CN107955346B - Preparation method of polylactic acid plasticized compound - Google Patents
Preparation method of polylactic acid plasticized compound Download PDFInfo
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- CN107955346B CN107955346B CN201610901483.1A CN201610901483A CN107955346B CN 107955346 B CN107955346 B CN 107955346B CN 201610901483 A CN201610901483 A CN 201610901483A CN 107955346 B CN107955346 B CN 107955346B
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
Abstract
The invention provides a preparation method of a polylactic acid plasticized compound. The polylactic acid plasticized compound comprises the following components in parts by weight: 70-95 parts of polylactic acid and 5-30 parts of compound plasticizer. The compound plasticizer is prepared from the following components in parts by weight of 1-5: 1-25 of a component A and a component B. The component A is one or more of glycerol, xylitol and sorbitol of polyalcohol in any proportion; the component B is one or more of dioctyl phthalate, polyethylene glycol with the molecular weight of 1000-8000, triethyl citrate, tributyl citrate, trioctyl citrate, acetyl triethyl citrate, acetyl tributyl citrate and acetyl trioctyl citrate in any proportion. Compared with polylactic acid plasticized by a single plasticizer, the prepared polylactic acid plasticized by the polylactic acid plasticized compound has the advantages that the tensile strength is increased by 15.74%, the elongation at break is increased by 11.05%, and meanwhile, the using amount of the polylactic acid plasticized compound is reduced by 41.67% compared with that of the single plasticizer.
Description
Technical Field
The invention relates to a preparation method of a polylactic acid plasticizing compound, belonging to the field of processing of high polymer materials.
Background
With the rapid development of science and technology, the polymer material has become an indispensable material in people's life. Renewable, biodegradable polylactic acid is considered to be one of the most promising materials to replace petroleum-based plastics. The polylactic acid has higher transparency and glossiness, good heat resistance and good biocompatibility, and can be completely degraded into water and carbon dioxide. However, the processing and use of polylactic acid are limited due to the disadvantages of high brittleness, poor impact strength, lack of flexibility and elasticity, low melt strength, narrow processing temperature range, high raw material cost and the like. The best mode for improving the use of the polylactic acid is to improve the mechanical property and the processing property of the polylactic acid and ensure the degradability of the material.
The currently preferred approach is to improve the processing and use of polylactic acid by blending with plasticizers. Chinese patent CN1687233A discloses a plasticizing method of polylactic resin particles, and the plasticizer related in the material comprises tributyl citrate, polyethylene glycol with the molecular weight of 200-8000 and glyceryl triacetate. Chinese patent CN1532216A discloses a preparation method of a polylactic acid composition film, and plasticizers applied in the material comprise tributyl citrate, acetyl tributyl citrate, polyethylene glycol and oligomeric lactic acid. Chinese patent CN1793228A adopts polyol esters, oligomeric polyesters and citric acid esters as plasticizers to obtain a plasticized polylactic acid system. And introducing crosslinking into a plasticized polylactic acid system by using methods such as electron beams and the like to obtain the high-performance polylactic acid. Chinese patent CN1857235 discloses a method for plasticizing with polymeric plasticizer and polylactic acid, but the elongation at break of polylactic acid is only improved by 1.5 times, and the preparation method of the material is complicated and is not beneficial to application. The Effect of The amount of a single Citrate plasticizer used on The plasticization of polylactic acid is reported in Journal of applied Polymer Science in The Effect of Citrate Plasticizers on The thermal and Mechanical Properties of Poly (DL-lactate) 2012. However, the use of a single plasticizer often requires high levels to achieve the best material properties.
Disclosure of Invention
The invention provides a preparation method of a polylactic acid plasticized compound, aiming at the problem of high usage amount of polylactic acid plasticized by using a single plasticizer. The composite plasticizer is simple to prepare, the use amount of a single plasticizer can be reduced, and the processing performance and the usability of the material can be improved.
The invention relates to a preparation method of a polylactic acid plasticized compound, which comprises the following components in parts by weight: 70-95 parts of polylactic acid and 5-30 parts of compound plasticizer; the polylactic acid is semi-crystalline polylactic acid; the compound plasticizer consists of a component A and a component B, wherein the component A is one or more of glycerol, xylitol and sorbitol of polyalcohol in any proportion; the component B is one or more of dioctyl phthalate, polyethylene glycol with the molecular weight of 1000-8000, triethyl citrate, tributyl citrate, trioctyl citrate, acetyl triethyl citrate, acetyl tributyl citrate and acetyl trioctyl citrate in any proportion; the weight part ratio of the component A to the component B is 1-5: 1-25;
the preparation steps and conditions are as follows:
(1) the polylactic acid is placed in a vacuum oven in advance for drying;
(2) uniformly mixing the component A and the component B of the compound plasticizer according to the proportion to obtain the compound plasticizer;
(3) banburying and blending: adding polylactic acid and compound plasticizer according to the proportion at the temperature of 160-190 ℃, and mixing for 5-10 minutes at the speed of 30-60 r/min;
(4) and (3) pressing and forming: placing the internally mixed and blended materials in a mold, preheating at the temperature of 190 ℃ at 170 ℃ and under the pressure of 10-20MPa, and carrying out hot pressing for 2-5 minutes; the pressure is 10-20MPa, and then cold pressing is carried out for 3-10 minutes at room temperature to obtain the polylactic acid plasticizing compound.
Has the advantages that: the invention provides a preparation method of a polylactic acid plasticized compound, and test results show that: compared with polylactic acid plasticized by a single plasticizer, the polylactic acid plasticized by the polylactic acid plasticized compound prepared by the invention has the advantages that the tensile strength is increased by 15.74 percent, the elongation at break is increased by 11.05 percent, and meanwhile, the using amount of the polylactic acid plasticized compound is reduced by 41.67 percent compared with that of the single plasticizer. Saves the cost and enhances the technical function index of the polylactic acid material.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the present invention by way of example, and it is to be understood that the description is intended to illustrate and not limit the scope of the invention as claimed.
Example 1 preparation method of polylactic acid plasticized Compound
(1) The polylactic acid is placed in a vacuum oven to be dried for 8 hours at the temperature of 80 ℃; the polylactic acid is semi-crystalline polylactic acid;
(2) 5 parts of glycerol and 10 parts of polyethylene glycol with the weight-average molecular weight of 6000 are uniformly mixed to prepare the compound plasticizer.
(3) Banburying and blending: mixing 15 parts by weight of the compound plasticizer and 85 parts by weight of polylactic acid for 5 minutes by using a haake mixer at 180 ℃ and the rotating speed of 40 r/min;
(4) and (3) pressing and forming: placing the banburying and blending materials in a mold, preheating for 5 minutes at 170 ℃, and hot-pressing for 5 minutes under the pressure of 10 MPa; and (3) cold pressing at room temperature for 3 minutes under the pressure of 10MPa to obtain the polylactic acid plasticizing compound.
And (3) testing tensile property: according to the GB/T1043-1979 test standard, a universal electronic tensile machine model 3365 of the American Instron company is selected for testing, a tensile sample bar is of a standard dumbbell type, the size of the sample bar is 75mm multiplied by 4mm multiplied by 1mm, and the tensile rate is 20 mm/s.
The test result shows that: the tensile strength of the polylactic acid plasticized compound prepared by the invention is 13.4MPa, and the elongation at break is 175.8%.
Example 2 preparation method of polylactic acid plasticized Compound
(1) The same as in example 1.
(2) 5 parts by weight of glycerol and 15 parts by weight of polyethylene glycol with the weight average molecular weight of 6000 are uniformly mixed to prepare the compound plasticizer.
(3) Banburying and blending: 20 parts by weight of compound plasticizer and 80 parts by weight of polylactic acid are mixed and blended for 5min by Haake at 180 ℃ and 40 r/min.
(4) And (3) pressing and forming: then preheating for 5 minutes at 190 ℃, then carrying out hot pressing for 5 minutes, then carrying out cold pressing for 3 minutes at room temperature, wherein the pressure is 10MPa, and carrying out compression molding to obtain the polylactic acid plasticizing compound.
The impact and tensile properties were measured as in example 1. The test result shows that: the tensile strength of the polylactic acid plasticized compound prepared by the invention is 12.5MPa, and the elongation at break is 227.2%.
Example 3 preparation of a plasticized polylactic acid Compound
(1) The same as in example 1.
(2) 5 parts by weight of glycerol and 20 parts by weight of polyethylene glycol with the weight average molecular weight of 6000 are uniformly mixed to prepare the compound plasticizer.
(3) Banburying and blending: mixing 25 parts by weight of compound plasticizer and 75 parts by weight of polylactic acid with Haake for 5min at 180 ℃ and 40 r/min.
(4) And (3) pressing and forming: then preheating for 5 minutes at 190 ℃, then carrying out hot pressing for 5 minutes, then carrying out cold pressing for 10 minutes at room temperature, wherein the pressure is 15MPa, and carrying out compression molding to obtain the polylactic acid plasticizing compound.
The impact and tensile properties were measured as in example 1. The test result shows that: the tensile strength of the polylactic acid plasticized compound prepared by the invention is 16.4MPa, and the elongation at break is 15.26%.
Example 4 preparation of a plasticized polylactic acid Compound
(1) The same as in example 1.
(2) 2.5 parts by weight of glycerol and 2.5 parts by weight of polyethylene glycol with the weight average molecular weight of 6000 are uniformly mixed to prepare the compound plasticizer.
(3) Banburying and blending: 15 parts of compound plasticizer and 95 parts of polylactic acid are mixed and blended for 5min by Haake at 180 ℃ and 40 r/min.
(4) And (3) pressing and forming: then preheating at 190 ℃, after 2 minutes, hot-pressing for 5 minutes, cold-pressing for 10 minutes at room temperature, wherein the pressure is 10MPa, and performing compression molding to obtain the polylactic acid plasticizing compound.
The impact and tensile properties were measured as in example 1. The test result shows that: the tensile strength of the polylactic acid plasticized compound prepared by the invention is 10.2MPa, and the elongation at break is 55.3%.
Comparative example 1 polylactic acid was dried in a vacuum oven at 80 ℃ for 8 hours. 30 parts by weight of polyethylene glycol with the weight-average molecular weight of 6000 and 70 parts by weight of polylactic acid are mixed and blended for 5min by Haake at 180 ℃ and the rotating speed of 40 r/min. Then preheating for 5 minutes at 190 ℃, then carrying out hot pressing for 5 minutes, then carrying out cold pressing for 3 minutes at room temperature, wherein the pressure is 10MPa, and carrying out compression molding to obtain the polylactic acid plasticizing compound.
The impact and tensile properties were measured as in example 1. The test result shows that: the tensile strength is 10.8MPa, and the elongation at break is 204.6%.
Example 5 preparation of a plasticized polylactic acid Compound
(1) The same as in example 1.
(2) 5 parts by weight of glycerol and 10 parts by weight of acetyl tributyl citrate are uniformly mixed to prepare the compound plasticizer.
(3) Banburying and blending: 15 parts of compound plasticizer and 85 parts of polylactic acid are mixed and blended for 5min by Haake at 175 ℃ and 40 r/min.
(4) And (3) pressing and forming: then preheating for 5 minutes at 180 ℃, then carrying out hot pressing for 5 minutes, then carrying out cold pressing for 3 minutes at room temperature, wherein the pressure is 20MPa, and carrying out compression molding to obtain the polylactic acid plasticizing compound.
The impact and tensile properties were measured as in example 1. The test result shows that: the tensile strength of the polylactic acid plasticized compound prepared by the invention is 26.8MPa, and the elongation at break is 395.1%.
Example 6 preparation of a plasticized polylactic acid Compound
(1) The same as in example 1.
(2) 5 parts by weight of glycerol and 15 parts by weight of acetyl tributyl citrate are uniformly mixed to prepare the compound plasticizer.
(3) Banburying and blending: 20 parts of compound plasticizer and 80 parts of polylactic acid are mixed and blended by Haake for 10min at 190 ℃ and 60 r/min.
(4) And (3) pressing and forming: then preheating for 5 minutes at 180 ℃, then carrying out hot pressing for 5 minutes, then carrying out cold pressing for 3 minutes at room temperature, wherein the pressure is 10MPa, and carrying out compression molding to obtain the polylactic acid plasticizing compound.
The impact and tensile properties were measured as in example 1. The test result shows that: the tensile strength of the polylactic acid plasticized compound prepared by the invention is 23.9MPa, and the elongation at break is 430.7%.
Example 7 preparation of a plasticized polylactic acid Compound
(1) The same as in example 1.
(2) 5 parts by weight of glycerol and 25 parts by weight of acetyl tributyl citrate are uniformly mixed to prepare the compound plasticizer.
(3) Mixing 30 parts by weight of compound plasticizer and 70 parts by weight of polylactic acid with Haake for 5min at 160 ℃ and 30 r/min.
(4) Then preheating for 5 minutes at 180 ℃, then carrying out hot pressing for 5 minutes, then carrying out cold pressing for 3 minutes at room temperature, wherein the pressure is 10MPa, and carrying out compression molding to obtain the polylactic acid plasticizing compound.
The impact and tensile properties were measured as in example 1. The test result shows that: the tensile strength of the polylactic acid plasticized compound prepared by the invention is 20.6MPa, and the elongation at break is 476.1%.
Comparative example 2 polylactic acid resin was dried in a vacuum oven at 80 ℃ for 8 hours. 30 parts by weight of acetyl tributyl citrate and 70 parts by weight of polylactic acid are mixed and blended for 5min by Haake at the temperature of 175 ℃ and the rotating speed of 40 r/min. Then preheating for 5 minutes at 180 ℃, then carrying out hot pressing for 5 minutes, then carrying out cold pressing for 3 minutes at room temperature, wherein the pressure is 10MPa, and carrying out compression molding to obtain the polylactic acid plasticizing compound.
The impact and tensile properties were measured as in example 1. The test result shows that: the tensile strength was 21MPa and the elongation at break was 437%.
And (3) comparing the results: the weight ratio of the compound plasticizer to the polylactic acid in the embodiment 2 is 20: 80. that is, the compounded plasticizer accounts for 25% of the weight of the polylactic acid.
The weight ratio of plasticizer to polyethylene glycol of comparative example 1 was 30: 70. namely, the compounded plasticizer accounts for 42.86 percent of the weight of the polylactic acid.
The amount of compounded plasticizer of example 2 was reduced by 41.67% compared to the amount of plasticizer of comparative example 1.
The test result shows that: the compound prepared in example 2 plasticized polylactic acid, tensile strength was 12.5MPa, and elongation at break was 227.2%. Comparative example 1 had a tensile strength of 10.8MPa and an elongation at break of 204.6%. Example 2 has a 15.74% increase in tensile strength and 11.05% increase in elongation at break over comparative example 1.
Similarly, the amount of compounded plasticizer in the polylactic acid plasticized by the compound prepared in example 6 was reduced by 41.67% compared with the amount of plasticizer in comparative example 2.
The test result shows that: the compound plasticized polylactic acid prepared in example 6 had a tensile strength of 23.9MPa and an elongation at break of 430.7%. Comparative example 2 had a tensile strength of 21MPa and an elongation at break of 437%. Example 6 showed a 13.81% increase in tensile strength and a 1.44% decrease in elongation at break over comparative example 1.
Through comparison, the polylactic acid plasticized by the compound prepared by the method disclosed by the invention has the advantages that the dosage is reduced by 41.67% compared with that of polylactic acid prepared by a single plasticizer, and the mechanical property is similar or better.
Claims (3)
1. The preparation method of the polylactic acid plasticized compound is characterized in that the components of the polylactic acid plasticized compound are as follows according to the weight portion: 70-95 parts of polylactic acid and 5-30 parts of compound plasticizer; the compound plasticizer consists of a component A and a component B, wherein the component A is one of glycerol, xylitol and sorbitol of polyalcohol; the component B is one of dioctyl phthalate, polyethylene glycol with the molecular weight of 1000-8000, triethyl citrate, tributyl citrate, trioctyl citrate, acetyl triethyl citrate, acetyl tributyl citrate and acetyl trioctyl citrate; the weight part ratio of the component A to the component B is 1-5: 1-25;
the preparation steps and conditions are as follows:
(1) the polylactic acid is placed in a vacuum oven in advance for drying;
(2) uniformly mixing the component A and the component B of the compound plasticizer according to the proportion to obtain the compound plasticizer;
(3) banburying and blending: adding polylactic acid and compound plasticizer according to the proportion at the temperature of 175-190 ℃, and mixing for 5-10 minutes at the speed of 30-60 r/min;
(4) and (3) pressing and forming: placing the internally mixed and blended materials in a mold, preheating at the temperature of 190 ℃ at 170 ℃ and under the pressure of 10-20MPa, and carrying out hot pressing for 2-5 minutes; the pressure is 10-20MPa, and then cold pressing is carried out for 3-10 minutes at room temperature to obtain the polylactic acid plasticizing compound.
2. The method of claim 1, wherein the polylactic acid is a semi-crystalline polylactic acid.
3. The method for preparing a polylactic acid plasticized compound according to claim 1 or 2, wherein in the step (2), 5 parts by weight of glycerin and 15 parts by weight of polyethylene glycol having a weight average molecular weight of 6000 are uniformly mixed to prepare a compound plasticizer;
(3) banburying and blending: 20 parts by weight of compound plasticizer and 80 parts by weight of polylactic acid are mixed and blended for 5min by Haake at 180 ℃ and 40 r/min;
(4) and (3) pressing and forming: then preheating for 5 minutes at 190 ℃, then carrying out hot pressing for 5 minutes, then carrying out cold pressing for 3 minutes at room temperature, wherein the pressure is 10MPa, and carrying out compression molding to obtain the polylactic acid plasticizing compound.
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