CN113185815A - Biodegradable material for improving PBSeT puncture resistance by using vinegar residue and preparation method thereof - Google Patents
Biodegradable material for improving PBSeT puncture resistance by using vinegar residue and preparation method thereof Download PDFInfo
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- CN113185815A CN113185815A CN202110533150.9A CN202110533150A CN113185815A CN 113185815 A CN113185815 A CN 113185815A CN 202110533150 A CN202110533150 A CN 202110533150A CN 113185815 A CN113185815 A CN 113185815A
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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Abstract
The invention relates to the field of high polymer materials, in particular to a biodegradable material for improving the puncture resistance of PBSeT by using vinegar residue and a preparation method thereof; the biodegradable material is prepared from the following raw materials in parts by weight: 70-100 parts of PBSeT and 0-30 parts of vinegar residue; the preparation method comprises the following steps: firstly, crushing wet vinegar residues by using a crusher, and then drying the crushed wet vinegar residues in a forced air drying oven for 72 hours; then, sieving the dried vinegar residue with a sieve of 50 meshes and a sieve of 200 meshes in sequence; finally, blending the vinegar residue which passes through a 200-mesh sieve with the PBSeT at high temperature to obtain a biodegradable material with the vinegar residue for improving the puncture resistance of the PBSeT; the vinegar residue improves the puncture resistance of the PBSeT biodegradable material by 92.8 percent compared with the puncture resistance of a single PBSeT biodegradable material. The preparation method can improve the puncture resistance of the PBSeT biodegradable material and has higher market value.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a biodegradable material for improving the puncture resistance of PBSeT by using vinegar residue and a preparation method thereof.
Background
Environmental protection is one of the topics which is currently being highlighted, because environmental pollution is becoming more and more serious. Among them, white pollution is one of the most troublesome problems. Therefore, researchers have made efforts to develop degradable plastic products, and polyester-based plastics among them are gaining favor, such as polybutylene succinate (PBS), polylactic acid (PLA), poly (hydroxyalkanoate) (PHA), poly (butylene adipate-terephthalate) (PBAT), and poly (sebacic sebacate-butylene terephthalate) (PBSeT). Of course, these products are not perfect and present more problems. The high cost and unbalanced performance become a bottleneck problem that restricts the development of biodegradable materials, which limits their widespread use.
The vinegar residue is a byproduct in the vinegar making process and mainly comprises rice hulls, bran coat, sorghum hulls and the like. China is the largest world-wide country for producing and consuming edible vinegar, and the annual yield of vinegar residues is over 500 ten thousand tons and is increasing every year. The vinegar residue contains cellulose 30.78% on average and hemicellulose 18.05% on average. Meanwhile, the vinegar residue also contains lignin, starch, crude protein, crude fat and nutrient elements required by microorganisms. Based on some properties of the vinegar residue, the vinegar residue is mainly used as a feed raw material, an edible fungus cultivation material or a plant cultivation substrate and is applied to traditional Chinese medicines. The vinegar residue can be used for animal and plant production, but has the problems of small treatment amount, large energy consumption and the like. Therefore, the disposal of vinegar residue is one of the problems that are troublesome today. However, the pbsets synthesized by us are difficult to be popularized due to the problems of puncture, barrier properties, low melting point, high cost, and the like.
As is known from the mechanism of the puncture resistance of a material, in order to improve the puncture resistance of a material, the puncture resistance of a material can be improved by blending, increasing crystallinity, increasing intermolecular interaction force, or the like.
Disclosure of Invention
The invention provides a biodegradable material for improving the puncture resistance of PBSeT by using vinegar residue, aiming at solving the technical problem of poor puncture resistance of PBSeT material.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a biodegradable material for improving PBSeT puncture resistance by using vinegar residue is prepared from the following raw materials in parts by weight: 70-100 parts of PBSeT (poly sebacic acid glycol ester-butylene terephthalate) and 0-30 parts of vinegar residue.
The PBSeT used above was the PBSeT sample prepared in example 1 of the patent publication No. CN112280014A, namely: weighing 713g of SeA (sebacic acid), 900g of BDO (1, 4-butanediol) and 390.59g of TPA (terephthalic acid) by a one-step esterification method, adding 6g of Tetrabutyl Titanate (catalyst) for esterification when the temperature reaches 220 ℃, starting polycondensation when the quality of the produced water is equal to that of theoretical water, adding 3g of Tetrabutyl Titanate (catalyst) and heating to 230 ℃ for polycondensation, and finishing polycondensation when the torque on equipment is not changed after the polycondensation is carried out for a period of time.
The vinegar residue contains considerable amount of cellulose and hemicellulose, and part of lignin. Cellulose contains a great deal of hydroxyl, and when the cellulose enters a PBST matrix as a filler, PBSeT molecular chains can be attracted and acting force between the molecular chains is increased due to the existence of the surface hydroxyl. The lignin has benzene rings, so that the melting point, the puncture performance and the like of the material can be properly improved.
Preferably, the biodegradable material for improving the PBSeT puncture resistance by using the vinegar residue is prepared from the following raw materials in parts by weight: 76 parts of PBSeT (polysebacate-butylene terephthalate) and 24 parts of vinegar residue.
Further, the weight average molecular weight of the PBSeT is 23502.
Further, the polydispersity of the PBSeT is 1.09.
Further, the viscosity of the PBSeT is 0.77 dL/g.
In addition, the invention also provides a preparation method of the biodegradable material, which comprises the steps of firstly crushing the wet vinegar residue by using a crusher, and then drying the crushed wet vinegar residue in a forced air drying oven for 72 hours; then, sieving the dried vinegar residue with a sieve of 50 meshes and a sieve of 200 meshes in sequence; and finally, blending the vinegar residue which passes through a 200-mesh sieve with the PBSeT at high temperature to obtain the biodegradable material with the vinegar residue for improving the puncture resistance of the PBSeT.
Through the steps, the PBSeT material and the vinegar residue are blended at high temperature, and the vinegar residue comprises cellulose, lignin, a small amount of starch and the like. Cellulose and starch contain a large number of hydroxyl groups, and PBSeT can enhance the acting force between molecules whether the hydroxyl groups are blocked or the carboxyl groups are blocked. In addition, after passing through a 200-mesh sieve, the specific surface area of the particles is increased, so that the activity of the surface groups of the particles is higher. Of course, the benzene ring contained in the lignin has better effect on improving the performance of the material.
Furthermore, the used blending reaction equipment is a torque rheometer, and the temperatures of the front, middle and rear plates are 120-130 ℃, 150-180 ℃ and 150-180 ℃.
Further, adjusting the rotating speed of the rotor from 0 to 10-20 rad/min, and then adding weighed PBSeT into the rotor; then adjusting the rotating speed to 50-60 rad/min, adding a certain amount of vinegar residues into reaction equipment, blending for 1.5min, and taking out a first product; and then shearing the first product, putting the sheared first product into the torque rheometer again, blending for 1.5min, taking out the second product, and finally taking out the second product, wherein the sheared second product is put into the torque rheometer, blending for 3-6 min, and finishing to obtain the biodegradable material.
Purpose of three times of blending: firstly, in order to disperse the vinegar residue powder more uniformly, the broken vinegar residue powder can be dispersed better by blending for a plurality of times in a short time during blending; the other is to prevent the polyester material from lasting too long at high temperature, and the molecular chain becomes fragile and easy to break due to the long-time high temperature. In addition, the polyester is a biodegradable material, and the long-term high temperature can cause the oxidative breakage of molecular chains.
Compared with the prior art, the invention has the following beneficial effects:
the vinegar residue improves the puncture resistance of the PBSeT biodegradable material by 92.8 percent compared with the puncture resistance of a single PBSeT biodegradable material under the condition that the mass ratio of the vinegar residue to the PBSeT is 12/38 under the blending condition. The preparation method can improve the puncture resistance of the PBSeT biodegradable material and has higher market value.
Drawings
Fig. 1 is a schematic diagram of a preparation blending route of a biodegradable material for improving the puncture resistance of PBSeT by using vinegar residue.
Fig. 2 shows the tear strength test results of the biodegradable material control sample and the examples, which utilize vinegar residue to improve the puncture resistance of PBSeT.
Detailed Description
The present invention is further illustrated by the following specific examples.
The invention provides a biodegradable material, which is prepared from 70-100 parts by weight of PBSeT (poly sebacic acid glycol ester-butylene terephthalate) and 0-30 parts by weight of vinegar residue.
Provides a preparation method of a biodegradable material, adopts the raw materials, and comprises the following steps:
the wet vinegar residue is crushed by a crusher and then is put into an air-blast drying oven for drying for 72 hours. After the completion, the dried vinegar residue is sieved by a sieve with 50 meshes and a sieve with 200 meshes, and the vinegar residue powder sieved by the sieve with 200 meshes is used.
A torque rheometer is adopted as a blending reaction device, and the temperatures of the front, middle and rear plates are respectively set to be 120-130 ℃, 150-180 ℃ and 150-180 ℃. When the temperature rises to a designated temperature, the rotor speed is adjusted from 0 to 10 to 20rad/min, and then PBSeT (poly sebacic acid-butylene terephthalate) is added thereto. And then adjusting the rotating speed to 50-60 rad/min, adding the vinegar residue into the reaction equipment, blending for 1.5min, and taking out a first product. Then shearing the first product, putting the sheared first product into a torque rheometer again, blending for 1.5min, taking out the second product, and finally taking out the second product, wherein the sheared second product is put into the torque rheometer to blend for 3-6 min, and then ending the experiment; the group to which no vinegar residue was added was additionally set as a control group.
Example 1
By adopting the method, 47g of the synthesized PBSeT is weighed after being dried in a forced air drying oven for 12 hours, and the temperatures of the front, middle and rear plates of the torque rheometer are respectively set to be 120-130 ℃, 150-180 ℃ and 150-180 ℃. When the temperature rises to the specified temperature, the rotor speed is adjusted from 0 to 10 to 20rad/min, and then weighed PBSeT is added thereto. And then adjusting the rotating speed to 50-60 rad/min, adding 3g of vinegar residues into the reaction equipment, blending for 1.5min, and taking out a first product. And then shearing the first product, putting the sheared first product into the torque rheometer again, blending for 1.5min, taking out the second product, and finally taking out the second product, wherein the sheared second product is put into the torque rheometer to be blended for 3-6 min, and then ending the experiment.
Example 2
By adopting the method, 44g of the synthesized PBSeT is weighed after being dried in a forced air drying oven for 12 hours, and the temperatures of the front, middle and rear plates of the torque rheometer are respectively set to be 120-130 ℃, 150-180 ℃ and 150-180 ℃. When the temperature rises to the specified temperature, the rotor speed is adjusted from 0 to 10 to 20rad/min, and then weighed PBSeT is added thereto. And then adjusting the rotating speed to 50-60 rad/min, adding 6g of vinegar residue into the reaction equipment, blending for 1.5min, and taking out a first product. And then shearing the first product, putting the sheared first product into the torque rheometer again, blending for 1.5min, taking out the second product, and finally taking out the second product, wherein the sheared second product is put into the torque rheometer to be blended for 3-6 min, and then ending the experiment.
Example 3
By adopting the method, 41g of the synthesized PBSeT is weighed after being dried in a forced air drying oven for 12h, and the temperatures of the front, middle and rear plates of the torque rheometer are respectively set to be 120-130 ℃, 150-180 ℃ and 150-180 ℃. When the temperature rises to the specified temperature, the rotor speed is adjusted from 0 to 10 to 20rad/min, and then weighed PBSeT is added thereto. And then adjusting the rotating speed to 50-60 rad/min, adding 9g of vinegar residue into the reaction equipment, blending for 1.5min, and taking out a first product. And then shearing the first product, putting the sheared first product into the torque rheometer again, blending for 1.5min, taking out the second product, and finally taking out the second product, wherein the sheared second product is put into the torque rheometer to be blended for 3-6 min, and then ending the experiment.
Example 4
By adopting the method, 38g of the synthesized PBSeT is weighed after being dried in a forced air drying oven for 12 hours, and the temperatures of the front, middle and rear plates of the torque rheometer are respectively set to be 120-130 ℃, 150-180 ℃ and 150-180 ℃. When the temperature rises to the specified temperature, the rotor speed is adjusted from 0 to 10 to 20rad/min, and then weighed PBSeT is added thereto. And then adjusting the rotating speed to 50-60 rad/min, adding 12g of vinegar residue into the reaction equipment, blending for 1.5min, and taking out a first product. And then shearing the first product, putting the sheared first product into the torque rheometer again, blending for 1.5min, taking out the second product, and finally taking out the second product, wherein the sheared second product is put into the torque rheometer to be blended for 3-6 min, and then ending the experiment.
Example 5
By adopting the method, 35g of the synthesized PBSeT is weighed after being dried in a forced air drying oven for 12 hours, and the temperatures of the front, middle and rear plates of the torque rheometer are respectively set to be 120-130 ℃, 150-180 ℃ and 150-180 ℃. When the temperature rises to the specified temperature, the rotor speed is adjusted from 0 to 10 to 20rad/min, and then weighed PBSeT is added thereto. And then adjusting the rotating speed to 50-60 rad/min, adding 15g of vinegar residue into the reaction equipment, blending for 1.5min, and taking out a first product. And then shearing the first product, putting the sheared first product into the torque rheometer again, blending for 1.5min, taking out the second product, and finally taking out the second product, wherein the sheared second product is put into the torque rheometer to be blended for 3-6 min, and then ending the experiment.
And (3) detection results:
the puncture resistance of the vinegar residue modified PBSeT biodegradable material prepared in example 1, example 2, example 3, example 4 and example 5 and the puncture resistance of the biodegradable material prepared in the control group were measured. Wherein, the puncture strength test method in GB/T10004-. The test sample is hot pressed by a flat vulcanizing machine, then cold pressed and molded, and is cut into a sheet with the diameter of 30mm, and the test temperature is 25 ℃. The puncture resistance of the sample was determined as the average of 5 data from three experiments, and the test results are shown in table 1.
As can be seen from table 1, it can be seen from example 1 to example 5 that: the vinegar residue provided by the invention can improve the puncture resistance of the PBSeT biodegradable material, and along with the increase of the mass part of the vinegar residue, the vinegar residue can improve the puncture resistance of the PBSeT biodegradable material, and the puncture resistance is firstly increased and then decreased. The puncture resistance strength of the PBSeT biodegradable material is 3.23N without adding vinegar residue. The anti-puncture strength of the PBSeT biodegradable material added with 6 parts of vinegar residue is 5.56N. The puncture resistance of the PBSeT biodegradable material added with 12 parts of vinegar residue is 5.78N. With the addition of 18 parts of vinegar residue, the puncture resistance strength of the PBSeT biodegradable material was 5.84N. The anti-puncture strength of the PBSeT biodegradable material added with 24 parts of vinegar residue is increased to 6.23N. The puncture resistance of the PBSeT biodegradable material added with 30 parts of vinegar residue is reduced to 5.43N.
Table 1: detection result of improving puncture resistance of PBSeT biodegradable material embodiment by vinegar residue
As can be seen from the above table 1 and fig. 1, by using the blending method provided by the present invention, a certain amount of the synthesized PBSeT is weighed after being dried in the forced air drying oven for 12 hours, and the temperatures of the front, middle and rear plates of the torque rheometer are set to 120-130 ℃, 150-180 ℃ and 150-180 ℃ respectively. When the temperature rises to the specified temperature, the rotor speed is adjusted from 0 to 10 to 20rad/min, and then weighed PBSeT is added thereto. And then adjusting the rotating speed to 50-60 rad/min, adding a certain amount of vinegar residues into the reaction equipment, blending for 1.5min, and taking out a first product. And then shearing the first product, putting the sheared first product into the torque rheometer again, blending for 1.5min, taking out the second product, shearing the second product, putting the sheared second product into the torque rheometer, blending for 3-6 min, and ending the experiment, so that the puncture resistance of the PBSeT biodegradable material can be improved, and the puncture resistance strength is firstly increased and then reduced along with the increase of the content of the vinegar residue.
The experimental result shows that the vinegar residue provided by the invention improves the puncture resistance of the PBSeT biodegradable material, and the puncture resistance strength of the PBSeT biodegradable material added with 24 parts of vinegar residue is improved by about 92.8 percent compared with the puncture resistance strength of the PBSeT biodegradable material not added with vinegar residue.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (8)
1. The biodegradable material for improving the puncture resistance of PBSeT by using the vinegar residue is characterized by being prepared from the following raw materials in parts by weight: 70-100 parts of PBSeT and 0-30 parts of vinegar residue.
2. The biodegradable material for improving the PBSeT puncture resistance by using vinegar residue as claimed in claim 1, is characterized by being prepared from the following raw materials in parts by weight: PBSeT 76 parts and vinegar residue 24 parts.
3. The biodegradable material of PBSeT improved in puncture resistance by vinegar residue as claimed in claim 1, wherein the weight average molecular weight of PBSeT is 23502.
4. The biodegradable material of PBSeT with vinegar residue for improving the puncture resistance of PBSeT as claimed in claim 1, wherein the polydispersity of PBSeT is 1.09.
5. The biodegradable material of claim 1, wherein the viscosity of PBSeT is 0.77 dL/g.
6. The method for producing a biodegradable material according to any one of claims 1 to 5, wherein the wet vinegar residue is first pulverized by a crusher and then dried in a forced air drying oven for 72 hours; then, sieving the dried vinegar residue with a sieve of 50 meshes and a sieve of 200 meshes in sequence; and finally, blending the vinegar residue which passes through a 200-mesh sieve with the PBSeT at high temperature to obtain the biodegradable material with the vinegar residue for improving the puncture resistance of the PBSeT.
7. The method for preparing biodegradable material according to claim 6, wherein the blending reaction equipment is a torque rheometer, and the temperatures of the front, middle and rear plates are 120-130 ℃, 150-180 ℃ and 150-180 ℃.
8. The method for preparing biodegradable material according to claim 6, wherein the rotor speed is adjusted from 0 to 10-20 rad/min, and then the weighed PBSeT is added thereto; then adjusting the rotating speed to 50-60 rad/min, adding a certain amount of vinegar residues into reaction equipment, blending for 1.5min, and taking out a first product; and then shearing the first product, putting the sheared first product into the torque rheometer again, blending for 1.5min, taking out the second product, and finally taking out the second product, wherein the sheared second product is put into the torque rheometer, blending for 3-6 min, and finishing to obtain the biodegradable material.
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