CN112538241B - Aging-resistant hydrolysis-resistant biodegradable color master batch and preparation method and application thereof - Google Patents
Aging-resistant hydrolysis-resistant biodegradable color master batch and preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
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- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- C08K5/15—Heterocyclic compounds having oxygen in the ring
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Abstract
The invention discloses an anti-aging and anti-hydrolytic biodegradation color master batch, a preparation method and an application thereof, wherein the color master batch comprises the following components in parts by weight: 60-90 parts of biodegradable polyester; 6-8 parts of an anti-hydrolysis agent; 4-8 parts of a light stabilizer; 5-10 parts of an ultraviolet absorber; 1-5 parts of an antioxidant; 10-50 parts of pigment; 1 to 10 parts of a lubricant. According to the invention, PLA and PBAT are blended according to a certain proportion to be used as a carrier, epoxy compounds and bisoxazoline compounds are selected to be compounded according to a certain proportion for use, so that the compatibility among all components can be increased, the dispersibility is improved, and due to the crosslinking enhancement effect of the epoxy compounds and the chain extension tackifying effect of the bisoxazoline compounds, the prepared biodegradable color master batch has good aging resistance and hydrolysis resistance, can be added into a biodegradable agricultural mulching film according to a certain proportion, so that colored mulching films with different colors are obtained, meanwhile, the aging resistance and hydrolysis resistance of the mulching film can be well improved, and the service cycle of the mulching film is prolonged.
Description
Technical Field
The invention relates to the technical field of degradable plastics, in particular to an anti-aging and anti-hydrolytic biodegradable color master batch and a preparation method and application thereof.
Background
The agricultural mulching film is called agricultural film for short, is mainly used for covering farmlands, and has the effects of preserving heat, retaining water, promoting seed germination and rapid growth of seedlings and inhibiting weed growth. The agricultural films have various colors, the agricultural films with different colors have different absorption and reflection rules on spectra, and have different influences on the growth of crops, weeds, plant diseases and insect pests and the ground temperature; in the actual use process, the agricultural films with different colors are required to be selected according to the characteristics of different crops and planting seasons.
The traditional agricultural film mostly adopts Polyethylene (PE) plastics, and the manual recovery is difficult after the part disintegrates, and PE plastics are difficult to degrade under natural condition, if can not in time retrieve totally, remaining plastic film influences soil physical property and crop growth and development, causes planting income and ecological environment's dual loss. In order to practice the concept of green environmental protection and realize the sustainable development of plastic film mulching planting, the best approach is the development and development application of biodegradable agricultural films.
At present, various biodegradable agricultural films are available on the market, and mainly degradable materials such as polylactic acid (PLA) or poly adipic acid/polybutylene terephthalate (PBAT) are adopted. The current biodegradable agricultural film can not completely replace the traditional agricultural film, one of the main reasons is that the biodegradable agricultural film is easy to age and degrade, the service cycle is short, the problems that part of crops do not grow completely and the mulching film cracks and disintegrates can occur, the problem that the crop with longer growing season can not be met, the film covering significance is lost, and the use cost is increased. The environmental factors influencing the aging and degradation of the biodegradable agricultural film mainly comprise photoaging and hydrolysis, and PLA and PBAT contain a large number of carbonyl, double bonds and other groups, can absorb ultraviolet rays in sunlight, and cause molecular chain breakage, thereby causing photoaging; in addition, the polymer is easy to absorb water, so that ester bonds in a molecular chain are hydrolyzed, the thermal stability of the polymer is influenced, and the aging performance of the polymer is indirectly influenced. The problem that the biodegradable agricultural film is easy to age and degrade is solved, the service cycle of the biodegradable agricultural film is prolonged, and the biodegradable agricultural film is one of the main directions for replacing the traditional agricultural film.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide the aging-resistant and hydrolysis-resistant biodegradable color master batch which is suitable for preparing various colored biodegradable agricultural films and can obviously improve the aging-resistant and hydrolysis-resistant performance of the agricultural films.
The invention also aims to provide a preparation method of the aging-resistant and hydrolysis-resistant biodegradable color master batch.
The invention is realized by the following technical scheme:
the aging-resistant and hydrolysis-resistant biodegradable color master batch is characterized by comprising the following components in parts by weight:
the biodegradable polyester is polylactic acid (PLA) and polybutylene adipate/terephthalate (PBAT), wherein the weight ratio of the polylactic acid (PLA) to the polybutylene adipate/terephthalate (PBAT) is (3-4): 1;
the hydrolysis resistant agent is a bisoxazoline compound and an epoxy compound in a weight ratio of (1-2.5): 1, compounding.
The polylactic acid adopted by the invention is polylactic acid with the D-lactic acid content of more than 10 percent, the polylactic acid is amorphous non-crystalline polylactic acid generally, the thermal deformation temperature is lower, the polylactic acid is selected as a carrier, and the prepared master batch has better dispersibility in the using process.
The bisoxazoline compound is selected from any one of 2,2' -bis- (2-oxazoline) or 1, 4-bis- (2-oxazoline) benzene; the epoxy compound is selected from any one of phenyl glycidyl ether, bisphenol A diglycidyl ether, tetra (phenyl glycidyl ether) ethane or trimethoxy [3- (glycidyl ether) ] silane.
According to research, the bisoxazoline compound and the epoxy compound are selected to be compounded according to a specific proportion, so that the ageing resistance and the hydrolysis resistance of the material can be obviously improved in the formula of the invention. The bisoxazoline compound has strong reactivity with carboxyl, so that polymer molecular chains are coupled to achieve the effect of chain extension and viscosity increasing, and in addition, the bisoxazoline compound reacts with degradation product carboxylic acid to form a stable product, so that the polymer is prevented from being further degraded, and the stability of the polymer is improved; the epoxy compound can react with carboxyl and hydroxyl in PBAT and PLA respectively by virtue of the epoxy functional group of the epoxy compound, so that the interface compatibility of the PLA and the PBAT is obviously improved, the dispersibility of other components is improved, the carboxyl end group and the hydroxyl end group can be converted and reconnected to form a cross-linked structure, and the stability and the strength of the material are enhanced. The two are cooperated to cooperate, so that the material has good stability, excellent aging resistance and hydrolysis resistance and good mechanical property. Preferably, the weight ratio of the bisoxazoline compound to the epoxy compound is 2:1, compounding.
The light stabilizer is any one of light stabilizer 770 or light stabilizer GW-540; the ultraviolet stabilizer is selected from any one of UV-P, UV-326, UV-327, UV-328 or UV-329; the antioxidant is antioxidant 1010 and antioxidant DSTP according to the weight ratio (1.5-2): 1, compounding. Preferably, the light stabilizer, the ultraviolet stabilizer and the antioxidant are mixed according to the weight ratio of 2:3:1, the three assistants have good synergistic effect, so that the aging resistance of the material is obviously improved, and the service cycle of the mulching film is prolonged.
The invention can select and add pigment according to different requirements, and the pigment is selected from any one or more of titanium dioxide, iron oxide red, carbon black, ultramarine, phthalocyanine or organic yellow.
The lubricant is selected from any one or more of stearic acid and salt thereof, montan wax, erucic amide, oleamide or ethylene bis stearamide.
The invention also provides a preparation method of the aging-resistant and hydrolysis-resistant biodegradable color master batch, which comprises the following steps: according to the proportion, the components are stirred at a high speed and mixed uniformly, then the mixture is added into a double-screw extruder, and the mixture is melted and mixed at the temperature of 150-190 ℃, and then extrusion granulation is carried out, so as to obtain the aging-resistant and hydrolysis-resistant biodegradable color master batch; wherein the stirring speed is 500-550 rpm.
The invention also provides application of the aging-resistant hydrolysis-resistant biodegradable color master batch in biodegradable agricultural mulching films. The addition amount of the biodegradable color master batch in the agricultural mulching film is 4-10% (by weight). When preparing the agricultural mulching film, the anti-aging and anti-hydrolytic biodegradation color master batch is added according to different dosage proportions according to the actual application requirements.
The biodegradable agricultural mulching film can be prepared by the existing film blowing process.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, PLA and PBAT are blended according to a certain proportion to be used as a carrier, and the epoxy compound and the bisoxazoline compound are selected to be compounded according to a certain proportion for use, so that the compatibility among the components can be increased, the dispersibility is improved, and the prepared biodegradable color master batch has good aging resistance and hydrolysis resistance due to the crosslinking enhancement effect of the epoxy compound and the chain extension tackifying effect of the bisoxazoline compound.
(2) The aging-resistant hydrolysis-resistant color master batch prepared by the invention is a functional color master batch, has good dispersibility when used, is added into a biodegradable agricultural mulching film according to a certain proportion to obtain colored mulching films with different colors, and can well improve the aging-resistant hydrolysis-resistant performance of the mulching film and prolong the service cycle of the mulching film.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the concept of the invention. All falling within the scope of the present invention.
The raw materials used in the examples and comparative examples of the present invention are described below, but are not limited to these materials:
PLA1: natureWorks 4060D, the content of D-lactic acid is 12%;
PLA2: natureWorks 4032D, the content of L-lactic acid is 98.5 percent;
PBAT: jinfa science and technology Flex-64D;
bis-oxazolines: 2,2' -bis- (2-oxazoline), 1, 4-bis- (2-oxazolinyl) benzene, commercially available;
epoxy compounds: phenyl glycidyl ether, tetrakis (phenyl glycidyl ether) ethane, trimethoxy [3- (glycidyl ether) ] silane, commercially available;
light stabilizer: light stabilizer GW-540, light stabilizer 770, commercially available;
ultraviolet stabilizer: UV-326, UV-P, commercially available;
antioxidant: antioxidant 1010, antioxidant DSTP, commercially available;
pigment: titanium dioxide, commercially available;
lubricant: erucamide, commercially available.
Preparation methods of biodegradable color concentrates of examples 1 to 5 and comparative examples 1 to 5: according to the mixture ratio of the following table 1 and table 2, the components are stirred and mixed uniformly at the rotating speed of 500rpm, added into a double-screw extruder, melted and mixed at the temperature of 150-190 ℃, extruded and granulated to obtain the biodegradable color master batch.
The biodegradable color master batches prepared in the examples 1-5 and the comparative examples 1-5 are added into the fully dried PLA and PBAT according to the proportion of 6% for film blowing, 10 mu m biodegradable agricultural mulching film is prepared, and relevant performance tests are carried out.
Preparation method of comparative example 6: to the fully dried PLA and PBAT, 0.12% of 2,2' -bis- (2-oxazoline) was added; 0.12% phenyl glycidyl ether; 0.16% of light stabilizer GW-540;0.25% UV-326;0.05% of antioxidant 1010;0.03% of antioxidant DSTP;1.6% of pigment; 0.2% of a lubricant; stirring and mixing the components uniformly at the rotating speed of 500rpm, adding the components into a double-screw extruder, melting and mixing at the temperature of 150-190 ℃, and extruding and granulating to obtain the biodegradable color master batch; and directly adding the prepared biodegradable color master batch into a film blowing machine for film blowing to prepare a 10-micron biodegradable agricultural mulching film for relevant performance test.
The relevant performance test methods or criteria are as follows:
(1) And (3) testing tensile property: the test standard is ASTM D638-02; the mulching film materials prepared in the examples and the comparative examples are cut into 6.22mm 25mm dumbbell-shaped sample strips by using a mold, five standard sample strips are collected in the transverse direction and the longitudinal direction of each sample, the sample strips are fixed on a universal mechanical testing machine, the stretching speed is set to be 200mm/min, data are collected after the test is finished, and the final result is averaged.
(2) And (3) photo aging test: adopting a fluorescent ultraviolet lamp with the wavelength of 340nm and the irradiation intensity of 1.1W/m 2 Setting ultraviolet accelerated aging box test conditions, irradiating the sample film under ultraviolet light at 60 ℃ for 8h, then condensing in dark environment at 50 ℃ for 4h, taking 12h as a cycle, and repeating 10 cycles as a test period.
(3) Hydrolysis test: a constant temperature and humidity box is adopted, the constant temperature and humidity are kept for 8 hours in a 60 ℃ dark environment in the first stage, the constant temperature and humidity are kept for 4 hours in a 50 ℃ and 98% humidity dark environment in the second stage, 12 hours in the two stages are taken as a cycle, and 10 cycles are repeatedly carried out to serve as a test period.
Table 1: the specific proportions of the components in examples 1 to 5 (in parts by weight)
Table 2: the specific proportions (by weight) of the components in comparative examples 1 to 5
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
| PLA1 | 60 | 60 | 60 | 60 | |
| PLA2 | 60 | ||||
| PBAT | 20 | 20 | 20 | 20 | 20 |
| 2,2' -bis- (2-oxazoline) | 5 | 1 | 6 | 3 | |
| Phenyl glycidyl ether | 1 | 5 | 6 | 3 | |
| Light stabilizer GW-540 | 4 | 4 | 4 | 4 | 4 |
| UV-326 | 6 | 6 | 6 | 6 | 6 |
| Antioxidant 1010 | 1.2 | 1.2 | 1.2 | 1.2 | 1.2 |
| Antioxidant DSTP | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
| Pigment (I) | 40 | 40 | 40 | 40 | 40 |
| Lubricant agent | 5 | 5 | 5 | 5 | 5 |
The biodegradable color master batches prepared in the examples and comparative examples in the tables 1 and 2 are added into the fully dried PLA and PBAT according to the proportion of 6% for film blowing, 10-micron biodegradable agricultural mulching films are prepared, and relevant performance tests are carried out.
Table 3: tensile Property test results before and after aging test of examples 1 to 5 and comparative examples 1 to 6
Table 4: tensile Property test results before and after hydrolysis test of examples 1 to 5 and comparative examples 1 to 6
The embodiment and the comparative example show that the aging-resistant and hydrolysis-resistant biodegradable color master batch disclosed by the invention is added in a certain proportion to prepare the biodegradable agricultural mulching film, so that the aging-resistant and hydrolysis-resistant performance of the mulching film can be obviously improved.
Compared with the embodiment 1/2, the compounding ratio of the epoxy compound and the bisoxazoline compound in the color master batch is not in the required range, and the tensile strength reduction rate of the prepared mulching film is obviously increased after aging test and hydrolysis test, which shows that the effect of improving the aging resistance and hydrolysis resistance of the mulching film is poor.
Compared with the example 1, the epoxy compound or the bis-oxazoline compound is independently added into the color master batch, the improvement effect on the aging resistance and the hydrolysis resistance of the mulching film is poor, and the tensile strength reduction rate of the mulching film is obviously increased after an aging test and a hydrolysis test.
Comparative example 5 compared with example 1, the PLA with a content of 98.5% is crystalline polylactic acid, and the prepared color master batch has poor dispersibility when used, resulting in poor aging resistance and hydrolysis resistance of the prepared mulching film.
Comparative example 6 no functional color master batch is prepared, and all the components are directly added into PLA and PBAT resin in proportion to prepare the biodegradable mulching film, and the components have poor dispersibility and poor aging resistance and hydrolysis resistance.
Claims (7)
1. The aging-resistant and hydrolysis-resistant biodegradable color master batch is characterized by comprising the following components in parts by weight:
60-90 parts of biodegradable polyester;
6-8 parts of an anti-hydrolysis agent;
4-8 parts of a light stabilizer;
5-10 parts of an ultraviolet absorber;
1-5 parts of an antioxidant;
10-50 parts of pigment;
1 to 10 parts of a lubricant;
the biodegradable polyester is polylactic acid (PLA) and polybutylene adipate/terephthalate (PBAT), wherein the weight ratio of the polylactic acid (PLA) to the polybutylene adipate/terephthalate (PBAT) is (3-4): 1;
the content of D-lactic acid in the polylactic acid is 10-12 percent;
the hydrolysis resistant agent is a bisoxazoline compound and an epoxy compound in a weight ratio of 2:1, compounding;
the light stabilizer, the ultraviolet stabilizer and the antioxidant are mixed according to the weight ratio of 2:3:1, compounding.
2. The aging-resistant hydrolysis-resistant biodegradable color masterbatch according to claim 1, wherein the bisoxazoline compound is selected from any one of 2,2' -bis- (2-oxazoline) and 1, 4-bis- (2-oxazoline) benzene; the epoxy compound is selected from any one of phenyl glycidyl ether, bisphenol A diglycidyl ether, tetra (phenyl glycidyl ether) ethane or trimethoxy [3- (glycidyl ether) ] silane.
3. The aging resistant and hydrolysis resistant biodegradation color concentrate of claim 1 wherein said light stabilizer is any one of light stabilizer 770 or light stabilizer GW-540; the ultraviolet stabilizer is selected from any one of UV-P, UV-326, UV-327, UV-328 or UV-329; the antioxidant is composed of an antioxidant 1010 and an antioxidant DSTP according to the weight ratio of (1.5 to 2): 1, compounding.
4. The aging-resistant and hydrolysis-resistant biodegradable color masterbatch according to claim 1, wherein the pigment is selected from any one or more of titanium dioxide, iron oxide red, carbon black, ultramarine, phthalocyanine or organic yellow; the lubricant is selected from one or more of stearic acid and salt thereof, montan wax, erucic amide, oleic amide or ethylene bis stearamide.
5. The preparation method of the aging-resistant and hydrolysis-resistant biodegradable color master batch according to any one of claims 1 to 4, which is characterized by comprising the following steps: according to the proportion, the components are stirred at a high speed and mixed uniformly, then the mixture is added into a double-screw extruder, and the mixture is melted and mixed at the temperature of 150 to 190 ℃, and then extruded and granulated to obtain the aging-resistant and hydrolysis-resistant biodegradable color master batch; wherein the stirring speed is 500 to 550rpm.
6. The application of the aging-resistant and hydrolysis-resistant biodegradable color master batch according to any one of claims 1 to 4, which is used for preparing a biodegradable agricultural mulching film.
7. The application of the aging-resistant and hydrolysis-resistant biodegradable masterbatch according to claim 6, wherein the biodegradable masterbatch is added to the biodegradable agricultural mulching film in an amount of 4-10% by weight.
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| CN116333458B (en) * | 2023-02-24 | 2023-12-01 | 大禾科技发展(南京)有限公司 | High-temperature-resistant biodegradable agricultural film for rice based on graphene and multiwall carbon nanotube composite material |
| CN116589836A (en) * | 2023-07-13 | 2023-08-15 | 中国农业科学院农业环境与可持续发展研究所 | Green safe biodegradable material and preparation method and application thereof |
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| CN109535675A (en) * | 2018-12-07 | 2019-03-29 | 北京惠林苑生物科技有限公司 | The hydrolysis light of resistance to UV aging biodegradable plastic mulch and preparation method thereof |
| CN110330773A (en) * | 2019-07-19 | 2019-10-15 | 深圳利琒环保材料有限公司 | A kind of controllable full-biodegradable mulch and preparation method thereof |
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