CN110885541A - Biodegradable polylactic acid-based antirust master batch and preparation method thereof - Google Patents
Biodegradable polylactic acid-based antirust master batch and preparation method thereof Download PDFInfo
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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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- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
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Abstract
The invention relates to a biodegradable polylactic acid-based gas-phase antirust master batch and a preparation method thereof, wherein the gas-phase antirust master batch comprises the following components in parts by weight: 45-55 parts of surface modified polylactic acid, 8-12 parts of polyethylene, 10-15 parts of 3, 5-dinitrobenzoic acid hexamethylene imine, 3-8 parts of benzotriazole or a derivative thereof, 3-8 parts of sodium molybdate, 1-5 parts of sodium nitrite, 1-5 parts of thiadiazole or a derivative thereof, 4-8 parts of plasticizer and 4-8 parts of reinforcing agent, and the raw materials are mixed and blended and granulated according to a specific sequence to obtain the gas-phase antirust master batch. The gas-phase antirust master batch prepared by the invention has good biodegradability.
Description
Technical Field
The invention relates to a composition of biodegradable polylactic acid-based gas-phase antirust master batch and a preparation method thereof, belonging to the technical field of metal antirust.
Background
With the increasing global population and the increasing shortage of resources, the development of a resource-saving and environment-harmonized society has become a development direction. Statistically, the amount of plastic used globally in 2016 will reach 5 hundred million tons, and global plastic consumption is expected to increase at a rate of 8% per year, with annual consumption of plastic reaching more than 7 hundred million tons per 2030, and plastic waste amounts of approximately 2.6-3 million tons per year.
Plastic packages have become one of the major packaging materials in the consumer goods field, and the application range has been gradually expanded to various mass production fields and transport packaging fields. In the transportation and storage processes of the equipment such as automobiles, steel, machinery, electronics and the like and the inlet and outlet of a production line, gas-phase rust-proof plastic products such as a gas-phase rust-proof film, a gas-phase rust-proof bubble pad and the like are needed to be paved in a container or directly wrapped on a packaged object, so that the situation that oxygen and water react with metal to generate corrosion is prevented. These plastic products have a short service life, typically only one to several months, and become quickly waste after the goods arrive at their destination. The gas-phase rust-proof plastic product is produced by using petroleum as a basic raw material, adding a gas-phase corrosion inhibitor which has volatility and certain vapor pressure like camphor balls and applying a chemical synthesis method. Because of the volatility of the vapor phase corrosion inhibitor, the vapor phase rust-proof material is an environment-friendly material in literature, but the corrosion inhibitor contained in the material cannot be completely volatilized, and the plastic carrier can be naturally rotted after being buried in nature for at least 200 years and is difficult to degrade, so that the energy is consumed and the environment is polluted, therefore, the vapor phase rust-proof plastic product with short service life needs to be produced into a degradable product.
Disclosure of Invention
The invention aims to solve the technical problems and provides a biodegradable polylactic acid-based gas-phase antirust master batch and a preparation method thereof, so that a gas-phase antirust plastic product can be biodegraded, and the problems of environment and energy are solved.
The technical scheme adopted for solving the technical problem of the invention is as follows:
the biodegradable polylactic acid-based gas-phase antirust master batch comprises the following components in parts by weight: 45-55 parts of surface modified polylactic acid, 8-12 parts of polyethylene, 10-15 parts of 3, 5-dinitrobenzoic acid hexamethylene imine, 3-8 parts of benzotriazole or a derivative thereof, 3-8 parts of sodium molybdate, 1-5 parts of sodium nitrite, 1-5 parts of thiadiazole or a derivative thereof, 4-8 parts of plasticizer and 4-8 parts of reinforcing agent.
Specifically, the surface modified polylactic acid is used as a carrier, and a film forming substance replaces the non-degradable resin in the conventional plastic film, so that the product has better natural degradation performance. However, the molecular chain of polylactic acid contains a large amount of COO-bonds with strong polarity, which can cause too strong rigidity of the molecular chain and poor flexibility of the material, and can cause poor fusion of the components in the system, and finally influence the uniformity of the material and the function of the antirust components, so the polylactic acid needs to be subjected to surface modification to reduce the surface polarity and increase the compatibility with other components.
The 3,5 dinitrobenzoic acid hexamethylene imine, benzotriazole or derivatives thereof, sodium molybdate, sodium nitrite, thiadiazole or derivatives thereof and other 5 substances are rust-proof components, 4 synergistic effects are achieved among the 5 components, and the components are as follows: volatilization rate synergy, chemical reaction synergy, molecular spatial structure synergy, adsorption type synergy. The volatilization rate synergy and the adsorption type synergy mean that 5 components have different volatilization rates, the benzotriazole or the derivative thereof with higher vapor pressure and higher volatilization rate volatilizes to the metal surface firstly, quickly occupies the metal surface, is combined with the site in a physical adsorption mode, then the 3, 5-dinitrobenzoic acid hexamethylene imine and the thiadiazole or the derivative thereof volatilize to the metal surface, and then the previous benzotriazole or the derivative thereof is replaced in a chemical adsorption mode to form a more stable complex protective layer. The molecular space structure synergy means that the molecular volumes of 3,5 dinitrobenzoic acid hexamethylene imine and thiadiazole or derivatives thereof are greatly different, and relatively complete coverage can be formed on the metal surface. The chemical reaction synergy means that trace moisture and trace hydrogen ions in the space react with sodium molybdate and sodium nitrite to release strong oxidizing groups, and trace metal atoms are oxidized into metal ions, so that the combination of 3,5 dinitrobenzoic acid hexamethylene imine and thiadiazole or derivatives thereof is facilitated.
Further, the surface modified polylactic acid is prepared from polylactic acid, a coupling agent and a lubricant in a mass ratio of 1:0.015-0.03: 0.015-0.03. The specific method comprises the following steps: drying polylactic acid, crushing to below 300 meshes, adding the coupling agent and the lubricant under stirring, and reacting for 15-30min to obtain the polylactic acid.
In some embodiments of the present invention, the coupling agent is one or a combination of two or more selected from the group consisting of a silane coupling agent, a titanate coupling agent, and an aluminate coupling agent. Preferably, the coupling agent is a silane coupling agent KH 570.
In some embodiments of the invention, the lubricant is one or a combination of two or more of zinc stearate, calcium stearate, and magnesium stearate. Preferably, the lubricant is zinc stearate.
The invention also provides a method for preparing the biodegradable polylactic acid-based gas-phase antirust master batch, which comprises the following steps:
(1) mixing the surface modified polylactic acid, 3, 5-dinitrobenzoic acid hexamethylene imine, benzotriazole or derivatives thereof, sodium molybdate, sodium nitrite and thiadiazole or derivatives thereof, and stirring for 15min to obtain a mixed material 1;
(2) adding the plasticizer, the reinforcing agent and polyethylene into the mixed material 1, and stirring for 30min to obtain a mixed material 2;
(3) and blending and granulating the mixed material 2 to obtain the biodegradable polylactic acid-based gas-phase antirust master batch.
Further, the stirring temperature in the step (2) is 80 ℃.
The biodegradable polylactic acid-based gas-phase antirust master batch prepared by the invention takes biodegradable modified polylactic acid as a carrier material and takes components screened and compounded from national food additive catalogues as antirust core components, and has good biodegradability.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments.
Example 1: drying a plurality of polylactic acid for 24h at 100 ℃, carrying out superfine grinding by using an WZJ-6J type vibration superfine grinder, sieving by using a 300-mesh sieve, taking 100 parts of polylactic acid, adding 1.5 parts of silane coupling agent KH570 and 1.5 parts of zinc stearate into a high-speed stirring kettle while stirring, and carrying out stirring reaction for 30min to obtain the surface modified polylactic acid.
50 parts of the surface modified polylactic acid, 12 parts of 3, 5-dinitrobenzoic acid hexamethylene imine, 5 parts of benzotriazole, 6 parts of sodium molybdate, 2 parts of sodium nitrite and 3 parts of thiadiazole are taken and stirred for 15min to obtain a mixed material 1, and then 6 parts of plasticizer, 6 parts of reinforcing agent and 10 parts of polyethylene are added at 80 ℃. Stirring for 30min to obtain a mixed material 2, cooling, and granulating the mixed material 2 in a double-screw granulator to obtain the polylactic acid-based gas-phase antirust master batch. (record: Master batch 1#)
Example 2: the master batch No. 1 in the example 1 is directly blown into a degradable polylactic acid-based gas phase antirust film. (as: antirust film 1#)
Example 3: 45 parts of surface modified polylactic acid, 15 parts of 3, 5-dinitrobenzoic acid hexamethylene imine, 5 parts of benzotriazole, 5 parts of sodium molybdate, 3 parts of sodium nitrite and 3 parts of thiadiazole prepared in the embodiment 1 are stirred for 15min to obtain a mixed material 1, and then 8 parts of plasticizer, 8 parts of reinforcing agent and 8 parts of polyethylene are added at 80 ℃. Stirring for 30min to obtain a mixed material 2, cooling, and granulating the mixed material 2 in a double-screw granulator to obtain the polylactic acid-based gas-phase antirust master batch. (record: masterbatch 2#)
Example 4: the master batch No. 2 in the embodiment 3 is directly blown into a degradable polylactic acid-based gas-phase antirust film. (as: antirust film 2#)
Example 5: 55 parts of surface modified polylactic acid, 10 parts of 3, 5-dinitrobenzoic acid hexamethylene imine, 3 parts of benzotriazole, 3 parts of sodium molybdate, 2 parts of sodium nitrite and 5 parts of thiadiazole prepared in the embodiment 1 are stirred for 15min to obtain a mixed material 1, and then 5 parts of plasticizer, 5 parts of reinforcing agent and 12 parts of polyethylene are added at 80 ℃. Stirring for 30min to obtain a mixed material 2, cooling, and granulating the mixed material 2 in a double-screw granulator to obtain the polylactic acid-based gas-phase antirust master batch. (record: masterbatch 3#)
Example 6: the master batch No. 3 in the example 5 is directly blown into a degradable polylactic acid-based gas-phase antirust film. (as: antirust film 3#)
Comparative example 1: 50 parts of the surface-modified polylactic acid prepared in the example 1, 15 parts of 3, 5-dinitrobenzoic acid hexamethylene imine, 8 parts of benzotriazole and 5 parts of thiadiazole are stirred for 15min to obtain a mixed material 1, and then 6 parts of a plasticizer, 6 parts of a reinforcing agent and 10 parts of polyethylene are added at 80 ℃. Stirring for 30min to obtain a mixed material 2, cooling, and granulating the mixed material 2 in a double-screw granulator to obtain the polylactic acid-based gas-phase antirust master batch. (record: master batch 4#)
Comparative example 2: and taking the master batch No. 4 in the comparative example 1 to directly blow into the degradable polylactic acid-based gas-phase antirust film. (as: antirust film 4#)
Comparative example 3: 50 parts of the surface-modified polylactic acid prepared in the example 1, 15 parts of 3, 5-dinitrobenzoic acid hexamethylene imine, 5 parts of benzotriazole, 6 parts of sodium molybdate and 2 parts of sodium nitrite are stirred for 15min to obtain a mixed material 1, and then 6 parts of plasticizer, 6 parts of reinforcing agent and 10 parts of polyethylene are added at 80 ℃. Stirring for 30min to obtain a mixed material 2, cooling, and granulating the mixed material 2 in a double-screw granulator to obtain the polylactic acid-based gas-phase antirust master batch. (record: masterbatch 5#)
Comparative example 4: and taking the master batch No. 5 in the comparative example 3 to directly blow into the degradable polylactic acid-based gas-phase antirust film. (as: antirust film 5#)
Comparative example 5: 50 parts of the surface-modified polylactic acid prepared in example 1, 15 parts of 3, 5-dinitrobenzoic acid hexamethyleneimine, 8 parts of sodium molybdate, 2 parts of sodium nitrite and 3 parts of thiadiazole are stirred for 15min to obtain a mixed material 1, and then 6 parts of a plasticizer, 6 parts of a reinforcing agent and 10 parts of polyethylene are added at 80 ℃. Stirring for 30min to obtain a mixed material 2, cooling, and granulating the mixed material 2 in a double-screw granulator to obtain the polylactic acid-based gas-phase antirust master batch. (record: masterbatch 6#)
Comparative example 6: and taking the master batch No. 6 in the comparative example 5 to directly blow the degradable polylactic acid-based gas-phase antirust film. (as: antirust film 6#)
The rust inhibitive performance and biodegradability of the above examples and comparative examples were verified by the following tests.
1. Novel gas phase rust-proof discrimination test
This test was conducted to verify the gas phase rust inhibitive effects of the examples, comparative examples, and conventional films. The specific contents are as follows:
2g of degradable gas-phase antirust master batch is placed into a 100mL beaker, then is placed into an 800mL beaker filled with 20mL of aqueous solution, a metal test piece with the thickness of 50mm multiplied by 25mm multiplied by 2mm is fixed at the top of the beaker after being processed according to a standard method, sealing is carried out, the temperature of a water bath is set to be 40 ℃, and the experimental period is 7 days.
Will be 200cm2Degradable gas-phase antirust film and 200cm2The PE films with the same thickness are respectively attached to the inner wall of an 800mL beaker, then the beaker is placed into a 100mL beaker filled with 20mL of aqueous solution, a metal test piece with the thickness of 50mm multiplied by 25mm multiplied by 2mm is fixed at the top of the beaker after being processed according to a standard method, sealing is carried out, the temperature of a water bath is set to be 40 ℃, and the experimental period is 7 days.
The above aqueous solutions all contained 1000mg/L HCO3 -、2500mg/L SO4 2-、1500mg/L Cl-。
The test results are shown in table 1:
TABLE 1
According to the data, the antirust performance of the embodiment provided by the invention is obviously superior to that of the comparative example and the conventional film, namely, the antirust performance of the gas-phase antirust master batch and the gas-phase antirust film prepared from the gas-phase antirust master batch are obviously improved due to the synergistic effect of all antirust components in the gas-phase corrosion inhibitor.
2. Biodegradation test
Taking the samples in the embodiment 1 and the embodiment 2 as test samples, adopting a soil burying method, keeping the temperature at 25-30 ℃ during the test, taking the samples out of the soil at regular time, observing the degradation condition, calculating the weight loss rate of the samples, and testing the mechanical properties of the samples. After the soil is buried for 90 days, the surface of the sample is rough and has holes. The original mass of the polylactic acid-based gas phase rust prevention master batch (master batch 1#) and the polylactic acid-based gas phase rust prevention film (rust prevention film 1#) is 20.22g and 20.31g respectively.
The test results are shown in table 2:
TABLE 2
After 90 days of soil burying, the degradation rates of the polylactic acid-based gas-phase rust-proof master batch (master batch No. 1) and the polylactic acid-based gas-phase rust-proof film (rust-proof film No. 1) respectively reach 78.83% and 88.43%, and the degradation effect is excellent. The rust inhibitive degradation performance of examples 3-6 was comparable to that of examples 1 and 2.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. The biodegradable polylactic acid-based gas-phase antirust master batch is characterized by comprising the following raw materials, by weight, 45-55 parts of surface modified polylactic acid, 8-12 parts of polyethylene, 10-15 parts of 3, 5-dinitrobenzoic acid hexamethylene imine, 3-8 parts of benzotriazole or a derivative thereof, 3-8 parts of sodium molybdate, 1-5 parts of sodium nitrite, 1-5 parts of thiadiazole or a derivative thereof, 4-8 parts of a plasticizer and 4-8 parts of a reinforcing agent.
2. The biodegradable polylactic acid-based gas-phase antirust master batch according to claim 1, wherein the surface-modified polylactic acid is prepared from polylactic acid, a coupling agent and a lubricant in a mass ratio of 1:0.015-0.03: 0.015-0.03.
3. The biodegradable polylactic acid-based gas-phase antirust master batch according to claim 2, wherein the preparation method of the surface-modified polylactic acid comprises the following steps: and crushing the polylactic acid until the mesh number is less than 300 meshes, adding the coupling agent and the lubricant under stirring, and stirring and reacting for 15-30min to obtain the polylactic acid.
4. The biodegradable polylactic acid-based gas phase rust inhibitive masterbatch according to claim 2 or 3,
the coupling agent is selected from one or the combination of more than two of silane coupling agent, titanate coupling agent and aluminate coupling agent;
the lubricant is one or the combination of more than two of zinc stearate, calcium stearate and magnesium stearate.
5. The method for preparing the biodegradable polylactic acid-based gas-phase rust-proof masterbatch according to any one of claims 1 to 4, comprising the steps of:
(1) mixing the surface modified polylactic acid, 3,5 dinitrobenzoic acid hexamethylene imine, benzotriazole or derivatives thereof, sodium molybdate, sodium nitrite and thiadiazole or derivatives thereof, and uniformly stirring to obtain a mixed material 1;
(2) adding the plasticizer, the reinforcing agent and polyethylene into the mixed material 1, and uniformly stirring to obtain a mixed material 2;
(3) and blending and granulating the mixed material 2 to obtain the biodegradable polylactic acid-based gas-phase antirust master batch.
6. The method for preparing the biodegradable polylactic acid-based gas-phase antirust masterbatch according to claim 5, wherein the biodegradable polylactic acid-based gas-phase antirust masterbatch is prepared by the following steps: the stirring temperature in the step (2) was 80 ℃.
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| US5344589A (en) * | 1988-08-23 | 1994-09-06 | Cortec Corporation | Vapor phase corrosion inhibitor-desiccant material |
| CN105237969A (en) * | 2015-11-16 | 2016-01-13 | 重庆博浪塑胶股份有限公司 | Composite biodegradation gas-phase anti-rusting membrane and preparation process thereof |
| CN106380764A (en) * | 2016-08-31 | 2017-02-08 | 朱春英 | Functional biodegradable material and preparation method thereof |
| CN108997689A (en) * | 2018-08-24 | 2018-12-14 | 张万虎 | A kind of fully bio-degradable volatile rust preventive material and its application |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5344589A (en) * | 1988-08-23 | 1994-09-06 | Cortec Corporation | Vapor phase corrosion inhibitor-desiccant material |
| CN105237969A (en) * | 2015-11-16 | 2016-01-13 | 重庆博浪塑胶股份有限公司 | Composite biodegradation gas-phase anti-rusting membrane and preparation process thereof |
| CN106380764A (en) * | 2016-08-31 | 2017-02-08 | 朱春英 | Functional biodegradable material and preparation method thereof |
| CN108997689A (en) * | 2018-08-24 | 2018-12-14 | 张万虎 | A kind of fully bio-degradable volatile rust preventive material and its application |
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