CN105885115A - Cellulose-reinforced caprolactone-starch degradable thin film and method for preparing same - Google Patents
Cellulose-reinforced caprolactone-starch degradable thin film and method for preparing same Download PDFInfo
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- CN105885115A CN105885115A CN201610477712.1A CN201610477712A CN105885115A CN 105885115 A CN105885115 A CN 105885115A CN 201610477712 A CN201610477712 A CN 201610477712A CN 105885115 A CN105885115 A CN 105885115A
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- starch
- caprolactone
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- cellulose
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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
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
-
- 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
-
- 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
- C08J2403/06—Esters
-
- 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
- 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
-
- 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
-
- 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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The invention discloses a cellulose-reinforced caprolactone-starch degradable thin film. The cellulose-reinforced caprolactone-starch degradable thin film is characterized by comprising, by weight, 100 parts of corn starch, 8-10 parts of sweet potato starch, 5-8 parts of celluloses, 2-3 parts of sodium hydroxide, 3-4 parts of urea, 80-100 parts of DMF (dimethyl formamide), 8-10 parts of acetic anhydride, 100-120 parts of pyridine, 120-150 parts of diethylene glycol dimethyl ether, 15-20 parts of sodium naphthalene solution, 5-8 parts of caprolactone, 200-300 parts of petroleum ether, 200-300 parts of tetrahydrofuran, 5-8 parts of sorbitol and an appropriate quantity of water. The cellulose-reinforced caprolactone-starch degradable thin film has the advantages that the elastic modulus and the breaking elongation of the cellulose-reinforced caprolactone-starch degradable thin film are obviously improved as compared with starch matrixes; the starch and the celluloses can be biodegraded, can come from abundant sources, are low in cost and are environmentally friendly.
Description
Technical field
The present invention relates to thin film fabrication techniques field, be specifically related to caprolactone-starch degradable that a kind of cellulose strengthens
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
Caprolactone-starch degradable thin film that cellulose strengthens and preparation method thereof.
The technical problem to be solved uses following technical scheme to realize:
Caprolactone-starch degradable thin film that a kind of cellulose strengthens, it is characterised in that it is prepared by the raw material of following weight portion
Form: corn starch 100 parts, sweet potato starch 8-10 part, cellulose 5-8 part, sodium hydroxide 2-3 part, carbamide 3-4 part, DMF 80-
100 parts, acetic anhydride 8-10 part, pyridine 100-120 part, diethylene glycol dimethyl ether 120-150 part, sodium naphthalene solution 15-20 part, in oneself
Ester 5-8 part, petroleum ether 200-300 part, oxolane 200-300 part, sorbitol 5-8 part, water are appropriate.
A kind of cellulose strengthen caprolactone-starch degradable thin film, it is characterised in that its prepared by following steps and
Become:
(1) cellulose is joined sodium hydroxide, carbamide and be equivalent to its total weight parts 10-12 times water configuration solution in,
Under ultrasonic or stirring action fully dispersed, centrifugal, washing is to neutral.
(2) sweet potato 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 at 90-100 DEG C, be poured into cold after dripping
Water precipitates, filters, wash to neutrality, be dried, for white powder material, i.e. starch acetate；
(3) 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；
(4) starch, the sorbitol that corn starch, caprolactone are grafted add the water being equivalent to corn starch weight portion 15-20 times
In, it is warming up to 90-100 DEG C, ultrasonic disperse 20-30min；Add the cellulose after step (1) processes, ultrasonic disperse 20-
30min；After vacuum outgas, by casting method film forming, at a temperature of 50-80 DEG C, take off film after drying, obtain a kind of cellulose and increase
Strong caprolactone-starch degradable thin film.
Caprolactone-starch degradable thin film that a kind of cellulose strengthens, 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.
Caprolactone-starch degradable thin film that a kind of cellulose strengthens, 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 and cellulose can be biodegradable, abundance,
Cheap, environmentally friendly；Cellulose is as reinforcer, and at starch surface grafting caprolactone, effectively facilitates cellulose
With uniformly mixing between starch, the mechanical property of raising thin film；Starch is played plasticization by the addition of sorbitol；The present invention
The plastic sheeting intensity prepared is high, low cost and biodegradable, can effectively alleviate white pollution problems.
Detailed description of the invention
Caprolactone-starch degradable thin film that the cellulose of the present embodiment strengthens, it is prepared by the raw material of following weight portion
Form: corn starch 100 parts, sweet potato starch 8 parts, cellulose 5 parts, sodium hydroxide 3 parts, 4 parts of carbamide, DMF 100 parts, acetic anhydride
8 parts, pyridine 120 parts, diethylene glycol dimethyl ether 150 parts, sodium naphthalene solution 15 parts, caprolactone 5 parts, petroleum ether 300 parts, oxolane
300 parts, sorbitol 5 parts, water appropriate.
Caprolactone-starch degradable thin film that the cellulose of the present embodiment strengthens, it is prepared from by following steps:
(1) cellulose is joined sodium hydroxide, carbamide and be equivalent to its total weight parts 10 times water configuration solution in, ultrasonic
Or fully dispersed under stirring action, centrifugal, washing is to neutral.
(2) sweet potato starch is the driest, then under conditions of stirring, it is warmed up to 130 DEG C with DMF, keep 4h, cool to
100 DEG C, dropping acetic anhydride and pyridine, continue to react 6h, cooling after dripping at 100 DEG C, be poured in cold water precipitation, filter,
Washing, to neutral, is dried, for white powder material, i.e. starch acetate；
(3) 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 100 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 110 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；
(4) corn starch, the starch of caprolactone grafting, sorbitol are added in the water being equivalent to corn starch weight portion 15 times,
It is warming up to 100 DEG C, ultrasonic disperse 30min；Add the cellulose after step (1) processes, ultrasonic disperse 30min；Through vacuum outgas
After, by casting method film forming, at a temperature of 60 DEG C, take off film after drying, the caprolactone-starch obtaining the enhancing of a kind of cellulose can drop
Degrading film.
After tested, caprolactone-starch degradable thin film that the cellulose of the present embodiment strengthens, hot strength 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. caprolactone-starch degradable thin film that a cellulose strengthens, it is characterised in that it is by the raw material system of following weight portion
For forming: corn starch 100 parts, sweet potato starch 8-10 part, cellulose 5-8 part, sodium hydroxide 2-3 part, carbamide 3-4 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, sorbitol 5-8 part, water are appropriate.
2. caprolactone-starch degradable thin film that a cellulose strengthens, it is characterised in that it is prepared from by following steps:
Cellulose is joined sodium hydroxide, carbamide and be equivalent to its total weight parts 10-12 times water configuration solution in, ultrasonic
Or fully dispersed under stirring action, centrifugal, washing is to neutral；
Sweet potato 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；
Corn starch, the starch of caprolactone grafting, sorbitol are added in the water being equivalent to corn starch weight portion 15-20 times,
It is warming up to 90-100 DEG C, ultrasonic disperse 20-30min；Add the cellulose after step (1) processes, ultrasonic disperse 20-30min；Warp
After vacuum outgas, by casting method film forming, at a temperature of 50-80 DEG C, take off film after drying, obtain the own interior of a kind of cellulose enhancing
Ester-starch degradable thin film.
3. caprolactone-starch degradable thin film that a cellulose strengthens, it is characterised in that the preparation side 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. caprolactone-starch degradable thin film that a cellulose strengthens, 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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| CN201610477712.1A CN105885115A (en) | 2016-06-24 | 2016-06-24 | Cellulose-reinforced caprolactone-starch degradable thin film and method for preparing same |
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| CN201610477712.1A CN105885115A (en) | 2016-06-24 | 2016-06-24 | Cellulose-reinforced caprolactone-starch degradable thin film and method for preparing same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106349514A (en) * | 2016-08-30 | 2017-01-25 | 安徽锦鸿环保科技有限公司 | Biodegradable film made from caprolactone and starch enhanced by mica powder and preparing method thereof |
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| CN103965519A (en) * | 2014-05-16 | 2014-08-06 | 齐鲁工业大学 | Preparation method of regenerated cellulose reinforced starch film |
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| CN105694116A (en) * | 2016-04-15 | 2016-06-22 | 上海福助工业有限公司 | Adjustable-degradation-rate natural polymer film material |
-
2016
- 2016-06-24 CN CN201610477712.1A patent/CN105885115A/en active Pending
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| CN101906220A (en) * | 2010-07-16 | 2010-12-08 | 山东农业大学 | Starch-based edible film and preparation method thereof |
| CN103012856A (en) * | 2012-12-06 | 2013-04-03 | 湖南工业大学 | Microcrystalline cellulose and polyvinyl alcohol reinforced starch-based full-biodegradable blending material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106349514A (en) * | 2016-08-30 | 2017-01-25 | 安徽锦鸿环保科技有限公司 | Biodegradable film made from caprolactone and starch enhanced by mica powder and preparing method thereof |
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Application publication date: 20160824 |