CN114410080A - Composite material for manufacturing degradable disposable lunch box and preparation method thereof - Google Patents
Composite material for manufacturing degradable disposable lunch box and preparation method thereof Download PDFInfo
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- CN114410080A CN114410080A CN202210105626.3A CN202210105626A CN114410080A CN 114410080 A CN114410080 A CN 114410080A CN 202210105626 A CN202210105626 A CN 202210105626A CN 114410080 A CN114410080 A CN 114410080A
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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
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
Abstract
The invention relates to the field of degradable materials, in particular to a composite material for manufacturing a degradable disposable lunch box and a preparation method thereof. Mixing filler powder, a modifier and deionized water, standing, and removing supernatant to obtain a glue solution; wherein the mass ratio of the filler powder to the deionized water is 1 (3-6); making the glue solution in supercritical CO at 40-70 deg.C2Stirring and reacting under the atmosphere, then obtaining modified filler powder by a solid-liquid separation method, and then drying; mixing the modified filler powder, poly (butylene adipate)/terephthalate, polylactic acid and an initiator, and putting the mixture into a double-screw extruder at the temperature of 150-Then, the mixture is melted, blended, granulated and dried to obtain the composite material. The preparation method of the invention effectively improves the compatibility of the composite material, and the uniformly dispersed filler improves the mechanical property of the composite material.
Description
Technical Field
The invention relates to the technical field of degradable materials, in particular to a degradable composite material.
Background
In recent years, with the continuous development of economy in China, the plastic industry in China also increases at a rate of about 10% per year, the problem of environmental pollution is to be solved urgently, the waste amount of disposable products in plastic waste is the largest, and therefore the search for alternative environment-friendly completely degradable materials becomes a key point.
Taking a disposable lunch box product as an example, plastic products and paper products are mainly used at present, the plastic products are difficult to degrade and cause environmental pollution, and the raw materials of the paper products are trees, so that the environmental problem is also caused by the large-scale felling of the trees. Therefore, how to prepare degradable disposable meal box products has attracted extensive attention from scientists in the material field.
Poly adipic acid/butylene terephthalate (PBAT) is one of biodegradable materials widely used, is ternary copolyester which is polymerized by a direct esterification or ester exchange method on the basis of terephthalic acid, adipic acid, 1, 4-butanediol and a mode unit, has good flexibility and thermal stability, but the low modulus and the low strength limit the application and popularization of the PBAT in multiple fields.
Polylactic acid (PLA) is prepared by extracting and converting renewable plant resources, is one of the most common biodegradable materials, has good biocompatibility and degradability, and can not cause environmental pollution because the degraded final products are carbon dioxide and water. The polylactic acid has good comprehensive performance and high strength, but has very poor toughness and is easy to break.
Patent CN111606347A utilizes low molecular weight polylactic acid to modify calcium carbonate, thereby improving compatibility with polylactic acid, but this method is too complicated and cannot be mass-produced, and cannot meet the increasing practical demand.
The patent CN103589124A utilizes a melt blending method to prepare a PLA/PBAT composite film material, but the method adopts an isocyanate chain extender, and the isocyanate has certain toxicity, and the method has limited improvement on the compatibility of the filler.
Furthermore, the low modulus and strength of poly (butylene adipate terephthalate) (PBAT) limits the application scenarios, while polylactic acid (PLA), although having a high modulus, is inherently hard and brittle, and their combination can improve the respective disadvantages. Although the cost of the cheap filler powder can be reduced, the filler powder, the PBAT and the PLA are only simply and physically blended, the compatibility and the dispersibility are poor, and the improvement on the overall performance of the composite material is not ideal.
Disclosure of Invention
The invention aims to solve the technical problem of providing a composite material for manufacturing a degradable disposable lunch box and a preparation method thereof.
Specifically, the application provides the following technical scheme:
a preparation method of a composite material for manufacturing a degradable disposable lunch box comprises the following steps:
(1) mixing filler powder, a modifier and deionized water, standing, and removing supernatant to obtain glue solution; wherein the mass ratio of the filler powder to the deionized water is 1 (3-6);
(2) making the glue solution in supercritical CO at 40-70 deg.C2Stirring and reacting under the atmosphere, then obtaining modified filler powder by a solid-liquid separation method, and then drying;
(3) mixing the modified filler powder, the poly (butylene adipate)/terephthalate), the polylactic acid and the initiator, performing melt blending granulation on the mixed material in a double-screw extruder at the temperature of 150-200 ℃, and drying to obtain the composite material.
The method modifies the surface of filler powder to make the filler powder contain functional groups, and the filler powder is reactively blended with poly adipic acid/butylene terephthalate (PBAT) and polylactic acid (PLA). The initiator can further promote the reaction process, and simultaneously improve the three-phase compatibility of poly (adipic acid)/butylene terephthalate (PBAT), polylactic acid (PLA) and filler powder, thereby improving the comprehensive mechanical property of the composite material. The compatibility and the dispersibility of the filler are effectively improved by means of combining surface modification and chemical reaction, and the combination condition of the filler powder and the matrix resin interface is improved.
Wherein in the step (1), the rest time is 12-24 h.
Wherein, in the step (2), supercritical CO is adopted2The pressure of the atmosphere is 7-14MPa, the stirring speed is 200-400r/min, and the reaction time is 3-7 h; the drying temperature was 70 ℃.
Wherein, in the step (3), the rotating speed of the double-screw extruder is 150-; the drying temperature was 80 ℃.
Wherein the filler powder is 1-20 parts by weight; 0.1-3 parts of modifier; the total weight of the polybutylene adipate/terephthalate and the polylactic acid is 100 parts by weight; 0.1-2 parts of initiator.
Further, the weight-average molecular weight of the polybutylene adipate/terephthalate is 0-100 parts by weight and 15-40 ten thousand; 0-100 parts of polylactic acid, and the weight average molecular weight is 10-25 ten thousand.
Wherein the filler powder is one or more of calcium carbonate powder, egg shell powder and shell powder; the particle diameter of the filler powder is 50-500 nm.
Wherein, the modifier is organic acid containing various functional groups and/or unsaturated fatty acid and derivatives thereof;
the organic acid containing multiple functional groups is one or more of salicylic acid, malic acid, citric acid, alginic acid, quinic acid, glycolic acid, hydroxyethylidene diphosphonic acid, B-hydroxybutyric acid, gamma-hydroxybutyric acid and hydroxylauric acid;
the unsaturated fatty acid and the derivatives thereof are one or more of cinnamic acid, linoleic acid, linolenic acid, arachidonic acid, ricinoleic acid, hydroxyl-12-octadecanoic acid, 15-hydroxyl-9-cis-octadecanoic acid, 16-hydroxyl-9-cis-octadecanoic acid, 17-hydroxyl-9-cis-octadecanoic acid, 10-hydroxyl-12, 15-octadecanoic acid, 10, 12-dihydroxystearic acid, 10-hydroxystearic acid, 9, 10-dihydroxyoctadecanoic acid, 13, 14-dihydroxyeicosanoic acid and 13(14) -monohydroxy-docosanoic acid.
The initiator is one or more of dicumyl peroxide, benzoyl peroxide, dibenzoyl peroxide, tert-butyl peroxybenzoate, tert-butyl peroxypivalate, diisopropyl peroxydicarbonate, tert-butyl peroxybenzoate, dicyclohexyl peroxydicarbonate, 1-bis (tert-butylperoxy) -3,3, 5-trimethylcyclohexane and dibenzoyl peroxide bis (tert-butylperoxy) diisopropylbenzene.
The composite material prepared by the preparation method can be used for producing degradable disposable lunch boxes.
Compared with the prior art, the composite material for manufacturing the degradable disposable lunch box and the preparation method thereof have the following beneficial effects:
(1) the composite material for manufacturing the degradable disposable lunch box prepared by the method effectively improves the comprehensive mechanical property of the composite material.
(2) The composite material prepared by the method disclosed by the invention is completely degradable, accords with the development concept of green environmental protection, and can be widely applied to products such as disposable lunch boxes and the like.
(3) Compared with the existing method, the preparation method of the invention does not involve the use of organic solvent, has less selected additives, but has definite reaction mechanism and high reaction efficiency, better promotes the compatibility and the dispersibility of the filler, improves the comprehensive performance of the composite material and effectively reduces the cost.
(4) The preparation method of the composite material is simple and efficient, can be used for large-scale production, and has good application prospect.
The composite material for making the degradable disposable lunch box and the preparation method thereof according to the present invention will be further described with reference to the following embodiments.
Detailed Description
The following examples and comparative examples employ the following performance evaluation methods:
and (3) measuring tensile mechanical properties: an Instron 1211 type electronic universal tester is used for testing the tensile mechanical property, a sample is taken from the composite material after blending and granulation, a sheet with the thickness of 1mm is prepared by a flat vulcanizing machine at 180 ℃, the sheet is cut into dumbbell shapes with the size of 20mm multiplied by 4mm multiplied by 1mm according to the ISO527-1:2012 standard, and the final result is the average value of five sample strip measurement values.
Example 1
Raw materials:
poly (butylene adipate/terephthalate), weight average molecular weight 15 ten thousand, 90 parts by weight;
polylactic acid, weight average molecular weight is 10 ten thousand, 10 weight portions;
calcium carbonate powder, 100nm, 5 parts by weight;
glycolic acid, 0.1 part by weight;
dicumyl peroxide, 0.1 weight part.
The preparation process of the composite material of the degradable disposable lunch box comprises the following steps:
(1) mixing calcium carbonate powder, glycolic acid and 15 parts by weight of deionized water, standing for 12 hours, and removing supernatant.
(2) At 40 deg.C, making the glue solution in supercritical CO with pressure of 7MPa2Stirring and reacting for 3h at the speed of 200r/min under the atmosphere, then obtaining modified calcium carbonate powder by a solid-liquid separation method, and drying in a constant-temperature drying oven at 70 ℃.
(3) Mixing the modified calcium carbonate powder, poly (butylene adipate)/terephthalate, polylactic acid and dicumyl peroxide, performing melt blending granulation on the mixed material in a double-screw extruder at the temperature of 160 ℃, setting the rotating speed at 150 revolutions per minute, and drying in a constant-temperature drying oven at the temperature of 80 ℃ to obtain the composite material.
Through performance tests, the Young modulus is 160.4MPa, and the tensile strength is 18.8 MPa.
Example 2
Raw materials:
poly (butylene adipate/terephthalate), weight average molecular weight 20 ten thousand, 80 weight portions;
polylactic acid, the weight average molecular weight is 15 ten thousand, 20 weight portions;
10 parts of shell powder with the particle size of 200 nm;
glycolic acid, 0.1 part by weight;
0.1 part by weight of citric acid;
0.2 part by weight of benzoyl peroxide.
The preparation process of the composite material of the degradable disposable lunch box comprises the following steps:
(1) mixing shell powder, glycolic acid and citric acid with 35 parts by weight of deionized water, standing for 18h, and removing supernatant.
(2) At 45 deg.C, making the glue solution in supercritical CO at pressure of 8MPa2Stirring and reacting for 4h at the speed of 250r/min under the atmosphere, then obtaining modified shell powder by a solid-liquid separation method, and drying in a constant-temperature drying oven at 70 ℃.
(3) And mixing the modified shell powder, the polybutylene adipate/terephthalate, the polylactic acid and the benzoyl peroxide, performing melt blending granulation on the mixed material in a double-screw extruder at the temperature of 170 ℃, setting the rotating speed to be 170 revolutions per minute, and drying in a constant-temperature drying oven at the temperature of 80 ℃ to obtain the composite material.
Through performance tests, the Young modulus is 166.9MPa, and the tensile strength is 15.8 MPa.
Example 3
Raw materials:
poly (butylene adipate/terephthalate), weight average molecular weight 25 ten thousand, 75 weight parts;
polylactic acid, weight average molecular weight is 18 ten thousand, 25 weight portions;
shell powder with the particle size of 300nm in 6 parts by weight;
calcium carbonate powder with the particle size of 300nm and 6 parts by weight;
0.5 part by weight of arachidonic acid;
0.5 part by weight of citric acid;
0.5 part by weight of benzoyl peroxide; tert-butyl peroxypivalate, 0.5 part by weight.
The preparation process of the composite material of the degradable disposable lunch box comprises the following steps:
(1) mixing shell powder, calcium carbonate powder, arachidonic acid and citric acid with 50 parts by weight of deionized water, standing for 20h, and removing supernatant.
(2) At 50 deg.C, making the glue solution in supercritical CO at pressure of 10MPa2Stirring and reacting for 5h at the speed of 300r/min under the atmosphere, then obtaining modified mixed filler powder by a solid-liquid separation method, and drying in a constant-temperature drying oven at 70 ℃.
(3) And mixing the modified mixed filler powder, poly (butylene adipate)/terephthalate), polylactic acid, benzoyl peroxide and tert-butyl peroxypivalate, performing melt blending granulation on the mixed material in a double-screw extruder at 175 ℃, setting the rotating speed to be 190 revolutions per minute, and drying in a constant-temperature drying oven at 80 ℃ to obtain the composite material.
Through performance tests, the Young modulus is 232.9MPa, and the tensile strength is 12.4 MPa.
Example 4
Raw materials:
poly (butylene adipate/terephthalate), weight average molecular weight 30 ten thousand, 70 parts by weight;
polylactic acid, the weight average molecular weight is 20 ten thousand, 30 weight portions;
calcium carbonate powder, 400nm, 8 weight portions;
egg shell powder, 500nm, 8 weight portions;
1 part by weight of 17-hydroxy-9-cis-octadecanoic acid;
1 part by weight of 10, 12-dihydroxystearic acid;
0.5 part by weight of dicyclohexyl peroxydicarbonate;
0.5 part by weight of tert-butyl peroxypivalate;
0.5 part by weight of dibenzoyl peroxide.
The preparation process of the composite material of the degradable disposable lunch box comprises the following steps:
(1) mixing calcium carbonate powder, eggshell powder, 17-hydroxy-9-cis-octadecanoic acid, 10, 12-dihydroxystearic acid and 60 parts by weight of deionized water, standing for 22 hours, and removing supernatant.
(2) At 60 deg.C, making the glue solution in supercritical CO at pressure of 12MPa2Stirring and reacting for 6h at the speed of 350r/min under the atmosphere, then obtaining modified mixed filler powder by a solid-liquid separation method, and addingDrying in a constant-temperature drying oven at 70 ℃.
(3) And mixing the modified mixed filler powder, poly (butylene adipate)/terephthalate), polylactic acid, dicyclohexyl peroxydicarbonate, tert-butyl peroxypivalate and dibenzoyl peroxide, performing melt blending granulation on the mixed material in a double-screw extruder at 180 ℃, setting the rotation speed to be 200 revolutions per minute, and drying in a constant-temperature drying oven at 80 ℃ to obtain the composite material.
Through performance tests, the Young modulus is 402.9MPa, and the tensile strength is 15.4 MPa.
Example 5
Raw materials:
poly (butylene adipate/terephthalate), weight average molecular weight 40 ten thousand, 60 parts by weight;
polylactic acid, weight average molecular weight 25 ten thousand, 40 weight portions;
calcium carbonate powder, 500nm, 10 parts by weight;
10 parts of shell powder with the particle size of 500 nm;
1 part by weight of 15-hydroxy-9-cis-octadecanoic acid;
1 part by weight of cinnamic acid and 1 part by weight of ricinoleic acid;
1, 1-bis (t-butylperoxy) -3,3, 5-trimethylcyclohexane, 1 part by weight;
1 part by weight of dibenzoyl peroxide.
The preparation process of the composite material of the degradable disposable lunch box comprises the following steps:
(1) mixing calcium carbonate powder, shell powder, 15-hydroxy-9-cis-octadecanoic acid, cinnamic acid and ricinoleic acid with 70 parts by weight of deionized water, standing for 24 hours, and removing supernatant.
(2) At 70 deg.C, making the glue solution in supercritical CO at pressure of 14MPa2Stirring and reacting for 7h at the speed of 350r/min under the atmosphere, then obtaining modified mixed filler powder by a solid-liquid separation method, and drying in a constant-temperature drying oven at 70 ℃.
(3) Mixing the modified mixed filler powder, poly (butylene adipate)/terephthalate, polylactic acid, 1-bis (tert-butylperoxy) -3,3, 5-trimethylcyclohexane and dibenzoyl peroxide, carrying out melt blending granulation on the mixed material in a double-screw extruder at the temperature of 200 ℃, setting the rotating speed at 220 revolutions per minute, and drying in a constant-temperature drying box at the temperature of 80 ℃ to obtain the composite material.
Through performance tests, the Young modulus is 429.9MPa, and the tensile strength is 14.4 MPa.
Comparative example 1
Raw materials:
poly (butylene adipate/terephthalate), weight average molecular weight 30 ten thousand, 100 weight parts;
calcium carbonate powder, 200nm, 10 weight portions.
The preparation process of the composite material comprises the following steps:
mixing the poly (butylene adipate)/terephthalate with calcium carbonate powder, then carrying out melt blending granulation on the mixed material in a double-screw extruder at the temperature of 160 ℃, setting the rotating speed at 180 revolutions per minute, and drying in a constant-temperature drying box at the temperature of 80 ℃ to obtain the composite material.
Through performance tests, the Young modulus is 106.6MPa, and the tensile strength is 20.5 MPa.
Comparative example 2
Raw materials:
poly (butylene adipate/terephthalate), weight average molecular weight 30 ten thousand, 80 parts by weight;
polylactic acid, weight average molecular weight 25 ten thousand, 20 weight portions;
and 20 parts of shell powder with the particle size of 500 nm.
The preparation process of the composite material comprises the following steps:
mixing the polybutylene adipate/terephthalate, the polylactic acid and the calcium carbonate powder, then carrying out melt blending granulation on the mixed material in a double-screw extruder at 180 ℃, setting the rotating speed at 180 revolutions per minute, and drying in a constant-temperature drying oven at 90 ℃ to obtain the composite material.
Through performance tests, the Young modulus is 147.2MPa, and the tensile strength is 8.4 MPa.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (10)
1. A preparation method of a composite material for manufacturing a degradable disposable lunch box is characterized by comprising the following steps:
(1) mixing filler powder, a modifier and deionized water, standing, and removing supernatant to obtain glue solution; wherein the mass ratio of the filler powder to the deionized water is 1 (3-6);
(2) making the glue solution in supercritical CO at 40-70 deg.C2Stirring and reacting under the atmosphere, then obtaining modified filler powder by a solid-liquid separation method, and then drying;
(3) mixing the modified filler powder, the poly (butylene adipate)/terephthalate), the polylactic acid and the initiator, performing melt blending granulation on the mixed material in a double-screw extruder at the temperature of 150-200 ℃, and drying to obtain the composite material.
2. The method for preparing composite material for making degradable disposable lunch box according to claim 1 is characterized by that: 1-20 parts by weight of filler powder; 0.1-3 parts of modifier; the total weight of the polybutylene adipate/terephthalate and the polylactic acid is 100 parts by weight; 0.1-2 parts of initiator.
3. The method for preparing composite material for making degradable disposable lunch box according to claim 2 wherein: 0-100 parts of poly (butylene adipate/terephthalate), and the weight-average molecular weight of the poly (butylene adipate/terephthalate) is 15-40 ten thousand; 0-100 parts of polylactic acid, and the weight average molecular weight is 10-25 ten thousand.
4. The method for preparing composite material for making degradable disposable lunch box according to claim 3 is characterized by that: the filler powder is one or more of calcium carbonate powder, egg shell powder and shell powder; the particle diameter of the filler powder is 50-500 nm.
5. The method for preparing composite material for making degradable disposable lunch box according to claim 4 is characterized by that: the modifier is organic acid containing various functional groups and/or unsaturated fatty acid and derivatives thereof;
the organic acid containing multiple functional groups is one or more of salicylic acid, malic acid, citric acid, alginic acid, quinic acid, glycolic acid, hydroxyethylidene diphosphonic acid, B-hydroxybutyric acid, gamma-hydroxybutyric acid and hydroxylauric acid;
the unsaturated fatty acid and the derivatives thereof are one or more of cinnamic acid, linoleic acid, linolenic acid, arachidonic acid, ricinoleic acid, hydroxyl-12-octadecanoic acid, 15-hydroxyl-9-cis-octadecanoic acid, 16-hydroxyl-9-cis-octadecanoic acid, 17-hydroxyl-9-cis-octadecanoic acid, 10-hydroxyl-12, 15-octadecanoic acid, 10, 12-dihydroxystearic acid, 10-hydroxystearic acid, 9, 10-dihydroxyoctadecanoic acid, 13, 14-dihydroxyeicosanoic acid and 13(14) -monohydroxy-docosanoic acid.
6. The method for preparing composite material for making degradable disposable lunch box according to claim 5 is characterized by that: the initiator is one or more of dicumyl peroxide, benzoyl peroxide, dibenzoyl peroxide, tert-butyl peroxybenzoate, tert-butyl peroxypivalate, diisopropyl peroxydicarbonate, tert-butyl peroxybenzoate, dicyclohexyl peroxydicarbonate, 1-bis (tert-butylperoxy) -3,3, 5-trimethylcyclohexane and dibenzoyl peroxide bis (tert-butylperoxy) diisopropylbenzene.
7. The method for preparing composite material for making degradable disposable lunch box according to claim 1 is characterized by that: in the step (1), the rest time is 12-24 h.
8. The method for preparing composite material for making degradable disposable lunch box according to claim 1, characterized in thatIn the following steps: in the step (2), supercritical CO2The pressure of the atmosphere is 7-14MPa, the stirring speed is 200-400r/min, and the reaction time is 3-7 h; the drying temperature was 70 ℃.
9. The method for preparing composite material for making degradable disposable lunch box according to claim 1 is characterized by that: in the step (3), the rotating speed of the double-screw extruder is 150-; the drying temperature was 80 ℃.
10. A composite material for making a degradable disposable lunch box made by the method of any one of claims 1-9.
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| CN116041989A (en) * | 2023-01-10 | 2023-05-02 | 聚能新材料科技(荆门)有限公司 | Biomass carbon sphere, preparation method thereof, antistatic composite material and preparation method thereof |
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