CN109111667A - A kind of degradable, high moisture-inhibiting preservative film and preparation method thereof - Google Patents
A kind of degradable, high moisture-inhibiting preservative film and preparation method thereof Download PDFInfo
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- CN109111667A CN109111667A CN201810978459.7A CN201810978459A CN109111667A CN 109111667 A CN109111667 A CN 109111667A CN 201810978459 A CN201810978459 A CN 201810978459A CN 109111667 A CN109111667 A CN 109111667A
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C08K5/00—Use of organic ingredients
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- C08K5/098—Metal salts of carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a kind of degradable, high moisture-inhibiting preservative film and preparation method thereof, the preservative film of preparation has good mechanical property, and its rate of perviousness is higher, and fresh-keeping effect can extend 15 days or so, and degradation property is preferable.It using mustard oil processing tealeaf residue, can not only make tealeaf residue smooth phozy, promote its dispersion in the substrate to increase the action time of mustard oil moreover, tealeaf residue can largely adsorb mustard oil, to extend the fresh-keeping effect of preservative film；Kaolin, precipitated calcium carbonate can be made to be more fully mixed using oleamide, improve reunion degree, improve the mechanical property of preservative film.
Description
Technical field
The invention belongs to fresh-keeping technical field of membrane, especially a kind of degradable, high moisture-inhibiting preservative film and preparation method thereof.
Background technique
Respiration is continued to after fresh fruit picking, nutritional ingredient aoxidizes, and releases heat, generates moisture, two
The metabolites such as carbonoxide, ethylene are formed by closed environment in common freshness protection package, breathe ethylene, the titanium dioxide of generation
Carbon and moisture cannot be rejected to the external world in time, can be enriched in freshness protection package, to form high humidity environment, cause fruits and vegetables rotten
It is rotten, breed bacterium, thus, preservative film using more and more extensive.
As environmental pollution caused by the wasting of resources caused by preservative film material and its waste is got worse, people are to guarantor
Fresh film has higher requirement, to meet the market requirement.
Summary of the invention
In view of the above-mentioned problems, the present invention is intended to provide a kind of degradable, high moisture-inhibiting preservative film and preparation method thereof.
The invention is realized by the following technical scheme:
A kind of degradable, high moisture-inhibiting preservative film, which is characterized in that be made of raw material from the following weight:
Tealeaf residue 5-10, odium stearate 2-3, mustard oil 2-4, kaolin 3-4, sodium hydroxide solution 20-50, oleamide 3-6,
Precipitated calcium carbonate 2-3, polylactic acid, triethyl citrate mixed emulsion 30-60, sodium pyrophosphate 2-3, polyvinyl alcohol 80-100.
Further, preparation method includes the following steps:
(1) tealeaf residue is put into crucible, slow fire is dried to surface and turned to be yellow, and is put into ball milling 20-30min in ball mill, is obtained tea
Then leaf slag powder is added odium stearate, mustard oil, is transferred in high-speed kneading machine and mediates 30-40min, obtain modified tealeaves ground-slag；
(2) kaolin is immersed in the sodium hydroxide solution that concentration is 30-40%, is then boiled solution heating, and keep
20-30min, being cooled to temperature is 40-50 DEG C, is added in dilute hydrochloric acid and solution is to neutrality, oleamide, lightweight carbon is then added
Then sour calcium is filtered using 30-40Hz ultrasonic disperse 50-80min, dry at 60-70 DEG C, and being milled to partial size is 5-50 μ
m；
(3) ball milling is blended with step (2) gains in step (1) gains, is then added to polylactic acid, lemon triethylenetetraminehexaacetic acid
In ester mixed emulsion, sodium pyrophosphate is added, 40-50min is dispersed with stirring at 30-35 DEG C, 900-1000rpm, then in 5-10
1-2h is stood at DEG C, filter and is freeze-dried, and modified compounded mix is obtained；
(4) polyvinyl alcohol is added in 80-90 DEG C of the distilled water of 12-15 times of its volume, stirs 2-3h under 100-200rpm,
Then the distilled water for adding 10-30 times continues to obtain glue after stirring 1-2h, modified compounded mix obtained by step (3) is added,
Continue to utilize microwave treatment 10-12s after stirring 20-30min, obtains into film liquid, casting film-forming；
Further, step (2) the dilute hydrochloric acid concentration is 10-20%.
Further, step (2) precipitated calcium carbonate passes through following modification: precipitated calcium carbonate and zirconate is even
Connection agent is put into high-speed mixer, and at 2000-2300rpm then gains are put into tube furnace by mixed at high speed 5-10min
In, 1-2h is roasted at 200-250 DEG C, then roasts 50-60min at 350-400 DEG C, is down to the rate of 3-5 DEG C/min
Room temperature.
Further, step (3) polylactic acid, triethyl citrate mixed emulsion solid content are 15-20%, wherein gathering
The mass ratio of lactic acid and triethyl citrate is 10:1-3.
Beneficial effects of the present invention: the present invention, which provides a kind of degradable, high moisture-inhibiting preservative film, has good mechanical property,
And its rate of perviousness is higher, and fresh-keeping effect can extend 15 days or so, and degradation property is preferable.Using mustard oil processing tealeaf residue,
It can not only make tealeaf residue smooth phozy, promote its dispersion in the substrate, moreover, tealeaf residue can largely adsorb mustard oil,
The action time for increasing mustard oil, to extend the fresh-keeping effect of preservative film；It can make kaolin, lightweight carbon using oleamide
Sour calcium is more fully mixed, and is improved reunion degree, is improved the mechanical property of preservative film；The modification of precipitated calcium carbonate makes gently
Matter calcium carbonate enhances its adhesive force easily in conjunction with polylactic acid, triethyl citrate, meanwhile, polylactic acid, triethyl citrate mixing
After lotion is modified package to precipitated calcium carbonate, kaolin, tealeaves ground-slag, the dusting of filler is avoided, its intensity is improved, mentions
The interface binding power of high itself and substrate, to enhance the tensile strength of preservative film.
Specific embodiment
Illustrate the present invention with specific embodiment below, but is not limitation of the present invention.
Embodiment 1
A kind of degradable, high moisture-inhibiting preservative film, which is characterized in that be made of raw material from the following weight:
Tealeaf residue 5, odium stearate 2, mustard oil 2, kaolin 3, sodium hydroxide solution 20, oleamide 3, precipitated calcium carbonate 2 gather
Lactic acid, triethyl citrate mixed emulsion 30, sodium pyrophosphate 2, polyvinyl alcohol 80.
Further, preparation method includes the following steps:
(1) tealeaf residue is put into crucible, slow fire is dried to surface and turned to be yellow, and is put into ball milling 20min in ball mill, is obtained tealeaf residue
Then powder is added odium stearate, mustard oil, is transferred in high-speed kneading machine and mediates 30min, obtain modified tealeaves ground-slag；
(2) kaolin is immersed in the sodium hydroxide solution that concentration is 30%, is then boiled solution heating, and keep
20min, being cooled to temperature is 40 DEG C, and with solution to neutrality in addition dilute hydrochloric acid, oleamide, precipitated calcium carbonate is then added,
Using 30Hz ultrasonic disperse 50min, then filter, it is dry at 60 DEG C, and being milled to partial size is 5 μm；
(3) ball milling is blended with step (2) gains in step (1) gains, is then added to polylactic acid, lemon triethylenetetraminehexaacetic acid
In ester mixed emulsion, sodium pyrophosphate is added, 40min is dispersed with stirring at 30 DEG C, 900rpm, then stands 1h at 5 DEG C, filters
And be freeze-dried, obtain modified compounded mix；
(4) polyvinyl alcohol is added in 80 DEG C of the distilled water of 12 times of its volume, 2h is stirred under 100rpm, then adds 10
Distilled water again continues to obtain glue after stirring 1h, modified compounded mix obtained by step (3) is added, continues benefit after stirring 20min
With microwave treatment 10s, film liquid, casting film-forming are obtained into；
Further, step (2) the dilute hydrochloric acid concentration is 10%.
Further, step (2) precipitated calcium carbonate passes through following modification: precipitated calcium carbonate and zirconate is even
Connection agent is put into high-speed mixer, and gains, are then put into tube furnace by mixed at high speed 5min at 2000rpm, 200
1h is roasted at DEG C, then roasts 50min at 350 DEG C, and room temperature is down to the rate of 3 DEG C/min.
Further, step (3) polylactic acid, triethyl citrate mixed emulsion solid content are 15%, wherein polylactic acid
Mass ratio with triethyl citrate is 10:1.
Embodiment 2
A kind of degradable, high moisture-inhibiting preservative film, which is characterized in that be made of raw material from the following weight:
Tealeaf residue 6, odium stearate 3, mustard oil 3, kaolin 4, sodium hydroxide solution 30, oleamide 5, precipitated calcium carbonate 3 gather
Lactic acid, triethyl citrate mixed emulsion 50, sodium pyrophosphate 3, polyvinyl alcohol 90.
Further, preparation method includes the following steps:
(1) tealeaf residue is put into crucible, slow fire is dried to surface and turned to be yellow, and is put into ball milling 25min in ball mill, is obtained tealeaf residue
Then powder is added odium stearate, mustard oil, is transferred in high-speed kneading machine and mediates 35min, obtain modified tealeaves ground-slag；
(2) kaolin is immersed in the sodium hydroxide solution that concentration is 35%, is then boiled solution heating, and keep
25min, being cooled to temperature is 45 DEG C, and with solution to neutrality in addition dilute hydrochloric acid, oleamide, precipitated calcium carbonate is then added,
Using 35Hz ultrasonic disperse 60min, then filter, it is dry at 65 DEG C, and being milled to partial size is 30 μm；
(3) ball milling is blended with step (2) gains in step (1) gains, is then added to polylactic acid, lemon triethylenetetraminehexaacetic acid
In ester mixed emulsion, sodium pyrophosphate is added, 45min is dispersed with stirring at 32 DEG C, 950rpm, 2h is then stood at 8 DEG C, filters
And be freeze-dried, obtain modified compounded mix；
(4) polyvinyl alcohol is added in 85 DEG C of the distilled water of 13 times of its volume, 3h is stirred under 150rpm, then adds 20
Distilled water again continues to obtain glue after stirring 2h, modified compounded mix obtained by step (3) is added, continues benefit after stirring 25min
With microwave treatment 11s, film liquid, casting film-forming are obtained into；
Further, step (2) the dilute hydrochloric acid concentration is 15%.
Further, step (2) precipitated calcium carbonate passes through following modification: precipitated calcium carbonate and zirconate is even
Connection agent is put into high-speed mixer, and gains, are then put into tube furnace by mixed at high speed 8min at 2200rpm, 220
2h is roasted at DEG C, then roasts 55min at 380 DEG C, and room temperature is down to the rate of 4 DEG C/min.
Further, step (3) polylactic acid, triethyl citrate mixed emulsion solid content are 18%, wherein polylactic acid
Mass ratio with triethyl citrate is 5:1.
Embodiment 3
A kind of degradable, high moisture-inhibiting preservative film, which is characterized in that be made of raw material from the following weight:
Tealeaf residue 10, odium stearate 3, mustard oil 4, kaolin 4, sodium hydroxide solution 50, oleamide 6, precipitated calcium carbonate 3,
Polylactic acid, triethyl citrate mixed emulsion 60, sodium pyrophosphate 3, polyvinyl alcohol 100.
Further, preparation method includes the following steps:
(1) tealeaf residue is put into crucible, slow fire is dried to surface and turned to be yellow, and is put into ball milling 30min in ball mill, is obtained tealeaf residue
Then powder is added odium stearate, mustard oil, is transferred in high-speed kneading machine and mediates 40min, obtain modified tealeaves ground-slag；
(2) kaolin is immersed in the sodium hydroxide solution that concentration is 40%, is then boiled solution heating, and keep
30min, being cooled to temperature is 50 DEG C, and with solution to neutrality in addition dilute hydrochloric acid, oleamide, precipitated calcium carbonate is then added,
Using 40Hz ultrasonic disperse 80min, then filter, it is dry at 70 DEG C, and being milled to partial size is 50 μm；
(3) ball milling is blended with step (2) gains in step (1) gains, is then added to polylactic acid, lemon triethylenetetraminehexaacetic acid
In ester mixed emulsion, sodium pyrophosphate is added, 50min is dispersed with stirring at 35 DEG C, 1000rpm, 2h, mistake are then stood at 10 DEG C
It filters and is freeze-dried, obtain modified compounded mix；
(4) polyvinyl alcohol is added in 90 DEG C of the distilled water of 15 times of its volume, 3h is stirred under 200rpm, then adds 30
Distilled water again continues to obtain glue after stirring 2h, modified compounded mix obtained by step (3) is added, continues benefit after stirring 30min
With microwave treatment 12s, film liquid, casting film-forming are obtained into；
Further, step (2) the dilute hydrochloric acid concentration is 20%.
Further, step (2) precipitated calcium carbonate passes through following modification: precipitated calcium carbonate and zirconate is even
Connection agent is put into high-speed mixer, and gains, are then put into tube furnace by mixed at high speed 10min at 2300rpm,
2h is roasted at 250 DEG C, then roasts 60min at 400 DEG C, and room temperature is down to the rate of 5 DEG C/min.
Further, step (3) polylactic acid, triethyl citrate mixed emulsion solid content are 20%, wherein polylactic acid
Mass ratio with triethyl citrate is 10:3.
Comparative example 1
The addition of mustard oil is omitted compared to embodiment 2 in this comparative example, and method and step in addition to this is all the same.
Comparative example 2
The addition of oleamide is omitted compared to embodiment 2 in this comparative example, and method and step in addition to this is all the same.
Comparative example 3
The addition of polylactic acid, triethyl citrate mixed emulsion is omitted compared to embodiment 2 in this comparative example, except this it
Outer method and step is all the same.
Comparative example 4
The modification of precipitated calcium carbonate is omitted compared to embodiment 2 in this comparative example, and method and step in addition to this is equal
It is identical.
Performance test:
Mechanical property is measured referring to GB/T 1040.3-2006 " measurement of plastic tensile performance " method.
Rate of perviousness is measured referring to GB/T 16928-1997 " packaging material test method ".
Fresh keeping property test: using fresh honey peach as experimental subjects, the preservative film obtained by each embodiment and comparative example
It is wrapped up, is then placed at 25 DEG C and saves, the time of 1-3 small specks occurs in record, characterizes preservative film with this
Fresh-keeping effect.
Degradation property test: it by the embedment natural environment soil of preservative film obtained by each group of phase homogenous quantities, is specially embedded to
In farmland 100cm × 100cm × 100cm heatable adobe sleeping platform, testing its degradation rate is 95% required time, is recorded as degradation time.
Test result is as shown in table 1:
Table 1
As can be seen from Table 1, preservative film prepared by the present invention has good mechanical property, and its rate of perviousness is higher, fresh-keeping
Effect can extend 15 days or so, and degradation property is preferable.
Claims (5)
1. a kind of degradable, high moisture-inhibiting preservative film, which is characterized in that be made of raw material from the following weight:
Tealeaf residue 5-10, odium stearate 2-3, mustard oil 2-4, kaolin 3-4, sodium hydroxide solution 20-50, oleamide 3-6,
Precipitated calcium carbonate 2-3, polylactic acid, triethyl citrate mixed emulsion 30-60, sodium pyrophosphate 2-3, polyvinyl alcohol 80-100.
2. one kind according to claim 1 is degradable, high moisture-inhibiting preservative film, which is characterized in that preparation method include with
Lower step:
(1) tealeaf residue is put into crucible, slow fire is dried to surface and turned to be yellow, and is put into ball milling 20-30min in ball mill, is obtained tea
Then leaf slag powder is added odium stearate, mustard oil, is transferred in high-speed kneading machine and mediates 30-40min, obtain modified tealeaves ground-slag；
(2) kaolin is immersed in the sodium hydroxide solution that concentration is 30-40%, is then boiled solution heating, and keep
20-30min, being cooled to temperature is 40-50 DEG C, is added in dilute hydrochloric acid and solution is to neutrality, oleamide, lightweight carbon is then added
Then sour calcium is filtered using 30-40Hz ultrasonic disperse 50-80min, dry at 60-70 DEG C, and being milled to partial size is 5-50 μ
m；
(3) ball milling is blended with step (2) gains in step (1) gains, is then added to polylactic acid, lemon triethylenetetraminehexaacetic acid
In ester mixed emulsion, sodium pyrophosphate is added, 40-50min is dispersed with stirring at 30-35 DEG C, 900-1000rpm, then in 5-10
1-2h is stood at DEG C, filter and is freeze-dried, and modified compounded mix is obtained；
(4) polyvinyl alcohol is added in 80-90 DEG C of the distilled water of 12-15 times of its volume, stirs 2-3h under 100-200rpm,
Then the distilled water for adding 10-30 times continues to obtain glue after stirring 1-2h, modified compounded mix obtained by step (3) is added,
Continue to utilize microwave treatment 10-12s after stirring 20-30min, obtains into film liquid, casting film-forming.
3. one kind according to claim 1 is degradable, high moisture-inhibiting preservative film, which is characterized in that step (2) described dilute hydrochloric acid
Concentration is 10-20%.
4. one kind according to claim 1 is degradable, high moisture-inhibiting preservative film, which is characterized in that step (2) the lightweight carbon
Sour calcium passes through following modification: precipitated calcium carbonate and zirconium ester coupling agent being put into high-speed mixer, in 2000-
Gains, are then put into tube furnace by mixed at high speed 5-10min under 2300rpm, roast 1-2h at 200-250 DEG C, connect
Roast 50-60min at 350-400 DEG C, room temperature is down to the rate of 3-5 DEG C/min.
5. one kind according to claim 1 is degradable, high moisture-inhibiting preservative film, which is characterized in that step (3) the poly- cream
Acid, triethyl citrate mixed emulsion solid content are 15-20%, and wherein the mass ratio of polylactic acid and triethyl citrate is 10:1-
3。
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2018
- 2018-08-27 CN CN201810978459.7A patent/CN109111667A/en active Pending
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|---|---|---|---|---|
| CN101029173A (en) * | 2007-03-16 | 2007-09-05 | 许波 | Modified resin material for producing flexible film and shrinkaged film and its production |
| CN101735636A (en) * | 2008-11-12 | 2010-06-16 | 福建恒安集团有限公司 | Biodegradation time controlled plastic film and preparation method thereof |
| CN101864132A (en) * | 2010-05-26 | 2010-10-20 | 四川大学 | Fusion preparation method of polyvinyl alcohol film |
| CN104910440A (en) * | 2015-05-27 | 2015-09-16 | 铜陵方正塑业科技有限公司 | Antibacterial starch-blended full-degradable plastic film and preparation method thereof |
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Application publication date: 20190101 |