CN111040396B - Composite material and preparation method thereof - Google Patents
Composite material and preparation method thereof Download PDFInfo
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- CN111040396B CN111040396B CN201910440707.7A CN201910440707A CN111040396B CN 111040396 B CN111040396 B CN 111040396B CN 201910440707 A CN201910440707 A CN 201910440707A CN 111040396 B CN111040396 B CN 111040396B
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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
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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Abstract
The invention discloses a composite material and a preparation method thereof. The composite material is prepared from the following raw materials: 20-85 parts of polylactic acid, 10-75 parts of polyethylene terephthalate, 0.5-5 parts of lanthanum oxide, 2-8 parts of zinc stearate, 0.1-3 parts of hydrotalcite and 0.1-1 part of antioxidant. The composite material contains lanthanum oxide, zinc stearate and hydrotalcite, and can improve the mechanical property and the thermal stability of the composite material.
Description
Technical Field
The invention relates to a composite material and a preparation method thereof.
Background
Polylactic acid (PLA) is a novel completely degradable green biomaterial, has good biocompatibility and degradability, can be processed by adopting processes such as injection molding, extrusion, spinning and the like to prepare fibers, films, sheets, plates and the like, and products can be widely applied to the fields of clothing, packaging, agriculture, automobiles, electronics, biomedicine, tissue engineering and the like. Although PLA has many advantages, its poor mechanical properties and thermal stability still limit its application in many fields.
In recent years, polylactic acid materials have been modified in various ways. For example, CN104927323B discloses a PLA composite material, which is made from raw materials comprising the following components: 40-65 parts of polylactic acid (PLA), 10-20 parts of anhydrous sodium sulfate, 15-30 parts of polyethylene terephthalate (PET), 5-10 parts of a toughening agent, 0.2-0.6 part of a stabilizer, 2-6 parts of a plasticizer and 0.4-1 part of a lubricant. The above patent documents do not add agents for improving the mutual compatibility of PLA and PET, resulting in poor mutual compatibility of PLA and PET during the preparation of PLA composites.
For another example, CN107815078A discloses a medical degradable composite material, which contains polylactic acid (PLA), a toughening agent and an antioxidant, wherein each 100 parts by weight of the polylactic acid (PLA) contains 10-50 parts of the toughening agent and 0-1 part of the antioxidant; the degradable composite material contains rare earth elements, and the content of the rare earth elements is 50ppm-10000ppm by taking the weight of the composite material as a reference; the rare earth elements comprise cerium, lanthanum and the like, and are provided by compounds containing the rare earth elements, cerium nitrate, ammonium ceric nitrate, cerium dioxide, cerium dichloride, lanthanum oxide, lanthanum acetate and lanthanum carbonate can be selected, and the cerium lanthanum compounds can be used independently or in a compound way. The patent document adds rare earth elements to make the composite material have excellent antibacterial effect and can also improve the degradation performance of the material, but the patent document does not relate to the improvement of the mechanical property and the thermal stability of the PLA composite material.
For another example, CN106751629A discloses a fully biodegradable plastic wrap and a preparation method thereof: (1) drying polylactic acid (produced by Shenzhen Guanghua Wei corporation, film level) and biodegradable polyester PBSA (produced by Anqing and Xing corporation, film blowing level) in an oven at 70 ℃ for 3h, and drying inorganic filler ultrafine kaolin in the oven at 110 ℃ for 3 h; (2) weighing the following raw materials in parts by weight: 5 parts of polylactic acid, 95 parts of biodegradable polyester PBSA, 1 part of toughening agent (produced according to the method in the embodiment 1 of the invention patent ZL201410662335. X), 6 parts of ethylene decomposition absorbent rare earth oxide, 20 parts of inorganic filler superfine kaolin, 0.5 part of processing aid lubricant calcium stearate and 10100.3 parts of antioxidant; adding the above raw materials into a high-speed mixer, and mixing at normal temperature for 5-10 min; (3) adding the uniformly mixed raw materials in the step (2) into a double-screw extruder, melting and blending at the temperature of 120-190 ℃, and performing extrusion modification granulation to obtain a special modified material for the preservative film; (4) and (4) carrying out blow molding on the modified material special for the preservative film obtained in the step (3) at the temperature of 140-180 ℃ by using a single-screw extrusion film blowing machine to form a film, thus obtaining the full-biodegradable preservative film. In the patent document, the rare earth oxide is used as an ethylene decomposition absorbent, and the rare earth oxide has the function of decomposing ethylene gas released in the process of storing fruits and vegetables, so that the fresh-keeping storage time of the fruits and vegetables is greatly prolonged; however, the patent document does not deal with the improvement of mechanical properties and thermal stability.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a composite material containing lanthanum oxide, zinc stearate and hydrotalcite, which can improve the mechanical properties and thermal stability of the composite material.
The lanthanum oxide, the zinc stearate and the hydrotalcite added in the preparation method are mutually cooperated to promote the full mutual compatibility of the polylactic acid PLA and the polyethylene terephthalate PET, and the mechanical property and the thermal stability of the obtained composite material are improved.
The invention adopts the following technical scheme to achieve the purpose.
In one aspect, the present invention provides a composite material made from raw materials comprising: 20-85 parts of polylactic acid, 10-75 parts of polyethylene terephthalate, 0.5-5 parts of lanthanum oxide, 2-8 parts of zinc stearate, 0.1-3 parts of hydrotalcite and 0.1-1 part of antioxidant.
The composite material according to the invention is preferably made from raw materials comprising: 25-75 parts of polylactic acid, 15-60 parts of polyethylene terephthalate, 0.6-3.5 parts of lanthanum oxide, 2.5-6 parts of zinc stearate, 0.3-2 parts of hydrotalcite and 0.2-0.8 part of antioxidant.
The composite material according to the invention is preferably made from raw materials comprising: 30-70 parts of polylactic acid, 20-55 parts of polyethylene terephthalate, 0.8-2 parts of lanthanum oxide, 3-5 parts of zinc stearate, 0.5-1.5 parts of hydrotalcite and 0.3-0.6 part of antioxidant.
According to the composite material, the mass ratio of the polyethylene terephthalate to the polylactic acid is preferably 1/3-1/1.
According to the composite material, the mass ratio of lanthanum oxide, zinc stearate and hydrotalcite is preferably 1-3: 4-7: 1 to 2.
According to the composite material of the present invention, preferably, the antioxidant is selected from one or more of butylated hydroxyanisole, dibutyl hydroxytoluene, tert-butyl hydroquinone, diisodecyl phosphite, pentaerythritol diphosphite, [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tris (2, 4-di-tert-butylphenyl) phosphite, [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] octadecanol ester, and tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester.
In another aspect, the present invention provides a method for preparing the above composite material, comprising the steps of: uniformly mixing the lanthanum oxide, zinc stearate, an antioxidant, hydrotalcite and a PET/PLA blend to obtain a mixture; plasticizing, crushing and extruding the mixture to obtain the composite material;
wherein the PET/PLA blend is formed by mixing the polylactic acid and the polyethylene terephthalate.
According to the preparation method provided by the invention, the mixing time of the lanthanum oxide, the zinc stearate, the antioxidant, the hydrotalcite and the PET/PLA blend is preferably 3-10 min.
According to the preparation method provided by the invention, preferably, the mixing time of the lanthanum oxide, the zinc stearate, the antioxidant, the hydrotalcite and the PET/PLA blend is 4-8 min.
According to the preparation method provided by the invention, the plasticizing temperature is preferably 170-180 ℃.
The composite material contains lanthanum oxide, zinc stearate and hydrotalcite, and can improve the mechanical property and the thermal stability of the composite material. According to the preparation method of the composite material, lanthanum oxide, zinc stearate and hydrotalcite are mutually cooperated, so that the full mutual compatibility of PLA and PET is promoted, and the mechanical property and the thermal stability of the obtained composite material are improved.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
< composite Material >
The composite material is prepared from the following raw materials: polylactic acid (PLA), polyethylene terephthalate (PET), lanthanum oxide (La)2O3) Zinc stearate and hydrotalcite; antioxidants may also be included.
In the invention, the composite material is prepared from the following raw materials: 20-85 parts of polylactic acid, 10-75 parts of polyethylene terephthalate, 0.5-5 parts of lanthanum oxide, 2-8 parts of zinc stearate, 0.1-3 parts of hydrotalcite and 0.1-1 part of antioxidant.
In the present invention, the polylactic acid is 20 to 85 parts by weight, preferably 25 to 75 parts by weight, and more preferably 30 to 70 parts by weight. The amount of the polyethylene terephthalate is 10 to 75 parts by weight, preferably 15 to 60 parts by weight, and more preferably 20 to 55 parts by weight. The lanthanum oxide is 0.5 to 5 parts by weight, preferably 0.6 to 3.5 parts by weight, and more preferably 0.8 to 2 parts by weight. The zinc stearate accounts for 2-8 parts by weight, preferably 2.5-6 parts by weight, and more preferably 3-5 parts by weight. The amount of the hydrotalcite is 0.1 to 3 parts by weight, preferably 0.3 to 2 parts by weight, and more preferably 0.5 to 1.5 parts by weight. The antioxidant is 0.1 to 1 part by weight, preferably 0.2 to 0.8 part by weight, and more preferably 0.3 to 0.6 part by weight. When the content of each component is in the range, the composite material has good mechanical property and thermal stability.
In certain embodiments, the composite material is made from raw materials comprising: 25-75 parts of polylactic acid, 15-60 parts of polyethylene terephthalate, 0.6-3.5 parts of lanthanum oxide, 2.5-6 parts of zinc stearate, 0.3-2 parts of hydrotalcite and 0.2-0.8 part of antioxidant.
In certain embodiments, the composite material is made from raw materials comprising: 30-70 parts of polylactic acid, 20-55 parts of polyethylene terephthalate, 0.8-2 parts of lanthanum oxide, 3-5 parts of zinc stearate, 0.5-1.5 parts of hydrotalcite and 0.3-0.6 part of antioxidant.
In the invention, the mass ratio of the polyethylene terephthalate to the polylactic acid is preferably 1/3-1/1, and more preferably 3/7-1/1. Thus, the composite material with good mechanical property and thermal stability can be obtained.
In the present invention, the hydrotalcite is an inorganic compound containing magnesium and aluminum. In one aspect, the hydrotalcite natural product has a structure derived from Mg6Al2(OH)16CO3·4H2O represents a chemical structure. On the other hand, examples of the synthetic product of hydrotalcite other than hydrotalcite include hydrotalciteThe natural substance of (2) is a substance having a composition ratio of Mg to Al, for example, a substance represented by the formula Mg4Al2(OH)12CO3·3H2O、Mg5Al2(OH)14CO3·4H2O、Mg10Al2(OH)22(CO3)2·4H2And O, and the like. These hydrotalcites may be used alone, or 2 or more kinds thereof may be used in combination. The invention discovers that: the hydrotalcite, the lanthanum oxide and the zinc stearate are used for preparing the composite material according to a certain mass ratio, so that the full mutual compatibility of PLA and PET can be promoted, and the mechanical property and the thermal stability of the obtained composite material can be improved.
In the invention, the mass ratio of lanthanum oxide, zinc stearate and hydrotalcite is preferably 1-3: 4-7: 1-2; more preferably 1 to 2: 5-6: 1 to 2. According to a specific embodiment of the invention, the mass ratio of lanthanum oxide, zinc stearate and hydrotalcite is 1-2: 5-6: 1. therefore, lanthanum oxide, zinc stearate and hydrotalcite can better exert the mutual synergistic effect, promote the full mutual compatibility of PLA and PET, and improve the mechanical property and the thermal stability of the obtained composite material.
In the present invention, the antioxidant may be one or more selected from the group consisting of dibutylhydroxytoluene, tert-butylhydroquinone, diisodecyl phosphite, pentaerythritol diphosphite, [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tris (2, 4-di-tert-butylphenyl) phosphite, [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] octadecanoic carbonate, tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, and butylhydroxyanisole; preferably one or more selected from the group consisting of dibutylhydroxytoluene, tert-butylhydroquinone, diisodecyl phosphite, pentaerythritol diphosphite, pentaerythritol [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester, and tris (2, 4-di-tert-butylphenyl) phosphite; more preferably one or more selected from the group consisting of dibutylhydroxytoluene, tert-butylhydroquinone, diisodecyl phosphite, pentaerythritol diphosphite, and pentaerythritol [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
< method for producing composite Material >
The preparation method of the composite material comprises the following steps: (1) mixing the components; (2) and (3) processing the mixture.
In the step (1), the mixing steps of the components are as follows: uniformly mixing lanthanum oxide, zinc stearate, an antioxidant, hydrotalcite and a PET/PLA blend to obtain a mixture; wherein the PET/PLA blend is formed by mixing the polylactic acid and the polyethylene terephthalate. The proportions of lanthanum oxide, zinc stearate, antioxidant, hydrotalcite, PET and PLA are as described above and will not be described herein. The mixing time may be 3 to 10min, preferably 4 to 8min, and more preferably 4 to 6 min. The components can be dried before mixing, for example, the components are dried in an oven at 80-90 ℃ for 2-5 hours. The mixing equipment can be a mixer. Therefore, lanthanum oxide, zinc stearate and hydrotalcite can better exert the mutual synergistic effect, promote the mutual compatibility of PLA and PET, and improve the mechanical property and the thermal stability of the obtained composite material.
In the step (2), the mixture is processed by the following steps: and plasticizing, crushing and extruding the mixture to obtain the composite material. The plasticizing equipment can be a two-roller plastic mixing machine. The plasticizing temperature can be 170-180 ℃. The crushing equipment can be a crusher. The extrusion molding equipment can be an injection molding machine. The temperature of the extrusion molding can be 140-180 ℃, and preferably 160-180 ℃.
According to one embodiment of the invention, 0.5-5 parts by weight of lanthanum oxide, 2-8 parts by weight of zinc stearate, 0.1-1 part by weight of antioxidant, 0.1-3 parts by weight of hydrotalcite and PET/PLA blend are poured into a mixer and mixed for 4-6 min so as to be fully and uniformly mixed to obtain a mixture; wherein the weight parts of polylactic acid in the PET/PLA blend are 20-85, the weight parts of polyethylene terephthalate are 10-75, and the mass ratio of PET to PLA is 1/3-1/1; plasticizing the mixture by using a double-roller plastic mixing mill, standing for 18-30 h, and then crushing by using a crusher to obtain a crushed sample; and preparing the smashed sample into a sample strip to be tested by using an injection molding machine, so as to obtain the composite material.
< test methods >
The test standard for tensile strength is "determination of tensile Properties of GB/T1040 plastics part 1: general rules of care (general rules); the test standard of the bending strength is GB/T9341 determination of the bending performance of plastics; the test standard of the heat distortion temperature is GB/T1634 determination of plastic load distortion temperature.
Example 1
0.6g of La2O32.4g of zinc stearate, 0.3g of antioxidant, 0.45g of hydrotalcite and 60g of PET/PLA blend are poured into a mixer and mixed for 5min so as to be fully and uniformly mixed to obtain a mixture; wherein the mass ratio of PET to PLA in the PET/PLA blend is 5/5. Plasticizing the mixture by using a double-roller plastic mixing mill, standing for 24h, and crushing by using a crusher to obtain a crushed sample; and (4) preparing the smashed sample into a sample strip to be tested by using an injection molding machine, and obtaining the composite material. The performance parameters of the composite are shown in table 1.
Example 2
0.6g of La2O32.4g of zinc stearate, 0.3g of antioxidant, 0.45g of hydrotalcite and 60g of PET/PLA blend are poured into a mixer and mixed for 5min so as to be fully and uniformly mixed to obtain a mixture; wherein the mass ratio of PET to PLA in the PET/PLA blend is 3/7. Plasticizing the mixture by using a double-roller plastic mixing mill, standing for 24h, and crushing by using a crusher to obtain a crushed sample; and (4) preparing the smashed sample into a sample strip to be tested by using an injection molding machine, and obtaining the composite material. The performance parameters of the composite are shown in table 1.
Example 3
0.8g of La2O32.4g of zinc stearate, 0.3g of antioxidant, 0.45g of hydrotalcite and 60g of PET/PLA blend are poured into a mixer and mixed for 5min so as to be fully and uniformly mixed to obtain a mixture; wherein the mass ratio of PET to PLA in the PET/PLA blend is 3/7. Plasticizing the mixture by using a double-roller plastic mixing mill, standing for 24h, and crushing by using a crusher to obtain a crushed sample; and (4) preparing the smashed sample into a sample strip to be tested by using an injection molding machine, and obtaining the composite material. The performance parameters of the composite are shown in table 1.
Comparative example 1
Pouring 0.3g of antioxidant and 60g of PET/PLA blend into a mixer, and mixing for 5min to fully and uniformly mix to obtain a mixture; wherein the mass ratio of PET to PLA in the PET/PLA blend is 5/5. Plasticizing the mixture by using a double-roller plastic mixing mill, standing for 24h, and crushing by using a crusher to obtain a crushed sample; and (4) preparing the smashed sample into a sample strip to be tested by using an injection molding machine, and obtaining the composite material. The performance parameters of the composite are shown in table 1.
Comparative example 2
A composite material was obtained by replacing zinc stearate with calcium stearate and performing the same operation as in example 1. The performance parameters of the composite are shown in table 1.
TABLE 1 Properties of the composites
| Numbering | Tensile strength/MPa | Flexural Strength/MPa | Heat distortion temperature/. degree.C |
| Example 1 | 102 | 128 | 130 |
| Example 2 | 96 | 122 | 124 |
| Example 3 | 99 | 124 | 127 |
| Comparative example 1 | 45 | 60 | 58 |
| Comparative example 2 | 86 | 103 | 110 |
As is clear from Table 1, the composite materials of examples 1 to 3 are significantly improved in tensile strength, flexural strength and heat distortion temperature as compared with those of comparative examples 1 to 2. The results show that the composite material contains lanthanum oxide, zinc stearate and hydrotalcite, and can improve the mechanical property and the thermal stability of the composite material.
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.
Claims (8)
1. The composite material is characterized by being prepared from the following raw materials: 25-70 parts of polylactic acid, 15-55 parts of polyethylene terephthalate, 0.5-2 parts of lanthanum oxide, 2-3 parts of zinc stearate, 0.1-0.5 part of hydrotalcite and 0.1-1 part of antioxidant;
wherein the mass ratio of the polyethylene terephthalate to the polylactic acid is 1/3-1/1.
2. The composite material according to claim 1, wherein the mass ratio of the polyethylene terephthalate to the polylactic acid is 3/7-1/1.
3. The composite material of claim 1, wherein the mass ratio of lanthanum oxide, zinc stearate and hydrotalcite is 1-3: 4-7: 1 to 2.
4. The composite material according to claim 1, wherein the antioxidant is selected from one or more of butylated hydroxyanisole, dibutyl hydroxytoluene, tert-butyl hydroquinone, diisodecyl phosphite, pentaerythritol diphosphite, pentaerythritol [3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester, tris (2, 4-di-tert-butylphenyl) phosphite, [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] octadecanol ester, and pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
5. A method for preparing a composite material according to any one of claims 1 to 4, characterized by comprising the steps of: uniformly mixing lanthanum oxide, zinc stearate, an antioxidant, hydrotalcite and a PET/PLA blend to obtain a mixture; plasticizing, crushing and extruding the mixture to obtain the composite material;
wherein the PET/PLA blend is formed by mixing the polylactic acid and the polyethylene terephthalate.
6. The method for preparing the composite material according to claim 5, wherein the mixing time of the lanthanum oxide, the zinc stearate, the antioxidant, the hydrotalcite and the PET/PLA blend is 3-10 min.
7. The method for preparing the composite material according to claim 6, wherein the mixing time of the lanthanum oxide, the zinc stearate, the antioxidant, the hydrotalcite and the PET/PLA blend is 4-8 min.
8. The method for preparing the composite material according to claim 5, wherein the plasticizing temperature is 170-180 ℃.
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