CN108948680A - A kind of full biology base PBSA biodegradable plastic of starch conversion and preparation method thereof - Google Patents
A kind of full biology base PBSA biodegradable plastic of starch conversion and preparation method thereof Download PDFInfo
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- 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
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/02—Starch; Degradation products thereof, e.g. dextrin
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract
The invention discloses full biology base PBSA biodegradable plastic of a kind of starch conversion and preparation method thereof, which includes: that (1) provides full biological poly succinic acid/tetramethylene adipate (PBSA)；(2) full biological poly succinic acid/tetramethylene adipate (PBSA), starch are dried in vacuo respectively；(3) full biological poly succinic acid/tetramethylene adipate (PBSA), starch and chain extender, antioxidant, plasticizer, lubricant, heat stabilizer after drying is added in high mixer, are uniformly mixed；(4) gained mixed material is passed through into twin-screw extrusion machine extruding pelletization；(5) by the composite plastic grain carry out at a certain temperature blown film to get.Using the full biology base PBSA biodegradable plastic of starch conversion made from the method for the present invention, while degradable requirement is met after composite modified, the mechanical property of pure PBSA resin is enhanced, and effectively reduce production cost, be more advantageous to marketing.
Description
Technical field
The present invention relates to biodegradable plastic technical field more particularly to a kind of full biology base PBSA biology drops of starch conversion
Solve plastics and preparation method thereof.
Background technique
Currently, the consumption figure of plastic products is constantly increasing, and synthetic plastic is producing with the continuous development of national economy
It is played an increasingly important role in life.But can not degrade after being discarded due to most plastic products, it deposits for a long time
, constantly accumulation causes serious white pollution, and continuous with pollution is aggravated and the continuous enhancing of people's environmental consciousness,
Seeking a kind of plastic products for being not only able to satisfy people's use demand but also being able to satisfy ecological requirements seems more more and more urgent and causes
The broad interest of researcher, wherein degradable resin has become the heat of research due to its degradation characteristic and economic performance
Point,
Poly- is a kind of polyester material of complete biodegradable to succinic acid/tetramethylene adipate (PBSA), in natural item
Water and carbon dioxide can be finally degraded to by enzyme dispersion metabolism in multiple-microorganism and animal and plant body under part.Poly-succinic/
Tetramethylene adipate has the characteristic of poly adipate succinic acid ester and poly butylene succinate, existing good extension simultaneously
Property and elongation at break, also have preferably heat resistance and shock resistance, substantially improve the property of original binary polyester material
Energy.
The raw material of PBSA is succinic acid, adipic acid and butanediol respectively, and although PBSA plastics are biodegradable plastics, still
From the point of view of the process units of industrialization at present, its three kinds of raw material sources are still from being extracted by petrochemical industry,
So PBSA plastics are to consume petroleum resources and produce more carbon dioxide in process of production.The meaning of bio-based plastics
Think of is that the initial source of raw material of its plastics is naturally occurring biomass resource (animal and plant resource: straw, animal body
Deng).The low-carbon emission for following bad utilization and process of resource can be achieved.Europe have begun require to have in plastic products it is certain
Bio-based content, this trend are being more and more obvious, so the research of bio-based plastics application is just being become more and more important,
So the research and modification to biology base PBSA performance have great significance.
Starch is stored in the storage polysaccharide in cell with form of starch grains during being plant growth.It seed, stem tuber and
Content is very rich in the organs such as root tuber.Starch is a kind of bio-based materials with extensive source, it may have excellent biology
Degradation characteristic, while starch has relatively very cheap price, is had been widely used in biodegradable field at present, it is main
Wanting mode is that the mode of processing is blended with biodegradable plastic.
Summary of the invention
It is an object of the invention to provide full biology base PBSA biodegradable plastics of a kind of starch conversion and preparation method thereof.
The present invention introduces biological material starch on the basis of full biology base biodegradation material PBSA, after composite modified
While meeting degradable requirement, the mechanical property of full biology base PBSA resin is enhanced, and effectively reduce this kind
Plastics obtain cost, are allowed to be more advantageous to marketing.
To achieve the above object, the invention adopts the following technical scheme:
The first aspect of the invention is to provide a kind of preparation side of full biology base PBSA biodegradable plastic of starch conversion
Method specifically comprises the following steps:
(1) full biological poly succinic acid/tetramethylene adipate (PBSA) is provided；
(2) full biological poly succinic acid/tetramethylene adipate (PBSA), starch are dried in vacuo respectively；
(3) be added in high mixer it is dry after full biological poly succinic acid/tetramethylene adipate (PBSA), starch with
And chain extender, antioxidant, plasticizer, lubricant, heat stabilizer, it is uniformly mixed, mixed material is made；
(4) gained mixed material is passed through into twin-screw extrusion machine extruding pelletization, starch-PBSA composite plastic grain is made；
(5) the composite plastic grain is subjected to blown film at a certain temperature, prepares the full biology base PBSA biology drop of starch conversion
Solve plastics.
Further, the preparation method of the full biology base PBSA biodegradable plastic of the starch conversion, in parts by weight
Meter, the consumption proportion of each raw material are as follows:
It is further preferred that the preparation method of the full biology base PBSA biodegradable plastic of the starch conversion, by weight
The consumption proportion of number meter, each raw material is as follows:
Further more preferably, the preparation method of the full biology base PBSA biodegradable plastic of the starch conversion, is pressed
The consumption proportion of parts by weight meter, each raw material is as follows:
Further, in the preparation method of the full biology base PBSA biodegrade modeling of starch conversion, each raw material
Weight fraction is 100% calculating according to raw material effective content, and actual amount need to be converted according to the actually active content of raw material.
Further, the preparation method of the full biology base PBSA biodegradable plastic of starch conversion the step of (1)
In, full biological poly succinic acid/tetramethylene adipate (PBSA) synthesis material butanediol, adipic acid, succinic acid are to adopt
It is produced and is obtained with biology base route；The specific synthesis process of the full biological poly succinic acid/tetramethylene adipate (PBSA)
Are as follows: weigh 41.35 grams of biology base succinic acid respectively, 30.66 grams of biology base adipic acid, 90.72 grams of biology base 1,4-butanediol, two
Titanium oxide and 0.41 gram of silica composite (titanium silicon mol ratio is 8:2), 0.21 gram of triethyl phosphite and magnesium acetate
0.09 gram is added in the three-necked flask of 250mL, wherein connect stirring flatly, connects nitrogen protection flatly, another mouth connect water segregator with
And distillation column, stirring is started, heats reaction system to 130 degree, with 10 degree of heating rate heatings per minute after mashing 15 minutes
It to 235 degree, keeps the thermotonus after 140 minutes, removes water segregator and condenser pipe, connect vacuum pump interface, it is logical to close nitrogen
Road valve starts to be evacuated to absolute pressure 4000Pa or so, react 60 minutes, continues to be evacuated to the left side absolute pressure 50Pa
The right side keeps 235 degree of the reaction was continued 150 minutes getting the products.
Further, the preparation method of the full biology base PBSA biodegradable plastic of starch conversion the step of (2)
In, starch is one or more of cornstarch, tapioca, potato starch, pea starch or wheaten starch.
Further, the preparation method of the full biology base PBSA biodegradable plastic of starch conversion the step of (2)
In, drying temperature is 25~40 degrees Celsius, and drying time is 1.5h~3h, and vacuum degree is 0~5000Pa (absolute pressure)；It is preferred that
Ground, drying temperature are 28~35 degrees Celsius, and drying time is 2h~3h, and vacuum degree is 400~3000Pa (absolute pressure)；More
Preferably, drying temperature is 30~32 degrees Celsius, drying time 2.5h, and vacuum degree is 1000~1500Pa (absolute pressure).
Further, the preparation method of the full biology base PBSA biodegradable plastic of starch conversion the step of (3)
In, heat stabilizer is one of maleic anhydride, epoxidized soybean oil；Lubricant be calcium stearate, in zinc stearate or
Any one of oleamide series lubricant agent or two kinds or more mixture；Plasticizer be tributyl citrate, triethyl citrate,
The compound of any one of acetyl tri-n-butyl citrate, triacetyl glycerine, dibutyl sebacate or two kinds or more.
Further, the preparation method of the full biology base PBSA biodegradable plastic of starch conversion the step of (3)
In, antioxidant is butylated hydroxy anisole, dibutyl hydroxy toluene, butyl to biphenol, phosphorous acid benzene diisodecyl ester, season penta
Tetrol bis-phosphite, 3- (3,5- di-tert-butyl-hydroxy phenyl) propionate, (2, the 4- bis- tertiary fourths of phosphorous acid three
Base phenyl) ester, one of ten caprylate of 3,5- di-tert-butyl-hydroxy phenyl propionic acid or two or more compounds；Expand
Chain agent be hydroquinone two hydroxy ethyl ether, resorcinol dihydroxyethyl ether, bisphenol-A, ethylene glycol, 1,4- butanediol, 1,6- oneself two
One of alcohol, diethylene glycol or two or more compounds.
Further, the preparation method of the full biology base PBSA biodegradable plastic of starch conversion the step of (4)
In, extrusion temperature is 120~190 DEG C；Preferably, extrusion temperature is 130~180 DEG C；More preferably, extrusion temperature 165
~170 DEG C.
Further, the preparation method of the full biology base PBSA biodegradable plastic of starch conversion the step of (5)
In, blown film temperature is 130~160 DEG C；Preferably, blown film temperature is 135~155 DEG C；More preferably, blown film temperature is 150
~155 DEG C.
The second aspect of the invention is to provide a kind of raw using the full biology base PBSA of starch conversion of above method preparation
Object degradative plastics.
The third aspect of the invention is to provide a kind of full biology base PBSA biodegradable plastic of the starch conversion in life
It is applied in the fields such as object degradation shopping bag, refuse bag, mulch, green house of vegetables film.
The present invention by adopting the above technical scheme, compared with prior art, has the following technical effect that
Present invention employs the biomass being widely present from nature the starch for preparing to full bio-based source
PBSA Biodegradable resin, which is modified, to be modified to be prepared for the compound full biology base biodegradable plastic of starch-PBSA, can
The membrane materials such as shopping bag, refuse bag, mulch, awning film are widely used in, the film prepared relative to traditional petroleum base PBSA resin
Material reduces the consumption and carbon emission in the process of petroleum resources, effectively realizes while equally solving white pollution
Resource recycles, and complies fully with state-of-the-art environmental protection concept；The introducing of starch further promotes biology base PBSA film simultaneously
The mechanical property of material reduces the cost of material, effectively reduces marketing difficulty.
Specific embodiment
The major technique of the full biology base PBSA biodegradable plastic of starch conversion provided by the present invention and preparation method thereof
Scheme is, by introducing biological material starch on the basis of full biology base biodegradation material PBSA, to accord with after composite modified
While closing degradable requirement, the mechanical property of full biology base PBSA resin is enhanced, and effectively reduces this kind modeling
Expect to obtain cost, is allowed to be more advantageous to marketing.
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
Full biology base PBSA biodegradation material is synthesized first, in accordance with following specific method:
Succinic acid from biology base route is from Dutch Royal DSM company, the adipic acid and fourth two of biology base route
Alcohol is from BASF AG, and specific synthesis process is to weigh 41.35 grams of biology base succinic acid respectively, biology base adipic acid 30.66
Gram, 90.72 grams of biology base 1,4-butanediol, (titanium silicon mol ratio is 0.41 gram of 8:2), Asia for titanium dioxide and silica composite
0.21 gram of triethyl phosphate and 0.09 gram of magnesium acetate are added in the three-necked flask of 250mL, wherein connecing stirring flatly, are connect flatly
Nitrogen protection, another mouth connect water segregator and distillation column, start stirring, heat reaction system to 130 degree, after being beaten 15 minutes with
10 degree of heating rates per minute are warming up to 235 degree, keep the thermotonus after 140 minutes, remove water segregator and condenser pipe, connect
Upper vacuum pump interface closes channel of nitrogen valve, starts to be evacuated to absolute pressure 4000Pa or so, react 60 minutes, continues
It is evacuated to absolute pressure 50Pa or so, is kept for 235 degree the reaction was continued 150 minutes getting the products.
The preparation of 1 starch conversion PBSA biodegradable plastic of embodiment
(1) proportion (mass ratio) of raw material is as follows:
(2) it matches according to above-mentioned raw materials, is prepared using following steps:
(1) full biology base PBSA Biodegradable resin is synthesized according to the method described above；
(2) a certain amount of biology base PBSA, cornstarch are dried to 2.0h under the conditions of 25 degree, 0~5000Pa；
(3) dried biology base PBSA, cornstarch, bisphenol-A, dibutyl hydroxy toluene, lemon are added in high mixer
Lemon triethylenetetraminehexaacetic acid ester, epoxidized soybean oil, zinc stearate mix 15 minutes；
(4) gained mixed material is passed through into twin-screw extrusion machine extruding pelletization, starch-biology base PBSA composite plastic is made
Expect particle；
(5) composite plastic is passed through into blown film, can be made into various full biology base biodegradable plastic membrane materials.
The preparation of 2 starch conversion biology base PBSA biodegradable plastic of embodiment
(1) proportion (mass ratio) of raw material is as follows:
(2) it matches according to above-mentioned raw materials, is prepared using following steps:
(1) full biology base PBSA Biodegradable resin is synthesized according to the method described above；
(2) a certain amount of biology base PBSA, cornstarch are dried to 3h under the conditions of 25 degree, 0~5000Pa；
(3) dried biology base PBSA, starch, acetyl tri-n-butyl citrate, resorcinol are added in high mixer
Dihydroxyethyl ether, butyl mix biphenol, epoxidized soybean oil, calcium stearate 20 minutes；
(4) gained mixed material is passed through into twin-screw extrusion machine extruding pelletization, starch-PBSA composite plastic grain is made
Son；
(5) composite plastic is passed through into blown film, can be made into various full biology base biodegradable plastic membrane materials.
The preparation of 3 starch conversion biology base PBSA biodegradable plastic of embodiment
(1) proportion (mass ratio) of raw material is as follows:
(2) it matches according to above-mentioned raw materials, is prepared using following steps:
(1) full biology base PBSA Biodegradable resin is synthesized according to the method described above；
(2) a certain amount of biology base PBSA, tapioca are dried to 3h under the conditions of 25 degree, 0~5000Pa；
(3) biology base PBSA, tapioca, maleic anhydride, three triacetins after drying is added in high mixer
Ester, butyl mix biphenol, 1,4- butanediol, zinc stearate 25 minutes；
(4) gained mixed material is passed through into twin-screw extrusion machine extruding pelletization, starch-PBSA composite plastic grain is made；
(5) composite plastic is passed through into blown film, can be made into various full biology base biodegradable plastic membrane materials.
The preparation of 4 starch conversion biology base PBSA biodegradable plastic of embodiment
(1) proportion (mass ratio) of raw material is as follows:
(2) it matches according to above-mentioned raw materials, is prepared using following steps:
(1) full biology base PBSA Biodegradable resin is synthesized according to the method described above；
(2) a certain amount of biology base PBSA, cornstarch are dried to 3h under the conditions of 25 degree, 0~5000Pa；
(3) biology base PBSA, starch, triacetyl glycerine, bisphenol-A, phosphorous acid benzene after drying is added in high mixer
Diisodecyl ester, epoxidized soybean oil, zinc stearate mix 25 minutes；
(4) gained mixed material is passed through into twin-screw extrusion machine extruding pelletization, starch-PBSA composite plastic grain is made
Son；
(5) composite plastic is passed through into blown film, can be made into various full biology base biodegradable plastic membrane materials.
Performance test: the full biology base processed without starch conversion that will be synthesized according to method shown in [0022] content
PBSA Biodegradable resin as a comparison case 1, using universal electrical tensile testing machine (SUN500 type, by Italian GALDABINI
Company's manufacture) tensile strength of above-described embodiment 1-4,1 material of comparative example, elongation at break are measured respectively, and according to
National standard GB/T16716.7-2012 standard carries out biological compost degradation experiment to above-mentioned material, and specific test result is shown in Table an institute
Show:
The test result of one embodiment 1-4 of table, 1 material of comparative example
| Tensile strength/MPa | Elongation at break/% | 6 months compost degradation rate % | |
| Embodiment 1 | 27 | 542 | 99 |
| Embodiment 2 | 29 | 550 | 98 |
| Embodiment 3 | 32 | 562 | 98 |
| Embodiment 4 | 34 | 560 | 97 |
| Comparative example 1 | 24 | 542 | 99 |
From in above-mentioned table one using test result it can be seen that with the non-modified pure biological poly of degradable material to benzene
Dioctyl phthalate/tetramethylene adipate (PBSA) comparative example 1 is compared, basic in degradation property by the Examples 1 to 4 of starch conversion
In the case where constant, there is promotion in mechanical property by the PBSA of starch conversion, tensile strength is enhanced, wherein with
The increase of content of starch, this enhancing be more and more obvious, the above comparison can show advantage of the invention.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (10)
1. a kind of preparation method of the full biology base PBSA biodegradable plastic of starch conversion, which comprises the steps of:
(1) full biological poly succinic acid/tetramethylene adipate (PBSA) is provided；
(2) full biological poly succinic acid/tetramethylene adipate (PBSA), starch are dried in vacuo respectively；
(3) full biological poly succinic acid/tetramethylene adipate (PBSA), starch and expansion after drying is added in high mixer
Chain agent, antioxidant, plasticizer, lubricant, heat stabilizer are uniformly mixed, and mixed material is made；
(4) gained mixed material is passed through into twin-screw extrusion machine extruding pelletization, starch-PBSA composite plastic grain is made；
(5) the composite plastic grain is subjected to blown film at a certain temperature, prepares the full biology base PBSA biodegrade modeling of starch conversion
Material.
2. the preparation method of the full biology base PBSA biodegradable plastic of starch conversion according to claim 1, feature exist
According to parts by weight, the consumption proportion of each raw material is as follows:
3. the preparation method of the full biology base PBSA biodegradable plastic of starch conversion according to claim 1 or 2, feature
Be, in the step (1), full biological poly succinic acid/tetramethylene adipate (PBSA) synthesis material butanediol, oneself two
Acid, succinic acid are to be produced and obtained using biology base route；The full biological poly succinic acid/tetramethylene adipate (PBSA)
Specific synthesis process are as follows: weigh 41.35 grams of biology base succinic acid respectively, 30.66 grams of biology base adipic acid, biology base Isosorbide-5-Nitrae-fourth
90.72 grams of glycol, (titanium silicon mol ratio is 0.41 gram of 8:2), triethyl phosphite 0.21 for titanium dioxide and silica composite
Gram and 0.09 gram of magnesium acetate be added in the three-necked flask of 250mL, wherein connecing stirring flatly, connect nitrogen protection flatly, it is another
Mouthful water segregator and distillation column are connect, start stirring, heat reaction system to 130 degree, after being beaten 15 minutes per minute with 10 degree
Heating rate is warming up to 235 degree, keeps the thermotonus after 140 minutes, removes water segregator and condenser pipe, connects vacuum pump and connect
Mouthful, channel of nitrogen valve is closed, starts to be evacuated to absolute pressure 4000Pa or so, react 60 minutes, continues to be evacuated to absolutely
To pressure 50Pa or so, kept for 235 degree the reaction was continued 150 minutes getting the products.
4. the preparation method of the full biology base PBSA biodegradable plastic of starch conversion according to claim 1, feature exist
In in the step (2), starch is one in cornstarch, tapioca, potato starch, pea starch or wheaten starch
Kind is a variety of.
5. the preparation method of the full biology base PBSA biodegradable plastic of starch conversion according to claim 1 or 2, feature
Be, in the step (2), drying temperature be 25~40 degrees Celsius, drying time be 1.5h~3h, vacuum degree be 0~
5000Pa。
6. the preparation method of the full biology base PBSA biodegradable plastic of starch conversion according to claim 1 or 2, feature
It is, in the step (3), heat stabilizer is one of maleic anhydride, epoxidized soybean oil；Lubricant is stearic acid
In calcium, zinc stearate or any one of oleamide series lubricant agent or two kinds or more mixtures；Plasticizer is citric acid three
Butyl ester, triethyl citrate, any one of acetyl tri-n-butyl citrate, triacetyl glycerine, dibutyl sebacate or two
Kind or more compound.
7. the preparation method of the full biology base PBSA biodegradable plastic of starch conversion according to claim 1 or 2, feature
It is, in the step (3), antioxidant is butylated hydroxy anisole, dibutyl hydroxy toluene, butyl to biphenol, phosphorous
Sour benzene diisodecyl ester, pentaerythritol bis-phosphite, 3- (3,5- di-tert-butyl-hydroxy phenyl) propionate, Asia
One of tricresyl phosphate (2,4- di-tert-butyl-phenyl) ester, 3,5- di-tert-butyl-hydroxy phenyl propionic acid, ten caprylate or
Two or more compounds；Chain extender be hydroquinone two hydroxy ethyl ether, resorcinol dihydroxyethyl ether, bisphenol-A, ethylene glycol, 1,
One of 4- butanediol, 1,6-HD, diethylene glycol or two or more compounds.
8. the preparation method of the full biology base PBSA biodegradable plastic of starch conversion according to claim 1 or 2, feature
It is, in the step (4), extrusion temperature is 120~190 DEG C.
9. the preparation method of the full biology base PBSA biodegradable plastic of starch conversion according to claim 1 or 2, feature
It is, in the step (5), blown film temperature is 130~160 DEG C.
10. a kind of full biology base PBSA biodegradable plastic of starch conversion prepared such as any one of claim 1-9 the method.
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| CN111662537A (en) * | 2019-03-07 | 2020-09-15 | 大同股份有限公司 | Biodegradable plastic composition and method for producing the same |
| CN113444344A (en) * | 2020-03-26 | 2021-09-28 | 上海紫丹食品包装印刷有限公司 | High-temperature-resistant high-toughness full-bio-based degradable plastic and preparation method thereof |
| CN113881109A (en) * | 2020-07-01 | 2022-01-04 | 南京五瑞生物降解新材料研究院有限公司 | Multistage modified thermoplastic starch master batch and application thereof in preparation of starch-based biodegradable film |
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| CN113444344A (en) * | 2020-03-26 | 2021-09-28 | 上海紫丹食品包装印刷有限公司 | High-temperature-resistant high-toughness full-bio-based degradable plastic and preparation method thereof |
| CN113444344B (en) * | 2020-03-26 | 2023-08-18 | 上海紫丹食品包装印刷有限公司 | High-temperature-resistant high-toughness full-bio-based degradable plastic and preparation method thereof |
| CN113881109A (en) * | 2020-07-01 | 2022-01-04 | 南京五瑞生物降解新材料研究院有限公司 | Multistage modified thermoplastic starch master batch and application thereof in preparation of starch-based biodegradable film |
| CN113881109B (en) * | 2020-07-01 | 2022-12-30 | 南京五瑞生物降解新材料研究院有限公司 | Multistage modified thermoplastic starch master batch and application thereof in preparation of starch-based biodegradable film |
| US11732058B2 (en) | 2020-07-01 | 2023-08-22 | Nanjing Wurui Biodegradable New Material Research Institute Co., Ltd. | Thermoplastic starch and starch-based biodegradable film |
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Application publication date: 20181207 |