CN108102148B - A kind of processing method of high-barrier bacteriostatic starch based composites - Google Patents
A kind of processing method of high-barrier bacteriostatic starch based composites Download PDFInfo
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/02—Applications for biomedical use
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- 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
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention discloses a kind of processing methods of high-barrier bacteriostatic starch based composites, belong to modern food processing technology field.The present invention takes off the technologies such as branch modification, poly-blended polymerization, functionalized design recombination using common starch as raw material, by enzyme process to prepare high-barrier bacteriostatic starch based composites.Simple production process of the invention, technologically advanced, highly-safe, process is easily controllable, can be continuously produced, and product can be used as Biodegradable material applied to multiple fields such as food, medicine, household chemicals.
Description
Technical field
The present invention relates to a kind of processing methods of high-barrier bacteriostatic starch based composites, belong to modern food processing technology
Field.
Background technique
Starch has cheap and easy to get, degradability and is easily transformed into shallow lake as the reproducibility resource for being only second to cellulose
The features such as powder derivative.The development and utilization research of starch resource is all attached great importance in countries in the world for a long time, particularly by various
Method is always the research hotspot of scientific worker and production firm to the modification of starch.In China, starch resource is sufficient, and 2015
Year, total starch yield was up to 21,600,000 tons, and wherein converted starch yield is only 1,350,000 tons.Compared with European and American developed countries, China
Starch deep processing level is not high, and product quality is of low grade and of less types, and the universal energy consumption of traditional processing technology is high, pollution weight
Defect.
Currently protecting environment, economizing on resources has been the basic strategy of countries in the world realization sustainable development.In Global Oil
Resource provision day is becoming tight, and environmental issue becomes increasingly conspicuous, can be again under the increasingly strong severe situation of low-carbon economy growth requirement
Bio-based materials based on production-goods source, which rapidly develop, becomes inexorable trend.Using starch biomass as the biology of raw material conversion manufacture
Sill is paid attention to extensively as international strategies new industry, by developed country, and the fast-developing impetus is presented.The U.S.
Warner-lambert company, Novamont company, Italy, St.Lawrance company, Canada, Italy Ferruzzi are public
Si Deng trans-corporation is devoted for years to the research and development in starch-based material, has pushed the commercialization process of global bio-based materials, still
China still in its infancy, compared with international most advanced level, in properties of product, manufacturing cost, key technology and industrialization
There is also gaps for scale etc..
Currently, commercialization material is mostly the petroleum base sill of high-barrier or antibacterial simple function, but high-barrier is pressed down
The report of bacterium dual function material is less, and being primarily due to antibacterial agent addition frequently can lead to barrier property reduction, thus can not shape
At high-barrier antibacterial material.As China Patent Publication No. CN104672503A discloses a kind of high barrier degradative plastics and preparation
Method forms high barrier by barrier transesterification and chain extension by Microcrystalline Starch and carboxyl end group succinic acid-butanediol ester prepolymer
Degradative plastics.China Patent Publication No. CN104893007A discloses a kind of starch-based film containing antibacterial microcapsule and its preparation
Method is that auxiliary agents, the solution curtain coatings such as the microcapsules with antibiotic property and glycerol, gelatin is added and is made at film base material with starch.Base
In above-mentioned reason, a kind of processing method of high-barrier bacteriostatic starch based composites is studied in detail in the present invention.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of processing method of high-barrier bacteriostatic starch based composites,
It uses de- branch starch, antibacterial agent, poly- polysaccharide nano-crystalline for primary raw material, enhances mechanics, the antibacterial and barrier property of material.It is special
Branch starch is not taken off and increases starch amylose content, enhances the mechanical property of materials, and the poly- polysaccharide nano-crystalline added can
To play its nano effect, so as to improve the mechanics, calorifics and barrier property of material.Simple production process of the invention, technology
It is advanced, highly-safe, process is easily controllable, can be continuously produced, product can be used as Biodegradable material applied to food, doctor
The multiple fields such as medicine, household chemicals.
The processing method of high-barrier bacteriostatic starch based composites of the invention is that starch is first prepared starch milk solution,
Then Heat Gelatinization is added debranching enzyme after cooling and is handled, and antibacterial agent is added in after treatment enzyme deactivation, and stirring, crushes at drying
Obtain composites of starch；Composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender are uniformly mixed, then one section of dry process reaction
Time to get arrive high-barrier bacteriostatic starch based composites.
In one embodiment, the starch is common starch, including cereal starch, root tuber starch or bean starch.
In one embodiment, the starch can be cornstarch, wheaten starch, potato starch, tapioca,
Sweet potato starch, pea starch etc..
In one embodiment, the concentration of the starch milk solution is 5-30% (wt/wt).
In one embodiment, after the cooling be added debranching enzyme be temperature be adjusted to 35-55 DEG C, pH value be adjusted to 3.5-
6.0 and add 0.5-10U/g starch debranching enzyme processing 3-10h.
In one embodiment, the debranching enzyme can be isoamylase, Pullulanase etc..
In one embodiment, the antibacterial agent is epsilon-polylysine, nisin, natamycin, cinnamic acid
Etc. one or more.
In one embodiment, the antibacterial agent additive amount is the 1-5% of starch quality.
It in one embodiment, is in 4-20 DEG C of stir process 5-10min, then through xeraphium after the addition antibacterial agent
It is broken.
In one embodiment, amylose content is 40-80% in the composites of starch.
In one embodiment, the poly- polysaccharide nano-crystalline is that Cellulose nanocrystal, chitin be nanocrystalline, starch nano
In crystalline substance any one or it is a variety of.
In one embodiment, the molecule outer dimension (50-200) of the poly- polysaccharide nano-crystalline × (5-30) nm.
In one embodiment, the compatible chain extender be in esterifying agent, crosslinking agent, grafting agent etc. any one or
Person is a variety of.
In one embodiment, the composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender are according to mass ratio
100:(1-10): (0.5-3) mixing.
In one embodiment, the dry process reaction is in 80-120 DEG C of kneading temperature, revolving speed 70-150r/min, pressure
5-30min is reacted under power 0.1-10MPa.
In one embodiment, the processing method specifically comprises the following steps:
(1) common starch is made into the starch milk solution that concentration is 5-30%, is cooled to 35-50 after Heat Gelatinization processing
DEG C, it adjusts pH to 3.5-6.0 and adds debranching enzyme (0.5-10U/g starch) processing 3-10h；
(2) 1-5% antibacterial agent is added after destroy the enzyme treatment and is obtained in 4-20 DEG C of stir process 5-10min, then through drying and crushing
To composites of starch；
(3) by composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender according to mass percent 100:(1-10): (0.5-
3) it is uniformly mixed, the dry process reaction 5-30min under the conditions of 80-120 DEG C, revolving speed 70-150r/min, 0.1-10MPa, fully reacting
High-barrier bacteriostatic starch based composites are obtained afterwards.
A second object of the present invention is to provide the starch-based composite materials that the above method is prepared.
Third object of the present invention is to provide the applications of the starch-based composite material.
In one embodiment, the application includes multi-field for food, medicine, household chemicals etc..
In one embodiment, the application specifically can be for can be made into degradable food packaging, bio-medical
Material, daily consumables, kitchen articles, hotel's consumables etc..
Advantages of the present invention and effect:
1, raw material of the invention is using cereal starch, potato starch, kind of starch and other plants common on domestic market
The starch in source, raw material sources extensively, are not limited by the place of production and season；
2, step of the present invention is easy, and easily operated, reaction condition is controllable, advantage of lower cost, and using cleaning green
Production technology, it is substantially pollution-free to environment.
3, development of the processing method of a kind of high-barrier bacteriostatic starch based composites of the invention for starch-based material
It is of great significance, obtained material blocks water with good, hinders oxygen and fungistatic effect, can more great Cheng as food packaging
Degree ground extends Food Shelf-life, and degradable, no pollution to the environment.Products of the present invention can be applied to food, medicine, day
With multiple fields such as chemicals, market prospects are very good, and economic benefit is wide.
4, the present invention develops environmental-friendly and recyclable bio-based materials using biomass resource abundant, meets
The strategy and policy of national sustainable development, for solving oil crisis and plastic pollution, Resources for construction economizing type and environmental-friendly
Type society is of great significance.
Specific embodiment
Mechanical performance: using TAXT2i physical property instrument, and A/TG fixture is measured.It tests measurement process and uses Button mould
Formula, distance is 25mm between Initial grip, and tensile speed is 2.00mm/s when measurement, and return speed is 10.00mm/s after survey.Every group
Sample does 5 times in parallel.Calculation formula is as follows:
In formula, L --- the length after film stretching, mm
L0--- the initial length of film, mm
In formula, F --- axial tensile force, N
The width of D --- film, mm
The thickness of d --- film, mm
Moisture-vapor transmission measuring method: according to GB-1037-70, using quasi- agar diffusion method.Under the conditions of 25 DEG C of temperature, in glass
Anhydrous calcium chloride is put into glass cup, calcium chloride is using preceding grinding and two hours dry in 200 DEG C of baking oven, and 0.5 after cooling
It is added in glass, the amount of addition is to rim of a cup 5mm.Sample to be tested measure its thickness with micrometer caliper after again by its envelope
Mouthful, weighing.By the glass after weighing be put into bottom be deionized water, temperature be 25 DEG C under the conditions of drier in (keep phase
It is 100%), to make to keep certain steam pressure difference inside and outside film to humidity, takes out weighing at regular intervals later, reaching
After stabilization, was weighed once every 2 hours, continuous five times, record the variation of weight.The calculation formula of water steaming WVP vapor permeability
It is as follows:
In formula, WVP --- moisture-vapor transmission gmm/m2·h·kPa
The increment of Δ m --- stabilised quality, g
D --- sample thickness, mm
The test area of A --- sample, m2
Δ t --- minute interval, h
The vapor pressure difference of Δ P --- sample two sides, KPa
OTR oxygen transmission rate measuring method: being measured using gas permeability tester, and test condition is 23 DEG C, 50%RH.Oxygen
The calculation formula of transmitance is as follows:
In formula, Pg--- the OTR oxygen transmission rate of material, cm3·mm/m2·h·KPa
Δ P/ Δ T --- when stablizing transmission, the arithmetic mean of instantaneous value of low pressure indoor gas variation, KPa/h in the unit time
V --- low pressure building volume, cm3
The test area of S --- sample, m2
T --- test temperature, K
Temperature (273.15K) and pressure (101.33KPa) under T0, P0 --- standard state
D --- sample thickness, mm
P1-P2--- the pressure difference of sample two sides, KPa
Antibacterial coefficient determination method: sample is respectively provided with to the test tube of 2mL Escherichia coli and staphylococcus aureus bacterium solution
In, the test tube of sample is not added as blank, 37 DEG C of constant temperature oscillations calculate colony count for 24 hours, with colony counting method.Antibiotic rate calculates
Formula is as follows:
Here is that the present invention is specifically described.
Embodiment 1
High-barrier bacteriostatic starch based composites are prepared as follows:
(1) common starch is made into the starch milk solution that concentration is 5%, is cooled to 35 DEG C after heating complete gelatinization processing,
It adjusts pH to 3.5 and adds isoamylase (0.5U/g starch) processing 3h；
(2) 1% antibacterial agent is added after destroy the enzyme treatment and in 4 DEG C of stir process 5min, then through drying and crushing to obtain starch multiple
Close object；
(3) composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender are mixed according to mass percent 100:1:0.5 equal
Even, the dry process reaction 5min under the conditions of 80 DEG C, revolving speed 70r/min, 0.1MPa obtains high-barrier bacteriostatic starch after fully reacting
Based composites.
The starch-based composite material that the present embodiment is prepared, tensile strength 7.35MPa, elongation at break 45%,
Moisture-vapor transmission is 0.387gmm/m2HkPa, OTR oxygen transmission rate 0.486cm3·mm/m2·h·kPa；Starch base
Composite material antibacterial coefficient is 45% (for 24 hours).
Embodiment 2
High-barrier bacteriostatic starch based composites are prepared as follows:
(1) common starch is made into the starch milk solution that concentration is 30%, is cooled to 55 DEG C after heating complete gelatinization processing,
It adjusts pH to 6.0 and adds Pullulanase (10U/g starch) processing 10h；
(2) 5% antibacterial agent is added after destroy the enzyme treatment and obtains starch in 20 DEG C of stir process 10min, then through drying and crushing
Compound；
(3) composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender are mixed according to mass percent 100:10:3 equal
Even, the dry process reaction 30min under the conditions of 120 DEG C, revolving speed 150r/min, 10MPa obtains the antibacterial shallow lake of high-barrier after fully reacting
Powder based composites.
The starch-based composite material that the present embodiment is prepared, tensile strength 10.10MPa, elongation at break 70%,
Moisture-vapor transmission is 0.248gmm/m2HkPa, OTR oxygen transmission rate 0.352cm3·mm/m2·h·kPa；Starch base
Composite material antibacterial coefficient is 98% (for 24 hours).
Embodiment 3
High-barrier bacteriostatic starch based composites are prepared as follows:
(1) common starch is made into the starch milk solution that concentration is 15%, is cooled to 40 DEG C after heating complete gelatinization processing,
It adjusts pH to 4.5 and adds isoamylase (5U/g starch) processing 6h；
(2) 3% antibacterial agent is added after destroy the enzyme treatment and obtains starch in 10 DEG C of stir process 10min, then through drying and crushing
Compound；
(3) composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender are uniformly mixed according to mass percent 100:5:1,
The dry process reaction 15min under the conditions of 100 DEG C, revolving speed 100r/min, 5MPa obtains high-barrier bacteriostatic starch base after fully reacting
Composite material.
The starch-based composite material that the present embodiment is prepared, tensile strength 9.32MPa, elongation at break 48%,
Moisture-vapor transmission is 0.307gmm/m2HkPa, OTR oxygen transmission rate 0.405cm3·mm/m2·h·kPa；Starch base
Composite material antibacterial coefficient is 80% (for 24 hours).
Embodiment 4
High-barrier bacteriostatic starch based composites are prepared as follows:
(1) common starch is made into the starch milk solution that concentration is 30%, is cooled to 40 DEG C after heating complete gelatinization processing,
It adjusts pH to 3.5 and adds isoamylase (2U/g starch) processing 10h；
(2) 5% antibacterial agent is added after destroy the enzyme treatment and obtains starch in 20 DEG C of stir process 10min, then through drying and crushing
Compound；
(3) composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender are mixed according to mass percent 100:10:2 equal
Even, the dry process reaction 30min under the conditions of 80 DEG C, revolving speed 100r/min, 5MPa obtains high-barrier bacteriostatic starch after fully reacting
Based composites.
The starch-based composite material that the present embodiment is prepared, tensile strength 6.86MPa, elongation at break 55%,
Moisture-vapor transmission is 0.293gmm/m2HkPa, OTR oxygen transmission rate 0.419cm3·mm/m2·h·kPa；Starch base
Composite material antibacterial coefficient is 96% (for 24 hours).
Embodiment 5
Starch-based composite material (compared with Example 1, lacking enzymatic treatment step) is prepared as follows:
(1) common starch is made into the starch milk solution that concentration is 5%, heats that add 1% after complete gelatinization processing anti-
Microbial inoculum and in 4 DEG C of stir process 5min, obtains composites of starch through drying and crushing；
(2) composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender are mixed according to mass percent 100:1:0.5 equal
Even, the dry process reaction 5min under the conditions of 80 DEG C, revolving speed 70r/min, 0.1MPa obtains high-barrier bacteriostatic starch after fully reacting
Based composites.
The starch-based composite material that the present embodiment is prepared, tensile strength 3.86MPa, elongation at break 25%,
Moisture-vapor transmission is 0.626gmm/m2HkPa, OTR oxygen transmission rate 0.749cm3·mm/m2·h·kPa；Starch base
Composite material antibacterial coefficient is 56% (for 24 hours).
Embodiment 6
Starch-based composite material (compared with other embodiments, this is pure starch-based material) is prepared as follows:
Common starch is made into the starch milk solution that concentration is 5%, 35 DEG C is cooled to after heating complete gelatinization processing, adjusts
PH to 3.5 simultaneously adds isoamylase (0.5U/g starch) processing 3h, then obtains composites of starch through drying and crushing.
The starch-based composite material that the present embodiment is prepared, tensile strength 4.15MPa, elongation at break 15%,
Moisture-vapor transmission is 1.013gmm/m2HkPa, OTR oxygen transmission rate 1.289cm3·mm/m2·h·kPa；Starch base
Composite material antibacterial coefficient is 1% (for 24 hours).
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill
The people of art can do various change and modification, therefore protection model of the invention without departing from the spirit and scope of the present invention
Enclose answer 7 this subject to the definition of the claims.
Claims (7)
1. a kind of processing method of high-barrier bacteriostatic starch based composites, which is characterized in that the method is first to match starch
Starch milk solution processed, then Heat Gelatinization, is added debranching enzyme after cooling and is handled, and antibacterial agent is added in after treatment enzyme deactivation,
Stirring, dry, crushing obtain composites of starch；Composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender are uniformly mixed, so
Reaction kettle dry process reaction is placed on for a period of time to get to high-barrier bacteriostatic starch based composites；
The mass concentration of the starch milk solution is 30%；
It is that temperature is adjusted to 35-55 DEG C, pH value is adjusted to 3.5-6.0 and adds 0.5-10U/g starch that debranching enzyme is added after the cooling
Debranching enzyme handle 3-10h；
Amylose content is 40-80% in the composites of starch；
The composites of starch, poly- polysaccharide nano-crystalline, compatible chain extender are according to mass ratio 100:(1-10): (0.5-3) mixing.
2. the method according to claim 1, wherein the dry process reaction be 80-120 DEG C of kneading temperature, turn
5-30min is reacted under fast 70-150r/min, pressure 0.1-10MPa.
3. the method according to claim 1, wherein the starch is common starch, including cereal starch, root tuber
Starch or bean starch.
4. the method according to claim 1, wherein the poly- polysaccharide nano-crystalline is Cellulose nanocrystal, crust
In the nanocrystalline, nanometer starch crystal of element any one or it is a variety of.
5. the method according to claim 1, wherein the compatible chain extender is esterifying agent, crosslinking agent, grafting agent
In any one or it is a variety of.
6. the starch-based composite material that any the method is prepared according to claim 1~5, wherein content of starch is greater than
60%.
7. the application of starch-based composite material described in claim 6, the application includes being used for food, medicine, household chemicals
Field.
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| CN111904948B (en) * | 2020-07-08 | 2022-08-19 | 中国农业科学院农业环境与可持续发展研究所 | Preparation method of cinnamaldehyde nano microsphere suspending agent |
| CN112552554B (en) * | 2020-12-09 | 2021-11-23 | 江南大学 | Processing method of self-reinforced starch-based multifunctional material |
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| CN102295827A (en) * | 2010-06-25 | 2011-12-28 | 阳新五龙兴塑业高科技材料有限公司 | Method for preparing fully biodegradable nano-composite polyester plastic |
| CN103045702A (en) * | 2012-12-11 | 2013-04-17 | 淄博兰雁集团有限责任公司 | Method for producing modified starch size through bio-enzyme |
| CN103421215A (en) * | 2013-08-20 | 2013-12-04 | 华东理工大学 | Starch composition, starch-based film, and preparation method of starch-based film |
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| CN102295827A (en) * | 2010-06-25 | 2011-12-28 | 阳新五龙兴塑业高科技材料有限公司 | Method for preparing fully biodegradable nano-composite polyester plastic |
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