CN106633210A - Preparation method for completely-biodegraded food packaging material - Google Patents
Preparation method for completely-biodegraded food packaging material Download PDFInfo
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- CN106633210A CN106633210A CN201610897052.2A CN201610897052A CN106633210A CN 106633210 A CN106633210 A CN 106633210A CN 201610897052 A CN201610897052 A CN 201610897052A CN 106633210 A CN106633210 A CN 106633210A
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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
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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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
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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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
- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/04—Starch derivatives
- C08J2403/10—Oxidised 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
- C08J2451/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2451/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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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
- C08L2205/03—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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Biochemistry (AREA)
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- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biological Depolymerization Polymers (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a preparation method for completely-biodegraded food packaging material, and belongs to the technical field of the packaging material. The preparation method comprises the following steps: taking mature loofah to prepare loofah sponge, drying to obtain powder, extracting polysaccharide from the loofah sponge powder by using the ultrasonic digestion, mixing the polysaccharide with materials, such as oxidized starch and polycaprolactone, and adding to a double-screw extruder for extruding and pelleting, and adding master batch obtained by pelleting to a film blowing machine for film-blowing to obtain the completely-biodegraded food packaging material. The prepared packaging material is capable of using the polysaccharide extracted from the loofah sponge as the raw material, and completely biodegrading after combining the oxidized starch and the polycaprolactone. The preparation method is safe and environmental, and the biodegrading speed is fast. The prepared packaging material has high tensile strength, and has extensive application prospect.
Description
Technical field
The invention discloses a kind of preparation method of complete biodegradable packaging material for food, belongs to packaging material technology neck
Domain.
Background technology
Biological packing material refers to microorganism such as bacterium, mould that a class is existed by nature also known as biodegradation material
（Fungi）With the effect of algae and cause the material of degraded, it has the characteristic that can re-use, and extensive pass was caused in recent years
Note.
Biological packing material be it is a kind of can be by the degradable material of microorganism under suitable natural environment.It is overall next
Say, the price of the plastics that these biological packing materials are commonly used than day is much higher, but they do not have any destruction to environment,
And can preferably apply in some fields such as：Shopping bag, food Package, agriculture cover film, disposable product etc..Once
These discarded objects are placed in land or marine environment, and they all can be decomposed, or change metallogenic material by microorganism.
In fact, some high-polymer moleculars are very sensitive to microbial degradation, it is blocking that these microorganism cultures secretases decompose polymer
Shape, sheet, graininess, even thoroughly decompose.If condition is adapted to the growth of antimicrobial composition（Such as：Mineral matter nutritional supply is filled
Under conditions of foot, about between 20 DEG C -60 DEG C, pH value is between 5-8 for temperature）, then will be helpful to the degraded of microorganism.I.e.
Make to be thing such as vegetables, meat and paper that some are easy to degrade, if under conditions of not having oxygen and water, they were in 20 years
Substantially can not degrade in time.So during microbial degradation macromolecular material, the surface area of material, surface
The effect of power, configuration of surface in biodegradation process is very important.Preferably biological packing material is a kind of with excellent
Good performance, it is discarded after can completely be decomposed by environmental microorganism, finally by inorganization and become Carbon cycle in nature
A part macromolecular material.
The content of the invention
Present invention mainly solves technical problem：For the hygroscopic deformation of current biological packing material, easily tear, hinder moist
The defect of energy difference, the invention provides a kind of preparation method of complete biodegradable packaging material for food, the present invention takes ripe
Sponge gourd is prepared into chalina, after being dried powder, polysaccharide is extracted to obtain from chalina powder using ultrasonic-leaching, by polysaccharide and
Extruding pelletization in double screw extruder, the master batch that granulation is obtained is added to add after the material mixings such as oxidized starch, polycaprolactone
Blown film in inflation film manufacturing machine, you can obtain complete biodegradable packaging material for food.The packaging material that the present invention is prepared are with from silk
The polysaccharide extracted in melon pulp is raw material, and after combined oxidation starch and polycaprolactone, safety and environmental protection can be degradable, degradation speed
Hurry up, and packaging material tensile strength height is obtained to obtain, be with a wide range of applications.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）The ripe sponge gourds of 200～400g are weighed, is put into after crust of pruning under the sun and is exposed to the sun 5～7 days, extruded in flesh after being exposed to the sun
Seeds of Luffa cylindrica, the chalina in mass ratio 1 of remove seed:50 add immersion in the hydrochloric acid of mass fraction 3%, take out after 5～7h of immersion, extrusion
Deionized water is rinsed 2～4 times after liquid in flesh, is shredded with scissors after rinsing, is obtained chalina fragment and is put into baking oven, 60
10～12h is dried at a temperature of～70 DEG C, 10～15min of crushing in pulverizer is put into after being dried, obtain chalina powder；
（2）By above-mentioned chalina powder in mass ratio 1:30 mix with distilled water, at a temperature of 55～60 DEG C ultrasonic-leaching 1～
2h, extraction is cooled to room temperature after terminating, and suction filtration obtains filtrate, by filtrate by volume 1:5 add the ethanol solution of mass fraction 95%
In, 5～7h is stood after 10～20min of stirring, centrifugation after standing obtains sediment, sediment is put into baking oven, 50～
6～8h is dried at a temperature of 60 DEG C, dried object is obtained；
（3）Count by weight, choose respectively 50～60 parts of above-mentioned dried objects, 15～20 parts of oxidized starch, 10～15 parts gather oneself
Lactone, 1～3 part of calcium carbonate, 1～3 part of PCL-g-GMA, 1～3 part of silane coupler KH-560,1～3 part of antioxidant 1098 and 3
～6 parts of glycerine, add in double screw extruder after stirring mixing, are 120～140 DEG C in feeding section temperature, plastify shearind section temperature
To spend for 140～150 DEG C, head temperature is 160～180 DEG C, screw speed is 120～180r/min, stock-cutter rotating speed is 100～
Extruding pelletization under conditions of 150r/min, obtains masterbatch；
（4）Masterbatch after above-mentioned granulation is added in inflation film manufacturing machine, blown film under the conditions of being heated up to 180～200 DEG C is cooled down after the completion of blown film
To room temperature simultaneously flanging, the material for obtaining is added into Bag Making Machine, you can obtain complete biodegradable packaging material for food.
The complete biodegradable packaging material for food elongation at break that the present invention is prepared is 260～380%, and stretching is strong
Spend for 23.8～28.6MPa, water vapor transmission is 1.262～2.365g.m/m2DPa, in being put into soil, in micro- life
Can degrade with 100% in degraded more than 80% in 6～8 months, 12～15 months in the presence of thing.
The invention has the beneficial effects as follows：
（1）The packaging material that the present invention is prepared with the polysaccharide that extracts from chalina as raw material, combined oxidation starch and poly-
After caprolactone, safety and environmental protection can be degradable, and degradation speed is fast；
（2）The present invention is obtained to obtain packaging material tensile strength height, is with a wide range of applications.
Specific embodiment
The ripe sponge gourds of 200～400g are weighed, is put into after crust of pruning under the sun and is exposed to the sun 5～7 days, extruded in flesh after being exposed to the sun
Seeds of Luffa cylindrica, the chalina in mass ratio 1 of remove seed:50 add immersion in the hydrochloric acid of mass fraction 3%, take out after 5～7h of immersion, extrusion
Deionized water is rinsed 2～4 times after liquid in flesh, is shredded with scissors after rinsing, is obtained chalina fragment and is put into baking oven, 60
10～12h is dried at a temperature of～70 DEG C, 10～15min of crushing in pulverizer is put into after being dried, obtain chalina powder；By above-mentioned silk
Melon pulp powder in mass ratio 1:30 mix with distilled water, 1～2h of ultrasonic-leaching at a temperature of 55～60 DEG C, and extraction is cold after terminating
But to room temperature, suction filtration obtains filtrate, by filtrate by volume 1:5 add in the ethanol solution of mass fraction 95%, stir 10～20min
5～7h is stood afterwards, and centrifugation after standing obtains sediment, sediment is put into baking oven, dry 6 at a temperature of 50～60 DEG C～
8h, obtains dried object；Count by weight, choose respectively 50～60 parts of above-mentioned dried objects, 15～20 parts of oxidized starch, 10～15 parts
Polycaprolactone, 1～3 part of calcium carbonate, 1～3 part of PCL-g-GMA, 1～3 part of silane coupler KH-560,1～3 part of antioxidant 1098
With 3～6 parts of glycerine, add after stirring mixing in double screw extruder, be 120～140 DEG C in feeding section temperature, plastify shearind section
Temperature is 140～150 DEG C, and head temperature is 160～180 DEG C, and screw speed is 120～180r/min, and stock-cutter rotating speed is 100
Extruding pelletization under conditions of～150r/min, obtains masterbatch；Masterbatch after above-mentioned granulation is added in inflation film manufacturing machine, 180～200 are heated up to
Blown film under the conditions of DEG C, is cooled to room temperature and flanging after the completion of blown film, the material for obtaining is added into Bag Making Machine, you can given birth to completely
Thing degraded packaging material for food.
Example 1
The ripe sponge gourds of 200g are weighed, is put into after crust of pruning under the sun and is exposed to the sun 5 days, Seeds of Luffa cylindrica in flesh, remove seed are extruded after being exposed to the sun
Chalina in mass ratio 1:50 add immersion in the hydrochloric acid of mass fraction 3%, take out after immersion 5h, spend after liquid in extrusion flesh
Ionized water is rinsed 2 times, is shredded with scissors after rinsing, is obtained chalina fragment and is put into baking oven, and at a temperature of 60 DEG C 10h is dried,
It is put into after drying in pulverizer and crushes 10min, obtains chalina powder；By above-mentioned chalina powder in mass ratio 1:30 and distilled water
Mixing, the ultrasonic-leaching 1h at a temperature of 55 DEG C, extraction is cooled to room temperature after terminating, and suction filtration obtains filtrate, by filtrate by volume
1:5 add in the ethanol solution of mass fraction 95%, and after stirring 10min 5h is stood, and centrifugation after standing obtains sediment, will precipitate
Thing is put into baking oven, and at a temperature of 50 DEG C 6h is dried, and obtains dried object；Count by weight, choose respectively 50 parts of above-mentioned dried objects,
15 parts of oxidized starch, 10 parts of polycaprolactones, 1 part of calcium carbonate, 1 part of PCL-g-GMA, 1 part of silane coupler KH-560,1 part of antioxygen
Agent 1098 and 3 parts of glycerine, add in double screw extruder after stirring mixing, are 120 DEG C in feeding section temperature, plastify shearind section temperature
Spend for 140 DEG C, head temperature is 160 DEG C, screw speed is 120r/min, stock-cutter rotating speed is to extrude under conditions of 100r/min
Granulation, obtains masterbatch；Masterbatch after above-mentioned granulation is added in inflation film manufacturing machine, blown film under the conditions of being heated up to 180 DEG C is cooled down after the completion of blown film
To room temperature simultaneously flanging, the material for obtaining is added into Bag Making Machine, you can obtain complete biodegradable packaging material for food.
The complete biodegradable packaging material for food elongation at break that the present invention is prepared is 260%, and tensile strength is
23.8MPa, water vapor transmission is 1.262g.m/m2DPa, in being put into soil, can be at 6 in the presence of microorganism
Moon degraded 82%, 12 months can be with 100% degraded.
Example 2
The ripe sponge gourds of 300g are weighed, is put into after crust of pruning under the sun and is exposed to the sun 6 days, Seeds of Luffa cylindrica in flesh, remove seed are extruded after being exposed to the sun
Chalina in mass ratio 1:50 add immersion in the hydrochloric acid of mass fraction 3%, take out after immersion 6h, spend after liquid in extrusion flesh
Ionized water is rinsed 3 times, is shredded with scissors after rinsing, is obtained chalina fragment and is put into baking oven, and at a temperature of 65 DEG C 11h is dried,
It is put into after drying in pulverizer and crushes 13min, obtains chalina powder；By above-mentioned chalina powder in mass ratio 1:30 and distilled water
Mixing, the ultrasonic-leaching 1.5h at a temperature of 57 DEG C, extraction is cooled to room temperature after terminating, and suction filtration obtains filtrate, and filtrate is pressed into volume
Than 1:5 add in the ethanol solution of mass fraction 95%, and after stirring 15min 6h is stood, and centrifugation after standing obtains sediment, will be heavy
Starch is put into baking oven, and at a temperature of 55 DEG C 7h is dried, and obtains dried object；Count by weight, 55 parts of above-mentioned dryings are chosen respectively
Thing, 17 parts of oxidized starch, 13 parts of polycaprolactones, 2 parts of calcium carbonate, 2 parts of PCL-g-GMA, 2 parts of silane coupler KH-560,2 parts resist
Oxygen agent 1098 and 4 parts of glycerine, add in double screw extruder after stirring mixing, are 130 DEG C in feeding section temperature, plastify shearind section
Temperature is 145 DEG C, and head temperature is 170 DEG C, and screw speed is 160r/min, and stock-cutter rotating speed is to squeeze under conditions of 125r/min
Go out granulation, obtain masterbatch；Masterbatch after above-mentioned granulation is added in inflation film manufacturing machine, blown film under the conditions of being heated up to 190 DEG C is cold after the completion of blown film
But to room temperature simultaneously flanging, the material for obtaining is added into Bag Making Machine, you can obtain complete biodegradable packaging material for food.
The complete biodegradable packaging material for food elongation at break that the present invention is prepared is 300%, and tensile strength is
25.7MPa, water vapor transmission is 1.678g.m/m2DPa, in being put into soil, can be at 7 in the presence of microorganism
Moon degraded 84%, 14 months can be with 100% degraded.
Example 3
The ripe sponge gourds of 400g are weighed, is put into after crust of pruning under the sun and is exposed to the sun 7 days, Seeds of Luffa cylindrica in flesh, remove seed are extruded after being exposed to the sun
Chalina in mass ratio 1:50 add immersion in the hydrochloric acid of mass fraction 3%, take out after immersion 7h, spend after liquid in extrusion flesh
Ionized water is rinsed 4 times, is shredded with scissors after rinsing, is obtained chalina fragment and is put into baking oven, and at a temperature of 70 DEG C 12h is dried,
It is put into after drying in pulverizer and crushes 15min, obtains chalina powder；By above-mentioned chalina powder in mass ratio 1:30 and distilled water
Mixing, the ultrasonic-leaching 2h at a temperature of 60 DEG C, extraction is cooled to room temperature after terminating, and suction filtration obtains filtrate, by filtrate by volume
1:5 add in the ethanol solution of mass fraction 95%, and after stirring 20min 7h is stood, and centrifugation after standing obtains sediment, will precipitate
Thing is put into baking oven, and at a temperature of 60 DEG C 8h is dried, and obtains dried object；Count by weight, choose respectively 60 parts of above-mentioned dried objects,
20 parts of oxidized starch, 15 parts of polycaprolactones, 3 parts of calcium carbonate, 3 parts of PCL-g-GMA, 3 parts of silane coupler KH-560,3 parts of antioxygens
Agent 1098 and 6 parts of glycerine, add in double screw extruder after stirring mixing, are 140 DEG C in feeding section temperature, plastify shearind section temperature
Spend for 150 DEG C, head temperature is 180 DEG C, screw speed is 180r/min, stock-cutter rotating speed is to extrude under conditions of 150r/min
Granulation, obtains masterbatch；Masterbatch after above-mentioned granulation is added in inflation film manufacturing machine, blown film under the conditions of being heated up to 200 DEG C is cooled down after the completion of blown film
To room temperature simultaneously flanging, the material for obtaining is added into Bag Making Machine, you can obtain complete biodegradable packaging material for food.
The complete biodegradable packaging material for food elongation at break that the present invention is prepared is 380%, and tensile strength is
28.6MPa, water vapor transmission is 2.365g.m/m2DPa, in being put into soil, can be at 8 in the presence of microorganism
Moon degraded 85%, 15 months can be with 100% degraded.
Claims (1)
1. a kind of preparation method of complete biodegradable packaging material for food, it is characterised in that concrete preparation process is：
（1）The ripe sponge gourds of 200～400g are weighed, is put into after crust of pruning under the sun and is exposed to the sun 5～7 days, extruded in flesh after being exposed to the sun
Seeds of Luffa cylindrica, the chalina in mass ratio 1 of remove seed:50 add immersion in the hydrochloric acid of mass fraction 3%, take out after 5～7h of immersion, extrusion
Deionized water is rinsed 2～4 times after liquid in flesh, is shredded with scissors after rinsing, is obtained chalina fragment and is put into baking oven, 60
10～12h is dried at a temperature of～70 DEG C, 10～15min of crushing in pulverizer is put into after being dried, obtain chalina powder；
（2）By above-mentioned chalina powder in mass ratio 1:30 mix with distilled water, at a temperature of 55～60 DEG C ultrasonic-leaching 1～
2h, extraction is cooled to room temperature after terminating, and suction filtration obtains filtrate, by filtrate by volume 1:5 add the ethanol solution of mass fraction 95%
In, 5～7h is stood after 10～20min of stirring, centrifugation after standing obtains sediment, sediment is put into baking oven, 50～
6～8h is dried at a temperature of 60 DEG C, dried object is obtained；
（3）Count by weight, choose respectively 50～60 parts of above-mentioned dried objects, 15～20 parts of oxidized starch, 10～15 parts gather oneself
Lactone, 1～3 part of calcium carbonate, 1～3 part of PCL-g-GMA, 1～3 part of silane coupler KH-560,1～3 part of antioxidant 1098 and 3
～6 parts of glycerine, add in double screw extruder after stirring mixing, are 120～140 DEG C in feeding section temperature, plastify shearind section temperature
To spend for 140～150 DEG C, head temperature is 160～180 DEG C, screw speed is 120～180r/min, stock-cutter rotating speed is 100～
Extruding pelletization under conditions of 150r/min, obtains masterbatch；
（4）Masterbatch after above-mentioned granulation is added in inflation film manufacturing machine, blown film under the conditions of being heated up to 180～200 DEG C is cooled down after the completion of blown film
To room temperature simultaneously flanging, the material for obtaining is added into Bag Making Machine, you can obtain complete biodegradable packaging material for food.
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