CN110734631A - lignin-based biodegradable polybutylene succinate film and preparation method thereof - Google Patents
lignin-based biodegradable polybutylene succinate film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses lignin-based biodegradable polybutylene succinate films and a preparation method thereof, wherein the preparation process comprises surface treatment, filling master batch preparation, material preparation and blow molding, the film products have high degradation speed, high flexibility, low recovery cost and no pollution to the environment, the requirements of express delivery industry on degradable packaging films in rapid development can be met, the difficult trouble that the express delivery packaging films are difficult to degrade, recover and pollute is thoroughly solved, the requirement of combining sustainable development with scientific development is met, huge economic benefits are brought to enterprises while the ecological environment is protected, and the competitiveness of the enterprises is improved.
Description
Technical Field
The invention relates to the technical field of biodegradable films, in particular to lignin-based biodegradable polybutylene succinate films and a preparation method thereof.
Background
Since the 21 st century, along with the rapid development of electronic commerce in China, the express industry is also rapidly developed. The rapid development of the express delivery industry brings great convenience to the life of people, but the recycling problem of the express delivery packaging bag brings challenges to the environment.
At present, the recovery rate of film bags for express packaging in China is less than 20%, transparent adhesive tapes, foam films, plastic bags and the like for express packaging are mainly made of PVC-based high-molecular polymers, the packaging materials are difficult to recycle, the direct burying degradation speed is low, the natural degradation needs hundred years, if the packaging materials are subjected to incineration treatment, a large number of toxic and harmful substances are generated, and the environment is polluted.
Disclosure of Invention
The invention aims to solve the problems, provides lignin-based biodegradable poly (butylene succinate) films and a preparation method thereof, and the films have the advantages of high degradation speed, high flexibility, low recovery cost and no environmental pollution, can meet the large demand of the express industry for degradable packaging films in rapid development, thoroughly solves the difficult problems of difficult degradation, difficult recovery and easy pollution of the express packaging films, meets the requirement of combining sustainable development and scientific development, brings huge economic benefits for enterprises while protecting ecological environment, and improves the competitiveness of the enterprises.
In order to achieve the purpose, the invention adopts the technical scheme that lignin-based biodegradable polybutylene succinate films comprise, by weight, 47-75 parts of lignin, 0.235-0.75 part of dibenzoyl peroxide, 0.94-3.75 parts of maleic anhydride and 118.91-931.75 parts of polybutylene succinate.
A method for preparing a lignin-based biodegradable polybutylene succinate film, which comprises the following steps:
A. surface treatment, namely sending lignin into a high-speed ball mill for ball milling operation, controlling the rotating speed of a ball mill motor to be 900-950r/min, controlling the nodular time to be 1.5-2 hours, controlling the particle size of the lignin to be 45-55 microns to obtain fine lignin, then sending the fine lignin, maleic anhydride and dibenzoyl peroxide into a high-speed mixer, mixing at a high speed for 5-10 minutes to obtain a premix, sending the premix into a double-screw extruder for reaction and extrusion to obtain the surface treatment lignin;
B. preparing filling master batches, namely feeding the surface treatment lignin prepared in the step A and poly (butylene succinate) into a high-speed mixer, mixing at a high speed for 3-5 minutes to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the lignin filling master batches;
C. b, preparing materials, namely feeding the lignin filling master batch prepared in the step B and poly (butylene succinate) into a high-speed mixer, mixing at a high speed for 3-5 minutes to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the biodegradable film material;
D. and D, blow molding, namely feeding the biodegradable film material prepared in the step C into a blow molding machine, performing melt blow molding operation by adopting an upward blow molding method, and performing inflation, traction and rolling to prepare the lignin-based biodegradable film.
, in step A, the amount of maleic anhydride is 2-5% of the fine lignin by mass, and the amount of dibenzoyl peroxide is 0.5-1% of the fine lignin by mass.
, in the step A, the temperature of the twin-screw extruder is controlled to 35-45 ℃ in the region, 75-85 ℃ in the second region, 95-105 ℃ in the third region, 125 ℃ in the fourth region, 135 ℃ in the fifth region, 125 ℃ in the nose region, and the rotation speed of the main machine is controlled to 8-13 rpm.
, in the step B, the mass ratio of the poly butylene succinate to the surface treatment lignin is controlled to be 2: 3.
, in the step B, the temperature of the twin-screw extruder is controlled to region 100-.
And , in the step C, the mass ratio of the lignin filling master batch to the polybutylene succinate is 8: 92-125: 96.
, in the step C, the temperature of the twin-screw extruder is controlled to region 100-.
, in step D, the temperature of the blow molding machine is controlled to region 110-.
The invention has the beneficial effects that lignin-based biodegradable poly (butylene succinate) films and a preparation method thereof are provided, the film products have high degradation speed, high flexibility and low recovery cost, have no pollution to the environment, can meet a large amount of demands of the express industry developing at a high speed on degradable packaging films, thoroughly solve the difficult problems of difficult degradation, difficult recovery and easy pollution of the express packaging films, meet the requirement of combining sustainable development and scientific development, bring huge economic benefits to enterprises while protecting the ecological environment, and improve the competitiveness of the enterprises.
1. The main raw materials of the invention adopt poly butylene succinate, lignin and maleic anhydride, the lignin is renewable natural degradable organic high molecular substances, the industrial lignin is derived from byproducts of the paper industry, has high yield, can resist ultraviolet radiation and heat, has higher industrial value and huge potential, which is used as the main material of the invention has lower production cost and , the preparation process of the invention is scientific and reasonable, the preparation process is simple and the reliability is high, and the invention can meet the manufacturing requirement of producing and processing degradable films in large scale for enterprises.
2. According to the invention, the compatibility problem is well solved, and the lignin treated by maleic anhydride can generate an interface effect with a polybutylene succinate matrix, so that the compatibility of the lignin and the polybutylene succinate is good, and the lignin is uniformly dispersed in the polybutylene succinate matrix.
3. According to the invention, the polybutylene succinate is added to greatly enhance the flexibility, ductility and comfort of a film product, the polybutylene succinate has good flexibility and ductility, and the polybutylene succinate is introduced into the film as a master batch carrier material, so that the flexibility of the film can be obviously improved.
4. In the invention, the poly (butylene succinate) and the lignin are biodegradable materials, the prepared lignin-based biodegradable film can be rapidly degraded under the condition of composting after being used, the degradation end products are carbon dioxide and water, the damage to land resources and ecological environment can be prevented, the environment is non-toxic and pollution-free, the low-carbon, economic and green environment-friendly effects are achieved, in addition, the lignin-based biodegradable film can be rapidly degraded into non-toxic and harmless carbon dioxide and water after being used, the recovery treatment and the combustion are not needed, and the high post-treatment cost of the express packaging material is saved.
Detailed Description
The present invention is described in detail below with reference to examples for better understanding of technical solutions of the present invention by those skilled in the art, and the description of the present invention is only exemplary and explanatory and should not be construed as limiting the scope of the present invention in any way.
Example 1 Lignin-based biodegradable polybutylene succinate films comprise, by weight, 47 parts of Lignin, 0.235 parts of dibenzoyl peroxide, 0.94 parts of maleic anhydride, and 931.75 parts of polybutylene succinate.
A method for preparing a lignin-based biodegradable polybutylene succinate film, which comprises the following steps:
A. surface treatment, namely feeding lignin into a high-speed ball mill for ball milling operation, controlling the rotating speed of a motor of the ball mill to be 900r/min, controlling the ball milling time to be 1.5 hours, controlling the particle size of the lignin to be 45 microns to obtain fine lignin, then feeding the fine lignin, maleic anhydride and dibenzoyl peroxide into a high-speed mixer, mixing for 5 minutes at a high speed to obtain a premix, feeding the premix into a double-screw extruder for reaction and extrusion to obtain the surface treatment lignin, wherein the dosage of the maleic anhydride is 2% of the mass of the fine lignin, and the dosage of the dibenzoyl peroxide is 0.5% of the mass of the fine lignin, and the temperature of the double-screw extruder is controlled to be 35 ℃ in a area, 75 ℃ in a second area, 95 ℃ in a third area, 115 ℃ in a fourth area, 125.
B. And C, preparing filling master batches, namely feeding the surface treatment lignin prepared in the step A and poly (butylene succinate) into a high-speed mixer, mixing at a high speed for 3 minutes to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the lignin filling master batches, wherein the mass ratio of the poly (butylene succinate) to the surface treatment lignin is controlled to be 2: 3, the temperature of the double-screw extruder is controlled to be 100 ℃ in an area, 120 ℃ in a second area, 140 ℃ in a third area, 150 ℃ in a fourth area, 150 ℃ in a fifth area, 145 ℃ at a head, and the rotating speed of a main machine of the double-screw extruder is controlled.
C. And C, preparing the material, namely feeding the lignin filling master batch prepared in the step B and the poly butylene succinate into a high-speed mixer, mixing at a high speed for 3 minutes to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the biodegradable film material, wherein the mass ratio of the lignin filling master batch to the poly butylene succinate is 8: 92, the temperature of the double-screw extruder is controlled to be 100 ℃ in an area, 120 ℃ in a second area, 140 ℃ in a third area, 150 ℃ in a fourth area, 150 ℃ in a fifth area, 145 ℃ at a head of the double-screw extruder, and the rotating speed of a main machine of the double-screw extruder.
D. And D, blow molding, namely feeding the biodegradable film material prepared in the step C into a blow molding machine, performing melt blow molding operation by adopting an upward blow molding method, and performing blowing, traction and winding to prepare the lignin-based biodegradable film, wherein the temperature of the blow molding machine is controlled to be 110 ℃ in an area, 130 ℃ in a second area, 150 ℃ in a third area, 155 ℃ in a fourth area, 155 ℃ in a head, the rotating speed of a main machine of the blow molding machine is controlled to be 80rpm, and the blow ratio is controlled to be 2.2: 1.
Example 2A lignin-based biodegradable polybutylene succinate film comprises, by weight, 55 parts of lignin, 0.44 part of dibenzoyl peroxide, 1.65 parts of maleic anhydride and 118.91 parts of polybutylene succinate.
A method for preparing a lignin-based biodegradable polybutylene succinate film, which comprises the following steps:
A. surface treatment, namely feeding lignin into a high-speed ball mill for ball milling operation, controlling the rotating speed of a motor of the ball mill to be 930r/min, controlling the nodular time to be 1.8 hours, controlling the particle size of the lignin to be 50 microns to obtain fine lignin, then feeding the fine lignin, maleic anhydride and dibenzoyl peroxide into a high-speed mixer, mixing at a high speed for 8 minutes to obtain a premix, feeding the premix into a double-screw extruder for reaction and extrusion to obtain the surface treatment lignin, wherein the dosage of the maleic anhydride is 3% of the mass of the fine lignin, and the dosage of the dibenzoyl peroxide is 0.8% of the mass of the fine lignin, and the temperature of the double-screw extruder is controlled to be region 40 ℃, 80 ℃ of a second region, 100 ℃ of a third region, 120 ℃ of a fourth region, 130 ℃ of a fifth.
B. And C, preparing filling master batches, namely feeding the surface treatment lignin prepared in the step A and poly (butylene succinate) into a high-speed mixer, mixing at a high speed for 5 minutes to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the lignin filling master batches, wherein the mass ratio of the poly (butylene succinate) to the surface treatment lignin is controlled to be 2: 3, the temperature of the double-screw extruder is controlled to be 105 ℃ in an area, 125 ℃ in a second area, 145 ℃ in a third area, 155 ℃ in a fourth area, 155 ℃ in a fifth area, 150 ℃ at a nose, and the rotating speed of a main machine of the double-screw extruder is controlled.
C. And C, preparing the material, namely feeding the lignin filling master batch prepared in the step B and the poly butylene succinate into a high-speed mixer, mixing for 4 minutes at a high speed to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the biodegradable film material, wherein the mass ratio of the lignin filling master batch to the poly butylene succinate is 58: 52, the temperature of the double-screw extruder is controlled to be 105 ℃ in an area, 125 ℃ in a second area, 145 ℃ in a third area, 155 ℃ in a fourth area, 155 ℃ in a fifth area, 150 ℃ in a nose and the rotating speed of a main machine of the double-screw extruder is controlled to be 100 rpm.
D. And D, blow molding, namely feeding the biodegradable film material prepared in the step C into a blow molding machine, performing melt blow molding operation by adopting an upward blow molding method, and performing blowing, traction and winding to prepare the lignin-based biodegradable film, wherein the temperature of the blow molding machine is controlled to 115 ℃ in an area, 135 ℃ in a second area, 155 ℃ in a third area, 160 ℃ in a fourth area, 160 ℃ in a head, the rotating speed of a main machine of the blow molding machine is controlled to 90rpm, and the blow ratio is controlled to 3: 1.
Example 3A lignin-based biodegradable polybutylene succinate film comprises, by weight, 75 parts of lignin, 0.75 part of dibenzoyl peroxide, 3.75 parts of maleic anhydride and 146 parts of polybutylene succinate.
A method for preparing a lignin-based biodegradable polybutylene succinate film, which comprises the following steps:
A. surface treatment, namely feeding lignin into a high-speed ball mill for ball milling operation, controlling the particle size of the lignin to be 55 microns at the ball mill motor rotation speed of 950r/min for 2 hours for nodular time to obtain fine lignin, then feeding the fine lignin, maleic anhydride and dibenzoyl peroxide into a high-speed mixer for high-speed mixing for 10 minutes to obtain a premix, feeding the premix into a double-screw extruder for reaction and extrusion to obtain the surface-treated lignin, wherein the consumption of the maleic anhydride is 5% of the mass of the fine lignin, and the consumption of the dibenzoyl peroxide is 1% of the mass of the fine lignin, and the temperature of the double-screw extruder is controlled to be 45 ℃ in an area, 85 ℃ in a second area, 105 ℃ in a fourth area, 125 ℃ in a fifth area, 135 ℃ in a nose, and the rotation speed of.
B. And C, preparing filling master batches, namely feeding the surface treatment lignin prepared in the step A and poly (butylene succinate) into a high-speed mixer, mixing at a high speed for 5 minutes to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the lignin filling master batches, wherein the mass ratio of the poly (butylene succinate) to the surface treatment lignin is controlled to be 2: 3, the temperature of the double-screw extruder is controlled to be 110 ℃ in area, 130 ℃ in two areas, 150 ℃ in three areas, 160 ℃ in four areas, 160 ℃ in five areas, 155 ℃ in head, and the main machine rotating speed of the double-screw extruder is controlled to be 70 rpm.
C. And C, preparing the material, namely feeding the lignin filling master batch prepared in the step B and the poly butylene succinate into a high-speed mixer, mixing at a high speed for 5 minutes to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the biodegradable film material, wherein the mass ratio of the lignin filling master batch to the poly butylene succinate is 125: 96, the temperature of the double-screw extruder is controlled to be 110 ℃ in area, 130 ℃ in two areas, 150 ℃ in three areas, 160 ℃ in four areas, 160 ℃ in five areas, 155 ℃ at the head of the double-screw extruder, and the rotating speed of a main machine of the double-screw extruder is controlled to be 100.
D. And D, blow molding, namely feeding the biodegradable film material prepared in the step C into a blow molding machine, performing melt blow molding operation by adopting an upward blow molding method, and performing blowing, traction and winding to prepare the lignin-based biodegradable film, wherein the temperature of the blow molding machine is controlled to be 120 ℃ in an area, 140 ℃ in a second area, 160 ℃ in a third area, 165 ℃ in a fourth area, 165 ℃ in a head, the rotating speed of a main machine of the blow molding machine is controlled to be 100rpm, and the blow ratio is controlled to be 3: 1.
Control group 1: the preparation method is specifically adopted in example 1, but the surface treatment process operation in step A is not carried out, and the lignin and the polybutylene succinate are directly prepared into the filling master batch.
Control group 2: the preparation was carried out by the specific preparation method of example 2, but the filler masterbatch preparation operation of step B was not carried out, and the surface-treated lignin was directly subjected to the material preparation operation.
Control group 3: the preparation was carried out by the specific preparation method of example 3, but the treatment process operations of step a and step B were not carried out, and the lignin was directly subjected to the preparation material operation.
The indexes of the films prepared in the above examples and comparative examples were examined, summarized and collated as shown in the following table:
as can be seen from the detection results in the above table, in the examples and the comparative examples, the tensile strength and the elongation at break of the film manufactured in the example in which the surface treatment and the masterbatch filling process are performed are both improved, the film is also significantly improved in the compost degradation rate, and the manufactured film has high decomposition rate and good decomposition effect.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises the series of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts of the present invention. The foregoing is only a preferred embodiment of the present invention, and it should be noted that there are objectively infinite specific structures due to the limited character expressions, and it will be apparent to those skilled in the art that a plurality of modifications, decorations or changes may be made without departing from the principle of the present invention, and the technical features described above may be combined in a suitable manner; such modifications, variations, combinations, or adaptations of the invention using its spirit and scope, as defined by the claims, may be directed to other uses and embodiments.
Claims (9)
1, lignin-based biodegradable poly (butylene succinate) film, which is characterized by comprising the following components, by weight, 47-75 parts of lignin, 0.235-0.75 part of dibenzoyl peroxide, 0.94-3.75 parts of maleic anhydride and 118.91-931.75 parts of poly (butylene succinate).
2, A preparation method of a lignin-based biodegradable polybutylene succinate film, which is characterized by comprising the following steps:
A. surface treatment, namely sending lignin into a high-speed ball mill for ball milling operation, controlling the rotating speed of a ball mill motor to be 900-950r/min, controlling the nodular time to be 1.5-2 hours, controlling the particle size of the lignin to be 45-55 microns to obtain fine lignin, then sending the fine lignin, maleic anhydride and dibenzoyl peroxide into a high-speed mixer, mixing at a high speed for 5-10 minutes to obtain a premix, sending the premix into a double-screw extruder for reaction and extrusion to obtain the surface treatment lignin;
B. preparing filling master batches, namely feeding the surface treatment lignin prepared in the step A and poly (butylene succinate) into a high-speed mixer, mixing at a high speed for 3-5 minutes to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the lignin filling master batches;
C. b, preparing materials, namely feeding the lignin filling master batch prepared in the step B and poly (butylene succinate) into a high-speed mixer, mixing at a high speed for 3-5 minutes to obtain a premix, feeding the premix into a double-screw extruder, and carrying out melting, mixing, extruding and granulating operations to obtain the biodegradable film material;
D. and D, blow molding, namely feeding the biodegradable film material prepared in the step C into a blow molding machine, performing melt blow molding operation by adopting an upward blow molding method, and performing inflation, traction and rolling to prepare the lignin-based biodegradable film.
3. The method for preparing a lignin-based biodegradable polybutylene succinate film according to claim 2, wherein in step A, maleic anhydride is used in an amount of 2-5% by mass of the fine lignin, and dibenzoyl peroxide is used in an amount of 0.5-1% by mass of the fine lignin.
4. The method for preparing the lignin-based biodegradable polybutylene succinate film as claimed in claim 2, wherein in step A, the temperature of the twin-screw extruder is controlled to 35-45 ℃ in region, 75-85 ℃ in the second region, 95-105 ℃ in the third region, 115-125 ℃ in the fourth region, 135 ℃ in the fifth region, 125-135 ℃ in the nose, and 8-13rpm in the rotation speed of the main machine.
5. The method for preparing a lignin-based biodegradable polybutylene succinate film according to claim 2, wherein in step B, the mass ratio of polybutylene succinate to surface-treated lignin is controlled to 2: 3.
6. The method for preparing the lignin-based biodegradable polybutylene succinate film according to claim 2, wherein in step B, the temperature of the twin-screw extruder is controlled at region 100-.
7. The method for preparing A biodegradable polybutylene succinate film with lignin group according to claim 2, wherein in step C, the mass ratio of the lignin-filled masterbatch to the polybutylene succinate is 8: 92-125: 96.
8. The method for preparing the lignin-based biodegradable polybutylene succinate film according to claim 2, wherein in step C, the temperature of the twin-screw extruder is controlled at -.
9. The method for preparing A biodegradable polybutylene succinate film according to claim 2, wherein in step D, the temperature of the blow molding machine is controlled to region 110-.
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