CN113563730A - Ultrafine filler and fully-degradable composite material for vinasse protein purification residues, and preparation method and application thereof - Google Patents
Ultrafine filler and fully-degradable composite material for vinasse protein purification residues, and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to an ultramicro filler and a full-degradable composite material for vinasse protein purification residues, and a preparation method and application thereof, wherein the ultramicro filler is obtained by synchronously realizing surface modification in the ultramicro crushing process of the vinasse protein purification residues, the full-degradable composite material is obtained by taking the ultramicro filler as a raw material, adding dried biodegradable polyester, a plasticizer and a compatilizer for premixing after drying treatment, and extruding and granulating after carrying out melt blending composite modification on a premix, and the preparation and the application of the ultramicro filler and the full-degradable composite material are further provided. The fully-degradable composite material prepared by using the residue obtained after the purification of the vinasse protein as the matrix and matching with the biodegradable polyester and other additives has excellent processing performance and mechanical performance, can realize the recycling of all components of vinasse resources, has the advantage of cost compared with a plant fiber/biodegradable polyester fully-degradable packaging composite material, and has good industrial operability.
Description
Technical Field
The invention belongs to the technical field of forming and processing of full-biodegradable composite materials, and particularly relates to an ultrafine filler for purifying vinasse protein residues, a full-degradable composite material, and a preparation method and application thereof.
Background
Since birth, plastics have excellent performance and low cost, and are widely applied to aspects of production and life, however, the plastics generally need 200-700 years of degradation in natural environment, and the existence of a large amount of waste plastics causes 'white pollution', which threatens the health of wild animals and human beings to a great extent.
In order to solve the problem of white pollution, the fully biodegradable plastic and the product are produced at the same time. The fully biodegradable material (called fully degradable material for short) can be completely decomposed into low-molecular compounds (such as CO2 and H2O) by microorganisms (such as bacteria, fungi and algae) under proper and explicable natural environmental conditions or composting conditions, does not cause any secondary pollution to the ecological environment, is an ideal material for replacing disposable plastic products, and is an important way for solving the pollution of plastic wastes.
At present, the full-degradable products applied in a large scale on the market are basically realized based on polylactic acid (PLA), dibasic acid dihydric alcohol copolyester series (PBAT, PBS, PBSA and the like) and composite materials thereof, but the large-scale popularization and application of the full-degradable products are limited due to higher cost and production scale which cannot meet the market demand. Therefore, natural polymer materials based on agricultural and forestry wastes, such as protein, cellulose, lignin and the like, undoubtedly provide an effective solution for large-scale preparation, popularization and application of fully-degradable materials due to the characteristics of abundant resources, low price, no toxicity, nature and degradability. The fully-degradable bio-based material prepared from agricultural and forestry wastes not only can change waste into valuable, but also can reduce the consumption of petroleum-based resources, reduce environmental pollution and realize a real ecological closed loop.
Distillers' grains, which are the main by-products of the alcohol or brewing industry, are rich in a large amount of nutrients, such as proteins, crude fibers, fats, crude starch, minerals, enzymes, and various vitamins. Fermentation enterprises such as various wineries and alcohol production enterprises produce 1 ton of alcohol products and several tons of vinasse every year. At present, most enterprises or individuals can process the vinasse simply and roughly, and the vinasse is basically used as feed or fertilizer for direct sale after being simply dried and even directly buried. However, the abundant nutrients in the distiller's grains are not fully utilized, which not only causes serious waste of resources, but also causes environmental pollution. Therefore, how to realize high-value comprehensive utilization of the vinasse has profound significance for economic benefits of the wine making industry and sustainable development of environmental protection.
Disclosure of Invention
The invention aims to solve the problems and provides an ultrafine filler and a fully-degradable composite material for vinasse protein purification residues, and a preparation method and application thereof.
The invention realizes the purpose through the following technical scheme:
the ultrafine filler is obtained by synchronously realizing surface modification in the ultrafine grinding process of the distillers' grains protein purification residues.
As a further optimization scheme of the invention, the vinasse is beer vinasse, white spirit vinasse, red wine vinasse or yellow wine vinasse.
Use of an ultramicro filler as defined in any preceding claim in the preparation of a packaging material.
The fully-degradable composite material is prepared by taking any one of the ultramicro fillers as a raw material, drying, adding dried biodegradable polyester, a plasticizer and a compatilizer for premixing, performing melt blending composite modification on the premix, and extruding and granulating.
As a further optimized scheme of the invention, the premix comprises the following components in parts by weight: 50-80 parts of the ultrafine filler, 40-20 parts of biodegradable polyester, 5-10 parts of an environment-friendly plasticizer and 3-5 parts of a compatilizer.
Use of a fully degradable composite material as described in any one of the above in the preparation of a packaging material.
A preparation method of the ultramicro filler or the fully-degradable composite material mainly comprises the following steps:
(1) carrying out ultramicro crushing and surface modification treatment on the distilled grain protein purification residues to obtain modified micro-nano distilled grain protein purification residue powder, namely the ultramicro filler;
(2) drying the ultramicro filler obtained in the step (1) and biodegradable polyester at the temperature of 60-80 ℃, and blending the dried wine ultramicro filler and biodegradable polyester with a plasticizer and a compatilizer to obtain a premix;
(3) placing the premix obtained in the step (2) into a double-screw extruder, carrying out melt blending composite modification extrusion bracing under the processing condition of 140-180 ℃, cooling and dicing to obtain fully-degradable composite master batches of the distillers' grain protein purification residue powder, namely the fully-degradable composite material;
(4) and (4) performing injection molding on the fully-degradable composite material obtained in the step (3) to obtain a fully-degradable alcohol-dispelling denture packaging or a fully-degradable lunch box or tableware.
As a further optimization scheme of the invention, in the step (1), the grain size of the distillers' grains protein purification residue after the ultramicro pulverization treatment is 400-3000 meshes.
As a further optimization scheme of the invention, in the step (1), the distillers' grains protein purification residues are modified by adopting a silane coupling agent, a titanate coupling agent, an aluminate coupling agent or an isocyanate coupling agent.
As a further optimization scheme of the invention, in the step (2), the biodegradable polyester is polylactic acid (PLA), Polycaprolactone (PCL), polybutylene succinate (PBS) or a compound biodegradable polyester thereof; the plasticizer is glycerol, sorbitol or polyethylene glycol (PEG); the compatilizer is maleic anhydride grafted polylactic acid (MA-g-PLA) or glycidyl methacrylate grafted polylactic acid (GMA-g-PLA).
The invention has the beneficial effects that:
(1) the method is different from the prior method for directly filling and utilizing the vinasse, the residue of the vinasse after protein purification is utilized, the purified high-value-added protein can be used for preparing a fully-degradable film packaging material, and the purified residue is subjected to protein extraction treatment, so that the structure is looser compared with the original vinasse, the method is more favorable for next-step superfine grinding and surface modification treatment, the energy consumption in the superfine grinding process of the residue can be reduced to a certain extent, the preparation cost is reduced, the treated residue superfine filler can be used for preparing a fully-degradable hard composite packaging material, the full utilization of all components of the vinasse is realized, the existing high-quality wood and bamboo fibers are replaced, waste is changed into valuable, an industrial demonstration is formed, and the method has profound significance on high-value utilization of agricultural and forestry waste and sustainable development of environmental protection;
(2) according to the invention, an ultramicro crushing technology is adopted, so that the preparation of the micro-nano vinasse protein purification residue particles is realized, the specific surface area of the residue particles is greatly improved, the reaction accessibility of surface modification is greatly promoted, the uniform dispersion of the vinasse protein purification residue particles in biodegradable polyester is favorably realized, and the preparation of a high-performance and high-filling full-degradation composite packaging material can be realized;
(3) according to the invention, the coupling modifier is used for modifying the distillers 'grains protein purification residue powder and the like, so that the interface compatibility between distillers' grains protein purification residue particles and the biodegradable polyester is effectively improved, the interaction between distillers 'grains protein purification residue fiber particles can be weakened, the energy consumption in the ultramicro crushing process is reduced, and the high-performance and low-cost preparation of the distillers' grains protein purification residue/biodegradable polyester full-degradable composite material is realized;
(4) according to the invention, one-step method is adopted to realize ultramicro crushing micro-nano and modification treatment of the distillers 'grains protein purification residues, the ultramicro crushing and surface modification treatment are organically combined, the surface modification is utilized to reduce the interaction between the distillers' grains protein purification residues, the energy consumption in the ultramicro crushing process is reduced, meanwhile, the heat generated in the ultramicro crushing process and the specific surface are improved, the modification reaction is promoted, the interface compatibility between the distillers 'grains protein purification residues and the biodegradable polyester is effectively improved, the filling amount of the distillers' grains protein purification residues is greatly improved while good strength performance is maintained, and the preparation cost of the full-biodegradable composite packaging material is effectively reduced;
(5) according to the invention, by introducing compatilizers such as maleic anhydride grafted polylactic acid or glycidyl methacrylate grafted polylactic acid, the interface compatibility of the micro-nano vinasse protein purification residue and the biodegradable polyester is further improved, and the performance of the composite material is effectively improved;
(6) the ultrafine filler for the vinasse protein purification residues and the fully-degradable composite material thereof have excellent strength performance, price competitiveness and process operability, and can be applied to the fields of wine bottle inner holders, fully-degradable lunch boxes, tableware and the like.
Drawings
FIG. 1 is a flow chart of the preparation process of the lees protein purification residue/biodegradable polyester composite packaging material;
FIG. 2 is a particle size and particle size distribution diagram of KH550 modified distillers' grains protein purification residue powder after micronization.
Detailed Description
The present application will now be described in further detail with reference to the drawings, it should be noted that the following detailed description is given for illustrative purposes only and is not to be construed as limiting the scope of the present application, as those skilled in the art will be able to make numerous insubstantial modifications and adaptations to the present application based on the above disclosure.
A preparation method of an ultrafine filler or a fully-degradable composite material for vinasse protein purification residues comprises the following steps:
(1) preparation of the modified solution: preparing different coupling modifier solutions or emulsions according to the use modes of different coupling modifiers, firstly weighing a certain mass of coupling modifier, uniformly spreading the coupling modifier on the surface of the vinasse protein purification residue subjected to primary screening and drying treatment, wherein the use amount of the coupling modifier is 1-5% wt of the absolute dry mass of the vinasse protein purification residue, then placing the coupling modifier in a high-speed mixer, and mixing for 15min at a high speed at the revolution of 2000r/min to complete uniform dispersion of the coupling modifier in the vinasse protein purification residue to obtain a uniformly dispersed mixture;
(2) ultramicro crushing and modification treatment: and (2) feeding the mixture of the vinasse protein purification residue and the coupling modifier which are uniformly mixed at a high speed into a mechanical kinetic energy mill for ultramicro crushing treatment, realizing coupling modification of the vinasse protein purification residue by using heat generated in the ultramicro crushing process, and then obtaining modified micro-nano vinasse protein purification residue powder with a target size in a separation and classification mode, namely the ultramicro filler.
(3) Placing the modified micro-nano vinasse protein purification residue powder and biodegradable polyester at 60-80 ℃ for drying treatment to obtain dry modified micro-nano vinasse protein purification residue powder and biodegradable polyester, then weighing a certain mass of micro-nano vinasse protein purification residue powder, biodegradable polyester, a plasticizer, a compatilizer and the like, placing the powder, the biodegradable polyester, the plasticizer, the compatilizer and the like in a high-speed mixer, and uniformly mixing for 10min at the rotating speed of 1000r/min to obtain a premix, wherein the formula and the ratio of the premix are as follows: 50-80 parts of modified micro-nano vinasse protein purification residue powder (ultramicro filler), 50-20 parts of biodegradable polyester, 5-10 parts of plasticizer and 3-5 parts of compatilizer by mass;
(4) transferring the premix prepared in the step (3) into a double-screw extruder, setting the processing temperature between 140 and 180 ℃, setting the rotating speed of a main machine screw to be 100r/min and the feeding speed to be 30r/min, and preparing the vinasse protein purification residue/biodegradable polyester composite master batch after double-screw extrusion, bracing, cooling and grain cutting, namely the vinasse protein purification residue fully-degradable composite material;
(5) performing injection molding on the vinasse protein purification residue fully-degradable composite material prepared in the step (4) in an injection molding machine charging barrel temperature of 170-190 ℃, under an injection pressure of 40-60MPa and under a pressure maintaining time of 2-15s to obtain a vinasse protein purification residue/biodegradable polyester fully-degradable composite material product;
example 1
The embodiment provides a preparation method of an ultrafine filler or a fully-degradable composite material for vinasse protein purification residues, which mainly comprises the following steps:
(1) placing 20 parts of silane coupling agent KH550, 72 parts of absolute ethyl alcohol and 8 parts of water in a magnetic stirrer, adjusting the pH value to 4-5 by using glacial acetic acid, fully stirring and mixing to complete full alcoholysis of the silane coupling KH550, thereby realizing preparation of a KH550 modifier solution.
(2) Weighing a certain mass of KH550 modifier solution, uniformly spraying the solution on the surface of the vinasse protein purification residue after primary screening and drying treatment, wherein the dosage of the coupling modifier is 2% wt of the oven-dried mass of the vinasse protein purification residue, then placing the vinasse protein purification residue in a high-speed mixer, and mixing for 15min at a high speed under the revolution of 2000r/min to complete uniform dispersion of the coupling agent in the vinasse protein purification residue, thereby obtaining a uniformly dispersed mixture.
(3) And (3) feeding the mixture of the distillers 'grain protein purification residue and the coupling modifier which are uniformly mixed at a high speed into a mechanical kinetic energy mill for superfine grinding to obtain modified micro-nano distillers' grain protein residue powder with the size of about 600 meshes, namely the distillers 'grain protein purification residue superfine filler, wherein the particle size distribution of the modified micro-nano distillers' grain protein purification residue superfine filler is shown in figure 2.
(4) Placing the vinasse protein purification residue ultramicro filler and biodegradable polyester-polylactic acid (PLA) at 60 ℃ for drying treatment to obtain dry modified micro-nano vinasse protein purification residue powder (ultramicro filler) and biodegradable polyester-polylactic acid (PLA), adding a plasticizer and a compatilizer, placing the mixture in a high-speed mixer, uniformly mixing at the rotating speed of 1000r/min for 10min to obtain a premix, wherein the premix comprises 50 parts of the vinasse protein purification residue ultramicro filler, 40 parts of polylactic acid resin, 10 parts of glycerol and 3 parts of maleic anhydride grafted polylactic acid (MA-g-PLA) in parts by mass.
(5) The prepared uniformly mixed material is moved into a double-screw extruder, the temperature of each zone of each heating section is set to be 150 ℃, 160 ℃, 170 ℃, 180 ℃, 185 ℃, 180 ℃ and 180 ℃ in sequence, the head temperature is 180 ℃, the rotating speed of a main machine screw is 80r/min, the feeding speed is 30r/min, after double-screw extrusion, bracing, cooling and grain cutting, the vinasse protein purification residue/biodegradable polyester composite master batch is obtained, namely the fully degradable composite material is obtained, and then the fully degradable composite material is processed into a standard test sample strip through injection molding to carry out strength performance test.
Example 2
The difference from the embodiment 1 is that the premix comprises 50 parts of micro-nano KH550 vinasse protein purification residue ultramicro filler, 40 parts of polylactic acid resin, 10 parts of sorbitol and 3 parts of maleic anhydride grafted polylactic acid (MA-g-PLA) according to the mass parts.
Example 3
The difference from the embodiment 1 is that the premix comprises 50 parts of micro-nano KH550 vinasse protein purification residue ultramicro filler, 40 parts of polylactic acid resin, 10 parts of glycerol and 3 parts of glycidyl methacrylate grafted polylactic acid (GMA-g-PLA) according to the mass parts.
Example 4
The difference from the embodiment 1 is that the premix comprises 60 parts of micro-nano KH550 vinasse protein purification residue ultramicro filler, 30 parts of polylactic acid resin, 10 parts of glycerol and 3 parts of maleic anhydride grafted polylactic acid (MA-g-PLA) according to the mass parts.
Example 5
The difference from the embodiment 1 is that the vinasse protein purification residue ultrafine filler is aluminate coupling agent UP801 modified vinasse protein purification ultrafine grinding residue powder.
Example 6
The difference from the embodiment 3 is that the grain diameter of the micro-nano vinasse protein purification residue powder after the ultra-micro grinding treatment is 1000 meshes.
Example 7
The difference from example 6 is that the residue after purification of the distillers' grains protein was not subjected to surface modification with a coupling modifier and was subjected to micronization.
In order to verify the beneficial effects of the product of the present invention, the strength performance test was performed in sequence by using standard test sample bars and commercially available general fully degradable composite materials as blank control groups according to the preparation methods described in the above examples 1 to 7, and the results are shown in table 1:
according to experimental results, in examples 1-7, the tensile strength, the elongation at break, the bending strength and the impact strength of the fully-degradable composite material prepared by the preparation method in example 6 are superior to those of other examples, the particle size of the micro-nano vinasse protein purification residue powder subjected to surface modification and superfine grinding is 1000 meshes, the specific surface area of the residue particle is greatly increased, the reaction accessibility of subsequent surface modification is greatly promoted, the uniform dispersion of the vinasse protein purification residue particle in the biodegradable polyester is favorably realized, in addition, the interface compatibility of the micro-nano vinasse protein purification residue and the biodegradable polyester is further improved through the introduction of compatilizers such as glycidyl methacrylate grafted polylactic acid and the like, and the performance of the composite material is effectively improved;
in addition, in the embodiment 6, the ultramicro pulverization and the surface modification treatment are organically combined, the interaction between the distillers ' grain protein purification residues is reduced by utilizing the surface modification, the energy consumption in the ultramicro pulverization process is reduced, meanwhile, the heat generated in the ultramicro pulverization process and the improvement of the specific surface promote the modification reaction, the interface compatibility between the distillers ' grain protein purification residues and the biodegradable polyester is effectively improved, the filling amount of the distillers ' grain protein purification residues is greatly increased while the good strength performance is kept, and the preparation cost of the full-biodegradable composite packaging material is effectively reduced.
As used in the specification and claims, certain terms are used to refer to particular components or methods. As one skilled in the art will appreciate, different regions may refer to a component by different names. The present specification and claims do not intend to distinguish between components that differ in name but not in name. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, and a person skilled in the art can solve the technical problem within a certain error range to substantially achieve the technical effect. The description which follows is a preferred embodiment of the present application, but is made for the purpose of illustrating the general principles of the application and not for the purpose of limiting the scope of the application. The protection scope of the present application shall be subject to the definitions of the appended claims.
It is also noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a good or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such good or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a commodity or system that includes the element.
While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (12)
1. The ultrafine filler for the vinasse protein purification residues is characterized by being obtained by synchronously realizing surface modification in the ultrafine grinding process of the vinasse protein purification residues.
2. The ultrafine filler for the purification residue of distillers 'grains protein according to claim 1, wherein the distillers' grains are beer distillers 'grains, white spirit distillers' grains, red wine distillers 'grains, or yellow wine distillers' grains.
3. Use of an ultramicro filler according to any of claims 1-2 for the preparation of packaging material.
4. The fully-degradable composite material of the vinasse protein purification residues is characterized in that the fully-degradable composite material is obtained by taking the ultramicro filler of any one of claims 1-2 as a raw material, drying, adding dried biodegradable polyester, a plasticizer and a compatilizer for premixing, performing melt blending composite modification on the premix, and then extruding and granulating.
5. The fully-degradable composite material for the distillers' grains protein purification residue as claimed in claim 4, wherein the premix comprises the following components in parts by weight: 50-80 parts of the ultramicro filler of any one of claims 1-2, 40-20 parts of biodegradable polyester, 5-10 parts of environment-friendly plasticizer and 3-5 parts of compatilizer.
6. Use of a fully degradable composite material according to any of claims 4 to 5 for the preparation of a packaging material, wherein said packaging material is a wine bottle, a wine bottle inner holder, a fully degradable meal box or tableware.
7. A method for preparing the ultramicro-filler or fully-degradable composite material as claimed in claim 1 or 4, characterized by mainly comprising the following steps:
(1) carrying out ultramicro crushing and surface modification treatment on the distilled grain protein purification residues to obtain modified micro-nano distilled grain protein purification residue powder, namely the ultramicro filler;
(2) drying the ultramicro filler obtained in the step (1) and biodegradable polyester at the temperature of 60-80 ℃, and blending the dried wine ultramicro filler and biodegradable polyester with a plasticizer and a compatilizer to obtain a premix;
(3) placing the premix obtained in the step (2) into a double-screw extruder, carrying out melt blending composite modification extrusion bracing under the processing condition of 140-180 ℃, cooling and dicing to obtain fully-degradable composite master batches of the distillers' grain protein purification residue powder, namely the fully-degradable composite material;
(4) and (4) performing injection molding on the fully-degradable composite material obtained in the step (3) to obtain a fully-degradable alcohol-dispelling denture packaging or a fully-degradable lunch box or tableware.
8. The preparation method of the ultramicro-filler or fully-degradable composite material as claimed in claim 7, characterized in that: in the step (1), the grain size of the distillers' grains protein purification residue after the ultramicro crushing treatment is 400-3000 meshes.
9. The preparation method of the ultramicro-filler or fully-degradable composite material as claimed in claim 7, characterized in that: in the step (1), the residue after the purification of the distillers' grains protein is modified by adopting a silane coupling agent, a titanate coupling agent, an aluminate coupling agent or an isocyanate coupling agent.
10. The preparation method of the ultramicro-filler or fully-degradable composite material as claimed in claim 7, characterized in that: in the step (2), the biodegradable polyester is polylactic acid (PLA), Polycaprolactone (PCL), polybutylene succinate (PBS) or compound biodegradable polyester thereof.
11. The preparation method of the ultramicro-filler or fully-degradable composite material as claimed in claim 7, characterized in that: in the step (2), the plasticizer is glycerol, sorbitol or polyethylene glycol (PEG).
12. The preparation method of the ultramicro-filler or fully-degradable composite material as claimed in claim 7, characterized in that: in the step (2), the compatilizer is maleic anhydride grafted polylactic acid (MA-g-PLA) or glycidyl methacrylate grafted polylactic acid (GMA-g-PLA).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114806109A (en) * | 2022-05-31 | 2022-07-29 | 江林（贵州）高科发展股份有限公司 | Biodegradable material, application thereof, fully-degradable vinasse composite material and biodegradable mulching film |
| CN114806109B (en) * | 2022-05-31 | 2022-12-27 | 江林（贵州）高科发展股份有限公司 | Biodegradable material, application thereof, fully-degradable vinasse composite material and biodegradable mulching film |
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