CN106117629A - A kind of degradable biological starch film of repeatable utilization - Google Patents

A kind of degradable biological starch film of repeatable utilization Download PDF

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Publication number
CN106117629A
CN106117629A CN201610601053.8A CN201610601053A CN106117629A CN 106117629 A CN106117629 A CN 106117629A CN 201610601053 A CN201610601053 A CN 201610601053A CN 106117629 A CN106117629 A CN 106117629A
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starch
film
appropriate
stirring
degradable biological
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高绍彬
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MAANSHAN WUGU POULTRY INDUSTRY SPECIALIZED COOPERATIVE
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MAANSHAN WUGU POULTRY INDUSTRY SPECIALIZED COOPERATIVE
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Priority to CN201610601053.8A priority Critical patent/CN106117629A/en
Publication of CN106117629A publication Critical patent/CN106117629A/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
    • C08L3/04—Starch derivatives, e.g. crosslinked derivatives
    • C08L3/08—Ethers
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protecting plants
    • A01G13/02—Protective coverings for plants; Coverings for the ground; Devices for laying-out or removing coverings
    • A01G13/0256—Ground coverings
    • A01G13/0268—Mats or sheets, e.g. nets or fabrics
    • A01G13/0275—Films
    • 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
    • C08B31/003—Crosslinking of starch
    • C08B31/006—Crosslinking 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
    • C08B31/08—Ethers
    • C08B31/12—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl 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
    • C08J2303/04—Starch derivatives
    • C08J2303/08—Ethers
    • 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
    • C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • 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
    • C08L2205/03—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)
  • Medicinal Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Environmental Sciences (AREA)
  • Biological Depolymerization Polymers (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

The invention discloses the degradable biological starch film of a kind of repeatable utilization, be made up of the raw material of following weight portion: butt corn starch 64 70, ethanol 23 26, chloroacetic acid 11 15, silica 14 16, epoxychloropropane 0.08 0.1, dimethylformamide 60 80, laminarin 34, glycerol 24, tributyl citrate 46, antioxidant 1010 0.2 0.3, polyvinyl alcohol 68,85% ethanol solution is appropriate, deionized water is appropriate；Starch film prepared by the present invention has all biodegradability, can avoid the conventional plastic pollution to environment, simple to soil non-hazardous, environmental protection, and preparation technology, and low cost is worthy to be popularized.

Description

A kind of degradable biological starch film of repeatable utilization
Technical field
The present invention relates to agricultural mulching technical field, particularly relate to the degradable biological starch film of a kind of repeatable utilization.
Background technology
At present, film-mulching technique is widely popularized in agricultural, be applied to Semen Tritici aestivi, Oryza sativa L., corn and soybean, In the plantation of the crop such as Sorghum vulgare Pers., Cotton Gossypii, effect of increasing production is obvious, owing to the most a large amount of mulch films used are nondegradable macromolecules Compound, neither by microbial attack, can not decompose voluntarily.If things go on like this, insoluble dirt will necessarily be brought to descendant Dye harm.Therefore, research degradable mulch gradually comes into one's own.Starch is the Renewable resource that nature is abundant, its nontoxic nothing Evil, fully biodegradable, but poor mechanical property and water resistance but limit its application.Its application is restricted. Starch is a kind of Renewable resource, and not only wide material sources are cheap, and its goods in use have the feature of environmental protection of excellence Can, can degrade rapidly after discarding, come from nature, back to nature.But, owing to starch is a kind of highly polar crystal material, Intramolecular also exists substantial amounts of hydrogen bond with intermolecular, and under generic condition, thermoplasticity is poor, it is difficult to machine-shaping, and obtained product Also exist that mechanical strength is low, poor water resistance and the shortcoming such as wet strength is low, therefore, how to improve the intensity of starch material, toughness and Water proofing property is a urgent problem of the real substituted for plastic raw material of starch based full-biodegradable material energy.By to starch Modification, starch granules expands, and structure changes, and degree of crystallinity reduces, and has certain molecular flexibility, and good film-forming property, with The compatibility of macromolecule resin improves, and is so greatly improved the performance of starch mulch film so that it is range of application is wider.
In " research of hydrophobic modification starch/PVA biodegradable plastic mulch film " literary composition, author is former with corn starch Material, through carboxymethyl etherification, the double modification of crosslinking, wherein etherification temperature is 74.44 DEG C, the molar ratio of sodium hydroxide/starch 1.85, etherification time 2.33h, concentration of alcohol is 84.65%, cross-linking modified during, use epoxychloropropane as cross-linking agent, Consumption is 0.05%, and crosslinking time is 1.0h, and sodium hydroxide concentration is 1.5%, then obtains the cross-linking carboxymethyl that thermoplasticity is stronger Starch, recycles it and is blended with PVA, and through crosslinking, speedup, hydrophobic modification, the mechanical property of film reaches standard-required, water suction Rate is substantially reduced, but its combination property does not also reach actually used needs, needs its further modification is met various making By demand, to improve the mechanical performance of starch film, toughness, intensity and other attributes, expand range of application.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that the degradable biological of a kind of repeatable utilization forms sediment Powder film.
The present invention is achieved by the following technical solutions:
The degradable biological starch film of a kind of repeatable utilization, is made up of the raw material of following weight portion: butt corn starch 64-70, ethanol 23-2 chloroacetic acid 11-15, silica 1 4-16, epoxychloropropane 0.08-0.1, dimethylformamide 60- 80, laminarin 3-4, glycerol 2-4, tributyl citrate 4-6, antioxidant 1010 0.2-0.3, polyvinyl alcohol 6-8,85% second Alcoholic solution is appropriate, deionized water is appropriate.
The degradable biological starch film of described a kind of repeatable utilization, is made up of step in detail below:
(1) by the sodium hydroxide mix homogeneously of butt corn starch and 6-10 times amount, forwarding to stir in reactor, rotating speed is 80- 100r/min, at 35 DEG C, stirring reaction 30min, after ethanol solution and chloroacetic acid mix homogeneously, is sprayed on starch surface and continues Continuous stirring 10min, after reaction terminates, is cooled to room temperature, then washs above-mentioned modified starch with 85% ethanol solution and adds appropriate Glacial acetic acid, regulation pH is 7.0, sucking filtration, continues to wash filter cake 2-3 time with 85% ethanol water, then in blast drier 50 It is dried 2-3h at DEG C, pulverizes, be sieving through 100 mesh, obtain carboxymethyl starch；
(2) carboxymethyl starch prepared by step (1) is added to furnishing slurry in alkaline solution, alkaline solution and carboxymethyl starch press Mix than ml:g1.5-2:1 according to volume mass, be subsequently placed in the thermostat water bath of 70-80 DEG C and be stirred continuously, by epoxy chloropropionate Alkane is dissolved in appropriate alkaline liquor, all instills in starch milk, react 1-3h, use hydrochloric acid conditioning solution after completion of the reaction in 3-5min Ph value to 6-7, stand a period of time, washing, sucking filtration, be placed in drying baker at 55 DEG C of dry 4h, prepare cross-linking carboxymethyl and form sediment Powder；
(3) it is added to silicon dioxide in the thionyl chloride of 2-3 times amount stir, is subsequently added the dimethyl formyl of total amount 1/3 Amine, at 70 DEG C reflux 5-7h, reaction terminate after decompression distillation, be subsequently placed in vacuum drying oven is vacuum dried at 50 DEG C standby With；It is added to the product prepared remain in dimethylformamide under the conditions of the 4s of ultrasonic 4s interval, makes dispersion liquid, then add Entering laminarin and 1ml pyridine, control temperature, at 110-120 DEG C, reacts 6-8h, and reaction is cooled to room temperature after terminating, centrifugal point From, it is washed with deionized and is dried to obtain silicon dioxide grafting laminarin the most afterwards；
(4) product prepared by step (2) is configured to the starch milk that concentration is 38-48g/L, adds product prepared by step (3) Stirring 30-40min at 95-100 DEG C, stirring adds remaining surplus materials and continues stirring 50-60min after terminating, then will mixing Emulsion is transferred to homogenizer 18000r/min homogenizing 5min, forms uniform film forming liquid, then by film forming liquid in 0.09MPa vacuum Deaerate under degree 20min, casting film-forming.
The degradable biological starch film of described a kind of repeatable utilization, described alkaline solution is by sodium hydroxide and sodium chloride Mix according to mass ratio 2-3:1, be then uniformly mixing to obtain with the deionized water dissolving of gross weight 3-4 times amount.
The invention have the advantage that the present invention utilizes corn starch for raw material, through carboxymethyl etherification, the double modification of crosslinking, make Obtaining modified corn starch, greatly add the surface group of starch, the chemical bonding effect that intermolecular existence is strong, to flowing The viscous drag produced increases, and apparent viscosity rises, and hinders rearranging and associating between straight chain molecule in gelatinized corn starch, increases The water-retaining property of starch low temperature disperse system, greatly reduces retrogradation and gel tendency, and improves light transmittance and reduce parent Aqueous, meets the crops requirement to illumination, and improves Optimality and the stability of film forming, and polysaccharide has special Long-chain helical molecular structure, stable chemical nature, filming performance is preferable, and gas barrier property is the most excellent, and moisture barrier property is poor, present invention profit By the good advantage the best with starch mixed phase capacitive of the filming performance of polysaccharide own as the modifying agent of silicon dioxide, significantly improve The features such as the tensile strength of starch film, pliability, intensity, starch film prepared by the present invention has all biodegradability, can avoid passing The system plastics pollution to environment, simple to soil non-hazardous, environmental protection, and preparation technology, low cost, it is worthy to be popularized.
Detailed description of the invention
The degradable biological starch film of a kind of repeatable utilization, is made up of the raw material of following weight portion (kilogram): dry Base corn starch 64, ethanol 23, chloroacetic acid 11, silica 14, epoxychloropropane 0.08, dimethylformamide 60, Thallus Laminariae (Thallus Eckloniae) Polysaccharide 3, glycerol 2, tributyl citrate 4, antioxidant 1010 0.2, polyvinyl alcohol 6,85% ethanol solution are appropriate, deionized water In right amount.
The degradable biological starch film of described a kind of repeatable utilization, is made up of step in detail below:
(1) by the sodium hydroxide mix homogeneously of butt corn starch and 6 times amount, forwarding to stir in reactor, rotating speed is 80r/ Min, stirring reaction 30min at 35 DEG C, after ethanol solution and chloroacetic acid mix homogeneously, be sprayed on starch surface and continue stirring 10min, after reaction terminates, is cooled to room temperature, then washs above-mentioned modified starch with 85% ethanol solution and adds appropriate ice vinegar Acid, regulation pH is 7.0, sucking filtration, continues to wash filter cake 2 times with 85% ethanol water, then dry at 50 DEG C in blast drier Dry 2h, pulverizes, is sieving through 100 mesh, obtain carboxymethyl starch；
(2) carboxymethyl starch prepared by step (1) is added to furnishing slurry in alkaline solution, alkaline solution and carboxymethyl starch press Mix than ml:g1.5:1 according to volume mass, be subsequently placed in the thermostat water bath of 70 DEG C and be stirred continuously, epoxychloropropane is dissolved In appropriate alkaline liquor, all instill in starch milk in 3min, react 1h, after completion of the reaction by the ph value of hydrochloric acid conditioning solution to 6, Stand a period of time, washing, sucking filtration, it is placed in drying baker at 55 DEG C of dry 4h, prepares crosslinked carboxymethyl fecula；
(3) it is added to silicon dioxide in the thionyl chloride of 2 times amount stir, is subsequently added the dimethylformamide of total amount 1/3, At 70 DEG C reflux 5h, reaction terminate after decompression distillation, be subsequently placed in vacuum drying oven is vacuum dried at 50 DEG C standby；Will system The standby product obtained is added to remain in dimethylformamide under the conditions of the 4s of ultrasonic 4s interval, makes dispersion liquid, adds Thallus Laminariae (Thallus Eckloniae) Polysaccharide and 1ml pyridine, control temperature at 110 DEG C, is reacted 6h, is reacted and be cooled to room temperature, centrifugation after terminating, use deionized water Washing is dried to obtain silicon dioxide grafting laminarin the most afterwards；
(4) product prepared by step (2) being configured to the starch milk that concentration is 38g/L, product prepared by addition step (3) is 95 Stirring 30min at DEG C, stirring adds remaining surplus materials and continues stirring 50min after terminating, then mixed emulsion is transferred to homogenizing Device 18000r/min homogenizing 5min, forms uniform film forming liquid, and then deaerate under 0.09MPa vacuum 20min by film forming liquid, Casting film-forming.
The degradable biological starch film of described a kind of repeatable utilization, described alkaline solution is by sodium hydroxide and sodium chloride Mix according to mass ratio 2:1, be then uniformly mixing to obtain with the deionized water dissolving of gross weight 3 times amount.
Preparing starch film according to the method for embodiment, it is carried out performance test, result is as follows:
Tensile strength (MPa): 56.1；Elongation at break (%): 378%；Light transmittance (600nm, %): 72.4；Moisture-vapor transmission (g.cm.cm-2.s-1.Pa-1): 1.80 × 10-12；Water absorption rate (%): 2.6.

Claims (3)

1. the degradable biological starch film of a repeatable utilization, it is characterised in that be made up of the raw material of following weight portion: Butt corn starch 64-70, ethanol 23-26, chloroacetic acid 11-15, silica 1 4-16, epoxychloropropane 0.08-0.1, two Methylformamide 60-80, laminarin 3-4, glycerol 2-4, tributyl citrate 4-6, antioxidant 1010 0.2-0.3, poly-second Enol 6-8,85% ethanol solution is appropriate, deionized water is appropriate.
The degradable biological starch film of a kind of repeatable utilization, it is characterised in that by detail below Step is made:
(1) by the sodium hydroxide mix homogeneously of butt corn starch and 6-10 times amount, forwarding to stir in reactor, rotating speed is 80- 100r/min, at 35 DEG C, stirring reaction 30min, after ethanol solution and chloroacetic acid mix homogeneously, is sprayed on starch surface and continues Continuous stirring 10min, after reaction terminates, is cooled to room temperature, then washs above-mentioned modified starch with 85% ethanol solution and adds appropriate Glacial acetic acid, regulation pH is 7.0, sucking filtration, continues to wash filter cake 2-3 time with 85% ethanol water, then in blast drier 50 It is dried 2-3h at DEG C, pulverizes, be sieving through 100 mesh, obtain carboxymethyl starch；
(2) carboxymethyl starch prepared by step (1) is added to furnishing slurry in alkaline solution, alkaline solution and carboxymethyl starch press Mix than ml:g1.5-2:1 according to volume mass, be subsequently placed in the thermostat water bath of 70-80 DEG C and be stirred continuously, by epoxy chloropropionate Alkane is dissolved in appropriate alkaline liquor, all instills in starch milk, react 1-3h, use hydrochloric acid conditioning solution after completion of the reaction in 3-5min Ph value to 6-7, stand a period of time, washing, sucking filtration, be placed in drying baker at 55 DEG C of dry 4h, prepare cross-linking carboxymethyl and form sediment Powder；
(3) it is added to silicon dioxide in the thionyl chloride of 2-3 times amount stir, is subsequently added the dimethyl formyl of total amount 1/3 Amine, at 70 DEG C reflux 5-7h, reaction terminate after decompression distillation, be subsequently placed in vacuum drying oven is vacuum dried at 50 DEG C standby With；It is added to the product prepared remain in dimethylformamide under the conditions of the 4s of ultrasonic 4s interval, makes dispersion liquid, then add Entering laminarin and 1ml pyridine, control temperature, at 110-120 DEG C, reacts 6-8h, and reaction is cooled to room temperature after terminating, centrifugal point From, it is washed with deionized and is dried to obtain silicon dioxide grafting laminarin the most afterwards；
(4) product prepared by step (2) is configured to the starch milk that concentration is 38-48g/L, adds product prepared by step (3) Stirring 30-40min at 95-100 DEG C, stirring adds remaining surplus materials and continues stirring 50-60min after terminating, then will mixing Emulsion is transferred to homogenizer 18000r/min homogenizing 5min, forms uniform film forming liquid, then by film forming liquid in 0.09MPa vacuum Deaerate under degree 20min, casting film-forming.
The degradable biological starch film of a kind of repeatable utilization, it is characterised in that described alkalescence is molten Liquid is to be mixed according to mass ratio 2-3:1 by sodium hydroxide and sodium chloride, then stirs with the deionized water dissolving of gross weight 3-4 times amount Mix and uniformly obtain.
CN201610601053.8A 2016-07-28 2016-07-28 A kind of degradable biological starch film of repeatable utilization Withdrawn CN106117629A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110537441A (en) * 2019-09-12 2019-12-06 西北农林科技大学 conveniently-recycled type belt-shaped agricultural mulching film made of mixed materials and using method thereof
CN110713624A (en) * 2019-11-27 2020-01-21 安徽鼎洋生物基材料有限公司 Starch-based cellulose degradable plastic film

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104098781A (en) * 2014-06-20 2014-10-15 华中农业大学 Method utilizing tabasheer waste to produce degradable liquid mulching film

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104098781A (en) * 2014-06-20 2014-10-15 华中农业大学 Method utilizing tabasheer waste to produce degradable liquid mulching film

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
曹龙奎等: ""交联羧甲基玉米淀粉/PVA复合膜制备工艺的研究"", 《包装工程》 *
王霞等: ""几种成膜助剂对CCMS/PVA可降解薄膜力学及耐水性能影响的研究"", 《黑龙江八一农垦大学学报》 *
闫美珍: ""疏水化改性淀粉/PVA生物降解塑料地膜的研究"", 《中国优秀硕士学位论文全文数据库 农业科技辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110537441A (en) * 2019-09-12 2019-12-06 西北农林科技大学 conveniently-recycled type belt-shaped agricultural mulching film made of mixed materials and using method thereof
CN110713624A (en) * 2019-11-27 2020-01-21 安徽鼎洋生物基材料有限公司 Starch-based cellulose degradable plastic film

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Application publication date: 20161116