CN115772322A - Preparation method of degradable preservative film - Google Patents
Preparation method of degradable preservative film Download PDFInfo
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- CN115772322A CN115772322A CN202111036488.XA CN202111036488A CN115772322A CN 115772322 A CN115772322 A CN 115772322A CN 202111036488 A CN202111036488 A CN 202111036488A CN 115772322 A CN115772322 A CN 115772322A
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- polylactic acid
- attapulgite
- degradable
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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Abstract
The invention discloses a preparation method of a degradable preservative film, which comprises the following steps: s1, catalyzing polylactic acid and a catalyst at high speed and high temperature to change the polylactic acid and the catalyst into a polylactic acid master batch with plasticity; s2, uniformly mixing the polylactic acid master batch, the modified nano attapulgite and the filler, and then manufacturing completely biodegradable polylactic acid polymer particles by a granulator; s3, carrying out catalytic polymerization on the mixed raw materials at a high temperature; s4, granulating by using an extrusion granulation processing method, blowing the film to obtain the preservative film, uniformly mixing the polylactic acid master batch, the modified nano-attapulgite and the filler, and then manufacturing degradable polylactic acid polymer particles by using a granulator, wherein the water vapor generated in the storage process of the fresh fruits and vegetables can be adjusted, and meanwhile, the modified nano-attapulgite has a strong adsorption effect and can strongly adsorb ethylene gas generated in the storage process of the fresh fruits and vegetables, so that the quality guarantee period is prolonged, the loss is reduced, and no burden is caused to the environment.
Description
Technical Field
The invention relates to the technical field of films, in particular to a preparation method of a degradable preservative film.
Background
Most of preservative films (bags) used in the market at present are made of polyethylene, the polyethylene is a non-degradable material, serious pollution is caused to the environment for a long time, and a series of policy restrictions are issued in China or the production of non-degradable plastics is prohibited, so that the development of degradable preservative films is necessary. Polylactic acid is a world-recognized biodegradable material, and can be applied to the field of preservative films by overcoming the defects thereof through a modification technology.
In addition, most preservative films have a very limited preservation function, microorganisms are propagated in a large quantity to cause spoilage due to easy condensation of water vapor in the using process, and the storage of the products is directly influenced by after-ripening of fresh and alive agricultural products due to continuous respiration of the agricultural products after packaging and ethylene generation.
Disclosure of Invention
The invention provides a preparation method of a degradable preservative film, which can effectively solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the preparation method of the degradable preservative film comprises the following steps:
s1, catalyzing polylactic acid and a catalyst at high speed and high temperature to change the polylactic acid and the catalyst into a polylactic acid master batch with plasticity;
s2, uniformly mixing the polylactic acid master batch, the modified nano attapulgite and the filler, and then manufacturing degradable polylactic acid polymer particles by a granulator;
s3, carrying out catalytic polymerization on the mixed raw materials at high temperature;
and S4, granulating and blowing the film by using an extrusion granulation processing method to obtain the preservative film.
According to the technical scheme, the ratio of the polylactic acid master batch, the modified nano attapulgite and the filler in the S2 is as follows according to the mass ratio: 50-80% of polylactic acid, 5-10% of attapulgite and 15-25% of filler;
the temperature in the S3 is 180-200 ℃.
According to the technical scheme, the modified nano attapulgite is a fresh-keeping material;
the preparation method comprises the following steps:
A. firstly, immersing attapulgite in a hydrochloric acid solution with the mass fraction of 3% for 10min, then filtering and immersing in a sodium hydroxide solution with the mass fraction of 10% for 10min, filtering and washing with deionized water for one time and airing for later use, then placing in a high-temperature calcining furnace for treating at 950-980 ℃ for 1h, and taking out for later use;
B. preparing a modifier:
a. putting methyl lignocaonate and glycerol into a reaction kettle together, then adding potassium hydroxide accounting for 2% of the total mass of the methyl lignocaonate and the glycerol, continuously stirring for 30min, then adding octyl phenol polyoxyethylene ether into the reaction kettle, and stirring for 30min at 70-74 ℃ under the pressure of 0.25-0.35MPa to obtain a modifier M1;
b. putting tetradecyl trimethyl ammonium bromide and hexadecyl sodium sulfonate into a stirring tank according to the weight ratio of 1.9-2.1, stirring and mixing at 35-38 ℃ for 35-40min, and taking out to obtain a modifier M2;
C. b, putting the attapulgite treated in the step A into a modifier M1, stirring for 50-55min, and filtering;
then adding the mixture into a modifier M2, stirring for 35-40min, filtering, and drying;
D. and grinding the treated attapulgite by using a superfine grinding dispersion machine to obtain the modified nano material with the diameter of about 20 nm.
According to the technical scheme, the filler is PBAT (poly (butylene terephthalate)/adipate) plastic particles.
Compared with the prior art, the invention has the beneficial effects that: polylactic acid is catalyzed at high temperature and then becomes polylactic acid master batch with plasticity, the polylactic acid master batch, modified nano-attapulgite and filling materials are mixed uniformly, degradable polylactic acid polymer particles are manufactured by a granulator, the prepared film has good breathing function, water vapor generated during storage of fresh fruits and vegetables can be adjusted, meanwhile, the modified nano-attapulgite has strong adsorption effect and can strongly adsorb ethylene gas generated in the storage process of the fresh fruits and vegetables, thereby prolonging the shelf life and reducing the loss.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings:
FIG. 1 is a schematic diagram of the structure of the process steps of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it should be understood that they are presented herein only to illustrate and explain the present invention and not to limit the present invention.
Example (b): as shown in figure 1, the invention provides a technical scheme that the preparation method of the degradable preservative film comprises the following steps:
s1, catalyzing polylactic acid and a catalyst at high speed and high temperature to change the polylactic acid and the catalyst into a polylactic acid master batch with plasticity;
s2, uniformly mixing the polylactic acid master batch, the modified nano attapulgite and the filler, and then manufacturing completely biodegradable polylactic acid polymer particles by a granulator;
s3, carrying out catalytic polymerization on the mixed raw materials at high temperature;
and S4, granulating by using an extrusion granulation processing method, and blowing the film to obtain the preservative film.
According to the technical scheme, the ratio of the polylactic acid master batch, the modified nano-attapulgite and the filler in the S2 is as follows according to the mass ratio: 70% of polylactic acid, 10% of attapulgite and 20% of filler;
the temperature in S3 is 190 ℃.
According to the technical scheme, the modified nano attapulgite is used as a fresh-keeping material;
the preparation method comprises the following steps:
A. firstly, immersing attapulgite in a hydrochloric acid solution with the mass fraction of 3% for 10min, then filtering and immersing in a sodium hydroxide solution with the mass fraction of 10% for 10min, filtering and washing with deionized water for one time and airing for later use, then placing in a high-temperature calcining furnace for treating at 950 ℃ for 1h and taking out for later use;
B. preparing a modifier:
a. putting methyl lignocerate and glycerol into a reaction kettle together, adding 2% of potassium hydroxide by mass, continuously stirring for 30min, adding octylphenol polyoxyethylene ether into the reaction kettle, and stirring at 72 ℃ and 0.35MPa for 30min to obtain a modifier M1;
b. putting tetradecyl trimethyl ammonium bromide and hexadecyl sodium sulfonate into a stirring tank together according to a weight ratio of 1.9-2.1, stirring and mixing for 38min at 36 ℃, and taking out to obtain a modifier M2;
C. b, putting the attapulgite treated in the step A into a modifier M1, stirring for 50min, and filtering;
then adding the mixture into a modifier M2, stirring for 37min, filtering, and drying;
D. and grinding the treated attapulgite by using a superfine grinding dispersion machine to obtain the modified nano material with the diameter of about 20 nm.
According to the technical scheme, the filler is PBAT (poly (butylene terephthalate)/adipate) plastic particles.
Compared with the prior art, the invention has the following beneficial effects: polylactic acid is catalyzed at high temperature to become polylactic acid master batch with plasticity, the polylactic acid master batch, modified nano attapulgite and a filling material are uniformly mixed, and degradable polylactic acid polymer particles are manufactured by a granulator, so that the manufactured film has a good breathing function, water vapor generated during storage of fresh fruits and vegetables can be regulated, meanwhile, the modified nano attapulgite has a strong adsorption effect and can strongly adsorb ethylene gas generated during storage of the fresh fruits and vegetables, so that the quality guarantee period is prolonged, the loss is reduced, more importantly, the functional preservative film can be completely degraded under a certain condition, the final products are carbon dioxide and water, no burden is caused to the environment, the preservative film is granulated and blown by an extrusion granulation processing method to manufacture a 2-filament-thick preservative film which is manufactured into a bag, seventy-eight mature green bananas are placed into the bag for sealing under the condition of 13-14 ℃, the preservative film can be stored for 45 days without color change, and anhydrous bananas, the traditional storage mode is that an ethylene absorbent is added into the PE bag for 30 days, and the quality guarantee period can be prolonged for 15 days; testing the sweet peaches at the normal temperature of 25-30 ℃, putting 20 sweet peaches picked from a tree into a bag, tying the bag, then putting the bag into a carton, and performing logistic test for 7 days, wherein no rotten fruit exists, the color, the smell and the taste are normal, and the contrast PE freshness protection bag sold on the market is 50% bad fruit, so the freshness protection film disclosed by the invention is also suitable for the transportation and freshness protection of fruits at the normal temperature.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The preparation method of the degradable preservative film is characterized by comprising the following steps: the method comprises the following steps:
s1, catalyzing polylactic acid and a catalyst at high speed and high temperature to change the polylactic acid and the catalyst into a polylactic acid master batch with plasticity;
s2, uniformly mixing the polylactic acid master batch, the modified nano attapulgite and the filler, and then manufacturing degradable polylactic acid polymer particles by a granulator;
s3, carrying out catalytic polymerization on the mixed raw materials at a high temperature;
and S4, granulating and blowing the film by using an extrusion granulation processing method to obtain the preservative film.
2. The preparation method of the degradable preservative film according to claim 1, wherein the ratio of the polylactic acid master batch, the modified nano attapulgite and the filler in the S2 is as follows according to the mass ratio: 50-80% of polylactic acid, 5-10% of attapulgite and 15-25% of filler;
the temperature in the S3 is 180-200 ℃.
3. The method for preparing the degradable preservative film according to claim 1, wherein the modified nano attapulgite is a preservative material;
the preparation method comprises the following steps:
A. firstly, immersing attapulgite in a hydrochloric acid solution with the mass fraction of 3% for 10min, then filtering and immersing in a sodium hydroxide solution with the mass fraction of 10% for 10min, filtering and washing with deionized water for one time and airing for later use, then placing in a high-temperature calcining furnace for treating at 950-980 ℃ for 1h, and taking out for later use;
B. preparing a modifier:
a. putting methyl lignocaonate and glycerol into a reaction kettle together, then adding potassium hydroxide accounting for 2% of the total mass of the methyl lignocaonate and the glycerol, continuously stirring for 30min, then adding octyl phenol polyoxyethylene ether into the reaction kettle, and stirring for 30min at 70-74 ℃ under the pressure of 0.25-0.35MPa to obtain a modifier M1;
b. putting tetradecyl trimethyl ammonium bromide and hexadecyl sodium sulfonate into a stirring tank according to the weight ratio of 1.9-2.1, stirring and mixing at 35-38 ℃ for 35-40min, and taking out to obtain a modifier M2;
C. b, putting the attapulgite treated in the step A into a modifier M1, stirring for 50-55min, and filtering;
then adding the mixture into a modifier M2, stirring for 35-40min, filtering out, and drying;
D. and grinding the treated attapulgite by using a superfine grinding dispersion machine to obtain the modified nano material with the diameter of about 20 nm.
4. The method for preparing the degradable plastic wrap of claim 1, wherein the filler is PBAT (polybutylene terephthalate/adipate) plastic particles.
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| CN202111036488.XA CN115772322A (en) | 2021-09-06 | 2021-09-06 | Preparation method of degradable preservative film |
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| CN202111036488.XA CN115772322A (en) | 2021-09-06 | 2021-09-06 | Preparation method of degradable preservative film |
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| CN106479143A (en) * | 2016-10-31 | 2017-03-08 | 河南龙都天仁生物材料有限公司 | A kind of attapulgite/poly lactic acid nano composite material and preparation method thereof |
| CN106751629A (en) * | 2017-01-24 | 2017-05-31 | 威海共达塑胶化工制品有限公司 | Complete biodegradable preservative film and preparation method thereof |
| CN108238607A (en) * | 2018-01-31 | 2018-07-03 | 安徽金丰新型建材有限公司 | A kind of modification processing method of attapulgite |
| CN108384381A (en) * | 2018-01-31 | 2018-08-10 | 安徽金丰新型建材有限公司 | A kind of preparation method of heatproof noise reduction architectural decoration coating material |
| CN110452509A (en) * | 2019-08-01 | 2019-11-15 | 山东省农业科学院农产品研究所 | One kind is fresh-keeping to use film |
| US20200291225A1 (en) * | 2017-09-12 | 2020-09-17 | Jiangsu Golden-Poly Alloy Material Co.,Ltd. | Low cost bio-based full degradable film and preparation method thereof |
| CN112280261A (en) * | 2020-11-10 | 2021-01-29 | 吴建 | Full-biodegradable high-barrier PLA/PBAT composite packaging film |
| CN112341655A (en) * | 2020-12-15 | 2021-02-09 | 宁波柯恩生物材料有限公司 | Full-biodegradable blown film composite material with high polylactic acid content and preparation method thereof |
| CN112538242A (en) * | 2020-12-03 | 2021-03-23 | 辽宁金科塑胶科技有限公司 | Environment-friendly full-degradable novel garbage bag and preparation thereof |
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2021
- 2021-09-06 CN CN202111036488.XA patent/CN115772322A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106479143A (en) * | 2016-10-31 | 2017-03-08 | 河南龙都天仁生物材料有限公司 | A kind of attapulgite/poly lactic acid nano composite material and preparation method thereof |
| CN106751629A (en) * | 2017-01-24 | 2017-05-31 | 威海共达塑胶化工制品有限公司 | Complete biodegradable preservative film and preparation method thereof |
| US20200291225A1 (en) * | 2017-09-12 | 2020-09-17 | Jiangsu Golden-Poly Alloy Material Co.,Ltd. | Low cost bio-based full degradable film and preparation method thereof |
| CN108238607A (en) * | 2018-01-31 | 2018-07-03 | 安徽金丰新型建材有限公司 | A kind of modification processing method of attapulgite |
| CN108384381A (en) * | 2018-01-31 | 2018-08-10 | 安徽金丰新型建材有限公司 | A kind of preparation method of heatproof noise reduction architectural decoration coating material |
| CN110452509A (en) * | 2019-08-01 | 2019-11-15 | 山东省农业科学院农产品研究所 | One kind is fresh-keeping to use film |
| CN112280261A (en) * | 2020-11-10 | 2021-01-29 | 吴建 | Full-biodegradable high-barrier PLA/PBAT composite packaging film |
| CN112538242A (en) * | 2020-12-03 | 2021-03-23 | 辽宁金科塑胶科技有限公司 | Environment-friendly full-degradable novel garbage bag and preparation thereof |
| CN112341655A (en) * | 2020-12-15 | 2021-02-09 | 宁波柯恩生物材料有限公司 | Full-biodegradable blown film composite material with high polylactic acid content and preparation method thereof |
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