CN111057356B - Polylactic acid-based biomass composite material plate and preparation method thereof - Google Patents

Polylactic acid-based biomass composite material plate and preparation method thereof Download PDF

Info

Publication number
CN111057356B
CN111057356B CN201911341931.7A CN201911341931A CN111057356B CN 111057356 B CN111057356 B CN 111057356B CN 201911341931 A CN201911341931 A CN 201911341931A CN 111057356 B CN111057356 B CN 111057356B
Authority
CN
China
Prior art keywords
powder
straw powder
polylactic acid
talcum powder
modified
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201911341931.7A
Other languages
Chinese (zh)
Other versions
CN111057356A (en
Inventor
周才良
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Guansen New Material Co ltd
Original Assignee
Jiangsu Yulinsheng Plastic Wood Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu Yulinsheng Plastic Wood Technology Co ltd filed Critical Jiangsu Yulinsheng Plastic Wood Technology Co ltd
Priority to CN201911341931.7A priority Critical patent/CN111057356B/en
Publication of CN111057356A publication Critical patent/CN111057356A/en
Application granted granted Critical
Publication of CN111057356B publication Critical patent/CN111057356B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • C08L67/04Polyesters derived from hydroxycarboxylic acids, e.g. lactones
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/06Biodegradable
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • 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
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Biological Depolymerization Polymers (AREA)

Abstract

The polylactic acid-based biomass composite material plate is prepared by compounding polylactic acid, polybutylene succinate, modified straw powder, a talcum powder/lignin composite material, a plasticizer DOP and acetyl tributyl citrate. The polylactic acid-based biomass composite material plate is biodegradable, non-toxic, pollution-free, light in weight, high in strength, good in heat resistance, safe and environment-friendly in use process, can reduce the cost of polylactic acid, and expands the application field of agricultural wastes. The forming process is relatively simple, fast and convenient, has strong designability, can be used for manufacturing products with different shapes, and has lower manufacturing cost. Can be used for manufacturing disposable products such as buried flowerpots, gift packaging boxes, disposable lunch boxes and the like.

Description

Polylactic acid-based biomass composite material plate and preparation method thereof
Technical Field
The invention relates to a composite material, in particular to a polylactic acid-based biomass composite material plate and a preparation method thereof. Is suitable for manufacturing disposable products such as buried flowerpots, gift packaging boxes, disposable lunch boxes and the like, and belongs to the technical field of composite materials.
Background
When flowers (saplings) are bought from the market and are to be transplanted, the disposable flower pots can be used for cultivating the flowers (saplings) in the flowers (saplings), after the flowers (saplings) are bought back by a user, the flowers (saplings) and the flower pots are buried in soil, the disposable flower pots are degraded along with time, the flowers (saplings) can thrive in the soil, and the death rate of the flowers (saplings) in the transplanting process can be reduced; packaging boxes are used in a large amount when gifts are packaged, traditionally, the packaging boxes are generally made of hard paper, plastic, wood or metal, and the packaging boxes made of the materials have certain limitations, such as low strength of the hard paper packaging boxes and waste of a large amount of paper resources in the using process; the plastic packaging box has low strength, is not easy to degrade, and is easy to pollute the environment after being discarded; the wooden packing box has higher cost, and trees are inevitably felled in the manufacturing process, which is not beneficial to ecological protection; the metal packing box is heavy, poor in touch feeling, high in cost and the like; the disposable lunch box is made of foamed plastic, is not degraded and is easy to pollute the environment, and in recent years, the disposable lunch box made of wood is available, and the disposable lunch box can be degraded after being discarded, but can destroy forest resources.
In summary, there is a need in the market for a degradable, environmentally friendly, safe, hygienic, and inexpensive material for manufacturing the above products.
The polylactic acid is thermoplastic aliphatic polyester formed by polymerizing lactic acid monomers formed by fermenting plants such as corn, starch and beet, can realize 100% degradation in natural environment, is green and environment-friendly, has good biocompatibility, excellent mechanical property and high strength, and is easy to process and form, so the polylactic acid is one of the best choices in the field of research of biomass composite materials and is expected to replace non-renewable petroleum-based fossil energy.
However, the polylactic acid material still has many defects in the using process, such as high price, high brittleness, low toughness and the like of the polylactic acid used as a plastic matrix, thereby limiting the application range of the polylactic acid.
Agricultural wastes such as rice straws, sesame straws, corn straws, wheat straws and the like are wide in source, low in price, green and environment-friendly, high in specific strength and specific modulus, low in density, biodegradable, non-toxic and pollution-free in structural materials prepared by compounding with polylactic acid, capable of replacing petroleum-based resources, capable of replacing more glass fibers or aramid fibers used at present, capable of improving the utilization value of the agricultural wastes, capable of reducing the problem of high cost of the polylactic acid in the application aspect, and important in economic and environment-friendly significance.
Therefore, it is necessary to invent a degradable composite material plate using polylactic acid as a matrix and agricultural wastes as fillers and a preparation method thereof.
Disclosure of Invention
The invention aims at the above purpose and provides a polylactic acid-based biomass composite material plate and a preparation method thereof.
The polylactic acid-based biomass composite material plate comprises the following components:
Figure BSA0000198167870000021
the modified straw powder is one of modified rice straw powder, modified sesame straw powder, modified corn straw powder and modified wheat straw powder, and has an average particle size of 80-160 meshes.
The talcum powder/lignin composite material is a powdery material, and the average grain diameter is 1-5 mu m.
A preparation method of a polylactic acid-based biomass composite plate comprises the following molding process:
(1) completely immersing the straw powder in an acetone solution for 30-60min, filtering until no acetone solution drops in the straw powder, completely immersing the filtered straw powder in a hydrochloric acid solution with the mass percent concentration of 6-10% for 20-30min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered straw powder in a NaOH aqueous solution with the mass percent concentration of 10-20% for 60-90min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and screening into 20-100 meshes of powder to obtain the pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 1500-2000: 0.1-0.3: 1-3: 230-330, adding the pretreated straw powder, water, tetrabutylammonium acetate and N, N-dimethylacetamide into a container, stirring and dispersing for 15-25min at 50-70 ℃, then adding butyl acrylate, reacting for 60-80min at 70-78 ℃, cooling the mixture to room temperature after the reaction is finished, drying, and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.08-0.12mol/L phenol ethanol solution according to the mass ratio of 100: 1200-1800, mixing, stirring for 3-4h at 90-100 ℃, standing, performing suction filtration, and repeatedly washing a filter cake by using NaOH aqueous solution with the mass percentage concentration of 3-5% and water until the filtrate is neutral; then, drying the filter cake at 60-70 ℃ to constant weight, grinding and sieving into powder with the particle size of 0.8-1.2 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 50-90: 5-7, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 60-70 ℃ for 2-3h, standing for 2-3h, filtering, drying a filter cake at the temperature of 80-90 ℃ to constant weight, and dividing the filter cake into powder with the particle size of 0.1-0.5 mu m by a grinding sieve to obtain surface activated talcum powder;
(5) respectively weighing surface activated talcum powder, lignin and water according to the mass ratio of 100: 40-60: 50-70, mixing the surface activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing at a high speed for 10-20min, then putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 6-8h on a ball mill at the rotating speed of 240-280rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate according to the metering ratio;
(8) uniformly mechanically mixing polylactic acid, modified straw powder and a plasticizer DOP, then placing the mixture into a double-screw extruder, and preparing polylactic acid-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 165-170 ℃, 170-172 ℃ and 180-186 ℃;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 110-;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are respectively 155-.
The polylactic acid-based biomass composite material plate disclosed by the invention is biodegradable, non-toxic, pollution-free, light in weight, high in strength, good in heat resistance, safe and environment-friendly in use process, and capable of reducing the cost of polylactic acid and expanding the application field of agricultural wastes. The forming process is relatively simple, fast and convenient, has strong designability, can be used for manufacturing products with different shapes, and has lower manufacturing cost. Can be used for manufacturing disposable products such as buried flowerpots, gift packaging boxes, disposable lunch boxes and the like.
Detailed Description
The following specific examples are intended to further illustrate the invention, but are not intended to limit the scope of the invention.
Example 1: the polylactic acid-based biomass composite material plate comprises the following components:
Figure BSA0000198167870000031
the modified straw powder is modified corn straw powder, and the average grain size is 120 meshes.
The talcum powder/lignin composite material is a powdery material, and the average grain diameter is 3 mu m.
A preparation method of a polylactic acid-based biomass composite plate comprises the following molding process:
(1) completely immersing the straw powder in an acetone solution for 45min, then filtering until no acetone solution drops in the straw powder, completely immersing the filtered and dried straw powder in a hydrochloric acid solution with the mass percent concentration of 8% for 25min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered and dried straw powder in a NaOH aqueous solution with the mass percent concentration of 15% for 75min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and screening into 60-mesh powder to obtain pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 1750: 0.2: 2: 280, adding the pretreated straw powder, the water, the tetrabutylammonium acetate and the N, N-dimethylacetamide into a container, stirring and dispersing for 20min at the temperature of 60 ℃, then adding butyl acrylate, reacting for 70min at the temperature of 74 ℃, cooling the mixture to room temperature after the reaction is finished, drying and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.1mol/L phenol ethanol solution according to the mass ratio of 100: 1500, mixing, stirring at 95 ℃ for 3.5h, standing, carrying out suction filtration, and repeatedly washing a filter cake by using 4% NaOH aqueous solution and water in sequence until a filtrate is neutral; then, drying the filter cake at 65 ℃ to constant weight, and grinding and screening the filter cake into powder with the particle size of 1.0 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 70: 6, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 65 ℃ for 2.5h, standing for 2.5h, filtering, drying a filter cake at the temperature of 85 ℃ to constant weight, and dividing the filter cake into powder with the particle size of 0.3 mu m by a grinding sieve to obtain surface-activated talcum powder;
(5) respectively weighing surface-activated talcum powder, lignin and water according to the mass ratio of 100: 50: 60, mixing the surface-activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing for 15min at a high speed, putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 7h on a ball mill at the rotating speed of 260rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate according to the metering ratio;
(8) uniformly mechanically mixing polylactic acid, modified straw powder and a plasticizer DOP, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization, extrusion and granulation to prepare polylactic acid-based blending granules, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are 167.5 ℃, 171 ℃ and 183 ℃ respectively;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 112 ℃, 115 ℃ and 118 ℃;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are 158 ℃, 161 ℃ and 170 ℃ respectively.
Example 2: the polylactic acid-based biomass composite material plate comprises the following components:
Figure BSA0000198167870000041
the modified rice straw powder is modified rice straw powder, and the average particle size is 80 meshes.
The talcum powder/lignin composite material is a powdery material, and the average grain diameter is 1 mu m.
A preparation method of a polylactic acid-based biomass composite plate comprises the following molding process:
(1) completely immersing the straw powder in an acetone solution for 30min, filtering until no acetone solution drops in the straw powder, completely immersing the filtered straw powder in a hydrochloric acid solution with the mass percent concentration of 6% for 20min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered straw powder in a NaOH aqueous solution with the mass percent concentration of 10% for 60min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and screening into 20-mesh powder to obtain the pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 1500: 0.1: 1: 230, adding the pretreated straw powder, the water, the tetrabutylammonium acetate and the N, N-dimethylacetamide into a container, stirring and dispersing for 15min at 50 ℃, then adding butyl acrylate, reacting for 60min at 70 ℃, cooling the mixture to room temperature after the reaction is finished, drying, and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.08mol/L phenol ethanol solution according to the mass ratio of 100: 1200, mixing, stirring for 3 hours at 90 ℃, standing, carrying out suction filtration, and repeatedly washing a filter cake by using NaOH aqueous solution with the mass percentage concentration of 3% and water until a filtrate is neutral; then, drying the filter cake at 60 ℃ to constant weight, and grinding and screening the filter cake into powder with the particle size of 0.8 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 50: 5, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 60 ℃ for 2h, standing for 2h, filtering, drying a filter cake at the temperature of 80 ℃ to constant weight, and grinding and sieving the filter cake into powder with the particle size of 0.1 mu m to obtain surface-activated talcum powder;
(5) respectively weighing surface-activated talcum powder, lignin and water according to the mass ratio of 100: 40: 50, mixing the surface-activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing for 10min at a high speed, putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 6h on a ball mill at the rotating speed of 240rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate according to the metering ratio;
(8) uniformly mixing polylactic acid, modified straw powder and a plasticizer DOP mechanically, then placing the mixture into a double-screw extruder, and preparing polylactic acid-based blended granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are 165 ℃, 170 ℃ and 180 ℃ respectively;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 110 ℃, 113 ℃ and 115 ℃;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are 155 ℃, 160 ℃ and 165 ℃ respectively.
Example 3: the polylactic acid-based biomass composite material plate comprises the following components:
Figure BSA0000198167870000061
the modified straw powder is modified sesame straw powder, and the average particle size is 160 meshes.
The talcum powder/lignin composite material is a powdery material, and the average grain diameter is 5 mu m.
A preparation method of a polylactic acid-based biomass composite plate comprises the following molding process:
(1) completely immersing the straw powder in an acetone solution for 60min, then filtering until no acetone solution drops in the straw powder, completely immersing the filtered and dried straw powder in a hydrochloric acid solution with the mass percentage concentration of 10% for 30min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered and dried straw powder in a NaOH aqueous solution with the mass percentage concentration of 20% for 90min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and screening into 100-mesh powder to obtain pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 2000: 0.3: 3: 330, adding the pretreated straw powder, the water, the tetrabutylammonium acetate and the N, N-dimethylacetamide into a container, stirring and dispersing for 25min at 70 ℃, then adding butyl acrylate, reacting for 80min at 78 ℃, cooling the mixture to room temperature after the reaction is finished, drying and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.12mol/L phenol ethanol solution according to the mass ratio of 100: 1800, mixing, stirring for 4 hours at 100 ℃, standing, carrying out suction filtration, and repeatedly washing a filter cake by using NaOH aqueous solution with the mass percentage concentration of 5% and water until a filtrate is neutral; then, drying the filter cake at 70 ℃ to constant weight, and grinding and screening the filter cake into powder with the particle size of 1.2 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 90: 7, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 70 ℃ for 3h, standing for 3h, filtering, drying a filter cake at the temperature of 90 ℃ to constant weight, and grinding and sieving the filter cake into powder with the particle size of 0.5 mu m to obtain surface-activated talcum powder;
(5) respectively weighing surface-activated talcum powder, lignin and water according to the mass ratio of 100: 60: 70, mixing the surface-activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing at a high speed for 20min, then putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 8h on a ball mill at the rotating speed of 280rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate according to the metering ratio;
(8) uniformly mixing polylactic acid, modified straw powder and a plasticizer DOP mechanically, then placing the mixture into a double-screw extruder, and preparing polylactic acid-based blended granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are 170 ℃, 172 ℃ and 186 ℃ respectively;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 114 ℃, 117 ℃ and 121 ℃;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are 161 ℃, 162 ℃ and 175 ℃ respectively.
Example 4: the polylactic acid-based biomass composite material plate comprises the following components:
Figure BSA0000198167870000071
the modified straw powder is modified wheat straw powder, and the average particle size is 80 meshes.
The talcum powder/lignin composite material is a powdery material, and the average grain diameter is 3 mu m.
A preparation method of a polylactic acid-based biomass composite plate comprises the following molding process:
(1) completely immersing the straw powder in an acetone solution for 60min, then filtering until no acetone solution drops in the straw powder, completely immersing the filtered and dried straw powder in a hydrochloric acid solution with the mass percent concentration of 6% for 25min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered and dried straw powder in a NaOH aqueous solution with the mass percent concentration of 20% for 60min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and screening into 60-mesh powder to obtain pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 2000: 0.1: 2: 330, adding the pretreated straw powder, the water, the tetrabutylammonium acetate and the N, N-dimethylacetamide into a container, stirring and dispersing for 20min at 50 ℃, then adding butyl acrylate, reacting for 60min at 78 ℃, cooling the mixture to room temperature after the reaction is finished, drying and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.12mol/L phenol ethanol solution according to the mass ratio of 100: 1500, mixing, stirring at 90 ℃ for 3.5h, standing, carrying out suction filtration, and repeatedly washing a filter cake by using 5% NaOH aqueous solution and water in sequence until the filtrate is neutral; then, drying the filter cake at 60 ℃ to constant weight, and grinding and screening the filter cake into powder with the particle size of 1.0 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 90: 5, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 65 ℃ for 3 hours, standing for 2 hours, filtering, drying a filter cake at the temperature of 85 ℃ to constant weight, and grinding and sieving the filter cake into powder with the particle size of 0.5 mu m to obtain surface-activated talcum powder;
(5) respectively weighing surface-activated talcum powder, lignin and water according to the mass ratio of 100: 40: 60, mixing the surface-activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing at a high speed for 20min, then putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 7h on a ball mill at the rotating speed of 240rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate according to the metering ratio;
(8) uniformly mixing polylactic acid, modified straw powder and a plasticizer DOP mechanically, then placing the mixture into a double-screw extruder, and preparing polylactic acid-based blended granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are 170 ℃, 170 ℃ and 183 ℃ respectively;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 114 ℃, 113 ℃ and 118 ℃;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are 161 ℃, 160 ℃ and 170 ℃ respectively.
Example 5: the polylactic acid-based biomass composite material plate comprises the following components:
Figure BSA0000198167870000081
the modified rice straw powder is modified rice straw powder, and the average particle size is 120 meshes.
The talcum powder/lignin composite material is a powdery material, and the average grain diameter is 5 mu m.
A preparation method of a polylactic acid-based biomass composite plate comprises the following molding process:
(1) completely immersing the straw powder in an acetone solution for 30min, then filtering until no acetone solution drops in the straw powder, completely immersing the filtered and dried straw powder in a hydrochloric acid solution with the mass percent concentration of 8% for 30min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered and dried straw powder in a NaOH aqueous solution with the mass percent concentration of 10% for 75min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and screening into 100-mesh powder to obtain the pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 1500: 0.2: 3: 230, adding the pretreated straw powder, the water, the tetrabutylammonium acetate and the N, N-dimethylacetamide into a container, stirring and dispersing for 25min at the temperature of 60 ℃, then adding butyl acrylate, reacting for 70min at the temperature of 70 ℃, cooling the mixture to room temperature after the reaction is finished, drying and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.08mol/L phenol ethanol solution according to the mass ratio of 100: 1800, mixing, stirring at 95 ℃ for 4 hours, standing, carrying out suction filtration, and repeatedly washing a filter cake by using NaOH aqueous solution with the mass percentage concentration of 3% and water until a filtrate is neutral; then, drying the filter cake at 65 ℃ to constant weight, and grinding and screening the filter cake into powder with the particle size of 1.2 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 50: 6, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 70 ℃ for 2h, standing for 2.5h, filtering, drying a filter cake at the temperature of 90 ℃ to constant weight, and grinding and sieving into powder with the particle size of 0.1 mu m to obtain the surface-activated talcum powder;
(5) respectively weighing surface-activated talcum powder, lignin and water according to the mass ratio of 100: 50: 70, mixing the surface-activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing at a high speed for 10min, then putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 8h on a ball mill at the rotating speed of 260rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate according to the metering ratio;
(8) uniformly mechanically mixing polylactic acid, modified straw powder and a plasticizer DOP, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization, extrusion and granulation to prepare polylactic acid-based blending granules, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 165 ℃, 171 ℃ and 186 ℃;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 110 ℃, 115 ℃ and 121 ℃;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are 155 ℃, 161 ℃ and 175 ℃ respectively.
Example 6: the polylactic acid-based biomass composite material plate comprises the following components:
Figure BSA0000198167870000091
Figure BSA0000198167870000101
the modified straw powder is modified sesame straw powder, and the average particle size is 160 meshes.
The talcum powder/lignin composite material is a powdery material, and the average grain diameter is 1 mu m.
A preparation method of a polylactic acid-based biomass composite plate comprises the following molding process:
(1) completely immersing the straw powder in an acetone solution for 45min, then filtering until no acetone solution drops in the straw powder, completely immersing the filtered and dried straw powder in a hydrochloric acid solution with the mass percentage concentration of 10% for 20min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered and dried straw powder in a NaOH aqueous solution with the mass percentage concentration of 15% for 90min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and screening into 20-mesh powder to obtain pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 1750: 0.3: 1: 280, adding the pretreated straw powder, the water, the tetrabutylammonium acetate and the N, N-dimethylacetamide into a container, stirring and dispersing for 15min at 70 ℃, then adding butyl acrylate, reacting for 80min at 74 ℃, cooling the mixture to room temperature after the reaction is finished, drying and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.08mol/L phenol ethanol solution according to the mass ratio of 100: 1800, mixing, stirring at 95 ℃ for 4 hours, standing, carrying out suction filtration, and repeatedly washing a filter cake by using NaOH aqueous solution with the mass percentage concentration of 3% and water until a filtrate is neutral; then, drying the filter cake at 65 ℃ to constant weight, and grinding and screening the filter cake into powder with the particle size of 1.2 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 50: 6, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 70 ℃ for 2h, standing for 2.5h, filtering, drying a filter cake at the temperature of 90 ℃ to constant weight, and grinding and sieving into powder with the particle size of 0.1 mu m to obtain the surface-activated talcum powder;
(5) respectively weighing surface-activated talcum powder, lignin and water according to the mass ratio of 100: 50: 70, mixing the surface-activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing at a high speed for 10min, then putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 8h on a ball mill at the rotating speed of 260rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate according to the metering ratio;
(8) uniformly mixing polylactic acid, modified straw powder and a plasticizer DOP mechanically, then placing the mixture into a double-screw extruder, and preparing polylactic acid-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are 167.5 ℃, 172 ℃ and 180 ℃ respectively;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 114 ℃, 113 ℃ and 118 ℃;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are 161 ℃, 160 ℃ and 170 ℃ respectively.
Example 7: the polylactic acid-based biomass composite material plate comprises the following components:
Figure BSA0000198167870000111
the modified straw powder is modified corn straw powder, and the average grain size is 120 meshes.
The talcum powder/lignin composite material is a powdery material, and the average grain diameter is 3 mu m.
A preparation method of a polylactic acid-based biomass composite plate comprises the following molding process:
(1) completely immersing the straw powder in an acetone solution for 30min, then filtering until no acetone solution drops in the straw powder, completely immersing the filtered and dried straw powder in a hydrochloric acid solution with the mass percent concentration of 6% for 30min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered and dried straw powder in a NaOH aqueous solution with the mass percent concentration of 20% for 60min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and screening into 20-mesh powder to obtain the pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 2000: 0.3: 2: 280, adding the pretreated straw powder, the water, the tetrabutylammonium acetate and the N, N-dimethylacetamide into a container, stirring and dispersing for 15min at 50 ℃, then adding butyl acrylate, reacting for 70min at 74 ℃, cooling the mixture to room temperature after the reaction is finished, drying and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.12mol/L phenol ethanol solution according to the mass ratio of 100: 1800, mixing, stirring at 95 ℃ for 3.5h, standing, carrying out suction filtration, and repeatedly washing a filter cake by using 5% NaOH aqueous solution and water in sequence until a filtrate is neutral; then, drying the filter cake at 70 ℃ to constant weight, and grinding and screening the filter cake into powder with the particle size of 0.8 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 50: 7, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 60 ℃ for 2.5h, standing for 2h, filtering, drying a filter cake at the temperature of 85 ℃ to constant weight, and grinding and sieving into powder with the particle size of 0.3 mu m to obtain the surface-activated talcum powder;
(5) respectively weighing surface-activated talcum powder, lignin and water according to the mass ratio of 100: 60: 50, mixing the surface-activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing at a high speed for 20min, then putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 6h on a ball mill at the rotating speed of 280rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate according to the metering ratio;
(8) uniformly mixing polylactic acid, modified straw powder and a plasticizer DOP mechanically, then placing the mixture into a double-screw extruder, and preparing polylactic acid-based blended granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are 165 ℃, 172 ℃ and 180 ℃ respectively;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 112 ℃, 117 ℃ and 115 ℃;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are 158 ℃, 162 ℃ and 165 ℃ respectively.
Example 8: the polylactic acid-based biomass composite material plate comprises the following components:
Figure BSA0000198167870000121
the modified straw powder is modified wheat straw powder, and the average grain size is 100 meshes.
The talcum powder/lignin composite material is a powdery material, and the average grain diameter is 2 mu m.
A preparation method of a polylactic acid-based biomass composite plate comprises the following molding process:
(1) completely immersing the straw powder in an acetone solution for 35min, then filtering until no acetone solution drops in the straw powder, completely immersing the filtered and dried straw powder in a hydrochloric acid solution with the mass percent concentration of 7% for 26min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered and dried straw powder in a NaOH aqueous solution with the mass percent concentration of 12% for 70min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and sieving into 80-mesh powder to obtain the pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 1600: 0.15: 1.3: 260, adding the pretreated straw powder, the water, the tetrabutylammonium acetate and the N, N-dimethylacetamide into a container, stirring and dispersing for 18min at 55 ℃, then adding butyl acrylate, reacting for 68min at 72 ℃, cooling the mixture to room temperature after the reaction is finished, drying and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.09mol/L phenol ethanol solution according to the mass ratio of 100: 1300, mixing, stirring at 96 ℃ for 3.4h, standing, carrying out suction filtration, and repeatedly washing a filter cake by using NaOH aqueous solution with the mass percentage concentration of 3.5% and water until a filtrate is neutral; then, drying the filter cake at 66 ℃ to constant weight, and grinding and screening the filter cake into powder with the particle size of 0.9 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 60: 5.6, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 66 ℃ for 2.3h, standing for 2.3h, filtering, drying a filter cake at the temperature of 84 ℃ to constant weight, and dividing the filter cake into powder with the particle size of 0.4 mu m by a grinding sieve to obtain surface-activated talcum powder;
(5) respectively weighing surface-activated talcum powder, lignin and water according to the mass ratio of 100: 45: 56, mixing the surface-activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing at a high speed for 12min, then putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 6.5h on a ball mill at the rotating speed of 270rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate according to the metering ratio;
(8) uniformly mixing polylactic acid, modified straw powder and a plasticizer DOP mechanically, then placing the mixture into a double-screw extruder, and preparing polylactic acid-based blended granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are 167 ℃, 170.5 ℃ and 182 ℃ respectively;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are 111 ℃, 116 ℃ and 119 ℃ respectively;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are 159 ℃, 161.5 ℃ and 168 ℃ respectively.
The following tests reflect the effects of example 1:
the bending strength is 48.68MPa, the bending modulus is 822.02MPa, the tensile strength is 26.25MPa, and the tensile modulus is 526.82 MPa; the bending strength retention rate is 54.25 percent and the bending modulus retention rate is 46.26 percent when the natural environment is buried for 3 months; the tensile strength retention rate is 46.32 percent, and the tensile modulus retention rate is 32.88 percent.
The detection result shows that the composite material plate has higher mechanical property and can meet the use requirement of a common non-bearing structure; after 3 months of soil burying, the bending property and the tensile property are obviously reduced, and the soil burying has higher degradation rate and excellent degradability under the condition of soil burying.

Claims (1)

1. The manufacturing method of the polylactic acid-based biomass composite material plate is characterized by comprising the following steps of:
(1) completely immersing the straw powder in an acetone solution for 30-60min, filtering until no acetone solution drops in the straw powder, completely immersing the filtered straw powder in a hydrochloric acid solution with the mass percent concentration of 6-10% for 20-30min, filtering again until no hydrochloric acid solution drops in the straw powder, completely immersing the filtered straw powder in a NaOH aqueous solution with the mass percent concentration of 10-20% for 60-90min, washing with water, ethanol and acetone in sequence after treatment until the washing liquid is neutral, drying the washed straw powder to constant weight, grinding, and screening into 20-100 meshes of powder to obtain the pretreated straw powder;
(2) respectively weighing pretreated straw powder, water, tetrabutylammonium acetate, N-dimethylacetamide and butyl acrylate according to the mass ratio of 100: 1500-2000: 0.1-0.3: 1-3: 230-330, adding the pretreated straw powder, water, tetrabutylammonium acetate and N, N-dimethylacetamide into a container, stirring and dispersing for 15-25min at 50-70 ℃, then adding butyl acrylate, reacting for 60-80min at 70-78 ℃, cooling the mixture to room temperature after the reaction is finished, drying, and screening to obtain modified straw powder;
(3) respectively weighing talcum powder and 0.08-0.12mol/L phenol ethanol solution according to the mass ratio of 100: 1200-1800, mixing, stirring for 3-4h at 90-100 ℃, standing, performing suction filtration, and repeatedly washing a filter cake by using NaOH aqueous solution with the mass percentage concentration of 3-5% and water until the filtrate is neutral; then, drying the filter cake at 60-70 ℃ to constant weight, grinding and sieving into powder with the particle size of 0.8-1.2 mu m to obtain modified talcum powder;
(4) respectively weighing modified talcum powder, water and hexadecyl trimethyl ammonium bromide according to the mass ratio of 100: 50-90: 5-7, uniformly mixing the modified talcum powder and the water, adding the hexadecyl trimethyl ammonium bromide, stirring at the constant temperature of 60-70 ℃ for 2-3h, standing for 2-3h, filtering, drying a filter cake at the temperature of 80-90 ℃ to constant weight, and dividing the filter cake into powder with the particle size of 0.1-0.5 mu m by a grinding sieve to obtain surface activated talcum powder;
(5) respectively weighing surface activated talcum powder, lignin and water according to the mass ratio of 100: 40-60: 50-70, mixing the surface activated talcum powder and the lignin at room temperature, then adding the water, mechanically mixing at a high speed for 10-20min, then putting the mixture into a ball milling tank, and carrying out wet ball milling on the mixture for 6-8h on a ball mill at the rotating speed of 240-280rpm to obtain lignin-talcum powder composite slurry;
(6) fully drying the lignin-talcum powder composite slurry to constant weight, grinding and screening to obtain a talcum powder/lignin composite material;
(7) respectively weighing 100kg, 23kg, 46kg, 12kg, 4.6kg and 12kg of polylactic acid, polybutylene succinate, modified straw powder, talcum powder/lignin composite material, plasticizer DOP and acetyl tributyl citrate;
(8) uniformly mechanically mixing polylactic acid, modified straw powder and a plasticizer DOP, then placing the mixture into a double-screw extruder, and preparing polylactic acid-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 165-170 ℃, 170-172 ℃ and 180-186 ℃;
(9) mechanically and uniformly mixing polybutylene succinate and a talcum powder/lignin composite material, then placing the mixture into a double-screw extruder, and preparing polybutylene succinate-based blending granules through high-temperature melting plasticization, extrusion and granulation, wherein the extrusion temperatures of a feeding section, a melting section and a homogenizing section are respectively 110-;
(10) mechanically and uniformly mixing polylactic acid-based blending granules, polybutylene succinate-based blending granules and acetyl tributyl citrate, then placing the mixture into a double-screw extruder, and carrying out high-temperature melting plasticization and extrusion to obtain a polylactic acid-based biomass composite plate; the extrusion temperatures of the feeding section, the melting section and the homogenizing section are respectively 155-;
the modified straw powder is one of modified rice straw powder, modified sesame straw powder, modified corn straw powder and modified wheat straw powder, and has an average particle size of 80-160 meshes;
the talcum powder/lignin composite material is a powdery material, and the average grain diameter is 1-5 mu m.
CN201911341931.7A 2019-12-23 2019-12-23 Polylactic acid-based biomass composite material plate and preparation method thereof Active CN111057356B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201911341931.7A CN111057356B (en) 2019-12-23 2019-12-23 Polylactic acid-based biomass composite material plate and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201911341931.7A CN111057356B (en) 2019-12-23 2019-12-23 Polylactic acid-based biomass composite material plate and preparation method thereof

Publications (2)

Publication Number Publication Date
CN111057356A CN111057356A (en) 2020-04-24
CN111057356B true CN111057356B (en) 2021-11-12

Family

ID=70302641

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201911341931.7A Active CN111057356B (en) 2019-12-23 2019-12-23 Polylactic acid-based biomass composite material plate and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111057356B (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112724612B (en) * 2020-12-09 2022-06-14 南京林业大学 Preparation method of heterogeneous lignin/polylactic acid composite material
CN112920567A (en) * 2021-03-05 2021-06-08 柳州塑友科技有限公司 Wheat straw filled modified PLA fully-degradable plastic and preparation method thereof
CN114517006B (en) * 2022-02-23 2024-01-02 佛山市湘聚新材料有限公司 Bio-based degradable plastic and preparation method thereof
CN115141495A (en) * 2022-07-25 2022-10-04 江苏中科睿赛污染控制工程有限公司 Reinforced and toughened degradable material and preparation method thereof
CN116396596A (en) * 2022-12-15 2023-07-07 富岭科技股份有限公司 Nanocellulose fully degradable cutlery box and preparation process

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104072957A (en) * 2014-06-20 2014-10-01 清华大学深圳研究生院 Food grade biodegradable polylactic acid-based composite material and application thereof
CN105315688A (en) * 2014-07-31 2016-02-10 南京工业大学 Modification and use methods for straw biomass
CN106336531A (en) * 2016-09-12 2017-01-18 葛袁园 Modified corn straw granule enhanced PBAT [poly(butyleneadipate-co-terephthalate)] starch composite material and preparation method thereof
CN108117712A (en) * 2017-11-14 2018-06-05 云南大学 A kind of preparation method of plastic stalk door-window section bar PP Pipe Compound
CN108467577A (en) * 2018-04-08 2018-08-31 赵建平 A kind of preparation method of self-reinforcing lactic acid composite material

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1363625A (en) * 2001-11-15 2002-08-14 天津丹海股份有限公司 Process for preparing bio-degradable resin
CN106189325A (en) * 2016-08-04 2016-12-07 南京工业大学 A kind of lignin enhancement mode Wood-plastic material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104072957A (en) * 2014-06-20 2014-10-01 清华大学深圳研究生院 Food grade biodegradable polylactic acid-based composite material and application thereof
CN105315688A (en) * 2014-07-31 2016-02-10 南京工业大学 Modification and use methods for straw biomass
CN106336531A (en) * 2016-09-12 2017-01-18 葛袁园 Modified corn straw granule enhanced PBAT [poly(butyleneadipate-co-terephthalate)] starch composite material and preparation method thereof
CN108117712A (en) * 2017-11-14 2018-06-05 云南大学 A kind of preparation method of plastic stalk door-window section bar PP Pipe Compound
CN108467577A (en) * 2018-04-08 2018-08-31 赵建平 A kind of preparation method of self-reinforcing lactic acid composite material

Also Published As

Publication number Publication date
CN111057356A (en) 2020-04-24

Similar Documents

Publication Publication Date Title
CN111057356B (en) Polylactic acid-based biomass composite material plate and preparation method thereof
CN102504560B (en) Degradable seedling culture container, and preparation method and application thereof
CN101602882B (en) Bamboo powder filled biomass-based resin composite material and preparation method thereof
CN104693707B (en) A kind of polylactic acid/starch/flaxen fiber Biobased degradable composite material and preparation method thereof
CN101781467B (en) Biomass-synthetic plastic product and method for preparing same
CN101942117B (en) Starch-based fully degraded packaging material and preparation method thereof
WO2009043580A1 (en) Biodegradable composition, preparation method and their application in the manufacture of functional containers for agricultural and/or forestry use
CN103275472B (en) All-bio-based hard polylactic acid composite material and preparation method thereof
CN103214695B (en) Chaff starch completely-biodegradable environmental protection material
CN110467736B (en) Biodegradable plastic woven bag production process
CN103183936A (en) Biodegradable composite material prepared by excessive processing materials of high-starch crops and preparation method thereof
Bastioli Starch-based technology
CN101693773A (en) Acorn powder/polycaprolactone composite material and preparation method thereof
CN103709773B (en) The preparation method of alkali urea disentanglement stalk/resin composite plates
CN107603254A (en) A kind of degradable disponsable tableware and preparation method thereof
CN104499380A (en) Method for producing seedling breeding container from fibrous solid wastes
CN107793780A (en) A kind of Based Full-degradable Plastics Film and preparation method thereof
CN101735484A (en) Degradable plastic, container prepared by same, and preparation method thereof
Bastioli et al. Starch
CN108285603A (en) A kind of degradable high-barrier composite material and preparation method thereof
CN111848998A (en) Environment-friendly degradable cotton cellulose plastic film and preparation method and application thereof
CN106046835A (en) Corn stalk plant fiber synthetic resin and preparation technology thereof
CN111574813A (en) Polylactic acid-based biomass composite material and 3D printing forming thereof
CN107840991A (en) A kind of Based Full-degradable Plastics Film and preparation method thereof
CN111334060A (en) Preparation method of bamboo fiber polylactic acid composite plastic capable of being rapidly refined and degraded

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20240528

Address after: 313118 Baixian Industrial Concentration Area, Meishan Town, Changxing County, Huzhou City, Zhejiang Province

Patentee after: ZHEJIANG GUANSEN NEW MATERIAL CO.,LTD.

Country or region after: China

Address before: 214264 Fangqiao Village, Fangqiao Street, Yixing City, Jiangsu Province

Patentee before: Jiangsu yulinsheng plastic wood technology Co.,Ltd.

Country or region before: China