CN108752881A - A kind of modified polylactic acid and preparation method thereof - Google Patents
A kind of modified polylactic acid and preparation method thereof Download PDFInfo
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- CN108752881A CN108752881A CN201810312474.8A CN201810312474A CN108752881A CN 108752881 A CN108752881 A CN 108752881A CN 201810312474 A CN201810312474 A CN 201810312474A CN 108752881 A CN108752881 A CN 108752881A
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- polylactic acid
- modified polylactic
- ethyl acetate
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- polyurethane
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/06—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from hydroxycarboxylic acids
- C08G63/08—Lactones or lactides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/91—Polymers modified by chemical after-treatment
- C08G63/912—Polymers modified by chemical after-treatment derived from hydroxycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- 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
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Biological Depolymerization Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of modified polylactic acid, the formula of the modified polylactic acid includes following component：Lactic acid 50%-55%, potato starch 6%-9%, propylene 8%-12%, polyurethane 2%-6%, stannous octoate 1%-5%, ethyl acetate 2%-6%, absolute ethyl alcohol 1%-4%, remaining is washings, and the invention also discloses a kind of modified polylactic acid and preparation method thereof, which includes the following steps：S1：It quantitatively weighs, S2：Dehydration, S3：Cyclisation is handled, S4：Wash crystallization, S5：Polymerisation, S6：Cooling drying；Formula of the present invention is national regulations raw material, and the polylactic acid that the present invention prepares is highly improved, its elasticity and wearability is set to get a promotion, its article produced is set to be suitable for more occasions, and the cost of present invention preparation polylactic acid decreases, increase enterprise income, is suitble to promote.
Description
Technical field
The present invention relates to polylactic acid preparing technical field, specially a kind of modified polylactic acid.
Background technology
Plastic products are that essential but traditional plastic products generally require a century even more in people's lives
The long time could be degradable, results in serious " white pollution ", while traditional plastic raw materials derive from oil etc.
Non-renewable resources, as the traditional plastics industry of the exhaustion of fossil resources is also on the hazard, therefore Devoting Major Efforts To Developing is environmental-friendly
Biodegradable polymer substitute petroleum-based plastics product, it has also become the hot spot of current research exploitation, wherein polylactic acid
（PLA）It is very important a kind of biodegradable plastics, is the lactic acid that is refined using agricultural product corn as monomer, through chemical synthesis
Biodegradable high molecular material, have nontoxic, nonirritant, good biocompatibility, intensity high and biodegradable
And the features such as absorbing, it has a wide range of applications in packaging material, biological medicine and pharmaceuticals industry, and the degradation speed of polylactic acid
Degree is very fast, is mixed with microorganism and compound organic waste materials, and CO2 and H2O can be resolved within some months, therefore increases to poly- breast
Acids product development and application can solve " white pollution " that perplexs environmental protection for a long time, and can be held to realization
Supervention exhibition has great importance, but polylactic acid poor flexibility wear-resisting property in the market is weak so that the article that polylactic acid is produced
A variety of use occasions can not be adapted to, for this purpose, the present invention proposes a kind of modified polylactic acid.
Invention content
The purpose of the present invention is to provide a kind of modified polylactic acid, to solve the problems mentioned in the above background technology.
To achieve the above object, the present invention provides the following technical solutions：A kind of modified polylactic acid, the modified polylactic acid
Formula include following component：Lactic acid 50%-55%, potato starch 6%-9%, propylene 8%-12%, polyurethane 2%-6%, octanoic acid are sub-
Tin 1%-5%, ethyl acetate 2%-6%, absolute ethyl alcohol 1%-4%, remaining is washings.
Preferably, including lactic acid 50%, potato starch 6%, propylene 8%, polyurethane 2%, stannous octoate 1%, ethyl acetate
2%, absolute ethyl alcohol 1%, remaining is washings.
Preferably, including lactic acid 55%, potato starch 7%, propylene 12%, polyurethane 6%, stannous octoate 3%, ethyl acetate
5%, absolute ethyl alcohol 3%, remaining is washings.
Preferably, including lactic acid 52%, potato starch 9%, propylene 10%, polyurethane 3%, stannous octoate 5%, ethyl acetate
3%, absolute ethyl alcohol 4%, remaining is washings.
Preferably, including lactic acid 54%, potato starch 8%, propylene 9%, polyurethane 5%, stannous octoate 2%, ethyl acetate
4%, absolute ethyl alcohol 2%, remaining is washings.
Preferably, the purity of the lactic acid, propylene, polyurethane, stannous octoate, ethyl acetate, absolute ethyl alcohol is not less than
98%, potato starch is in powdered.
Preferably, the washings select deionized water or one kind of distilled water.
A kind of a kind of modified polylactic acid as described above and preparation method thereof, which includes the following steps：
S1：It quantitatively weighs, all raw materials is weighed according to above-mentioned component；
S2：Dehydration obtains lactic acid after weighing and is put into sealing container, connects vacuum pump, to sealing container heating
Pumping decompression is carried out to its inside simultaneously, 140 °C is gradually warming up to, is depressurized to 0.035MPa, temperature is controlled at 130-140 °
C is dehydrated, and dewatering time was controlled at 1-2 hours；
S3：Cyclisation is handled, and dewatered lactic acid is warming up to 180 °C or more, increases the air pressure of sealed container interior extremely
0.098MPa occurs being cyclized when light yellow or yellow organic liquid in container to be sealed, and cyclisation time control is in 45-
75min；
S4：Sealing container is rapidly heated to 240 °C by wash crystallization, waits for that it steams light yellow liquid, then be added washings into
Row washing, washing times are 1-2 times, and then liquid internal after washing is added ethyl acetate and is recrystallized, recrystallization
Number is 1-2 times, is then filtered with vacuum pump, obtains white clear crystal, is used in combination molecular sieve that processing is dried；
S5：White clear crystal after drying is put into sealing container and is heated slowly to 110 °C by polymerisation, is used in combination true
Sky pump is depressurized to high vacuum, and propylene, polyurethane and potato starch are sequentially added when white clear crystal starts thawing, after
Continuous heating, at 140-160 °C, heating time controlled at 4-6 hours heating and temperature control；
S6：Cooling drying, the polymer after polymerisation is cooled to room temperature, and is subsequently added into anhydrous ethylene and is carried out precipitation process,
Then ethyl acetate is added in the polymer after precipitation and carries out second of crystallization treatment, be then put into the polymer after crystallization
Processing is dried in drying box.
Compared with prior art, the beneficial effects of the invention are as follows：Formula of the present invention is national regulations raw material,
And the polylactic acid that the present invention prepares is highly improved, its elasticity and wearability is made to get a promotion, and keeps the article that it is produced suitable
Cost for more occasions, and present invention preparation polylactic acid decreases, and increases enterprise income, is suitble to promote.
Specific implementation mode
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment one
The present invention provides a kind of technical solution：The formula of a kind of modified polylactic acid, the modified polylactic acid includes following component：
Including lactic acid 50%, potato starch 6%, propylene 8%, polyurethane 2%, stannous octoate 1%, ethyl acetate 2%, absolute ethyl alcohol 1%,
Remaining is washings.
Wherein, the purity of lactic acid, propylene, polyurethane, stannous octoate, ethyl acetate, absolute ethyl alcohol is not less than 98%, horse
Bell sweet potato starch is in powdered, washings selection distilled water.
A kind of a kind of modified polylactic acid as described above and preparation method thereof, which includes the following steps：
S1：It quantitatively weighs, all raw materials is weighed according to above-mentioned component；
S2：Dehydration obtains lactic acid after weighing and is put into sealing container, connects vacuum pump, to sealing container heating
Pumping decompression is carried out to its inside simultaneously, 140 °C is gradually warming up to, is depressurized to 0.035MPa, by temperature control at 130 °C, into
Row dehydration, dewatering time were controlled at 1 hour；
S3：Cyclisation is handled, and dewatered lactic acid is warming up to 180 °C or more, increases the air pressure of sealed container interior extremely
0.098MPa occurs being cyclized when light yellow or yellow organic liquid in container to be sealed, and cyclisation time control exists
45min；
S4：Sealing container is rapidly heated to 240 °C by wash crystallization, waits for that it steams light yellow liquid, then be added washings into
Row washing, washing times are 1 time, and then liquid internal after washing is added ethyl acetate and is recrystallized, and recrystallizes number
It is 2 times, is then filtered with vacuum pump, obtain white clear crystal, molecular sieve is used in combination that processing is dried；
S5：White clear crystal after drying is put into sealing container and is heated slowly to 110 °C by polymerisation, is used in combination true
Sky pump is depressurized to high vacuum, and propylene, polyurethane and potato starch are sequentially added when white clear crystal starts thawing, after
Continuous heating, at 140 °C, heating time controlled at 4 hours heating and temperature control；
S6：Cooling drying, the polymer after polymerisation is cooled to room temperature, and is subsequently added into anhydrous ethylene and is carried out precipitation process,
Then ethyl acetate is added in the polymer after precipitation and carries out second of crystallization treatment, be then put into the polymer after crystallization
Processing is dried in drying box.
Embodiment two
The present invention provides a kind of technical solution：The formula of a kind of modified polylactic acid, the modified polylactic acid includes following component：
Including lactic acid 55%, potato starch 7%, propylene 12%, polyurethane 6%, stannous octoate 3%, ethyl acetate 5%, absolute ethyl alcohol 3%,
Remaining is washings.
Wherein, the purity of lactic acid, propylene, polyurethane, stannous octoate, ethyl acetate, absolute ethyl alcohol is not less than 98%, horse
Bell sweet potato starch is in powdered, washings selection deionized water.
A kind of a kind of modified polylactic acid as described above and preparation method thereof, which includes the following steps：
S1：It quantitatively weighs, all raw materials is weighed according to above-mentioned component；
S2：Dehydration obtains lactic acid after weighing and is put into sealing container, connects vacuum pump, to sealing container heating
Pumping decompression is carried out to its inside simultaneously, 140 °C is gradually warming up to, is depressurized to 0.035MPa, by temperature control at 133 °C, into
Row dehydration, dewatering time were controlled at 1.3 hours；
S3：Cyclisation is handled, and dewatered lactic acid is warming up to 180 °C or more, increases the air pressure of sealed container interior extremely
0.098MPa occurs being cyclized when light yellow or yellow organic liquid in container to be sealed, and cyclisation time control exists
52min；
S4：Sealing container is rapidly heated to 240 °C by wash crystallization, waits for that it steams light yellow liquid, then be added washings into
Row washing, washing times are 2 times, and then liquid internal after washing is added ethyl acetate and is recrystallized, and recrystallizes number
It is 2 times, is then filtered with vacuum pump, obtain white clear crystal, molecular sieve is used in combination that processing is dried；
S5：White clear crystal after drying is put into sealing container and is heated slowly to 110 °C by polymerisation, is used in combination true
Sky pump is depressurized to high vacuum, and propylene, polyurethane and potato starch are sequentially added when white clear crystal starts thawing, after
Continuous heating, at 145 °C, heating time controlled at 4.3 hours heating and temperature control；
S6：Cooling drying, the polymer after polymerisation is cooled to room temperature, and is subsequently added into anhydrous ethylene and is carried out precipitation process,
Then ethyl acetate is added in the polymer after precipitation and carries out second of crystallization treatment, be then put into the polymer after crystallization
Processing is dried in drying box.
Embodiment three
The present invention provides a kind of technical solution：The formula of a kind of modified polylactic acid, the modified polylactic acid includes following component：
Including lactic acid 52%, potato starch 9%, propylene 10%, polyurethane 3%, stannous octoate 5%, ethyl acetate 3%, absolute ethyl alcohol 4%,
Remaining is washings.
Wherein, the purity of lactic acid, propylene, polyurethane, stannous octoate, ethyl acetate, absolute ethyl alcohol is not less than 98%, horse
Bell sweet potato starch is in powdered, washings selection distilled water.
A kind of a kind of modified polylactic acid as described above and preparation method thereof, which includes the following steps：
S1：It quantitatively weighs, all raw materials is weighed according to above-mentioned component；
S2：Dehydration obtains lactic acid after weighing and is put into sealing container, connects vacuum pump, to sealing container heating
Pumping decompression is carried out to its inside simultaneously, 140 °C is gradually warming up to, is depressurized to 0.035MPa, by temperature control at 135 °C, into
Row dehydration, dewatering time were controlled at 1.5 hours；
S3：Cyclisation is handled, and dewatered lactic acid is warming up to 180 °C or more, increases the air pressure of sealed container interior extremely
0.098MPa occurs being cyclized when light yellow or yellow organic liquid in container to be sealed, and cyclisation time control exists
55min；
S4：Sealing container is rapidly heated to 240 °C by wash crystallization, waits for that it steams light yellow liquid, then be added washings into
Row washing, washing times are 1 time, and then liquid internal after washing is added ethyl acetate and is recrystallized, and recrystallizes number
It is 1 time, is then filtered with vacuum pump, obtain white clear crystal, molecular sieve is used in combination that processing is dried；
S5：White clear crystal after drying is put into sealing container and is heated slowly to 110 °C by polymerisation, is used in combination true
Sky pump is depressurized to high vacuum, and propylene, polyurethane and potato starch are sequentially added when white clear crystal starts thawing, after
Continuous heating, at 156 °C, heating time controlled at 5.4 hours heating and temperature control；
S6：Cooling drying, the polymer after polymerisation is cooled to room temperature, and is subsequently added into anhydrous ethylene and is carried out precipitation process,
Then ethyl acetate is added in the polymer after precipitation and carries out second of crystallization treatment, be then put into the polymer after crystallization
Processing is dried in drying box.
Example IV
The present invention provides a kind of technical solution：The formula of a kind of modified polylactic acid, the modified polylactic acid includes following component：
Including lactic acid 54%, potato starch 8%, propylene 9%, polyurethane 5%, stannous octoate 2%, ethyl acetate 4%, absolute ethyl alcohol 2%,
Remaining is washings.
Wherein, the purity of lactic acid, propylene, polyurethane, stannous octoate, ethyl acetate, absolute ethyl alcohol is not less than 98%, horse
Bell sweet potato starch is in powdered, washings selection deionized water.
A kind of a kind of modified polylactic acid as described above and preparation method thereof, which includes the following steps：
S1：It quantitatively weighs, all raw materials is weighed according to above-mentioned component；
S2：Dehydration obtains lactic acid after weighing and is put into sealing container, connects vacuum pump, to sealing container heating
Pumping decompression is carried out to its inside simultaneously, 140 °C is gradually warming up to, is depressurized to 0.035MPa, by temperature control at 139 °C, into
Row dehydration, dewatering time were controlled at 1-2 hours；
S3：Cyclisation is handled, and dewatered lactic acid is warming up to 180 °C or more, increases the air pressure of sealed container interior extremely
0.098MPa occurs being cyclized when light yellow or yellow organic liquid in container to be sealed, and cyclisation time control exists
69min；
S4：Sealing container is rapidly heated to 240 °C by wash crystallization, waits for that it steams light yellow liquid, then be added washings into
Row washing, washing times are 2 times, and then liquid internal after washing is added ethyl acetate and is recrystallized, and recrystallizes number
It is 2 times, is then filtered with vacuum pump, obtain white clear crystal, molecular sieve is used in combination that processing is dried；
S5：White clear crystal after drying is put into sealing container and is heated slowly to 110 °C by polymerisation, is used in combination true
Sky pump is depressurized to high vacuum, and propylene, polyurethane and potato starch are sequentially added when white clear crystal starts thawing, after
Continuous heating, at 158 °C, heating time controlled at 5.8 hours heating and temperature control；
S6：Cooling drying, the polymer after polymerisation is cooled to room temperature, and is subsequently added into anhydrous ethylene and is carried out precipitation process,
Then ethyl acetate is added in the polymer after precipitation and carries out second of crystallization treatment, be then put into the polymer after crystallization
Processing is dried in drying box.
By carrying out composition detection to four groups of embodiments, and one group of polypropylene is picked from the market and is compared, examine
It is as follows to survey result：
From the experimental data of upper table it is found that the 4th group of polylactic acid of this programme elasticity and wear-resisting property it is best, therefore with compared with
Good promotional value.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of modified polylactic acid, it is characterised in that：The formula of the modified polylactic acid includes following component：Lactic acid 50%-
55%, potato starch 6%-9%, propylene 8%-12%, polyurethane 2%-6%, stannous octoate 1%-5%, ethyl acetate 2%-6%, anhydrous second
Alcohol 1%-4%, remaining is washings.
2. a kind of modified polylactic acid according to claim 1, it is characterised in that：Including lactic acid 50%, potato starch
6%, propylene 8%, polyurethane 2%, stannous octoate 1%, ethyl acetate 2%, absolute ethyl alcohol 1%, remaining is washings.
3. a kind of modified polylactic acid according to claim 1, it is characterised in that：Including lactic acid 55%, potato starch
7%, propylene 12%, polyurethane 6%, stannous octoate 3%, ethyl acetate 5%, absolute ethyl alcohol 3%, remaining is washings.
4. a kind of modified polylactic acid according to claim 1, it is characterised in that：Including lactic acid 52%, potato starch
9%, propylene 10%, polyurethane 3%, stannous octoate 5%, ethyl acetate 3%, absolute ethyl alcohol 4%, remaining is washings.
5. a kind of modified polylactic acid according to claim 1, it is characterised in that：Including lactic acid 54%, potato starch
8%, propylene 9%, polyurethane 5%, stannous octoate 2%, ethyl acetate 4%, absolute ethyl alcohol 2%, remaining is washings.
6. a kind of modified polylactic acid according to claim 1, it is characterised in that：It is the lactic acid, propylene, polyurethane, pungent
The purity of sour stannous, ethyl acetate, absolute ethyl alcohol is not less than 98%, and potato starch is in powdered.
7. a kind of modified polylactic acid according to claim 1, it is characterised in that：The washings select deionized water or
One kind of person's distilled water.
8. a kind of modified polylactic acid a kind of as described in claim 1 and preparation method thereof, it is characterised in that：The preparation method
Include the following steps：
S1：It quantitatively weighs, all raw materials is weighed according to above-mentioned component；
S2：Dehydration obtains lactic acid after weighing and is put into sealing container, connects vacuum pump, to sealing container heating
Pumping decompression is carried out to its inside simultaneously, 140 °C is gradually warming up to, is depressurized to 0.035MPa, temperature is controlled at 130-140 °
C is dehydrated, and dewatering time was controlled at 1-2 hours；
S3：Cyclisation is handled, and dewatered lactic acid is warming up to 180 °C or more, increases the air pressure of sealed container interior extremely
0.098MPa occurs being cyclized when light yellow or yellow organic liquid in container to be sealed, and cyclisation time control is in 45-
75min；
S4：Sealing container is rapidly heated to 240 °C by wash crystallization, waits for that it steams light yellow liquid, then be added washings into
Row washing, washing times are 1-2 times, and then liquid internal after washing is added ethyl acetate and is recrystallized, recrystallization
Number is 1-2 times, is then filtered with vacuum pump, obtains white clear crystal, is used in combination molecular sieve that processing is dried；
S5：White clear crystal after drying is put into sealing container and is heated slowly to 110 °C by polymerisation, is used in combination true
Sky pump is depressurized to high vacuum, and propylene, polyurethane and potato starch are sequentially added when white clear crystal starts thawing, after
Continuous heating, at 140-160 °C, heating time controlled at 4-6 hours heating and temperature control；
S6：Cooling drying, the polymer after polymerisation is cooled to room temperature, and is subsequently added into anhydrous ethylene and is carried out precipitation process,
Then ethyl acetate is added in the polymer after precipitation and carries out second of crystallization treatment, be then put into the polymer after crystallization
Processing is dried in drying box.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810312474.8A CN108752881A (en) | 2018-04-09 | 2018-04-09 | A kind of modified polylactic acid and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810312474.8A CN108752881A (en) | 2018-04-09 | 2018-04-09 | A kind of modified polylactic acid and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108752881A true CN108752881A (en) | 2018-11-06 |
Family
ID=63981446
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810312474.8A Withdrawn CN108752881A (en) | 2018-04-09 | 2018-04-09 | A kind of modified polylactic acid and preparation method thereof |
Country Status (1)
| Country | Link |
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| CN (1) | CN108752881A (en) |
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2018
- 2018-04-09 CN CN201810312474.8A patent/CN108752881A/en not_active Withdrawn
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