CN114181498A - Degradable polyester material and preparation method thereof - Google Patents
Degradable polyester material and preparation method thereof Download PDFInfo
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- CN114181498A CN114181498A CN202111539342.7A CN202111539342A CN114181498A CN 114181498 A CN114181498 A CN 114181498A CN 202111539342 A CN202111539342 A CN 202111539342A CN 114181498 A CN114181498 A CN 114181498A
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- polyester material
- degradable polyester
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- active
- calcium carbonate
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- 239000000463 material Substances 0.000 title claims abstract description 64
- 229920000728 polyester Polymers 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title abstract description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 56
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 23
- 229920000229 biodegradable polyester Polymers 0.000 claims abstract description 18
- 239000004622 biodegradable polyester Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000000945 filler Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000010008 shearing Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 239000003963 antioxidant agent Substances 0.000 claims description 8
- 230000003078 antioxidant effect Effects 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000000314 lubricant Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 239000003381 stabilizer Substances 0.000 claims description 7
- 239000003607 modifier Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 150000003377 silicon compounds Chemical class 0.000 claims description 5
- 230000003213 activating effect Effects 0.000 claims description 3
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 3
- 239000000454 talc Substances 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- 235000012222 talc Nutrition 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 abstract description 10
- 239000006185 dispersion Substances 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 4
- 229920001896 polybutyrate Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000010621 bar drawing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000005258 radioactive decay Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of degradable materials, in particular to a degradable polyester material; the composite material comprises the following components in percentage by mass: filling agent: 9-30 parts of a solvent; biodegradable polyester: 70-90 parts; a compatilizer: 3-5 parts; the preparation method comprises the following steps: fully mixing the active talcum powder, the active calcium carbonate, the biodegradable polyester, the compatilizer and the auxiliary materials in a stirring pot for 5-8min to form a mixture; and sequentially carrying out mixing, shearing, extruding, strip drawing, cooling and granulating on the mixture to form the degradable polyester material. The invention adds two fillers of active talcum powder and active calcium carbonate with high polarity, high performance, high fluidity, high dispersion and high lubricity into biodegradable polyester and compatilizer for blending modification, thereby obtaining the fully degradable polyester material with low cost, high performance and rapid degradation.
Description
Technical Field
The invention relates to the technical field of degradable materials, in particular to a degradable polyester material and a preparation method thereof.
Background
Biodegradable Polyester (PBAT) is a novel fully degradable polyester material. The PBAT contains flexible aliphatic chains and rigid aromatic bonds, so that the PBAT has high toughness and high temperature resistance, and the PBAT also has biodegradability due to the existence of ester bonds. But due to the existence of aromatic PBT chain segments, the degradation rate is relatively slow, the application of the aromatic PBT chain segments is limited, and the application cost is increased.
Although the existing modified degradable polyester material can meet the mechanical properties such as tensile strength or elongation, the existing modified degradable polyester material has low degradation rate, so that the production cost is high, and the large-scale production operation is not facilitated.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a degradable polyester material and a preparation method thereof, and aims to solve the problem that the existing degradable polyester material is low in degradation rate and high in production cost.
In order to achieve the purpose, the invention adopts the following technical scheme: the degradable polyester material comprises the following components in parts by weight:
filling agent: 9-30 parts of a solvent;
biodegradable polyester: 70-90 parts;
a compatilizer: 3-5 parts; and
and (5) auxiliary materials.
Preferably, the filler comprises activated talc and activated calcium carbonate.
Preferably, the active talcum powder and the active calcium carbonate comprise the following specific components in parts by weight:
active talc powder: 3-10 parts;
activated calcium carbonate: 6-20 parts.
Preferably, the auxiliary material comprises one of a mouth-opening agent, a thermal oxygen stabilizer or an antioxidant and one of an organic silicon compound or a lubricant.
Preferably, the thermal oxygen stabilizer or the antioxidant is 0.1 part by mass, the organic silicon compound or the lubricant is 0.2 part by mass, and the opening agent is 0.3 part by mass.
Preferably, the degradable polyester material is dumbbell-shaped.
The invention also provides a preparation method of the degradable polyester material, which comprises the following steps:
fully mixing the active talcum powder, the active calcium carbonate, the biodegradable polyester, the compatilizer and the auxiliary materials in a stirring pot for 5-8min to form a mixture;
and sequentially carrying out mixing, shearing, extruding, strip drawing, cooling and granulating on the mixture to form the degradable polyester material.
Preferably, the mixture is subjected to mixing, shearing, extruding, bar drawing, cooling and granulation in sequence by a double-screw extruder to form the degradable polyester material.
Preferably, the active talcum powder is prepared by performing active treatment on talcum powder by using a surfactant.
Preferably, the activated calcium carbonate is prepared by activating calcium carbonate by using a surfactant.
The beneficial effect that this scheme produced is:
the fully degradable polyester material with low cost, high performance and quick degradation is obtained by adding two fillers, namely active talcum powder and active calcium carbonate, which have high polarity, high performance, high fluidity, high dispersion and high lubricity, into the biodegradable polyester and the compatilizer for blending modification.
Detailed Description
The following describes embodiments of the present invention in detail. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
A degradable polyester material comprises the following components in parts by mass:
filling agent: 9-30 parts of a solvent;
biodegradable polyester: 70-90 parts;
a compatilizer: 3-5 parts; and
and (5) auxiliary materials.
Wherein the auxiliary material consists of one of an opening agent, a thermal oxygen stabilizer or an antioxidant and one of an organic silicon compound or a lubricant. Specifically, the content of the thermal oxygen stabilizer or the antioxidant is 0.1 part, the content of the organic silicon compound or the lubricant is 0.2 part, and the content of the opening agent is 0.3 part.
Wherein the filler comprises active talcum powder and active calcium carbonate.
The active talcum powder and the active calcium carbonate comprise the following specific components:
active talc powder: 3-10 parts;
activated calcium carbonate: 6-20 parts.
Specifically, the active talcum powder is prepared by performing active treatment on talcum powder by using a surfactant or a powder modifier.
The active calcium carbonate is prepared by carrying out active treatment on calcium carbonate by using a surfactant or a powder modifier.
The talcum powder and the calcium carbonate are subjected to active treatment by using a surfactant or a powder modifier, so that the surfactant or the powder modifier is combined with the particle surface in an adsorption or chemical bond mode, the particle surface is changed from hydrophilic to hydrophobic, new properties are endowed to the particles, and the compatibility of the particles and a polymer is improved. So as to obtain the active talcum powder and active calcium carbonate filler with high polarity, high performance, high fluidity, high dispersion and high lubricity.
The invention also provides a preparation method of the degradable polyester material, which comprises the following specific preparation steps:
step one, fully mixing the active talcum powder, the active calcium carbonate, the biodegradable polyester, the compatilizer and the auxiliary materials in a stirring pot for 5min to form a mixture. Wherein, the active talcum powder, the active calcium carbonate, the biodegradable polyester, the compatilizer and the auxiliary materials can also be fully mixed in a stirring pot for 6min or 8min to form a mixture.
And step two, sequentially carrying out mixing, shearing, extruding, strip drawing, cooling and granulating on the mixture to form the degradable polyester material.
Example one
Weighing the following components in parts by weight:
active talc powder: 10 parts.
Activated calcium carbonate: and 20 parts.
Biodegradable polyester: 70 parts of (A).
A compatilizer: and 3 parts.
The auxiliary materials are specifically as follows:
antioxidant: 0.1 part.
An organosilicon compound: 0.2 part.
An opening agent: 0.3 part.
Meanwhile, the preparation method of the invention is as follows:
fully mixing the active talcum powder, the active calcium carbonate, the biodegradable polyester, the compatilizer and the auxiliary materials in a stirring pot for 5min to form a mixture;
and sequentially mixing, shearing, extruding, drawing, cooling and granulating the mixture to form the degradable polyester material. And then the degradable polyester material is made into dumbbell-shaped sample strips for standard tensile experiments.
The performance results of the obtained degradable polyester material according to the mechanical property detection are shown in tables 1 and 2.
Example two
Weighing the following components in parts by weight:
active talc powder: 6 parts.
Activated calcium carbonate: 14 parts of (A).
Biodegradable polyester: 80 parts of the raw materials.
A compatilizer: 4 parts.
The auxiliary materials are specifically as follows:
antioxidant: 0.1 part.
An organosilicon compound: 0.2 part.
An opening agent: 0.3 part.
Meanwhile, the preparation method of the invention is as follows:
fully mixing the active talcum powder, the active calcium carbonate, the biodegradable polyester, the compatilizer and the auxiliary materials in a stirring pot for 5min to form a mixture;
and sequentially mixing, shearing, extruding, drawing, cooling and granulating the mixture to form the degradable polyester material. And then the degradable polyester material is made into dumbbell-shaped sample strips for standard tensile experiments.
The performance results of the obtained degradable polyester material according to the mechanical property detection are shown in tables 1 and 2.
EXAMPLE III
Weighing the following components in parts by weight:
active talc powder: and 3 parts.
Activated calcium carbonate: 6 parts.
Biodegradable polyester: and 90 parts.
A compatilizer: 5 parts of the raw materials.
The auxiliary materials are specifically as follows:
thermal oxygen stabilizer: 0.1 part.
Lubricant: 0.2 part.
An opening agent: 0.3 part.
Meanwhile, the preparation method of the invention is as follows:
and fully mixing the active talcum powder, the active calcium carbonate, the biodegradable polyester, the compatilizer and the auxiliary materials in a stirring pot for 5min to form a mixture.
And sequentially mixing, shearing, extruding, drawing, cooling and granulating the mixture to form the degradable polyester material. The degradable polyester material was then made into dumbbell-shaped bars for standard tensile testing.
The performance results of the obtained degradable polyester material according to the mechanical property detection are shown in tables 1 and 2.
Table 1 is a comparative table of the components with the adjuvants removed in examples one to three.
TABLE 1
Table 2 is a table of testing mechanical properties and degradation rates performed in examples one to three, wherein the standard in the testing project is an enterprise standard of eastern guan global environmental protection technology ltd.
The method for detecting the mechanical property and the degradation rate specifically comprises the following steps:
by radioactivity C14Marking method: with C14Respectively marking the detected degradable polyester material to generate CO under the action of microorganisms for 45 days2Absorption with alkaline solution and titration method for CO determination2Total amount, and measuring C by radioactive decay rate method14CO of2Amount of C14CO of2Accounting for CO produced2The percentage of (b) represents the degree of microbial attack (i.e., the degradation rate) to derive the biodegradability of the test sample.
TABLE 2
By comparing the parameter values in the first to third embodiments with the parameter values in the comparative sample, the degradable polyester material of the invention can efficiently play the synergistic effect of the two fillers of the active talcum powder and the active calcium carbonate in the product under the condition that the mechanical properties such as tensile strength, elongation and the like are well met, and the degradation rate is greatly improved.
Meanwhile, according to the comparative test, when the ratio of the active calcium carbonate to the active talcum powder is 2:1 and the sum of the active calcium carbonate and the active talcum powder accounts for about 10 percent by mass, the degradable polyester material has good mechanical property and high degradation rate. According to the preparation method, the raw materials used are few, so that the production cost is low, and the preparation method is favorable for large-scale production operation.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (10)
1. The degradable polyester material is characterized by comprising the following components in parts by weight:
filling agent: 9-30 parts of a solvent;
biodegradable polyester: 70-90 parts;
a compatilizer: 3-5 parts; and
and (5) auxiliary materials.
2. The degradable polyester material of claim 1 wherein the filler comprises activated talc and activated calcium carbonate.
3. The degradable polyester material of claim 2, wherein the active talc powder and the active calcium carbonate comprise the following specific components in parts by weight:
active talc powder: 3-10 parts;
activated calcium carbonate: 6-20 parts.
4. The degradable polyester material of claim 1 or 3, wherein the auxiliary material comprises one of a mouth-opening agent, a thermal oxygen stabilizer or an antioxidant and one of an organosilicon compound or a lubricant.
5. The degradable polyester material of claim 4, wherein the thermal oxygen stabilizer or antioxidant is 0.1 part by weight, the organic silicon compound or lubricant is 0.2 part by weight, and the opening agent is 0.3 part by weight.
6. The degradable polyester material of claim 1, wherein the degradable polyester material is dumbbell-shaped.
7. A method for preparing degradable polyester material according to any one of claims 1-6, characterized by comprising the following steps:
fully mixing a filler comprising active talcum powder and active calcium carbonate, biodegradable polyester, a compatilizer and auxiliary materials in a stirring pot for 5-8min to form a mixture;
and sequentially carrying out mixing, shearing, extruding, strip drawing, cooling and granulating on the mixture to form the degradable polyester material.
8. The method for preparing the degradable polyester material according to claim 7, wherein the mixture is subjected to mixing, shearing, extruding, drawing, cooling and granulating in sequence by using a twin-screw extruder to form the degradable polyester material.
9. The method for preparing the degradable polyester material according to claim 7, wherein the active talc powder is prepared by activating talc powder with a surfactant or a powder modifier.
10. The method for preparing a degradable polyester material according to claim 7, wherein the activated calcium carbonate is prepared by activating calcium carbonate with a surfactant or a powder modifier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111539342.7A CN114181498A (en) | 2021-12-15 | 2021-12-15 | Degradable polyester material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111539342.7A CN114181498A (en) | 2021-12-15 | 2021-12-15 | Degradable polyester material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114181498A true CN114181498A (en) | 2022-03-15 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111539342.7A Pending CN114181498A (en) | 2021-12-15 | 2021-12-15 | Degradable polyester material and preparation method thereof |
Country Status (1)
| Country | Link |
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| CN (1) | CN114181498A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2889039A1 (en) * | 2012-11-15 | 2014-05-22 | Basf Se | Biodegradable polyester mixture |
| CN104059342A (en) * | 2013-03-19 | 2014-09-24 | 上海杰事杰新材料(集团)股份有限公司 | Inorganic-filling material full-biodegradation composite material with high compatibility and preparation method thereof |
| CN111303594A (en) * | 2020-03-25 | 2020-06-19 | 贵州科泰天兴农业科技有限公司 | Full-biodegradable mulching film for cigarettes and preparation method thereof |
| CN113652063A (en) * | 2021-08-02 | 2021-11-16 | 安徽瑞鸿新材料科技有限公司 | Calcium carbonate filled PBAT/PLA degradable film and preparation method thereof |
-
2021
- 2021-12-15 CN CN202111539342.7A patent/CN114181498A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2889039A1 (en) * | 2012-11-15 | 2014-05-22 | Basf Se | Biodegradable polyester mixture |
| CN104059342A (en) * | 2013-03-19 | 2014-09-24 | 上海杰事杰新材料(集团)股份有限公司 | Inorganic-filling material full-biodegradation composite material with high compatibility and preparation method thereof |
| CN111303594A (en) * | 2020-03-25 | 2020-06-19 | 贵州科泰天兴农业科技有限公司 | Full-biodegradable mulching film for cigarettes and preparation method thereof |
| CN113652063A (en) * | 2021-08-02 | 2021-11-16 | 安徽瑞鸿新材料科技有限公司 | Calcium carbonate filled PBAT/PLA degradable film and preparation method thereof |
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