Solvent corrosion resistant sweet sorghum residue composite material and preparation method thereof Download PDF

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CN112852177B
CN112852177B CN202110047672.8A CN202110047672A CN112852177B CN 112852177 B CN112852177 B CN 112852177B CN 202110047672 A CN202110047672 A CN 202110047672A CN 112852177 B CN112852177 B CN 112852177B
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sweet sorghum
composite material
slag
residue
parts
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CN112852177A (en
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蔡红珍
韩祥生
卢文玉
于文凡
原研浩
豆小航
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Shandong University of Technology
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00Compositions of lignin-containing materials
    • C08L97/02Lignocellulosic material, e.g. wood, straw or bagasse
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04Homopolymers or copolymers of ethene
    • C08L23/06Polyethene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/14Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/16Fibres; Fibrils
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/06Properties of polyethylene
    • C08L2207/062HDPE

Abstract

The invention belongs to the technical field of novel composite materials, and particularly relates to a solvent corrosion resistant sweet sorghum residue composite material and a preparation method thereof. The raw materials of the composite material consist of baked modified sweet sorghum slag, high-density polyethylene and a lubricant; the sweet sorghum residue modified by baking is prepared by crushing sweet sorghum residue, screening 80-100 mesh powder, and drying to make the water content less than 2%; and then, taking nitrogen as a carrier, preserving the heat of the dried sweet sorghum slag powder at 200-300 ℃ for 30-60min, and cooling to room temperature to obtain the baking modified sweet sorghum slag. According to the solvent corrosion resistant sweet sorghum residue composite material, the sweet sorghum residue is baked and modified, so that the fiber hydrophilicity is effectively reduced, and the stability of the composite material is improved; meanwhile, the utilization value of the waste sweet sorghum slag is improved, and the high-value utilization of the waste sweet sorghum slag in the aspect of materials is realized.

Description

Solvent corrosion resistant sweet sorghum residue composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of novel composite materials, and particularly relates to a solvent corrosion resistant sweet sorghum residue composite material and a preparation method thereof.
Background
Sweet sorghum is a promising energy plant, sugar is extracted from the sweet sorghum and is widely used for producing fuel ethanol by a fermentation method, but the residue after fermentation is not comprehensively utilized. With the rapid development of the fuel ethanol industry, the content of sweet sorghum dregs is continuously increased. Although the sweet sorghum slag is a waste in the fuel ethanol industry, the sweet sorghum slag still has more cellulose, hemicellulose and lignin contents, and has high resource utilization value and great development potential. At present, the sweet sorghum dregs are mainly used as animal feed, biofuel and other useful products, and most of the sweet sorghum dregs are regarded as wastes due to the complex synthesis process, expensive disposal cost and high transportation cost, so that serious resource waste and environmental pollution are caused.
Torrefaction, which is a promising thermochemical pretreatment method of biomass, can improve fuel quality of biomass, improve grindability of fiber and enhance hydrophobicity at a temperature of 200 to 300 ℃ in the absence of oxygen, is generally used as a pretreatment method for pyrolysis, gasification or combustion of biomass, and few studies have been made on using torrefied biomass as a filler of biocomposites. Therefore, the sweet sorghum residue wood-plastic composite material is prepared by baking and pretreating the sweet sorghum residue waste, the application range of the sweet sorghum residue is widened, the waste with low additional value is converted into a material product with high additional value, and the economic benefit and the social benefit are excellent.
Disclosure of Invention
The purpose of the invention is: provides a sweet sorghum residue composite material with solvent corrosion resistance. The composite material widens the application range of the sweet sorghum slag and has excellent solvent corrosion resistance; the invention also provides a preparation method thereof.
The solvent corrosion resistant sweet sorghum residue composite material provided by the invention comprises the following raw materials in parts by weight: 30-60 parts of baking modified sweet sorghum slag, 30-60 parts of high-density polyethylene and 1-5 parts of lubricant;
the preparation method of the baked modified sweet sorghum slag comprises the following steps:
(1) pulverizing sweet sorghum residue, screening 80-100 mesh powder, and drying to make its water content less than 2%;
(2) and (3) taking nitrogen as a carrier gas, preserving the heat of the dried sweet sorghum slag powder at the temperature of 200-300 ℃ for 30-60min, and cooling to room temperature to obtain the baking modified sweet sorghum slag.
Wherein:
the drying temperature in the step (1) is 60-100 ℃, and the drying time is 12-24 h.
The flow rate of the nitrogen in the step (2) is 100-300ml/min, and the temperature is raised to 200-300 ℃ at the temperature raising rate of 10-20 ℃/min for heat preservation.
The High Density Polyethylene (HDPE) has a density in the range of 0.941 to 0.960g/cm 3 The melt flow rate is 0.05-0.10g/10min, the softening point is 100-130 ℃, and the melting point is 120-140 ℃.
The lubricant is polyethylene wax, and the melting point is 100-130 ℃.
The preparation method of the solvent corrosion resistant sweet sorghum residue composite material comprises the following steps:
(1) pulverizing sweet sorghum residue with pulverizer, sieving to obtain 80-100 mesh powder, and drying to water content less than 2%;
(2) putting the dried sweet sorghum slag powder into a quartz boat, then putting the quartz boat into a box-type muffle furnace, heating to 200-300 ℃ at the speed of 10-20 ℃/min, preserving the heat for 30-60min, taking nitrogen as carrier gas and the flow of 300ml/min, and cooling to room temperature to obtain baking modified sweet sorghum slag;
(3) weighing the required raw materials in parts by weight, and fully mixing for 15-30 min to obtain a uniform material;
(4) and putting the mixed materials into a miniature double-screw extruder for melt blending, extruding into a charging barrel, and putting into a miniature injection molding machine for injection molding to obtain the solvent corrosion resistant sweet sorghum slag composite material.
Wherein:
in the step (4), the rotating speed of the micro double-screw extruder is 50-70r/min, the extrusion temperature is 170-.
According to the solvent corrosion resistant sweet sorghum residue composite material, the baked and modified sweet sorghum residue has high fixed carbon and cellulose content, low hydrophilic hydroxyl, a rough porous structure and good thermal stability. Due to the reduction of hydrophilic groups and the formation of a porous structure, the rough porous surface of the baked and modified sweet sorghum slag is beneficial to the permeation of an HDPE matrix, the interface bonding force between the baked and modified sweet sorghum slag fiber and a high-density polyethylene matrix is enhanced, and the obtained composite material has enhanced thermal stability, excellent mechanical properties (including creep resistance and stress relaxation resistance), hydrophobicity and solvent resistance.
The proper roasting temperature of the sweet sorghum slag effectively improves the rigidity of the composite material, because the roasted sweet sorghum slag can be uniformly distributed in the HDPE matrix, and the rough surface of the roasted sweet sorghum slag is beneficial to the permeation of the HDPE matrix and has excellent interface compatibility, thereby improving the strength and rigidity of the composite material. The roasting treatment helps to reduce the water absorption of the sweet sorghum bagasse, further limits the movement of HDPE molecules, prevents water from entering the interior, and therefore changes the hydrophobicity and solvent corrosion resistance of the composite material.
Compared with the prior art, the invention has the following beneficial effects:
(1) the solvent corrosion resistant sweet sorghum residue composite material provided by the invention takes sweet sorghum residue and high-density polyethylene as raw materials, is low in price, has a positive effect on the recovery of the sweet sorghum residue and the high-density polyethylene, is beneficial to relieving resource shortage and environmental pollution to a certain extent, widens the application range of the sweet sorghum residue, converts waste with low added value into a material product with high added value, and has excellent economic benefit and social benefit.
(2) The sweet sorghum residue/high-density polyethylene composite material capable of resisting solvent corrosion is prepared by taking baked and modified sweet sorghum residue as a filler and high-density polyethylene as a matrix and adding a certain lubricant through melt co-extrusion and injection molding, can be recycled, and has high stability and better solvent corrosion resistance.
(3) According to the solvent corrosion resistant sweet sorghum residue composite material, the sweet sorghum residue is baked and modified, so that the fiber hydrophilicity is effectively reduced, and the stability of the composite material is improved; meanwhile, waste is changed into valuable, the utilization value of the waste sweet sorghum slag is improved, and high-value utilization of the waste sweet sorghum slag in the aspect of materials is realized.
(4) The preparation method of the solvent corrosion resistant sweet sorghum residue composite material has the advantages of simple process, environmental protection, no pollution and easy realization of industrial production.
Drawings
FIG. 1 is a flow chart of a process for preparing a solvent corrosion resistant sweet sorghum bagasse composite;
FIG. 2 is an SEM image of a cross-section of the composite material prepared in comparative example 1;
FIG. 3 is an SEM image of a cross-section of the composite material prepared in example 1;
FIG. 4 is an SEM image of a cross-section of the composite material prepared in example 2;
fig. 5 is an SEM image of a cross section of the composite material prepared in example 3.
Detailed Description
The present invention is further described below with reference to examples.
Comparative example 1
The sweet sorghum residue composite material of the comparative example 1 is prepared from the following raw materials in parts by weight: 40 parts of sweet sorghum residues, 55 parts of high-density polyethylene and 5 parts of polyethylene wax.
The preparation method of the sweet sorghum residue composite material according to the comparative example 1 comprises the following steps:
(1) screening the sweet sorghum residues of 80-100 meshes, and drying in an oven at 80 ℃ for 24 h;
(2) taking the following raw materials in parts by weight: fully mixing 40 parts of sweet sorghum residues, 55 parts of high-density polyethylene and 5 parts of polyethylene wax for 15min to obtain a uniform material;
(3) putting the mixed materials into a miniature double-screw extruder for melt blending, and extruding into a charging barrel, wherein the rotating speed of the extruder is 60r/min, and the extrusion temperature and the charging barrel temperature are both 175 ℃;
(4) the mixture is put into a micro injection molding machine through a charging barrel for injection molding to obtain a composite material; the injection temperature of the micro injection molding machine is 175 ℃, the injection pressure is 5MPa, the pressure maintaining time is 5s, and the cooling temperature of the injection molding machine mold is 45 ℃.
Example 1
The solvent corrosion resistant sweet sorghum residue composite material described in the embodiment 1 is composed of the following raw materials in parts by weight: 40 parts of baked modified sweet sorghum slag, 55 parts of high-density polyethylene and 5 parts of polyethylene wax.
The high density polyethylene (A), (B) and (C)HDPE) has a density in the range of 0.950g/cm 3 The melt flow rate was 0.05g/10min, the softening point was 123 ℃ and the melting point was 130 ℃.
The lubricant is polyethylene wax, and the melting point of the lubricant is 116 ℃.
The preparation method of the baked modified sweet sorghum slag comprises the following steps:
(1) pulverizing sweet sorghum residue, screening to obtain 80-100 mesh powder, and drying in 80 deg.C oven for 24 hr to make its water content less than 2%;
(2) and (3) putting the dried sweet sorghum slag powder into a quartz boat, then putting the quartz boat into a box-type muffle furnace, heating to 200 ℃ at the speed of 10 ℃/min, preserving the temperature for 30min, taking nitrogen as carrier gas and cooling to room temperature, thus obtaining the baking modified sweet sorghum slag, wherein the flow rate is 200 ml/min.
The parameter analysis of the sweet sorghum residue after being baked at 200 ℃ shows that the content of volatile substances, fixed carbon, carbon content, hydrogen content and oxygen content of the unmodified sweet sorghum residue are respectively 71.4% and 21.3%, the content of carbon, hydrogen and oxygen are respectively 42.5%, 5.9% and 51.0%, the content of cellulose, hemicellulose and lignin are respectively 42.1%, 29.2% and 2.1%, the content of volatile substances, fixed carbon and oxygen after being baked at 200 ℃ is respectively 71.3% and 21.2%, the content of carbon, hydrogen and oxygen are respectively 43.9%, 5.8% and 49.6%, and the content of cellulose, hemicellulose and lignin are respectively 46.1%, 26.7% and 2.5%. After baking at 200 ℃, the content of volatile substances and oxygen is respectively reduced by 0.1 percent and 2.7 percent, the content of carbon is increased by 3.3 percent, the content of cellulose is increased by 9.5 percent, and the content of hemicellulose is reduced by 8.6 percent.
The preparation method of the solvent corrosion resistant sweet sorghum residue composite material in the embodiment 1 comprises the following steps:
(1) sieving to obtain 80-100 mesh sweet sorghum residue, and drying in 80 deg.C oven for 24 hr.
(2) Putting the materials into a quartz boat, weighing, then putting the quartz boat into a box-type muffle furnace, heating to 200 ℃ at the speed of 10 ℃/min, keeping the temperature for 30min, taking nitrogen as carrier gas and the flow rate of 200ml/min, and cooling to room temperature to obtain the modified sweet sorghum slag.
(3) Taking the following raw materials in parts by weight: 40 parts of sweet sorghum residues, 55 parts of high-density polyethylene and 5 parts of polyethylene wax, and fully mixing for 15min to obtain a uniform material.
(4) And putting the fully mixed materials into a conical double-screw extruder for melt blending, and extruding into a charging barrel. The rotation speed of the extruder is 60r/min, and the extrusion temperature and the cylinder temperature are both 175 ℃. And putting the mixture into a micro injection molding machine through a charging barrel for injection molding to obtain the composite material. The injection temperature is 175 ℃, the injection pressure is 5MPa, the pressure maintaining time is 5s, and the cooling temperature of the injection molding machine mold is 45 ℃.
Example 2
The solvent corrosion resistant sweet sorghum residue composite material described in the embodiment 2 is composed of the following raw materials in parts by weight: 40 parts of baked modified sweet sorghum slag, 55 parts of high-density polyethylene and 5 parts of polyethylene wax.
The High Density Polyethylene (HDPE) has a density in the range of 0.950g/cm 3 The melt flow rate was 0.05g/10min, the softening point was 123 ℃ and the melting point was 130 ℃.
The lubricant is polyethylene wax, and the melting point of the lubricant is 116 ℃.
The preparation method of the baked modified sweet sorghum slag comprises the following steps:
(1) pulverizing sweet sorghum residue, screening to obtain 80-100 mesh powder, and drying in 80 deg.C oven for 24 hr to make its water content less than 2%;
(2) and (3) putting the dried sweet sorghum slag powder into a quartz boat, then putting the quartz boat into a box-type muffle furnace, heating to 250 ℃ at the speed of 10 ℃/min, preserving the heat for 30min, taking nitrogen as carrier gas and cooling to room temperature, thus obtaining the baking modified sweet sorghum slag, wherein the flow rate is 200 ml/min.
The parameter analysis of the sweet sorghum residue after being baked at 250 ℃ shows that the content of volatile substances, fixed carbon, carbon content, hydrogen content and oxygen content of the unmodified sweet sorghum residue are respectively 71.4% and 21.3%, the content of carbon, hydrogen and oxygen are respectively 42.5%, 5.9% and 51.0%, the content of cellulose, hemicellulose and lignin are respectively 42.1%, 29.2% and 2.1%, the content of volatile substances, fixed carbon and oxygen after being baked at 250 ℃ is respectively 60.4% and 31.2%, the content of carbon, hydrogen and oxygen is respectively 45.6%, 5.5% and 48.0%, and the content of cellulose, hemicellulose and lignin is respectively 53.8%, 10.8% and 9.7%. After the baking at 250 ℃, the content of volatile substances and oxygen is respectively reduced by 15.4 percent and 5.9 percent, the content of fixed carbon and carbon is respectively increased by 46.5 percent and 7.3 percent, the content of cellulose is increased by 27.8 percent, and the content of hemicellulose is reduced by 63.0 percent.
The preparation method of the solvent corrosion resistant sweet sorghum residue composite material in the embodiment 2 comprises the following steps:
(1) sieving to obtain 80-100 mesh sweet sorghum residue, and drying in 80 deg.C oven for 24 hr.
(2) And (3) putting the materials into a quartz boat, then putting the quartz boat into a box type muffle furnace, heating to 250 ℃ at the speed of 10 ℃/min, keeping the temperature for 30min, taking nitrogen as carrier gas and the flow rate of 200ml/min, and cooling to room temperature to obtain the modified sweet sorghum slag.
(3) Taking the following raw materials in parts by weight: 40 parts of sweet sorghum residues, 55 parts of high-density polyethylene and 5 parts of polyethylene wax, and fully mixing for 15min to obtain a uniform material.
(4) And putting the fully mixed materials into a conical double-screw extruder for melt blending, and extruding into a charging barrel. The rotation speed of the extruder is 60r/min, and the extrusion temperature and the cylinder temperature are both 175 ℃. The mixture is put into a micro injection molding machine through a charging barrel for injection molding to obtain the required material. The injection temperature is 175 ℃, the injection pressure is 5MPa, the pressure maintaining time is 5s, and the cooling temperature of the injection molding machine mold is 45 ℃.
Example 3
The solvent corrosion resistant sweet sorghum residue composite material described in the embodiment 3 is composed of the following raw materials in parts by weight: 40 parts of baked modified sweet sorghum slag, 55 parts of high-density polyethylene and 5 parts of polyethylene wax.
The High Density Polyethylene (HDPE) has a density in the range of 0.950g/cm 3 The melt flow rate was 0.05g/10min, the softening point was 123 ℃ and the melting point was 130 ℃.
The lubricant is polyethylene wax, and the melting point of the lubricant is 116 ℃.
The preparation method of the baked modified sweet sorghum slag comprises the following steps:
(1) pulverizing sweet sorghum residue, screening to obtain 80-100 mesh powder, and drying in 80 deg.C oven for 24 hr to make its water content less than 2%;
(2) and (3) putting the dried sweet sorghum slag powder into a quartz boat, then putting the quartz boat into a box-type muffle furnace, heating to 300 ℃ at the speed of 10 ℃/min, preserving the temperature for 30min, taking nitrogen as carrier gas and cooling to room temperature, thus obtaining the baking modified sweet sorghum slag, wherein the flow rate is 200 ml/min.
The parameter analysis of the sweet sorghum residue after being baked at 300 ℃ shows that the content of volatile substances, fixed carbon, carbon content, hydrogen content and oxygen content of the unmodified sweet sorghum residue are respectively 71.4% and 21.3%, the content of carbon, hydrogen and oxygen are respectively 42.5%, 5.9% and 51.0%, the content of cellulose, hemicellulose and lignin are respectively 42.1%, 29.2% and 2.1%, the content of volatile substances, fixed carbon and oxygen after being baked at 300 ℃ is respectively 35.6% and 53.3%, the content of carbon, hydrogen and oxygen are respectively 51.6%, 5.2% and 42.2%, and the content of cellulose, hemicellulose and lignin are respectively 72.3%, 1.4% and 26.7%. After being baked at 300 ℃, the content of volatile substances and oxygen are respectively reduced by 50.1 percent and 17.3 percent, the content of fixed carbon and carbon is respectively increased by 150.2 percent and 21.4 percent, the content of cellulose is increased by 71.7 percent, and the content of hemicellulose is reduced by 95.2 percent.
The preparation method of the solvent corrosion resistant sweet sorghum residue composite material in the embodiment 3 comprises the following steps:
(1) sieving to obtain 80-100 mesh sweet sorghum residue, and drying in 80 deg.C oven for 24 hr.
(2) And (3) putting the materials into a quartz boat, then putting the quartz boat into a box type muffle furnace, heating to 300 ℃ at the speed of 10 ℃/min, keeping the temperature for 30min, taking nitrogen as carrier gas and the flow rate of 200ml/min, and cooling to room temperature to obtain the modified sweet sorghum slag.
(3) Taking the following raw materials in parts by weight: 40 parts of sweet sorghum slag, 55 parts of high-density polyethylene and 5 parts of lubricant polyethylene wax, and fully mixing for 15min to obtain a uniform material.
(4) And putting the fully mixed materials into a conical double-screw extruder for melt blending, and extruding into a charging barrel. The rotation speed of the extruder is 60r/min, and the extrusion temperature and the cylinder temperature are both 175 ℃. The mixture is put into a micro injection molding machine through a charging barrel for injection molding to obtain the required material. The injection temperature is 175 ℃, the injection pressure is 5MPa, the pressure maintaining time is 5s, and the mold temperature is 40 ℃.
Testing the mechanical properties of the composite material according to related national standards (the tensile strength is tested according to GB/T1040.2-2006, the bending strength is tested according to GB/T9341-2008), testing the contact angle of the composite material before water absorption (the test liquid is deionized water), testing the water absorption property of the composite material according to GB/T1034-2008, calculating and testing the water absorption rate (WA) and the thickness expansion rate (TS) of the composite material after 28 days of water absorption according to formulas (1) and (2), testing the tensile strength and the retention rate (R) of the tensile mechanical strength of the composite material after the composite material is soaked in different solvents for 7 days according to GB/T1040.2-2006 ts ) The calculation is performed according to equation (3).
WA=(W t -W 0 )/W 0 ×100% (1)
TS=(T t -T 0 )/T 0 ×100% (2)
R ts =(Ts 0 -Ts t )/Ts 0 ×100% (3)
In the formula, Ts 0 、W 0 And T 0 The tensile strength, mass and thickness at the initial moment are respectively; ts t 、W t And T t Tensile strength, mass and thickness after 28 days of water absorption, respectively; t in the following table S 、F S Respectively, tensile strength and bending strength.
The test results for comparative example 1 and examples 1-3 are shown in tables 1-3:
TABLE 1 mechanical Properties of the composites obtained in comparative example 1 and examples 1 to 3
Serial number Tensile Strength (T) S /MPa) Flexural Strength (F) S /MPa)
Comparative example 1 21.24 28.06
Example 1 22.16 28.77
Example 2 24.84 30.54
Example 3 23.80 31.68
TABLE 2 hydrophobicity analysis of composites obtained in comparative example 1 and examples 1-3
Figure BDA0002897969700000071
The larger the contact angle, the better the hydrophobicity of the composite; lower water absorption and thickness expansion indicate better hydrophobicity of the material.
TABLE 3 Retention of mechanical Strength after 7 days of immersion in various solvents
Figure BDA0002897969700000072
As can be seen from the above tables 1 and 2, the mechanical properties and surface hydrophobicity of the composite material prepared by using the baked pretreated sweet sorghum slag are greatly improved. As can be seen from table 3, compared with the unmodified sweet sorghum residue composite material, after the composite material is soaked in different solvents for 7 days, the tensile strength retention rate of the baked modified sweet sorghum residue composite material is higher, which indicates that the baked modified sweet sorghum residue composite material has better solvent resistance stability.
Fig. 2 (comparative example 1) shows that the interaction between the original sweet sorghum bagasse fibers and the high density polyethylene matrix is poor, and some gaps exist in the interface, which results in the reduction of the interfacial bonding force of the composite material.
As the baking temperature is increased, the surface of the baked sweet sorghum residue fiber is gradually rough and porous, and the surface is shown in the figure
Figure BDA0002897969700000081
(corresponding to examples 1-3, respectively) intimate contact between the baked sweet sorghum bagasse fibers and the high density polyethylene matrix, particularly the baking pretreatment at 300 ℃, further forms a porous structure in the sweet sorghum bagasse fibers (fig. 5), which facilitates the influx of the polymer matrix, leads to intimate entanglement between the baked sweet sorghum bagasse fibers and the high density polyethylene matrix, enhances interfacial compatibility between the filler and the matrix, and thus facilitates the enhancement of the mechanical properties of the composite.
Comparative example 2
The sweet sorghum residue composite material of the comparative example 2 is prepared from the following raw materials in parts by weight: 40 parts of alkali modified sweet sorghum residues, 55 parts of high-density polyethylene and 5 parts of polyethylene wax.
The preparation method of the sweet sorghum residue composite material according to the comparative example 2 comprises the following steps:
(1) screening the sweet sorghum residues of 80-100 meshes, and drying in an oven at 80 ℃ for 24 h;
(2) preparing a 6% sodium hydroxide solution, putting the sweet sorghum slag into the sodium hydroxide solution according to the solid-to-liquid ratio of 1:10, and stirring at room temperature (25 ℃) for 2 hours at the stirring speed of 600 r/min;
(3) after the reaction is finished, washing the sweet sorghum slag to be neutral by using ultrapure water, and drying the sweet sorghum slag in an oven at the temperature of 80 ℃ for 24 hours;
(4) taking the following raw materials in parts by weight: 40 parts of alkali modified sweet sorghum slag, 55 parts of high-density polyethylene and 5 parts of polyethylene wax. Mixing thoroughly for 15min to obtain a homogeneous material;
(5) and putting the mixed materials into a miniature double-screw extruder for melt blending, and extruding into a charging barrel, wherein the rotating speed of the extruder is 60r/min, and the extrusion temperature and the charging barrel temperature are both 175 ℃.
(6) The mixture is put into a micro injection molding machine through a charging barrel for injection molding to obtain a composite material; the injection temperature of the micro injection molding machine is 175 ℃, the injection pressure is 5MPa, the pressure maintaining time is 5s, and the cooling temperature of the injection molding machine mold is 45 ℃.
Example 4
The preparation method of the solvent corrosion resistant sweet sorghum residue composite material described in the embodiment 4 is the same as that of the composite material described in the embodiment 3, and the only difference is that the raw material composition is different. The solvent corrosion resistant sweet sorghum residue composite material described in the embodiment 4 is composed of the following raw materials in parts by weight: 30 parts of baked modified sweet sorghum slag, 65 parts of high-density polyethylene and 5 parts of polyethylene wax.
Comparative example 3
Comparative example 3 differs from example 4 only in that unmodified sweet sorghum bagasse is used.
Example 5
The solvent corrosion resistant sweet sorghum bagasse composite material described in this example 5 was prepared in the same manner as the composite material described in example 3, except that the raw material composition was different. The solvent corrosion resistant sweet sorghum residue composite material described in this embodiment 5 is composed of the following raw materials in parts by weight: 60 parts of baked modified sweet sorghum slag, 35 parts of high-density polyethylene and 5 parts of polyethylene wax.
Comparative example 4
Comparative example 4 differs from example 5 only in that unmodified sweet sorghum bagasse is used.
Example 6
The solvent corrosion resistant sweet sorghum bagasse composite material described in this example 6 was prepared in the same manner as the composite material described in example 3, except that the baking and holding time was different. In the solvent corrosion resistant sweet sorghum residue composite material described in this example 6, the baking modification process was changed to: and (3) putting the materials into a quartz boat, then putting the quartz boat into a box type muffle furnace, heating to 300 ℃ at the speed of 10 ℃/min, keeping the temperature for 60min, taking nitrogen as carrier gas and the flow rate of 200ml/min, and cooling to room temperature to obtain the modified sweet sorghum slag.
TABLE 4 analysis of mechanical Properties of composites obtained in comparative examples 2 to 4 and examples 4 to 6
Serial number Tensile Strength (T) S /MPa)
Comparative example 2 20.41
Example 4 28.86
Comparative example 3 25.02
Example 5 20.48
Comparative example 4 18.42
Example 6 25.34
As can be seen from table 4, compared to the sweet sorghum bagasse/high density polyethylene composite material prepared from alkali-modified sweet sorghum bagasse, the modified sweet sorghum bagasse/high density polyethylene composite material obtained by the baking modification treatment method has better tensile strength. The weight parts of the sweet sorghum slag are reduced or increased, the mechanical properties of the sweet sorghum slag/high-density polyethylene composite material obtained by the baking modification treatment mode are superior to those of the unmodified sweet sorghum slag/high-density polyethylene composite material with the same parts, and the baking modification has positive significance for improving the tensile strength of the composite material. Higher tensile strengths can also be obtained by extending the residence time of the bake. On the whole, the sweet sorghum residue/high-density polyethylene composite material obtained by adopting a baking modification treatment mode has better mechanical property.

Claims (4)

1. A solvent corrosion resistant sweet sorghum residue composite material is characterized in that: the composite material is prepared from the following raw materials in parts by weight: 30-60 parts of baking modified sweet sorghum slag, 30-60 parts of high-density polyethylene and 1-5 parts of lubricant;
the preparation method of the baked modified sweet sorghum slag comprises the following steps:
(1) pulverizing sweet sorghum residue, screening 80-100 mesh powder, and drying to make its water content less than 2%;
(2) taking nitrogen as a carrier, preserving the heat of the dried sweet sorghum slag powder at the temperature of 200-300 ℃ for 30-60min, and cooling to room temperature to obtain baked modified sweet sorghum slag;
wherein:
the drying temperature in the step (1) is 60-100 ℃, and the drying time is 12-24 h;
the flow rate of the nitrogen in the step (2) is 100-300ml/min, and the temperature is raised to 200-300 ℃ at the temperature raising rate of 10-20 ℃/min for heat preservation;
the density of the high density polyethylene is in the range of 0.950g/cm 3 The melt flow rate was 0.05g/10min, the softening point was 123 ℃ and the melting point was 130 ℃.
2. The solvent corrosion resistant sweet sorghum bagasse composite according to claim 1, characterized in that: the lubricant is polyethylene wax, and the melting point is 100-130 ℃.
3. A method for preparing the solvent corrosion resistant sweet sorghum residue composite material of claim 1, which is characterized by comprising the following steps: the method comprises the following steps:
(1) pulverizing sweet sorghum residue with pulverizer, sieving to obtain 80-100 mesh powder, and drying to water content less than 2%;
(2) putting the dried sweet sorghum slag powder into a quartz boat, then putting the quartz boat into a box-type muffle furnace, heating to 200-300 ℃ at the speed of 10-20 ℃/min, preserving the heat for 30-60min, taking nitrogen as carrier gas and the flow of 300ml/min, and cooling to room temperature to obtain baking modified sweet sorghum slag;
(3) weighing the required raw materials in parts by weight, and fully mixing for 15-30 min to obtain a uniform material;
(4) and putting the mixed materials into a miniature double-screw extruder for melt blending, extruding into a charging barrel, and putting into a miniature injection molding machine for injection molding to obtain the solvent corrosion resistant sweet sorghum slag composite material.
4. The method for preparing the solvent corrosion resistant sweet sorghum bagasse composite material according to claim 3, characterized in that: in the step (4), the rotating speed of the micro double-screw extruder is 50-70r/min, the extrusion temperature is 170-.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580640A (en) * 2009-06-23 2009-11-18 福建师范大学 Method for preparing wood-plastic composite by blending heat-treated plant fiber with plastic
CN102690525A (en) * 2012-05-29 2012-09-26 北京化工大学 Wood-plastic composite material using sweet sorghum slag as enhanced phase and preparation method for wood-plastic composite material
CN103834093A (en) * 2014-03-19 2014-06-04 福建师范大学 Ethylene-vinyl alcohol copolymer-based wood/plastic composite board
CN112029168A (en) * 2020-08-11 2020-12-04 西安理工大学 Preparation method of waste tobacco stalk fiber reinforced resin matrix composite material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101580640A (en) * 2009-06-23 2009-11-18 福建师范大学 Method for preparing wood-plastic composite by blending heat-treated plant fiber with plastic
CN102690525A (en) * 2012-05-29 2012-09-26 北京化工大学 Wood-plastic composite material using sweet sorghum slag as enhanced phase and preparation method for wood-plastic composite material
CN103834093A (en) * 2014-03-19 2014-06-04 福建师范大学 Ethylene-vinyl alcohol copolymer-based wood/plastic composite board
CN112029168A (en) * 2020-08-11 2020-12-04 西安理工大学 Preparation method of waste tobacco stalk fiber reinforced resin matrix composite material

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