CN106243403A - A kind of tear-resistant starch degradable thin film of caprolactone grafting and preparation method thereof - Google Patents
A kind of tear-resistant starch degradable thin film of caprolactone grafting and preparation method thereof Download PDFInfo
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- CN106243403A CN106243403A CN201610755379.6A CN201610755379A CN106243403A CN 106243403 A CN106243403 A CN 106243403A CN 201610755379 A CN201610755379 A CN 201610755379A CN 106243403 A CN106243403 A CN 106243403A
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- starch
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- caprolactone
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/02—Starch; Degradation products thereof, e.g. dextrin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/02—Starch; Degradation products thereof, e.g. dextrin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/04—Starch derivatives
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
A kind of starch degradable thin film of tear-resistant caprolactone grafting, it is characterized in that, it is prepared from by the raw material of following weight portion: corn starch 100 parts, wheaten starch 8 10 parts, Polyethylene Glycol 58 parts, citrate 24 parts, 58 parts of superfine wool powder, diisocyanate 24 parts, DMF 80 100 parts, acetic anhydride 8 10 parts, pyridine 100 120 parts, diethylene glycol dimethyl ether 120 150 parts, sodium naphthalene solution 15 20 parts, caprolactone 58 parts, petroleum ether 200 300 parts, oxolane 200 300 parts, polycaprolactone 58 parts, water are appropriate.Starch of the present invention can be biodegradable, abundance, cheap, environmentally friendly；The tear-resistant starch degradable thin film heatproof of caprolactone grafting that the present invention prepares, tear-resistant, stretch-proof, and can be with complete biodegradable, non-environmental-pollution, can effectively alleviate white pollution problems.
Description
Technical field
The present invention relates to thin film fabrication techniques field, be specifically related to the starch degradable of a kind of tear-resistant caprolactone grafting
Thin film and preparation method thereof.
Technical background
Flourish along with plastics industry, the environmental pollution that waste plastic film rubbish brings also is on the rise, white
Pollute and become the environmental problem attracted attention in the whole world.Therefore, people have to go into overdrive to develop biological degredation plastic thin film,
Administer plastic refuse pollution problem brought to environment.
Starch is a kind of abundance, cheap natural macromolecular material, is also a kind of inexhaustible
Renewable resource, it can be biodegradable in a variety of environmental conditions, and final catabolite carbon dioxide and water can pass through
The photosynthesis recirculation of plant, will not cause any pollution to environment.Therefore, to be widely used in degradation plastic thin for starch
The research of film and product development, and have been achieved for great progress.
Author Song little Li, in the preparation and performance study one literary composition of starch-based degradable laminated film, utilizes starch, shell poly-
Sugar, glycerol, Paligorskite are prepared for a kind of starch-based degradable laminated film, and glycerol is starch film plasticizer, and Paligorskite changes
The mechanical property of kind starch film, the starch-based degradable laminated film of preparation has good biodegradability.
Summary of the invention
The technical problem to be solved is to provide that a kind of technique is simple, production cost is low and environment amenable
Tear-resistant starch degradable thin film of caprolactone grafting and preparation method thereof.
The technical problem to be solved uses following technical scheme to realize:
The starch degradable thin film of a kind of tear-resistant caprolactone grafting, it is characterised in that it is by the raw material system of following weight portion
For forming: corn starch 100 parts, wheaten starch 8-10 part, Polyethylene Glycol 5-8 part, citrate 2-4 part, superfine wool powder 5-8
Part, diisocyanate 2-4 part, DMF 80-100 part, acetic anhydride 8-10 part, pyridine 100-120 part, diethylene glycol dimethyl ether 120-
150 parts, sodium naphthalene solution 15-20 part, caprolactone 5-8 part, petroleum ether 200-300 part, oxolane 200-300 part, polycaprolactone
5-8 part, water are appropriate.
A kind of starch degradable thin film of tear-resistant caprolactone grafting, it is characterised in that its prepared by following steps and
Become:
(1) wheaten starch is the driest, then under conditions of stirring, it is warmed up to 130-140 DEG C with DMF, keep 4-5h, cooling
To 90-100 DEG C, dropping acetic anhydride and pyridine, continue to react 5-6h, cooling at 90-100 DEG C, be poured in cold water after dripping
Precipitation, filters, washs to neutrality, is dried, for white powder material, i.e. starch acetate；
(2) in the reactor equipped with agitator, thermometer, reflux condensing tube and logical nitrogen device, diethylene glycol dimethyl ether is added
And starch acetate, it is warmed up to 90-100 DEG C and makes it dissolve fully, be then down to room temperature, add naphthalene sodium under nitrogen protection molten
Liquid, after reacting about 15-20min, adds caprolactone, reacts 10-12h at 110-130 DEG C, and product is carried out with the petroleum ether of 1/3
After precipitation, then with oxolane dissolving, remaining petroleum ether precipitation secondary, product is white solid thing, i.e. caprolactone after drying
The starch of grafting；
(3) full and uniform mixing 2-is carried out in Polyethylene Glycol and citrate being delivered to homogenizer by automatic conveying device
3h, adds corn starch, the starch of caprolactone grafting, superfine wool powder, diisocyanate, polycaprolactone, carries out full and uniform
Mixing 5-6h, the material of mix homogeneously melt extrudes in double screw extruder；Carrying out on sharp cooling roll surface, chilling temperature is
25-30℃；70-80 DEG C, carry out under 8-10MPa preheating 40-45min after, carry out cross directional stretch, be then cooled to 25-30
DEG C shape；90-100 DEG C, preheat 30-35min under 8-10MPa, carry out longitudinal stretching, be then cooled to 25-30 DEG C
Shape；Rolling, obtains the starch degradable thin film of a kind of tear-resistant caprolactone grafting.
The starch degradable thin film of a kind of tear-resistant caprolactone grafting, it is characterised in that the system of described sodium naphthalene solution
Preparation Method is: naphthalene and metallic sodium are placed in oxolane, reacts 10-12h under room temperature and nitrogen are protected, and obtaining concentration is 0.8-
The sodium naphthalene solution of 1mol/L.
The starch degradable thin film of a kind of tear-resistant caprolactone grafting, it is characterised in that described DMF and pyridine use
Before all need to be dried through anhydrous sodium sulfate.
The invention has the beneficial effects as follows: starch of the present invention can be biodegradable, abundance, price are low
Honest and clean, environmentally friendly；The addition of superfine wool powder, utilizes the characteristics such as its grain size is little, specific surface area is big, plays starch film
To the effect strengthening and reducing fragility；Polycaprolactone can be as binding agent and plasticizer, and at starch surface grafting caprolactone,
Effectively facilitate uniformly mixing between polycaprolactone with starch, improve the mechanical property of thin film；The starch film that the present invention prepares
Heatproof, tear-resistant, stretch-proof, low cost and biodegradable, can effectively alleviate white pollution problems.
Detailed description of the invention
The starch degradable thin film of the tear-resistant caprolactone grafting of the present embodiment, it is prepared by the raw material of following weight portion
Form: corn starch 100 parts, wheaten starch 8 parts, Polyethylene Glycol 8 parts, citrate 4 parts, 8 parts of superfine wool powder, two Carbimide .s
Ester 4 parts, DMF 100 parts, acetic anhydride 8 parts, pyridine 120 parts, diethylene glycol dimethyl ether 150 parts, sodium naphthalene solution 15 parts, caprolactone 5
Part, petroleum ether 300 parts, oxolane 300 parts, polycaprolactone 5 parts, water are appropriate.
The starch degradable thin film of the tear-resistant caprolactone grafting of the present embodiment, it is prepared from by following steps:
(1) wheaten starch is the driest, then under conditions of stirring, it is warmed up to 130 DEG C with DMF, keep 4h, cool to 90 DEG C,
Dropping acetic anhydride and pyridine, continues to react 6h, cooling at 90 DEG C, is poured in cold water precipitation after dripping, filter, wash in
Property, it is dried, for white powder material, i.e. starch acetate；
(2) in the reactor equipped with agitator, thermometer, reflux condensing tube and logical nitrogen device, diethylene glycol dimethyl ether is added
And starch acetate, it is warmed up to 90 DEG C and makes it dissolve fully, be then down to room temperature, add sodium naphthalene solution under nitrogen protection, instead
Caprolactone should be added after about 20min, at 130 DEG C, react 10h, after product precipitates with the petroleum ether of 1/3, then with tetrahydrochysene
Furan dissolves, remaining petroleum ether precipitation secondary, and product is white solid thing after drying, i.e. the starch of caprolactone grafting；
(3) full and uniform mixing is carried out in Polyethylene Glycol and citrate being delivered to homogenizer by automatic conveying device
3h, adds corn starch, the starch of caprolactone grafting, superfine wool powder, diisocyanate, polycaprolactone, carries out full and uniform
Mixing 6h, the material of mix homogeneously melt extrudes in double screw extruder；Carrying out on sharp cooling roll surface, chilling temperature is 30
℃；70 DEG C, carry out under 10MPa preheating 45min after, carry out cross directional stretch, be then cooled to 30 DEG C and shape；90
DEG C, preheat 35min under 10MPa, carry out longitudinal stretching, be then cooled to 30 DEG C and shape；Rolling, obtains a kind of tear-resistant
Caprolactone grafting starch degradable thin film.
After tested, the starch degradable thin film hot strength of the tear-resistant caprolactone grafting of the present embodiment is more than 30MPa,
Elongation at break is more than 150%, and light transmittance is more than 90%, and thin film both sides temperature difference is more than 5 DEG C.
Claims (4)
1. the starch degradable thin film of a tear-resistant caprolactone grafting, it is characterised in that it is by the raw material of following weight portion
It is prepared from: corn starch 100 parts, wheaten starch 8-10 part, Polyethylene Glycol 5-8 part, citrate 2-4 part, superfine wool powder
5-8 part, diisocyanate 2-4 part, DMF 80-100 part, acetic anhydride 8-10 part, pyridine 100-120 part, diethylene glycol dimethyl ether
120-150 part, sodium naphthalene solution 15-20 part, caprolactone 5-8 part, petroleum ether 200-300 part, oxolane 200-300 part, poly-oneself
Lactone 5-8 part, water are appropriate.
2. the starch degradable thin film of a tear-resistant caprolactone grafting, it is characterised in that it is prepared from by following steps:
Wheaten starch is the driest, then under conditions of stirring, it is warmed up to 130-140 DEG C with DMF, keep 4-5h, cool to
90-100 DEG C, dropping acetic anhydride and pyridine, continue to react 5-6h, cooling after dripping at 90-100 DEG C, it is heavy to be poured in cold water
Form sediment, filter, wash to neutrality, be dried, for white powder material, i.e. starch acetate；
In the reactor equipped with agitator, thermometer, reflux condensing tube and logical nitrogen device, add diethylene glycol dimethyl ether and shallow lake
Powder acetas, is warmed up to 90-100 DEG C and makes it dissolve fully, be then down to room temperature, add sodium naphthalene solution under nitrogen protection, instead
Should add caprolactone after about 15-20min, react 10-12h at 110-130 DEG C, product precipitates with the petroleum ether of 1/3
After, then with oxolane dissolving, remaining petroleum ether precipitation secondary, product is white solid thing after drying, i.e. caprolactone grafting
Starch；
Full and uniform mixing 2-3h is carried out in Polyethylene Glycol and citrate are delivered to homogenizer by automatic conveying device,
Add corn starch, the starch of caprolactone grafting, superfine wool powder, diisocyanate, polycaprolactone, carry out full and uniform mixing
5-6h, the material of mix homogeneously melt extrudes in double screw extruder；Carrying out on sharp cooling roll surface, chilling temperature is 25-30
℃；70-80 DEG C, carry out under 8-10MPa preheating 40-45min after, carry out cross directional stretch, be then cooled to 25-30 DEG C and carry out
Sizing；90-100 DEG C, preheat 30-35min under 8-10MPa, carry out longitudinal stretching, be then cooled to 25-30 DEG C carry out fixed
Type；Rolling, obtains the starch degradable thin film of a kind of tear-resistant caprolactone grafting.
3. the starch degradable thin film of a tear-resistant caprolactone grafting, it is characterised in that the preparation of described sodium naphthalene solution
Method is: naphthalene and metallic sodium are placed in oxolane, reacts 10-12h under room temperature and nitrogen are protected, and obtaining concentration is 0.8-
The sodium naphthalene solution of 1mol/L.
4. the starch degradable thin film of a tear-resistant caprolactone grafting, it is characterised in that before described DMF and pyridine use
All need to be dried through anhydrous sodium sulfate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610755379.6A CN106243403A (en) | 2016-08-30 | 2016-08-30 | A kind of tear-resistant starch degradable thin film of caprolactone grafting and preparation method thereof |
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| CN201610755379.6A CN106243403A (en) | 2016-08-30 | 2016-08-30 | A kind of tear-resistant starch degradable thin film of caprolactone grafting and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109575576A (en) * | 2018-11-18 | 2019-04-05 | 西南交通大学 | A kind of starch-grafted isocyanates of polyurethane-- polyisocyanate polymer blend and its preparation method and application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1640919A (en) * | 2004-12-20 | 2005-07-20 | 陈明忠 | Starchlike biological degradatable plastic mother material and its preparation method |
-
2016
- 2016-08-30 CN CN201610755379.6A patent/CN106243403A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1640919A (en) * | 2004-12-20 | 2005-07-20 | 陈明忠 | Starchlike biological degradatable plastic mother material and its preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109575576A (en) * | 2018-11-18 | 2019-04-05 | 西南交通大学 | A kind of starch-grafted isocyanates of polyurethane-- polyisocyanate polymer blend and its preparation method and application |
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