CN109535671B - Polybutylene succinate composite material and preparation method thereof - Google Patents
Polybutylene succinate composite material and preparation method thereof Download PDFInfo
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- CN109535671B CN109535671B CN201811515124.8A CN201811515124A CN109535671B CN 109535671 B CN109535671 B CN 109535671B CN 201811515124 A CN201811515124 A CN 201811515124A CN 109535671 B CN109535671 B CN 109535671B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C08F8/14—Esterification
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Abstract
The application relates to a polybutylene succinate composite material and a preparation method thereof. The preparation method of the PBS composite material comprises the following steps: providing maleic anhydride grafted starch; mixing maleic anhydride grafted starch, 1, 4-butanediol and biomass carbon sulfonic acid to obtain a precursor; performing reaction extrusion on the precursor to obtain modified starch; and mixing, melting and extruding the modified starch and the poly (butylene succinate) to obtain the PBS composite material. According to the PBS composite material, the biomass carbon sulfonic acid is used as a catalyst, a reaction extrusion method is adopted, the 1, 4-butanediol and the maleic anhydride grafted starch are subjected to esterification reaction to obtain the modified starch with good compatibility with the PBS, the modified starch and the PBS are subjected to melt extrusion to obtain the PBS composite material, and the reaction extrusion and the melt extrusion are carried out through extrusion, so that the efficiency is greatly improved, the process flow is simplified, the equipment investment is reduced, and the field area is greatly reduced.
Description
Technical Field
The invention relates to the technical field of biodegradation, and particularly relates to a polybutylene succinate composite material and a preparation method thereof.
Background
Polybutylene succinate (PBS) is a biodegradable plastic with good ductility and flexibility, has a very good application value in the field of films, but is limited in application due to low tensile strength and high price, so that researches on improving the tensile strength of the PBS and reducing the cost of the PBS are paid attention, and the preparation of the PBS composite material by compounding starch and the PBS is one of effective ways. At present, a plurality of PBS composite materials are prepared by a chemical modification method, wherein the chemical modification method has the best effect, but the existing chemical method has the defects of complex process, high equipment investment and low efficiency.
Disclosure of Invention
Accordingly, there is a need for a method for synthesizing a PBS composite material with simple process, low equipment investment cost, and high efficiency.
A preparation method of poly (butylene succinate) comprises the following steps:
providing maleic anhydride grafted starch;
mixing the maleic anhydride grafted starch, 1, 4-butanediol and biomass carbon sulfonic acid to obtain a precursor;
performing reaction extrusion on the precursor to obtain modified starch;
and mixing the modified starch with the poly (butylene succinate), and performing melt extrusion to obtain the poly (butylene succinate) composite material.
In one embodiment, the mass of the 1, 4-butanediol is 5-25% of the mass of the maleic anhydride grafted starch.
In one embodiment, the mass of the biomass carbon sulfonic acid is 0.2-0.8% of the mass of the maleic anhydride grafted starch.
In one embodiment, the temperature of the reactive extrusion is, in order from the material advancing direction: 80-90 ℃, 95-105 ℃, 105-115 ℃, 115-125 ℃ and 110-120 ℃.
In one embodiment, the mass of the modified starch is 20-50% of that of the polybutylene succinate.
In one embodiment, the melt extrusion temperature is, in order from the material advancing direction: 80-90 ℃, 90-100 ℃, 100-120 ℃, 110-130 ℃, 120-140 ℃, 135-155 ℃ and 135-140 ℃.
In one embodiment, the maleic anhydride grafted starch is prepared by the following method:
mixing starch, maleic anhydride, water and ammonium persulfate, and performing reaction extrusion to obtain maleic anhydride grafted starch.
In one embodiment, the mass of the maleic anhydride is 2-5% of the mass of the starch; the mass of the water is 25-35% of the mass of the starch; the mass of the ammonium persulfate is 0.5-1% of the mass of the starch.
In one embodiment, in the step of mixing starch, maleic anhydride, water and ammonium persulfate and performing reactive extrusion, the temperature of reactive extrusion is as follows in the material advancing direction: 85-95 deg.C, 90-100 deg.C, 93-103 deg.C, 95-105 deg.C, 100-110 deg.C, 105-115 deg.C.
The application also provides a polybutylene succinate composite material, and the specific scheme is as follows:
the polybutylene succinate composite material prepared by the preparation method of the polybutylene succinate composite material.
According to the PBS composite material, the biomass carbon sulfonic acid is used as a catalyst, a reaction extrusion method is adopted, the 1, 4-butanediol and the maleic anhydride grafted starch are subjected to esterification reaction to obtain the modified starch with good compatibility with the PBS, the modified starch and the PBS are subjected to melt extrusion to obtain the PBS composite material, and the reaction extrusion and the melt extrusion are carried out through extrusion, so that the efficiency is greatly improved, the process flow is simplified, and the equipment investment is greatly reduced.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a PBS composite material according to an embodiment.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, a method for preparing a PBS composite material according to an embodiment includes the following steps S110 to S140:
and S110, providing maleic anhydride grafted starch.
In this embodiment, the maleic anhydride grafted starch is prepared by the following method:
mixing starch, maleic anhydride, water and ammonium persulfate, and performing reactive extrusion to obtain the maleic anhydride grafted starch.
Wherein the mass of the maleic anhydride is 2-5% of the mass of the starch. The mass of the water is 25-35% of the mass of the starch. The mass of the ammonium persulfate is 0.5-1% of that of the starch.
In this embodiment, starch, maleic anhydride, water, and ammonium persulfate are mixed in a high mixing mill. Reactive extrusion is carried out in a twin-screw extruder.
Further, the temperature of the reaction extrusion is as follows according to the advancing direction of the materials in sequence: 85-95 deg.C, 90-100 deg.C, 93-103 deg.C, 95-105 deg.C, 100-110 deg.C, 105-115 deg.C.
That is, the material is added from the reinforced section of twin-screw extruder, extrudes from the aircraft nose of twin-screw extruder, and the reaction extrusion temperature is from reinforced section to aircraft nose and is in proper order: 85-95 deg.C, 90-100 deg.C, 93-103 deg.C, 95-105 deg.C, 100-110 deg.C, 105-115 deg.C.
Furthermore, the rotating speed of the screw is 5 rpm-20 rpm in the reaction extrusion process.
It should be noted that the maleic anhydride grafted starch is not limited to be prepared by the above method, and in other embodiments, the maleic anhydride grafted starch may be prepared by other methods.
And S120, mixing the maleic anhydride grafted starch, 1, 4-butanediol and biomass carbon sulfonic acid to obtain a precursor.
Wherein the mass of the 1, 4-butanediol is 5-25% of that of the maleic anhydride grafted starch. The mass of the biomass carbon sulfonic acid is 0.2-0.8% of that of the maleic anhydride grafted starch.
In this embodiment, the maleic anhydride grafted starch, 1, 4-butanediol, and biomass carbon sulfonic acid are mixed in a high mixing machine.
And S130, carrying out reaction extrusion on the precursor to obtain the modified starch.
In the present embodiment, the reactive extrusion described above is carried out in a twin-screw extruder.
Further, the temperature of the reaction extrusion is as follows according to the advancing direction of the materials in sequence: 80-90 ℃, 95-105 ℃, 105-115 ℃, 115-125 ℃ and 110-120 ℃.
That is, the material is added from the reinforced section of twin-screw extruder, extrudes from the aircraft nose of twin-screw extruder, and the reaction extrusion temperature is from reinforced section to aircraft nose and is in proper order: 80-90 ℃, 95-105 ℃, 105-115 ℃, 115-125 ℃ and 110-120 ℃.
Furthermore, the rotating speed of the screw is 5 rpm-25 rpm in the reaction extrusion process.
S140, mixing, melting and extruding the modified starch and the poly (butylene succinate) to obtain the poly (butylene succinate) composite material.
Wherein the mass of the modified starch is 20-50% of that of the poly (butylene succinate).
In this embodiment, the modified starch and the polybutylene succinate are mixed in a high-speed mixer and then melt-extruded through a twin-screw extruder.
Further, the melt extrusion temperature is as follows according to the material advancing direction: 80-90 ℃, 90-100 ℃, 100-120 ℃, 110-130 ℃, 120-140 ℃, 135-155 ℃ and 135-140 ℃.
The material is added from the charging section of the double-screw extruder, and is extruded from the machine head of the double-screw extruder, and the reaction extrusion temperature is sequentially from the charging section to the machine head: 80-90 ℃, 90-100 ℃, 100-120 ℃, 110-130 ℃, 120-140 ℃, 135-155 ℃ and 135-140 ℃.
Further, the modified starch and the poly (butylene succinate) are mixed, and the step of granulation is also included after melt extrusion, so that the PBS composite material with uniform particle size distribution is obtained.
According to the PBS composite material, the biomass carbon sulfonic acid is used as a catalyst, a reaction extrusion method is adopted, the 1, 4-butanediol and the maleic anhydride grafted starch are subjected to esterification reaction to obtain modified starch with good compatibility with PBS, the modified starch and the PBS are subjected to melt extrusion to obtain the PBS composite material, and the reaction extrusion and the melt extrusion are carried out in a double-screw extruder, so that the efficiency is greatly improved, the process flow is simplified, the equipment investment is reduced, and the field area is greatly reduced.
In addition, the biomass charcoal sulfonic acid is used as a catalyst, so that the biomass charcoal sulfonic acid is non-toxic, efficient, green and environment-friendly.
The following are specific examples.
Example 1
Uniformly mixing 1000g of starch, 20g of maleic anhydride, 25g of water and 5g of ammonium persulfate in a high-speed mixer to obtain a first precursor; and (2) performing reactive extrusion on the first precursor by using a double-screw extruder to obtain maleic anhydride grafted starch, wherein the reactive extrusion temperature from a feeding section to a machine head is as follows in sequence: 90 deg.C, 95 deg.C, 98 deg.C, 100 deg.C, 105 deg.C, 110 deg.C, screw speed 5 rpm.
Uniformly mixing 1000g of maleic anhydride grafted starch, 50g of 1, 4-butanediol and 2g of biomass carbon sulfonic acid in a high-speed mixer to obtain a second precursor; and (3) carrying out reactive extrusion on the second precursor by using a double-screw extruder to obtain modified starch, wherein the reactive extrusion temperature is from a feeding section to a machine head: 85 ℃, 100 ℃, 110 ℃, 120 ℃, 115 ℃ and the screw rotating speed of 5 rpm.
Mixing 1000g of PBS and 200g of modified starch in a high-speed mixer, and then carrying out melt extrusion and granulation by a double-screw extruder to obtain the PBS composite material, wherein the melt extrusion temperature is from a feeding section to a machine head: 90 deg.C, 100 deg.C, 120 deg.C, 130 deg.C, 140 deg.C, 150 deg.C, 140 deg.C, screw speed 50 rpm.
The PBS composite material prepared in the example 1 is detected to have the tensile strength of 34 MPa.
Example 2
Mixing 1000g of starch, 50g of maleic anhydride, 350g of water and 1g of ammonium persulfate uniformly in a high-speed mixer to obtain a first precursor; and (2) performing reactive extrusion on the first precursor by using a double-screw extruder to obtain maleic anhydride grafted starch, wherein the reactive extrusion temperature from a feeding section to a machine head is as follows in sequence: 90 deg.C, 95 deg.C, 98 deg.C, 100 deg.C, 105 deg.C, 110 deg.C, screw rotation speed 5-20 rpm.
Uniformly mixing 1000g of maleic anhydride grafted starch, 250g of 1, 4-butanediol and 8g of biomass carbon sulfonic acid in a high-speed mixer to obtain a second precursor; and (3) carrying out reactive extrusion on the second precursor by using a double-screw extruder to obtain modified starch, wherein the reactive extrusion temperature is from a feeding section to a machine head: 85 ℃, 100 ℃, 110 ℃, 120 ℃, 115 ℃ and the screw rotating speed of 5-25 rpm.
Mixing 1000g of PBS and 500g of modified starch in a high-speed mixer, and then carrying out melt extrusion and granulation by a double-screw extruder to obtain the PBS composite material, wherein the melt extrusion temperature is from a feeding section to a machine head: 90 deg.C, 100 deg.C, 120 deg.C, 130 deg.C, 140 deg.C, 150 deg.C, 140 deg.C, screw rotation speed 50-150 rpm.
Through detection, the tensile strength of the PBS composite material prepared in the example 2 is 30 MPa.
Example 3
Uniformly mixing 1000g of starch, 30g of maleic anhydride, 300g of water and 8g of ammonium persulfate in a high-speed mixer to obtain a first precursor; and (2) performing reactive extrusion on the first precursor by using a double-screw extruder to obtain maleic anhydride grafted starch, wherein the reactive extrusion temperature from a feeding section to a machine head is as follows in sequence: 90 deg.C, 95 deg.C, 98 deg.C, 100 deg.C, 105 deg.C, 110 deg.C, screw rotation speed 5-20 rpm.
Uniformly mixing 1000g of maleic anhydride grafted starch, 150g of 1, 4-butanediol and 5g of biomass carbon sulfonic acid in a high-speed mixer to obtain a second precursor; and (3) carrying out reactive extrusion on the second precursor by using a double-screw extruder to obtain modified starch, wherein the reactive extrusion temperature is from a feeding section to a machine head: 85 ℃, 100 ℃, 110 ℃, 120 ℃, 115 ℃ and the screw rotating speed of 5-25 rpm.
Mixing 1000g of PBS and 350g of modified starch in a high-speed mixer, and then carrying out melt extrusion and granulation by a double-screw extruder to obtain the PBS composite material, wherein the melt extrusion temperature is from a feeding section to a machine head: 90 deg.C, 100 deg.C, 120 deg.C, 130 deg.C, 140 deg.C, 150 deg.C, 140 deg.C, screw rotation speed 50-150 rpm.
Through detection, the tensile strength of the PBS composite material prepared in the example 3 is 36 MPa.
Comparative example 1
Comparative example 1 is essentially the same as example 1 except that no biomass carbon sulfonic acid was added to comparative example 1.
The composite material prepared in comparative example 1 was tested for tensile strength of 22 MPa.
Comparative example 2
Comparative example 2 is essentially the same as example 1 except that in comparative example 2 the maleic anhydride grafted starch is replaced with starch and 1, 4-butanediol and biomass carbon sulfonic acid are mixed.
The composite material prepared in comparative example 2 was tested to have a tensile strength of 19 MPa.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the polybutylene succinate composite material is characterized by comprising the following steps:
providing maleic anhydride grafted starch;
mixing the maleic anhydride grafted starch, 1, 4-butanediol and biomass carbon sulfonic acid to obtain a precursor;
performing reactive extrusion on the precursor to perform esterification reaction on the 1, 4-butanediol and the maleic anhydride grafted starch to obtain modified starch;
and mixing the modified starch with the poly (butylene succinate), and performing melt extrusion to obtain the poly (butylene succinate) composite material.
2. The method for preparing the polybutylene succinate composite material according to claim 1, wherein the mass of the 1, 4-butanediol is 5-25% of that of the maleic anhydride grafted starch.
3. The preparation method of the polybutylene succinate composite material according to claim 1, wherein the mass of the biomass carbon sulfonic acid is 0.2-0.8% of the mass of the maleic anhydride grafted starch.
4. The preparation method of the polybutylene succinate composite material according to claim 1, wherein the reaction extrusion temperature sequentially comprises the following steps in the material advancing direction: 80-90 ℃, 95-105 ℃, 105-115 ℃, 115-125 ℃ and 110-120 ℃.
5. The preparation method of the polybutylene succinate composite material according to claim 1, wherein the mass of the modified starch is 20-50% of the mass of the polybutylene succinate.
6. The preparation method of the polybutylene succinate composite material according to claim 1, wherein the melt extrusion temperature sequentially comprises the following steps in the material advancing direction: 80-90 ℃, 90-100 ℃, 100-120 ℃, 110-130 ℃, 120-140 ℃, 135-155 ℃ and 135-140 ℃.
7. The preparation method of the polybutylene succinate composite material according to any one of claims 1 to 6, wherein the maleic anhydride grafted starch is prepared by the following method:
mixing starch, maleic anhydride, water and ammonium persulfate, and performing reactive extrusion to obtain the maleic anhydride grafted starch.
8. The preparation method of the polybutylene succinate composite material according to claim 7, wherein the mass of the maleic anhydride is 2-5% of the mass of the starch; the mass of the water is 25-35% of the mass of the starch; the mass of the ammonium persulfate is 0.5-1% of the mass of the starch.
9. The preparation method of the polybutylene succinate composite material according to claim 7, wherein in the step of mixing starch, maleic anhydride, water and ammonium persulfate and performing reactive extrusion, the reactive extrusion temperature is as follows in the material advancing direction: 85-95 deg.C, 90-100 deg.C, 93-103 deg.C, 95-105 deg.C, 100-110 deg.C, 105-115 deg.C.
10. The polybutylene succinate composite material prepared by the preparation method of the polybutylene succinate composite material as claimed in any one of claims 1 to 9.
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Effective date of registration: 20210624 Address after: 523000 Room 101, 102 yangkeng Road, Changping Town, Dongguan City, Guangdong Province Patentee after: Dongguan Huiguo New Material Technology Co.,Ltd. Address before: 418000 Huai Dong Road, Hecheng District, Huaihua, Hunan Province, No. 180 Patentee before: HUAIHUA University |