CN106349514A - Biodegradable film made from caprolactone and starch enhanced by mica powder and preparing method thereof - Google Patents

Biodegradable film made from caprolactone and starch enhanced by mica powder and preparing method thereof Download PDF

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Publication number
CN106349514A
CN106349514A CN201610761248.9A CN201610761248A CN106349514A CN 106349514 A CN106349514 A CN 106349514A CN 201610761248 A CN201610761248 A CN 201610761248A CN 106349514 A CN106349514 A CN 106349514A
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China
Prior art keywords
starch
parts
caprolactone
mica powder
enhanced
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CN201610761248.9A
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Chinese (zh)
Inventor
严荣楼
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ANHUI JINHON GREENISM TECHNOLOGY Co Ltd
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ANHUI JINHON GREENISM TECHNOLOGY Co Ltd
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Priority to CN201610761248.9A priority Critical patent/CN106349514A/en
Publication of CN106349514A publication Critical patent/CN106349514A/en
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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
    • 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
    • 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
    • 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
    • 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

Biodegradable film made from caprolactone A biodegradable film made from caprolactone and starch enhanced by mica powder is characterized in that the film is prepared from, by weight, 100 parts of corn starch, 8-10 parts of wheat starch, 80-100 parts of DMF, 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, 4-5 parts of calcium stearate, 2-3 parts of hydroxyl-stearic acid, 5-8 parts of sorbide-2-acetat,3-5 parts of mica powder,5-8 parts of polycaprolactone, a proper amount of water. The starch, polyglycolic acid, polycaprolactone used in the invention is biodegradable, rich in resource, low in price, environment friendly. As the enhancer,the mica powder plays a role in enhancing and toughening the starch film so that the mechanical property of the starch film can be greatly improved; the biodegradable film made from caprolactone and starch enhanced by mica powder prepared by the invention is high strength, low in cost, biodegradable, and can effectively alleviate white pollution problem.

Description

Enhanced caprolactone-starch degradable thin film of a kind of mica powder and preparation method thereof
Technical field
The present invention relates to thin film fabrication techniques field is and in particular to a kind of enhanced caprolactone-starch degradable of mica powder Thin film and preparation method thereof.
Technical background
Flourishing with plastics industry, the environmental pollution that waste plastic film rubbish brings also is on the rise, white Pollution becomes 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 of starch-based degradable laminated film and performance study one literary composition, is gathered using starch, shell 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.
Content of the invention
The technical problem to be solved is to provide a kind of process is simple, low production cost and environment amenable The enhanced caprolactone of mica powder-starch degradable thin film and preparation method thereof.
The technical problem to be solved to be realized using following technical scheme:
A kind of enhanced caprolactone-starch degradable thin film of mica powder it is characterised in that its by following weight portion raw material preparation Form: 100 parts of corn starch, wheaten starch 8-10 part, dmf 80-100 part, acetic anhydride 8-10 part, pyridine 100-120 part, two 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, calcium stearate 4-5 part, hydroxy stearic acid 2-3 part, acetic acid sorbitol ester 5-8 part, mica powder 3-5 part, PVOH Sour 10-15 part, polycaprolactone 5-8 part, appropriate amount of water.
A kind of enhanced caprolactone-starch degradable thin film of mica powder it is characterised in that its prepared by following steps and Become:
(1) sweet potato starch is fully dry, then it is warmed up to 130-140 DEG C with dmf under conditions of stirring, keep 4-5h, cooling To 90-100 DEG C, Deca acetic anhydride and pyridine, continue to react 5-6h, cooling at 90-100 DEG C, are poured in cold water after dripping Precipitation, filters, washs to neutrality, be dried, be white powder material, i.e. starch acetate；
(2) equipped with agitator, the reactor of thermometer, reflux condensing tube and logical nitrogen device, add diethylene glycol dimethyl ether And starch acetate, being warmed up to 90-100 DEG C makes it dissolve fully, is then down to room temperature, adds naphthalene sodium molten under nitrogen protection Liquid, after reaction about 15-20min, adds caprolactone, reacts 10-12h at 110-130 DEG C, and product is carried out with 1/3 petroleum ether After precipitation more secondary with oxolane dissolving, remaining petroleum ether precipitation, be white solid thing after product is dry, i.e. caprolactone The starch of grafting；
(3) by corn starch, the starch of caprolactone grafting, calcium stearate, hydroxy stearic acid, acetic acid sorbitol ester, mica powder, gather Glycolic, polycaprolactone add mix homogeneously in high-speed mixer, put into after carrying out in comminutor kneading, melt, extrude, cooling down Pelletizing；It is added to making thin film in inflation film manufacturing machine, obtain a kind of enhanced caprolactone of mica powder-starch degradable thin film.
A kind of enhanced caprolactone-starch degradable thin film of mica powder is it is characterised in that the preparation of described sodium naphthalene solution Method is: naphthalene and metallic sodium is placed in oxolane, in room temperature and nitrogen protection lower reaction 10-12h, obtaining concentration is 0.8- The sodium naphthalene solution of 1mol/l.
A kind of enhanced caprolactone-starch degradable thin film of mica powder is it is characterised in that described dmf and pyridine use Front all need to be dried through anhydrous sodium sulfate.
The invention has the beneficial effects as follows: starch of the present invention, polyglycolic acid and polycaprolactone can be dropped by biology Solution, abundance, cheap, environmentally friendly；Mica powder, as reinforcing agent, has enhancing and toughness reinforcing work to starch film With mechanical property can be made to be greatly enhanced；The addition of acetic acid sorbitol ester plays plasticization to starch；Hydroxyl is hard Fat acid and calcium stearate, as lubricant, play lubrication；Starch film intensity that the present invention is obtained is high, low cost and can giving birth to Thing is degraded, and can effectively alleviate white pollution problems.
Specific embodiment
The enhanced caprolactone of the mica powder-starch degradable thin film of the present embodiment, it is by the raw material preparation of following weight portion Form: 100 parts of corn starch, 8 parts of wheaten starch, 100 parts of dmf, 8 parts of acetic anhydride, 120 parts of pyridine, diethylene glycol dimethyl ether 150 parts, 15 parts of sodium naphthalene solution, 5 parts of caprolactone, 300 parts of petroleum ether, 300 parts of oxolane, 4 parts of calcium stearate, hydroxy stearic acid 3 parts, 5 parts of acetic acid sorbitol ester, 5 parts of mica powder, 10 parts of polyglycolic acid, 5 parts of polycaprolactone, appropriate amount of water.
The enhanced caprolactone of the mica powder-starch degradable thin film of the present embodiment, it is prepared from by following steps:
(1) sweet potato starch is fully dry, then it is warmed up to 130 DEG C with dmf under conditions of stirring, keep 4h, cool to 100 DEG C, Deca acetic anhydride and pyridine, continue to react 5h, cooling at 100 DEG C, are poured into precipitation in cold water, filter, washing after dripping To neutral, be dried, be white powder material, i.e. starch acetate；
(2) equipped with agitator, the reactor of thermometer, reflux condensing tube and logical nitrogen device, add diethylene glycol dimethyl ether And starch acetate, being warmed up to 90 DEG C makes it dissolve fully, is then down to room temperature, adds sodium naphthalene solution under nitrogen protection, instead Caprolactone should be added after about 20min, react 12h at 110 DEG C, after product is precipitated with 1/3 petroleum ether, then with tetrahydrochysene Furan dissolving, remaining petroleum ether precipitation are secondary, are white solid thing after product is dry, i.e. the starch of caprolactone grafting；
(3) by corn starch, the starch of caprolactone grafting, calcium stearate, hydroxy stearic acid, acetic acid sorbitol ester, mica powder, gather Glycolic, polycaprolactone add mix homogeneously in high-speed mixer, put into after carrying out in comminutor kneading, melt, extrude, cooling down Pelletizing；It is added to making thin film in inflation film manufacturing machine, obtain a kind of enhanced caprolactone of mica powder-starch degradable thin film.
After tested, the enhanced caprolactone of the mica powder of the present embodiment-starch degradable thin film, tensile 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. a kind of enhanced caprolactone-starch degradable thin film of mica powder it is characterised in that its by following weight portion raw material system Standby form: 100 parts of corn starch, wheaten starch 8-10 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, calcium stearate 4-5 part, hydroxy stearic acid 2-3 part, acetic acid sorbitol ester 5-8 part, mica powder 3-5 part, PVOH Sour 10-15 part, polycaprolactone 5-8 part, appropriate amount of water.
2. a kind of enhanced caprolactone-starch degradable thin film of mica powder is it is characterised in that it is prepared from by following steps:
Sweet potato starch is fully dry, then it is warmed up to 130-140 DEG C with dmf under conditions of stirring, keep 4-5h, cool to 90-100 DEG C, Deca acetic anhydride and pyridine, continue to react 5-6h, cooling at 90-100 DEG C, it is heavy to be poured in cold water after dripping Form sediment, filter, wash to neutrality, be dried, be white powder material, i.e. starch acetate；
Equipped with agitator, the reactor of thermometer, reflux condensing tube and logical nitrogen device, add diethylene glycol dimethyl ether and shallow lake Powder acetass, being warmed up to 90-100 DEG C makes it dissolve fully, is then down to room temperature, adds sodium naphthalene solution under nitrogen protection, instead Caprolactone should be added after about 15-20min, react 10-12h at 110-130 DEG C, product is precipitated with 1/3 petroleum ether Afterwards, more secondary with oxolane dissolving, remaining petroleum ether precipitation, be white solid thing after product is dry, i.e. caprolactone grafting Starch；
By corn starch, the starch of caprolactone grafting, calcium stearate, hydroxy stearic acid, acetic acid sorbitol ester, mica powder, poly- second Alkyd, polycaprolactone add mix homogeneously in high-speed mixer, put into carry out in comminutor kneading, melt, extrude, cool down after cut Grain；It is added to making thin film in inflation film manufacturing machine, obtain a kind of enhanced caprolactone of mica powder-starch degradable thin film.
3. a kind of enhanced caprolactone-starch degradable thin film of mica powder is it is characterised in that the preparation side of described sodium naphthalene solution Method is: naphthalene and metallic sodium is placed in oxolane, in room temperature and nitrogen protection lower reaction 10-12h, obtaining concentration is 0.8- The sodium naphthalene solution of 1mol/l.
4. a kind of enhanced caprolactone-starch degradable thin film of mica powder is it is characterised in that described dmf and pyridine are using front All need to be dried through anhydrous sodium sulfate.
CN201610761248.9A 2016-08-30 2016-08-30 Biodegradable film made from caprolactone and starch enhanced by mica powder and preparing method thereof Pending CN106349514A (en)

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CN105885114A (en) * 2016-06-24 2016-08-24 安徽德琳环保发展（集团）有限公司 Silica-enhanced caprolactone-starch degradable thin film and preparation method thereof
CN105885116A (en) * 2016-06-24 2016-08-24 安徽德琳环保发展（集团）有限公司 Polylactic acid-caprolactone-starch extrusion blown film and preparation method thereof
CN105885115A (en) * 2016-06-24 2016-08-24 安徽德琳环保发展（集团）有限公司 Cellulose-reinforced caprolactone-starch degradable thin film and method for preparing same

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101792591A (en) * 2009-12-30 2010-08-04 中国科学院广州化学研究所 Full-biodegradable plastic film and preparation method thereof
CN103627153A (en) * 2012-08-20 2014-03-12 上海杰事杰新材料(集团)股份有限公司 Entire biodegradation PLA/PBAT composite material and preparing method therefor
CN105885114A (en) * 2016-06-24 2016-08-24 安徽德琳环保发展（集团）有限公司 Silica-enhanced caprolactone-starch degradable thin film and preparation method thereof
CN105885116A (en) * 2016-06-24 2016-08-24 安徽德琳环保发展（集团）有限公司 Polylactic acid-caprolactone-starch extrusion blown film and preparation method thereof
CN105885115A (en) * 2016-06-24 2016-08-24 安徽德琳环保发展（集团）有限公司 Cellulose-reinforced caprolactone-starch degradable thin film and method for preparing same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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