CN113583438B - Biodegradable alkali lignin composite material, preparation method and application thereof - Google Patents
Biodegradable alkali lignin composite material, preparation method and application thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/04—Polyamides derived from alpha-amino carboxylic acids
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/04—Polyamides derived from alpha-amino carboxylic acids
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- C08J2497/00—Characterised by the use of lignin-containing materials
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
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Abstract
The invention discloses a biodegradable alkali lignin composite material, which comprises the following raw materials in parts by weight: 10-60 parts of alkali lignin, 20-80 parts of polyglutamic acid, 10-30 parts of montmorillonite, 20-40 parts of silane coupling agent, 30-200 parts of glycerol and 200-400 parts of solvent. The invention also discloses a preparation method of the biodegradable alkali lignin composite material and application of the biodegradable alkali lignin composite material in films, sheets or plates. The biodegradable alkali lignin composite material can fully utilize the biodegradable alkali lignin composite material of the papermaking byproduct alkali lignin, and simultaneously improve the performance of the raw material polyglutamic acid, so that the alkali lignin composite material has good barrier performance, tensile strength and low water absorption rate, thereby expanding the application range of the alkali lignin composite material.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a biodegradable alkali lignin composite material, a preparation method and application thereof.
Background
With the rapid development of economy and society, the wide use of polymer materials, especially plastic films, sheets and plates, brings great convenience to the life of people, most of plastic products are extracted from petroleum, the plastic products are difficult to degrade, the degradation time is hundreds of years, and the environment is polluted to a great extent, so that the plastic products are familiar with white pollution. After the new edition of "plastic forbidden" comes out of the platform in 1 month in 2020, the policy of "plastic forbidden" in each place is obviously accelerated. According to the content of the policies in the center and places, the plastic forbidden policy is about to be spread nationwide within the future 2-5 years. However, most enterprises focus on material synthesis, and the domestic strength of the research on improving the performance of the degradable plastic products is still weak.
Lignin is a renewable and degradable natural polymer substance and has the advantages of high impact strength, good heat resistance, water resistance, low cost, easy obtainment and the like. The lignin and the derivative structure thereof contain a large number of oxygen-containing active functional groups, but due to pi-pi action among aromatic rings, carboxyl and hydroxyl in the structure and hydrogen bond action among various ether bonds, the lignin is seriously aggregated, and hydrophobic chains are easy to wrap the active functional groups to form aggregates, so that the specific surface area is small; the pyrolysis temperature is between 100 and 180 ℃, and the heat resistance is good. As a byproduct of the pulping and papermaking industry, a large amount of alkali lignin produced each year is to be utilized. AL is chemically pulped by caustic soda or sulfate, is hydrophobic but soluble in alkaline media, has a lower sulfur content and higher reactivity. The lignin and the derivatives thereof can be blended with other materials to prepare the composite material with excellent performance, and the pollution of papermaking waste liquid to the environment can be reduced. Chirico et al blend lignin with polypropylene (PP) and compare with blending systems with added flame retardants such as melamine and monoammonium phosphate, demonstrating that the addition of lignin improves PP thermal stability and reduces heat release rate.
Polyglutamic acid (gamma-PGA) is a biodegradable amino acid polymer, and the synthesis method of gamma-PGA mainly comprises a chemical synthesis method, an extraction method and a microbial fermentation method, wherein the gamma-PGA is prepared by utilizing microbial fermentation, has the characteristics of easily available raw materials, recycling and meeting sustainable development, and has good economic value and application prospect. Currently, gamma-polyglutamic acid has been found to be a polyamino acid that can be used in packaging materials. The gamma-PGA has the advantages of good film forming property, plasticity, cohesiveness, biodegradability and the like, and is a polymer compound which is harmless to human bodies and the environment. However, γ -PGA has a strong water absorption property, and the barrier property of γ -PGA is not satisfactory when used for food packaging materials.
Therefore, in order to fully utilize byproducts of the paper industry and improve the performance of gamma-PGA in food packaging, processing technology, functional materials and the like, studies on blending of alkali lignin and polyglutamic acid have been conducted.
Disclosure of Invention
Therefore, the invention aims to provide the biodegradable alkali lignin composite material capable of fully utilizing the alkali lignin of the papermaking byproduct, and simultaneously improving the performance of the raw material polyglutamic acid, so that the alkali lignin composite material has good barrier property, tensile strength and low water absorption rate, and the application range of the alkali lignin composite material is widened.
The technical scheme of the invention is realized as follows:
a biodegradable alkali lignin composite material, comprising the following raw materials: alkali lignin, polyglutamic acid, montmorillonite and a silane coupling agent.
According to a further technical scheme, the raw material further comprises glycerin.
According to a further technical scheme, the raw materials further comprise a solvent dimethyl sulfoxide or N-methyl-2-pyrrolidone.
The further technical scheme is that the raw materials comprise, by weight, 10-60 parts of alkali lignin, 20-80 parts of polyglutamic acid, 10-30 parts of montmorillonite, 20-40 parts of a silane coupling agent, 30-200 parts of glycerol and 200-400 parts of a solvent.
The further technical scheme is that the raw materials comprise, by weight, 30 parts of alkali lignin, 50 parts of polyglutamic acid, 20 parts of montmorillonite, 30 parts of a silane coupling agent, 100 parts of glycerol and 150 parts of a solvent.
The preparation method of the biodegradable alkali lignin composite material comprises the following steps:
(1) Adding alkali lignin powder into glycerol, and stirring to prepare alkali lignin suspension;
(2) Dissolving polyglutamic acid in a solvent, and stirring to prepare a polyglutamic acid solution;
(3) Adding montmorillonite into the polyglutamic acid solution in the step (2), mixing, adding alkali lignin suspension and a silane coupling agent, and blending to prepare the alkali lignin composite material.
The further technical proposal is that the blending time is 12-48h, and the blending temperature is 70-85 ℃.
The application of the alkali lignin composite material is that the alkali lignin composite material is applied to films, sheets or plates.
The further technical scheme is that the alkali lignin composite material is prepared into a film, a sheet or a plate by a film blowing method, a casting method, a solution pouring method, a spin coating method, a calendaring method, a multilayer coextrusion method, a biaxial stretching method or a lamination method.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the method, the blocking performance of the alkali lignin composite material is improved by adding montmorillonite, the montmorillonite is a silicate with a 2:1 three-layer structure, the thickness of each lamellar layer and the original distance between lamellar layers are about 1nm, in addition, the two-dimensional dimensions are about 100nm, and the montmorillonite is filled into the alkali lignin composite material to improve the blocking capability to water vapor, so that the mechanism of the montmorillonite is similar to that of a blocking sheet formed by blocking resin in lamellar blending; in addition, the addition of alkali lignin further improves the barrier property of the alkali lignin composite material.
(2) The silane coupling agent improves the bonding strength of alkali lignin and polyglutamic acid, promotes the compatibility of the alkali lignin and the polyglutamic acid, and finally improves the tensile strength of the alkali lignin composite material.
(3) According to the method, the water absorption performance of the original polyglutamic acid is reduced by combining the alkali lignin and the polyglutamic acid, and the water absorption rate is about 15%.
(4) The glycerol is used as a solvent of the alkali lignin, so that the alkali lignin is dissolved in the glycerol, and meanwhile, the compatibility and permeability of the alkali lignin and polyglutamic acid are enhanced.
(5) The alkali lignin composite material adopts biodegradable alkali lignin and polyglutamic acid as main raw materials, but the biodegradation rate of polyglutamic acid is too high, and the addition of the alkali lignin slows down the biodegradation rate of the alkali lignin composite material, so that the application range of the alkali lignin composite material is widened; meanwhile, the alkali lignin composite material has the characteristics of easily available raw materials, recycling and meeting sustainable development.
Detailed Description
For a clear and complete description of the technical solutions of the present invention, it is apparent that the inventors have described in connection with the embodiments, but that the following embodiments describe only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A biodegradable alkali lignin composite material comprises the following raw materials in parts by weight: 30 parts of alkali lignin, 50 parts of polyglutamic acid, 20 parts of montmorillonite, 30 parts of silane coupling agent, 100 parts of glycerol and 150 parts of dimethyl sulfoxide.
The preparation method of the biodegradable alkali lignin composite material comprises the following steps:
(1) Adding alkali lignin powder into glycerol, and stirring to prepare alkali lignin suspension;
(2) Dissolving polyglutamic acid in a solvent, and stirring to prepare a polyglutamic acid solution;
(3) Adding montmorillonite into the polyglutamic acid solution in the step (2), mixing, adding alkali lignin suspension and a silane coupling agent, and blending to prepare the alkali lignin composite material. The blending time is 12 hours, and the blending temperature is 85 ℃.
The alkali lignin composite material is subjected to film blowing method to prepare a film.
Example 2
A biodegradable alkali lignin composite material comprises the following raw materials in parts by weight: 10 parts of alkali lignin, 20 parts of polyglutamic acid, 10 parts of montmorillonite, 20 parts of silane coupling agent, 30 parts of glycerol and 200 parts of N-methyl-2-pyrrolidone.
The preparation method of the biodegradable alkali lignin composite material comprises the following steps:
(1) Adding alkali lignin powder into glycerol, and stirring to prepare alkali lignin suspension;
(2) Dissolving polyglutamic acid in a solvent, and stirring to prepare a polyglutamic acid solution;
(3) Adding montmorillonite into the polyglutamic acid solution in the step (2), mixing, adding alkali lignin suspension and a silane coupling agent, and blending to prepare the alkali lignin composite material.
The further technical scheme is that the blending time is 48 hours, and the blending temperature is 70 ℃.
The alkali lignin composite material is made into a sheet material by a film blowing calendaring method.
Example 3
A biodegradable alkali lignin composite material comprises the following raw materials in parts by weight: 60 parts of alkali lignin, 80 parts of polyglutamic acid, 30 parts of montmorillonite, 40 parts of silane coupling agent, 200 parts of glycerol and 400 parts of dimethyl sulfoxide.
The preparation method of the biodegradable alkali lignin composite material comprises the following steps:
(1) Adding alkali lignin powder into glycerol, and stirring to prepare alkali lignin suspension;
(2) Dissolving polyglutamic acid in a solvent, and stirring to prepare a polyglutamic acid solution;
(3) Adding montmorillonite into the polyglutamic acid solution in the step (2), mixing, adding alkali lignin suspension and a silane coupling agent, and blending to prepare the alkali lignin composite material. The blending time is 24 hours, and the blending temperature is 80 ℃.
The alkali lignin composite material is prepared into a plate by a lamination method.
Comparative example 1
A biodegradable polyglutamic acid material comprises the following raw materials in parts by weight: 50 parts of polyglutamic acid, 20 parts of montmorillonite, 30 parts of silane coupling agent, 100 parts of glycerol and 150 parts of dimethyl sulfoxide.
The preparation method of the biodegradable polyglutamic acid material comprises the following steps: dissolving polyglutamic acid in dimethyl sulfoxide, and stirring to prepare polyglutamic acid solution; adding montmorillonite into the polyglutamic acid solution, mixing, adding glycerol and a silane coupling agent, and blending to prepare the polyglutamic acid material. The blending time is 12 hours, and the blending temperature is 85 ℃.
The alkali lignin composite material is subjected to film blowing method to prepare a film.
Comparative example 2
A biodegradable polyglutamic acid material comprises the following raw materials in parts by weight: 50 parts of polyglutamic acid, 20 parts of montmorillonite and 150 parts of dimethyl sulfoxide.
Comparative example 3
A biodegradable polyglutamic acid material comprises the following raw materials in parts by weight: 50 parts of polyglutamic acid and 150 parts of dimethyl sulfoxide.
The preparation method of the biodegradable polyglutamic acid material comprises the following steps: dissolving polyglutamic acid in dimethyl sulfoxide, and stirring to prepare polyglutamic acid solution; adding montmorillonite into the polyglutamic acid solution, mixing, and blending to obtain the polyglutamic acid material. The blending time is 12 hours, and the blending temperature is 85 ℃.
The alkali lignin composite material is subjected to film blowing method to prepare a film.
Comparative example 4
The raw material weight ratio of the biodegradable alkali lignin composite material is the same as that of the example 1. The preparation method of the biodegradable alkali lignin composite material comprises the following steps:
(1) Adding alkali lignin powder into glycerol, and stirring to prepare alkali lignin suspension;
(2) Dissolving polyglutamic acid in a solvent, and stirring to prepare a polyglutamic acid solution;
(3) And simultaneously adding montmorillonite, alkali lignin suspension and a silane coupling agent into the polyglutamic acid solution, stirring, and blending to prepare the alkali lignin composite material. The blending time is 12 hours, and the blending temperature is 85 ℃.
The alkali lignin composite material is subjected to film blowing method to prepare a film.
Performance testing
The alkali lignin composite materials described in examples 1-3 and the polyglutamic acid materials described in comparative examples 1-2 were subjected to performance tests (see Table 1), tensile performance tests were performed according to B/T1040-1992, the sample size was 320 x 150 x 3mm, and the tensile speed was 100mm/min; the water vapor permeation test was carried out according to GB/T1037-1988 at a temperature of 23℃and a humidity of 90%; the biodegradation rate testing method comprises the following steps: the film sample was dried to constant weight and then weighed m 0 Placing the film sample in Hainan outdoor red soil, taking out the film sample after 15 days, drying the film sample to constant weight, and weighing the film sample m 1 Degradation rate= (m 0 -m 1 )/m 0 100%; the water absorption test was carried out according to GB1034-2008, the sample thickness was 1mm by machining on one side of the machine and the sample was taken in water at 23 DEG CThe water absorption was tested.
TABLE 1
As can be seen from Table 1, the tensile strength of the alkali lignin composites described in examples 1-3 is significantly higher than that of comparative examples 1-3, indicating that the mechanical properties of the alkali lignin composites are better than those of polyglutamic acid materials. The alkali lignin composite material described in examples 1-3 has a lower water vapor transmission rate than comparative examples 1-3, indicating that the addition of alkali lignin further improves the barrier properties of the alkali lignin composite material, and the comparative examples 1-2 have a lower water vapor transmission rate than comparative example 3, indicating that montmorillonite can improve the barrier properties of polyglutamic acid. The water vapor transmission rate of example 1 is lower than that of comparative example 4, which shows that the water vapor transmission rate of the alkali lignin composite material prepared by adding montmorillonite, alkali lignin suspension and silane coupling agent simultaneously into polyglutamic acid solution is lower and the barrier property is better than that of the alkali lignin composite material prepared by adding montmorillonite, alkali lignin suspension and silane coupling agent into polyglutamic acid solution. The biodegradation rate and the water absorption rate of examples 1-3 are lower than those of comparative examples 1-3, which shows that the addition of alkali lignin slows down the biodegradation performance of the material and reduces the water absorption performance of the material, thereby expanding the application range of polyglutamic acid.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (8)
1. A biodegradable alkali lignin composite material, characterized in that: the preparation method comprises the following raw materials: alkali lignin, polyglutamic acid, montmorillonite and a silane coupling agent;
the preparation method of the biodegradable alkali lignin composite material comprises the following steps:
(1) Adding alkali lignin powder into glycerol, and stirring to prepare alkali lignin suspension;
(2) Dissolving polyglutamic acid in a solvent, and stirring to prepare a polyglutamic acid solution;
(3) Adding montmorillonite into the polyglutamic acid solution in the step (2), mixing, adding alkali lignin suspension and a silane coupling agent, and blending to prepare the alkali lignin composite material.
2. A biodegradable alkali lignin composite according to claim 1 wherein: the solvent comprises dimethyl sulfoxide or N-methyl-2-pyrrolidone.
3. A biodegradable alkali lignin composite according to claim 1 wherein: the silane coupling agent is one of alkyl triethoxy, methyl trimethoxy, triacetoxy and propyl triacetoxy silane.
4. A biodegradable alkali lignin composite according to claim 1 wherein: the raw materials comprise, by weight, 10-60 parts of alkali lignin, 20-80 parts of polyglutamic acid, 10-30 parts of montmorillonite, 20-40 parts of a silane coupling agent, 30-200 parts of glycerol and 200-400 parts of a solvent.
5. A biodegradable alkali lignin composite according to claim 1 wherein: the raw materials comprise, by weight, 30 parts of alkali lignin, 50 parts of polyglutamic acid, 20 parts of montmorillonite, 30 parts of a silane coupling agent, 100 parts of glycerol and 150 parts of a solvent.
6. A biodegradable alkali lignin composite according to claim 1 wherein: the blending time is 12-48h, and the blending temperature is 70-85 ℃.
7. Use of an alkali lignin composite according to any one of claims 1 to 6 wherein: the application of the alkali lignin composite material in films, sheets or plates.
8. The use of an alkali lignin composite according to claim 7 wherein: the alkali lignin composite material is prepared into a film, a sheet or a plate by a blowing method, a casting method, a solution casting method, a spin coating method, a calendaring method, a multilayer coextrusion method, a biaxial stretching method or a lamination method.
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| CN103396674A (en) * | 2013-08-08 | 2013-11-20 | 东北林业大学 | Preparation method of alkali lignin/corn starch/flax fiber thermoplastic composite material |
| AU2020101037A4 (en) * | 2019-06-24 | 2020-07-23 | Qilu University Of Technology | Preparation method of lignin-chitosan based fluoride-free high-strength super-hydrophobic paper |
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| AU2020101037A4 (en) * | 2019-06-24 | 2020-07-23 | Qilu University Of Technology | Preparation method of lignin-chitosan based fluoride-free high-strength super-hydrophobic paper |
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