CN113416399A - Plant-based material and preparation method and application thereof - Google Patents
Plant-based material and preparation method and application thereof Download PDFInfo
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- CN113416399A CN113416399A CN202110903448.4A CN202110903448A CN113416399A CN 113416399 A CN113416399 A CN 113416399A CN 202110903448 A CN202110903448 A CN 202110903448A CN 113416399 A CN113416399 A CN 113416399A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/06—Biodegradable
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The invention provides a plant-based material which is prepared from the following components in percentage by mass: polylactic acid: 60% -85%; toughening resin: 7% -15%; coffee grounds: 5% -30%; the balance of auxiliary agents; the sum of the mass percentages of the components is 100 percent. The invention uses eccentric rotor stretching rheological plasticizing extrusion equipment to process PLA, PBAT or PBS, coffee grounds, other auxiliary agents and the like according to a certain proportion to obtain modified materials or products.
Description
Technical Field
The invention relates to the field of plastic processing, in particular to a plant-based material and a preparation method and application thereof.
Background
Coffee is one of the most popular drinks and also one of the most widely traded commodities in international trade. Coffee grounds are a by-product remaining after extraction of coffee from coffee beans and account for approximately 2/3 parts by weight of the dried coffee beans. The coffee grounds contain rich grease, saccharides and protein, cellulose, acid (amino acid, chlorogenic acid, other fatty acid) and the like, wherein the content of the coffee oil is about 14 percent, and the coffee oil contains 4 main fatty acids accounting for 95.25 percent of the total amount of the fatty acids, namely, linoleic acid 34.79 percent, oleic acid 9.85 percent, palmitic acid 42.12 percent and stearic acid 8.49 percent respectively. Coffee grounds have a strong coffee aroma, in which volatile fats are the main source of coffee aroma and emit about forty aromatic substances. And the dyeing property is extremely strong. The application directions of the coffee grounds at present are as follows: animal functional feed, fungus culture medium, adsorptive active carbon, coffee oil extraction, fuel, etc.
The coffee grounds have the following characteristics: high water content, high acidity value and large organic load.
At present, food contact materials mainly comprise polypropylene, polystyrene, polyethylene and the like, but the materials can not be effectively degraded when being exposed in natural environment, white pollution is caused, and certain pressure is brought to environmental protection; 2. secreting biological enzyme to catalyze ester hydrolysis reaction, and breaking high molecular chain into low molecular chain fragments; 3. bioabsorption, and final conversion to carbon dioxide and water.
The traditional processing machinery and forming equipment have destructive effect on heat-sensitive PLA materials, poor compatibility between coffee grounds and PLA resin and poor dispersibility of the coffee grounds.
Disclosure of Invention
In a first aspect: therefore, aiming at the problems that the existing formula for producing the plant-based material by using the coffee grounds cannot be completely degraded, the degradation time is long, the cost is high, and some raw materials used do not meet the standard requirements of food contact materials, the invention provides the plant-based material which can be completely degraded, has short degradation time, lower preparation cost and environmental protection, and realizes the green cycle high-valued utilization of the coffee grounds.
The invention provides a plant-based material which is prepared from the following components in percentage by mass:
polylactic acid: 60% -85%;
toughening resin: 7% -15%;
coffee grounds: 5% -30%;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent.
Optionally, the composition is prepared from the following components in percentage by mass:
polylactic acid: 65-80 percent;
toughening resin: 9 to 12 percent;
coffee grounds: 15 to 25 percent;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent.
Optionally, the composition is prepared from the following components in percentage by mass:
polylactic acid: 67.2 percent;
toughening resin: 10 percent;
coffee grounds: 20 percent;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent;
or the like, or, alternatively,
polylactic acid: 70.2 percent;
toughening resin: 10 percent;
coffee grounds: 15 percent;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent;
or the like, or, alternatively,
polylactic acid: 77.2 percent;
toughening resin: 10 percent;
coffee grounds: 16 percent;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent;
or, polylactic acid: 84.2 percent;
toughening resin: 8 percent;
coffee grounds: 5 percent;
the balance of auxiliary agents.
Optionally, the auxiliary agent is at least one of a nucleating agent, a dispersing agent, a plasticizer and an antioxidant. Optionally, the auxiliary agent is a nucleating agent, an antioxidant and a plasticizer; optionally, the mass percentage of the nucleating agent is 0.5% -1%; the mass percentage of the plasticizer is 1-2%; the mass percentage of the antioxidant is 0.3-0.8%.
Optionally, the nucleating agent comprises at least one of talc, montmorillonite and silica;
the dispersant comprises at least one of N, N' -ethylene bis stearamide and N, N-ethylene oleamide;
the plasticizer comprises at least one of acetyl tributyl citrate and epoxidized soybean oil;
the antioxidant comprises at least one of an antioxidant 168, an antioxidant 1010, 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane, isooctyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) acrylate, pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and dilauryl thiodipropionate.
Optionally, the toughening resin comprises at least one of PBAT and PBS.
In a second aspect: therefore, aiming at the industry pain point that the traditional processing machinery and forming equipment have large damage and poor dispersion on the forming processing of the degradable materials and the coffee grounds, so that the prepared plant-based materials have poor tensile property and impact property, the invention provides the preparation method of the plant-based materials based on the concept of 'green environmental protection', which can improve the plasticizing forming and dispersion effects on the degradable materials and the coffee grounds, and finally improve the tensile property and the impact property of the plant-based materials, and the method can prepare the high-performance coffee grounds bio-based composite materials. The preparation method of the plant-based material realizes green cycle high-value utilization of coffee grounds.
The preparation method of the plant-based material comprises the following steps:
1) weighing polylactic resin, toughening resin and an auxiliary agent according to a proportion, adding into a mixer, and uniformly mixing to obtain a material 1;
2) adding coffee grounds into the material 1 and then uniformly mixing to obtain a material 2;
3) and (3) carrying out melt extrusion granulation by adopting an eccentric rotor extensional rheology plasticizing extrusion device.
Optionally, the eccentricity of the eccentric rotor extensional rheology plasticizing extrusion device is 1-5 mm; the number of the eccentric straight line segments of the rotor is 4-6; the compression ratio of the maximum pitch and the minimum pitch of the rotor is 2-5.
Optionally, the eccentricity of the eccentric rotor extensional rheology plasticizing extrusion equipment is 1.5-3 mm; the number of the rotor eccentric straight line segments is 5 or 6; the compression ratio of the maximum pitch and the minimum pitch of the rotor is 2.0-3.6.
Optionally, the extrusion temperature in the preparation process is as follows: 150 ℃ and 190 ℃, extrusion speed: 200 to 500 rpm.
Optionally, the coffee grounds are ground to a particle size of 40-150 mesh.
The application of the plant-based material in preparing food contact materials; optionally, the food contact material is a disposable beverage material or a disposable food packaging material; the food packaging material is a disposable plastic lunch box or a disposable food bag.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention provides a plant-based material which is prepared from the following components in percentage by mass: polylactic acid: 60% -85%; toughening resin: 7% -15%; coffee grounds: 5% -30%;
the balance of auxiliary agents; the sum of the mass percentages of the components is 100 percent. The plant-based material can be completely degraded, has short degradation time, lower preparation cost and environmental protection, and realizes the green cycle high-value utilization of coffee grounds.
2. The invention provides a preparation method of a plant-based material, and the processing technology of the used eccentric rotor extensional rheology extrusion equipment breaks through the international problem of processing of the plant-based biodegradable composite material. Aiming at the characteristics of the coffee grounds biodegradable composite material, the invention optimizes and improves the structure of the equipment, can improve the plasticizing and forming effect of the plant-based material and the dispersion effect of the coffee grounds, and finally improves the tensile property and the impact property of the plant-based material, the improved equipment can reduce the damage effect on the heat-sensitive PLA material, increases the compatibility of the coffee grounds and the PLA resin, is beneficial to the dispersion and orientation of the coffee grounds along the extrusion direction, and prepares the high-performance coffee grounds biodegradable composite material.
3. The invention expands the high-level application of the coffee grounds, so that the coffee grounds can be applied to food contact materials, such as disposable beverage materials and food packaging materials, and the materials can be naturally degraded. Meets different processing requirements, such as extrusion, injection molding and the like.
4. The plant based material of the invention meets the relevant regulations in chinese regulations regarding food contact materials.
5. Under the condition of high content of coffee grounds, the plasticizer can increase the fluidity of a melt, the nucleating agent is beneficial to refining crystals, the toughness is improved, the dispersity of the coffee grounds is increased, the addition amount of the coffee grounds is increased, the coffee aroma of the material is strong, the biodegradation performance of the biodegradable composite material is also greatly improved, and according to tests, a straw made of the raw material can be degraded by 90% within 4 months.
6. The application effectively utilizes the coffee grounds, improves the application range and the application depth of the coffee grounds, reduces the white garbage and lightens the environmental protection pressure.
7. The invention obtains the plant-based material by processing PLA, PBAT or PBS, coffee grounds, other auxiliary agents and the like according to a certain proportion through extensional rheology plasticizing extrusion.
Detailed Description
The melt index of the polylactic acid is 3-40g/min at the ambient temperature of 190 ℃ and the load of 2.16 Kg.
Example 1 plant-based Material and method of making the same
The formula of the plant-based material comprises: 67.2% of polylactic resin, 10% of PBAT, 20% of coffee grounds, 0.5% of nucleating agent, 2% of plasticizer and 0.3% of antioxidant; the percentages are mass percentages; the nucleating agent is talcum powder, the plasticizer is acetyl tributyl citrate, and the antioxidant is antioxidant 168.
The preparation method of the plant-based material comprises the following steps:
1. drying the polylactic resin, the toughening resin (PBAT) and the coffee grounds, and grinding the coffee grounds to 40 meshes.
2. Weighing polylactic resin, PBAT and auxiliaries (namely nucleating agent, plasticizer and antioxidant) according to a proportion, adding the weighed materials into a mixer, uniformly mixing, adding coffee grounds, uniformly mixing, and performing melt extrusion granulation by adopting an eccentric rotor extensional rheology plasticizing extrusion device, wherein in the embodiment, CN104002447A (an eccentric rotor volume pulsation deformation plasticizing and transporting method and device) is adopted, and the eccentric rotor volume pulsation deformation plasticizing and transporting device in embodiment 1 is independently used as an extruder to obtain a plant-based material; the rotor structure is designed to have the eccentricity e of 1.5mm, the number of the eccentric straight-line segments of the rotor is 4, and the compression ratio of the maximum pitch and the minimum pitch of the rotor is 2.0. Extrusion temperature in the preparation process: 150 ℃ and 190 ℃, extrusion speed: 200 to 500 rpm.
Example 2 plant-based Material and method of making the same
The formula of the plant-based material comprises: 67.2% of polylactic resin, 10% of PBS, 20% of coffee grounds, 0.5% of nucleating agent, 2% of plasticizer and 0.3% of antioxidant; the percentages are mass percentages; the nucleating agent is montmorillonite, the plasticizer is epoxidized soybean oil, and the antioxidant is antioxidant 1010.
The preparation method of the plant-based material comprises the following steps:
1. drying the polylactic resin, the toughened resin (PBS) and the coffee grounds, and grinding the coffee grounds to a particle size of 60 meshes.
2. Then weighing polylactic resin, PBS and auxiliary agents (namely nucleating agent, plasticizer and antioxidant) according to a certain proportion, adding the polylactic resin, PBS and auxiliary agents into a mixer, uniformly mixing, adding coffee grounds, uniformly mixing, and then carrying out melt extrusion granulation by adopting extensional rheology plasticizing extrusion equipment, wherein in the embodiment, CN104002447A (an eccentric rotor volume pulsation deformation plasticizing and transporting method and device) is adopted, and the eccentric rotor volume pulsation deformation plasticizing and transporting device in the embodiment 1 is independently used as an extruder to obtain a plant-based material; the rotor structure is designed to have the eccentricity e of 1.5mm, the number of the eccentric straight-line segments of the rotor is 4, and the compression ratio of the maximum pitch and the minimum pitch of the rotor is 3.6. Extrusion temperature in the preparation process: 150 ℃ and 190 ℃, extrusion speed: 200 to 500 rpm.
Example 3 plant-based Material and method of making the same
The formula of the plant-based material comprises: 72.2% of polylactic resin, 10% of PBAT, 15% of coffee grounds, 0.5% of nucleating agent, 2% of plasticizer and 0.3% of antioxidant; the percentages are mass percentages; the nucleating agent is silicon dioxide, the plasticizer is acetyl tributyl citrate, and the antioxidant is 1, 1, 3-tri (2-methyl-4-hydroxy-5-tert-butylphenyl) butane.
The preparation method of the plant-based material comprises the following steps:
1. drying the polylactic resin, the toughening resin (PBAT) and the coffee grounds, and grinding the coffee grounds to 150 meshes;
2. then weighing polylactic resin, PBAT and auxiliaries (namely nucleating agent, plasticizer and antioxidant) according to a proportion, adding the weighed materials into a mixer, uniformly mixing the materials, adding coffee grounds, uniformly mixing the materials, and then carrying out melt extrusion granulation by adopting extensional rheology plasticizing extrusion equipment, wherein in the embodiment, CN104002447A (an eccentric rotor volume pulsation deformation plasticizing and transporting method and device) is adopted, and the eccentric rotor volume pulsation deformation plasticizing and transporting device in the embodiment 1 is independently used as an extruder to obtain a plant-based material; the rotor structure is designed to have the eccentricity e of 3mm, the number of the eccentric straight-line segments of the rotor is 6, and the compression ratio of the maximum pitch and the minimum pitch of the rotor is 2.0. Extrusion temperature in the preparation process: 150 ℃ and 190 ℃, extrusion speed: 200 to 500 rpm.
Example 4 plant-based Material and method of making the same
The formula of the plant-based material comprises: 77.2 percent of polylactic resin, 10 percent of PBAT, 10 percent of coffee grounds, 0.5 percent of nucleating agent, 2 percent of plasticizer and 0.3 percent of antioxidant, wherein the percentages are mass percentages; the nucleating agent is talcum powder, the plasticizer is acetyl tributyl citrate, and the antioxidant is 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) isooctyl acrylate.
The preparation method of the plant-based material comprises the following steps:
1. drying the polylactic resin, the toughening resin (PBAT) and the coffee grounds, and grinding the coffee grounds to 150 meshes.
2. Weighing polylactic resin, PBAT and auxiliaries (namely nucleating agent, plasticizer and antioxidant) according to a proportion, adding the weighed materials into a mixer, uniformly mixing, adding coffee grounds, uniformly mixing, and then carrying out melt extrusion granulation by adopting an eccentric rotor extensional rheology plasticizing extrusion device, wherein in the embodiment, CN104002447A (an eccentric rotor volume pulsation deformation plasticizing and transporting method and device) is adopted, and the eccentric rotor volume pulsation deformation plasticizing and transporting device in the embodiment 1 is independently used as an extruder to obtain a plant-based material; the eccentricity e of the rotor is 3mm, the number of the eccentric straight-line segments of the rotor is 5, and the compression ratio of the maximum pitch and the minimum pitch of the rotor is 3.6.
Extrusion temperature in the preparation process: 150 ℃ and 190 ℃, extrusion speed: 200 to 500 rpm.
Example 5 plant-based Material and method of making the same
The formula of the plant-based material comprises: 84.2 percent of polylactic resin, 8 percent of PBAT, 5 percent of coffee grounds, 1 percent of nucleating agent, 1 percent of plasticizer and 0.8 percent of antioxidant, wherein the percentages are mass percentages; the nucleating agent is talcum powder, the plasticizer is acetyl tributyl citrate, and the antioxidant is 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) isooctyl acrylate.
The preparation method of the plant-based material comprises the following steps:
1. drying the polylactic resin, the toughening resin (PBAT) and the coffee grounds, and grinding the coffee grounds to 150 meshes.
2. Weighing polylactic resin, PBAT and auxiliaries (namely nucleating agent, plasticizer and antioxidant) according to a proportion, adding the weighed materials into a mixer, uniformly mixing, adding coffee grounds, uniformly mixing, and then carrying out melt extrusion granulation by adopting an eccentric rotor extensional rheology plasticizing extrusion device, wherein in the embodiment, CN104002447A (an eccentric rotor volume pulsation deformation plasticizing and transporting method and device) is adopted, and the eccentric rotor volume pulsation deformation plasticizing and transporting device in the embodiment 1 is independently used as an extruder to obtain a plant-based material; the eccentricity e of the rotor is 3mm, the number of the eccentric straight-line segments of the rotor is 6, and the compression ratio of the maximum pitch and the minimum pitch of the rotor is 3.6.
Extrusion temperature in the preparation process: 150 ℃ and 190 ℃, extrusion speed: 200 to 500 rpm.
Comparative example 1
The difference from the embodiment 1 is that the eccentric rotor volume pulsation deformation plasticizing and conveying device in the embodiment 1 is replaced by a double-screw extruder, namely, the double-screw extruder is used for melt extrusion granulation.
Comparative example 2
The only difference from example 1 is that no nucleating agent, plasticizer and antioxidant were added.
Comparative example 3
The difference from comparative example 1 is that the compression ratio of the maximum pitch to the minimum pitch of the rotor is 6.0.
Examples of the experiments
The method for detecting the melt index refers to the GB/T3682-2000 standard; the detection methods of tensile strength, elongation at break and impact property refer to the GB/T1040.1 standard; the detection method of the bending strength and the bending modulus refers to the GB/T9341 standard; the Vicat softening point detection method refers to the GB/T1633 standard, and the biodegradation performance detection method refers to the ISO 14855 standard.
The properties of examples 1 to 4 and comparative examples 1 to 3 are shown in table 1:
TABLE 1
As can be seen from the above table, example 1 has higher tensile strength, elongation at break, flexural strength, flexural modulus and impact property than comparative example 1, and proves that the material obtained by adopting the extensional rheology plasticizing extrusion of the invention has at least remarkable improvement in tensile property and impact property compared with the conventional twin-screw melt extrusion. Example 1 has higher impact properties and flow rate than comparative example 2, indicating that the processing aid used in the present invention facilitates the dispersion of coffee grounds and improves the compatibility of the coffee grounds with the resin matrix. Example 1 has higher tensile strength and impact properties than comparative example 3, which shows that the parameters of the eccentric rotor extensional rheological plasticizing extrusion equipment adopted by the embodiment of the invention reach the optimal structural parameters.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (12)
1. The plant-based material is characterized by being prepared from the following components in percentage by mass:
polylactic acid: 60% -85%;
toughening resin: 7% -15%;
coffee grounds: 5% -30%;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent.
2. The plant-based material according to claim 1, wherein the plant-based material is prepared from the following components in percentage by mass:
polylactic acid: 65-80 percent;
toughening resin: 9 to 12 percent;
coffee grounds: 15 to 25 percent;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent.
3. The plant-based material according to claim 1 or 2, characterized in that it is prepared from the following components in mass percent:
polylactic acid: 67.2 percent;
toughening resin: 10 percent;
coffee grounds: 20 percent;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent;
or the like, or, alternatively,
polylactic acid: 70.2 percent;
toughening resin: 10 percent;
coffee grounds: 15 percent;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent;
or the like, or, alternatively,
polylactic acid: 77.2 percent;
toughening resin: 10 percent;
coffee grounds: 16 percent;
the balance of auxiliary agents;
the sum of the mass percentages of the components is 100 percent;
or, polylactic acid: 84.2 percent;
toughening resin: 8 percent;
coffee grounds: 5 percent;
the balance of auxiliary agents.
4. The plant-based material of claim 1, wherein the adjuvant is at least one of a nucleating agent, a dispersant, a plasticizer, and an antioxidant; optionally, the auxiliary agent is a nucleating agent, an antioxidant and a plasticizer; optionally, the mass percentage of the nucleating agent is 0.5% -1%; the mass percentage of the plasticizer is 1-2%; the mass percentage of the antioxidant is 0.3-0.8%.
5. The plant-based material of claim 4, wherein the nucleating agent comprises at least one of talc, montmorillonite, and silica;
the dispersant comprises at least one of N, N' -ethylene bis stearamide and N, N-ethylene oleamide;
the plasticizer comprises at least one of acetyl tributyl citrate and epoxidized soybean oil;
the antioxidant comprises at least one of an antioxidant 168, an antioxidant 1010, 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane, isooctyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) acrylate, pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and dilauryl thiodipropionate.
6. The plant-based material of any one of claims 1-5, wherein the toughening resin comprises at least one of PBAT and PBS.
7. A method of preparing a plant based material according to any one of claims 1 to 6, comprising the steps of:
1) weighing polylactic resin, toughening resin and an auxiliary agent according to a proportion, adding into a mixer, and uniformly mixing to obtain a material 1;
2) adding coffee grounds into the material 1 and then uniformly mixing to obtain a material 2;
3) and (3) carrying out melt extrusion granulation by adopting an eccentric rotor extensional rheology plasticizing extrusion device.
8. The method of claim 7, wherein the eccentricity of the eccentric rotor extensional rheological plastification extrusion device is 1-5 mm; the number of the eccentric straight line segments of the rotor is 4-6; the compression ratio of the maximum pitch and the minimum pitch of the rotor is 2-5.
9. The method of claim 7 or 8, wherein the eccentricity of the eccentric rotor extensional rheological plastification extrusion device is 1.5-3 mm; the number of the rotor eccentric straight line segments is 5 or 6; the compression ratio of the maximum pitch and the minimum pitch of the rotor is 2.0-3.6.
10. The method according to any one of claims 7 to 9, wherein the extrusion temperature during the preparation is: 150 ℃ and 190 ℃, extrusion speed: 200 to 500 rpm.
11. The method according to any one of claims 7 to 10, wherein the coffee grounds are ground to a particle size of 40 to 150 mesh.
12. Use of a plant based material according to any one of claims 1 to 6 in the preparation of a food contact material; optionally, the food contact material is a disposable beverage material or a disposable food packaging material; the food packaging material is a disposable plastic lunch box or a disposable food bag.
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| CN112961479A (en) | 2021-06-15 |
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