CN109401220A - A method of antimicrobial preservative film is prepared with cloves extracting solution-garlic oil-beta cyclodextrin clathrate - Google Patents
A method of antimicrobial preservative film is prepared with cloves extracting solution-garlic oil-beta cyclodextrin clathrate Download PDFInfo
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- CN109401220A CN109401220A CN201811144031.9A CN201811144031A CN109401220A CN 109401220 A CN109401220 A CN 109401220A CN 201811144031 A CN201811144031 A CN 201811144031A CN 109401220 A CN109401220 A CN 109401220A
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- extracting solution
- preservative film
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- beta cyclodextrin
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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
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
- C08B37/0012—Cyclodextrin [CD], e.g. cycle with 6 units (alpha), with 7 units (beta) and with 8 units (gamma), large-ring cyclodextrin or cycloamylose with 9 units or more; Derivatives thereof
- C08B37/0015—Inclusion compounds, i.e. host-guest compounds, e.g. polyrotaxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- 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
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—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
- 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
- C08J2405/16—Cyclodextrin; Derivatives thereof
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2497/00—Characterised by the use of lignin-containing materials
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Abstract
The invention discloses a kind of methods for preparing antimicrobial preservative film with cloves extracting solution-garlic oil-beta cyclodextrin clathrate; distilled water is added into sodium lignin sulfonate; heating stirring dissolution is complete; maleic anhydride is added, after being alkaline reaction with sodium hydroxide adjusting pH, adds dilute sulfuric acid tune pH that precipitating is precipitated to be acid; filtering, washing; it dries in an oven, grinds sieving, maleylation lignin sulfonic acid is made；Deionized water is added into beta cyclodextrin, saturated solution is made, dehydrated alcohol dissolution is added into garlic oil, then mixes it in saturated solution for being added drop-wise to beta cyclodextrin with cloves extracting solution, it is included, crystallisation by cooling, is filtered by vacuum, it is washed with dehydrated alcohol, dry antibacterial inclusion compound；It after polyadipate-butylene terephthalate, polycaprolactone master batch are dried in a vacuum drying oven, is mixed with maleylation lignin sulfonic acid, antibacterial inclusion compound, injection twin-screw extrusion is cast unit, and extrusion obtains blending antibacterial preservative film.
Description
Technical field
The invention belongs to preservative film material fields, and in particular to a kind of to be included with cloves extracting solution-garlic oil-beta cyclodextrin
The method that object prepares antimicrobial preservative film.
Background technique
It becomes increasingly conspicuous with oil-fired increasingly depleted and white pollution problems, degradable, reproducible environmentally friendly material
Material has been to be concerned by more and more people.Lignin is a kind of biodegradable, nontoxic, reproducible aromatics high polymer, is certainly
Reserves are only second to the second largest natural macromolecular material of cellulose in right boundary.It is widely present among the lignum of plant,
Largely originate from industrial in slurrying and papermaking, bio-ethanol production etc., although yield is big, utilization rate is low.Therefore, this is made full use of
Kind natural polymer, is of great significance.In view of its polyhydroxy and fragrant rigid structure, it is unfavorable for independent machine-shaping, considers
It is subjected to blending and modifying with flexible polymer.Polycaprolactone is a kind of linear polyester synthesis macromolecule, and strand has good
Good flexibility, and there is biodegradability because of its molecular structure, but its price is costly, and rigidity is low.Therefore, will
The sodium lignin sulfonate and polycaprolactone of industrial mass production carry out melt blending and prepare preservative film.But there are anti-bacterial refreshings
It can be insufficient.
Garlic oil is that the collaboration after garlic is broken, by alliin in allinnase, phosphopyridoxal pyridoxal phosphate and metal ion is made
With the organic sulfur compound of lower formation, there is antibacterial, antiviral and antitumor, protect cardiovascular system, promote glycometabolism, improve machine
The effects of body immunity.Edible freshness-keeping thin coat, degradable preservative film and functional preservative film are the hairs of the following food packaging industry
Exhibition trend, antimicrobial preservative film are that one kind adds antimicrobial component in filmogen, are reached by the sustained release of antibacterial material antibacterial
Every bacterium, the functional preservative film of fresh-keeping purpose.A kind of natural antimicrobial substance of the garlic oil as broad-spectrum high efficacy, is antimicrobial preservative film
Excellent functional film-forming components.
The present invention is by adding fragrant extracting solution-garlic oil-beta cyclodextrin antibacterial inclusion compound, maleylation lignin sulfonic acid system
The standby antimicrobial preservative film haveing excellent performance.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of cloves extracting solution-garlic oil-beta cyclodextrin packet is provided
The method that object prepares antimicrobial preservative film is closed, the preservative film according to this method production has excellent anti-bacterial refreshing performance, and can
With biodegrade.
The present invention is achieved by the following technical solutions:
A method of antimicrobial preservative film is prepared with cloves extracting solution-garlic oil-beta cyclodextrin clathrate, which is characterized in that including
Following steps:
(1) preparation of maleylation lignin sulfonic acid:
Into 20-24 parts of sodium lignin sulfonates, distilled water is added in 1:5, and it is complete to be heated to 34-36 DEG C of stirring and dissolving, adds 18-
20 parts of maleic anhydrides, adjusting pH with sodium hydroxide is 10, after reacting 3-4h at 54-56 DEG C, adds dilute sulfuric acid tune pH for 1-2 precipitation
Precipitating, filtering, washing, dry 1-2d, grinds sieving in 40-50 DEG C of baking oven, and maleylation lignin sulfonic acid is made；
(2) preparation of cloves extracting solution-garlic oil-beta cyclodextrin antibacterial inclusion compound:
Deionized water is added into 10-20 parts of beta cyclodextrins, saturated solution is made, it is molten that dehydrated alcohol is added into 2-3 portions of garlic oils
Solution, then mixes it in saturated solution for being added drop-wise to beta cyclodextrin with cloves extracting solution, is 500W, includes temperature in inclusion power
Inclusion 1-2h is carried out under the conditions of 30-33 DEG C of degree, and crystallisation by cooling, vacuum filtration is washed 3-5 times with dehydrated alcohol, dry antibacterial
Inclusion compound；
(3) preparation of antimicrobial preservative film:
By 90-110 parts of polyadipate-butylene terephthalates, 27-33 parts of polycaprolactone master batches respectively in 60-63 DEG C and 30-
It in 33 DEG C of vacuum ovens after dry 20-24h, is mixed with resulting material in (1), (2), injects twin-screw extrusion casting machine
Group, extrusion obtain 50 μm of thickness of blending antibacterial preservative film.
Further, in step (2) cloves extracting solution preparation: cloves is dried at 60-63 DEG C, crush, cross 40 mesh
The ethyl alcohol of the Extraction solvent 95% of 10 times of volumes is added into 20-25 parts of cloves powder for sieve, and ultrasonic wave auxiliary mentions at 50-53 DEG C
1-2h is taken, is concentrated under reduced pressure after filtering, cloves extracting solution is made.
Further, extrusion temperature is 170-190 DEG C in step (3).
The present invention has the advantage that compared with prior art
(1) sodium lignin sulfonate and maleic anhydride are subjected in alkaline aqueous solution esterification modification, obtain maleylation lignin
Sulfonic acid is blended with polyadipate-butylene terephthalate, polycaprolactone and prepares antimicrobial preservative film；Maleylation sulfomethylated lignin
Interaction between acid and matrix is strong, is uniformly dispersed in the base, hence it is evident that improve its mechanical strength, especially tensile strength；
Modified preservative film is biodegradable.
(2) cloves is extracted by Extraction solvent of 95% ethyl alcohol, cloves extracting solution is made, corrosion-resistanting fresh-keeping effect is excellent, Ke Yizuo
Blending antibacterial preservative film is prepared for fungicide；Based on the antibacterial action of garlic oil, using beta cyclodextrin inclusion technique as means,
It is prepared for cloves extracting solution-garlic oil-beta cyclodextrin clathrate；Inclusion compound has no irritating odor, and shows good thermostabilization
Property, photostability and the stability that keeps sample for a long time, sufficiently meet subsequent
Film forming requires.
Specific embodiment
Embodiment 1
A method of antimicrobial preservative film is prepared with cloves extracting solution-garlic oil-beta cyclodextrin clathrate, which is characterized in that including
Following steps:
(1) preparation of maleylation lignin sulfonic acid:
Into 20 parts of sodium lignin sulfonates, distilled water is added in 1:5, and it is complete to be heated to 34-36 DEG C of stirring and dissolving, adds 18 portions of horses
Carry out acid anhydrides, adjusting pH with sodium hydroxide is 10, and after reacting 3h at 54-56 DEG C, adding dilute sulfuric acid tune pH is that precipitating, mistake is precipitated in 1-2
Filter, washing, dry 1d, grinds sieving in 40-50 DEG C of baking oven, and maleylation lignin sulfonic acid is made；
(2) preparation of cloves extracting solution-garlic oil-beta cyclodextrin antibacterial inclusion compound:
Deionized water is added into 10 parts of beta cyclodextrins, saturated solution is made, dehydrated alcohol dissolution is added into 2 portions of garlic oils, so
It is mixed in the saturated solution for being added drop-wise to beta cyclodextrin with cloves extracting solution afterwards, is 500W, includes temperature 30- in inclusion power
Carry out inclusion 1h under the conditions of 33 DEG C, crystallisation by cooling, vacuum filtration is washed 3 times with dehydrated alcohol, dry antibacterial inclusion compound；
(3) preparation of antimicrobial preservative film:
90 parts of polyadipate-butylene terephthalates, 27 parts of polycaprolactone master batches are true at 60-63 DEG C and 30-33 DEG C respectively
It in empty drying box after dry 20h, is mixed with resulting material in (1), (2), injection twin-screw extrusion is cast unit, squeezes out
To 50 μm of thickness of blending antibacterial preservative film.
Further, in step (2) cloves extracting solution preparation: cloves is dried at 60-63 DEG C, crush, cross 40 mesh
The ethyl alcohol of the Extraction solvent 95% of 10 times of volumes, the ultrasonic wave assisted extraction at 50-53 DEG C are added into 20 parts of cloves powder for sieve
1h is concentrated under reduced pressure after filtering, and cloves extracting solution is made.
Further, extrusion temperature is 170-190 DEG C in step (3).
Embodiment 2
A method of antimicrobial preservative film is prepared with cloves extracting solution-garlic oil-beta cyclodextrin clathrate, which is characterized in that including
Following steps:
(1) preparation of maleylation lignin sulfonic acid:
Into 24 parts of sodium lignin sulfonates, distilled water is added in 1:5, and it is complete to be heated to 34-36 DEG C of stirring and dissolving, adds 20 portions of horses
Carry out acid anhydrides, adjusting pH with sodium hydroxide is 10, and after reacting 4h at 54-56 DEG C, adding dilute sulfuric acid tune pH is that precipitating, mistake is precipitated in 1-2
Filter, washing, dry 2d, grinds sieving in 40-50 DEG C of baking oven, and maleylation lignin sulfonic acid is made；
(2) preparation of cloves extracting solution-garlic oil-beta cyclodextrin antibacterial inclusion compound:
Deionized water is added into 20 parts of beta cyclodextrins, saturated solution is made, dehydrated alcohol dissolution is added into 3 portions of garlic oils, so
It is mixed in the saturated solution for being added drop-wise to beta cyclodextrin with cloves extracting solution afterwards, is 500W, includes temperature 30- in inclusion power
Carry out inclusion 2h under the conditions of 33 DEG C, crystallisation by cooling, vacuum filtration is washed 5 times with dehydrated alcohol, dry antibacterial inclusion compound；
(3) preparation of antimicrobial preservative film:
110 parts of polyadipate-butylene terephthalates, 33 parts of polycaprolactone master batches are true at 60-63 DEG C and 30-33 DEG C respectively
It in empty drying box after drying for 24 hours, is mixed with resulting material in (1), (2), injection twin-screw extrusion is cast unit, squeezes out
To 50 μm of thickness of blending antibacterial preservative film.
Further, in step (2) cloves extracting solution preparation: cloves is dried at 60-63 DEG C, crush, cross 40 mesh
The ethyl alcohol of the Extraction solvent 95% of 10 times of volumes, the ultrasonic wave assisted extraction at 50-53 DEG C are added into 25 parts of cloves powder for sieve
2h is concentrated under reduced pressure after filtering, and cloves extracting solution is made.
Further, extrusion temperature is 170-190 DEG C in step (3).
There is excellent anti-bacterial refreshing performance according to the preservative film of the method for the present invention production, and can biodegrade；With
It is not added with maleylation lignin sulfonic acid, the preservative film of cloves extracting solution-garlic oil-beta cyclodextrin antibacterial inclusion compound preparation is sky
White control group；
38 times are improved by the penetrability of antimicrobial preservative film manufactured in the present embodiment, CO2And O2Tranmittance be up to 9.5, with this
The cherry tomato preservation term of preservative film packaging is up to 66 days；
Bacteria isolation rate to Escherichia coli and staphylococcus aureus is more than 99%, shows good microorganism isolation and inhibits effect
Fruit；
Soil burial test finds that the antimicrobial preservative film is biodegradable.
Claims (3)
1. a kind of method for preparing antimicrobial preservative film with cloves extracting solution-garlic oil-beta cyclodextrin clathrate, which is characterized in that packet
Include following steps:
(1) preparation of maleylation lignin sulfonic acid:
Into 20-24 parts of sodium lignin sulfonates, distilled water is added in 1:5, and it is complete to be heated to 34-36 DEG C of stirring and dissolving, adds 18-
20 parts of maleic anhydrides, adjusting pH with sodium hydroxide is 10, after reacting 3-4h at 54-56 DEG C, adds dilute sulfuric acid tune pH for 1-2 precipitation
Precipitating, filtering, washing, dry 1-2d, grinds sieving in 40-50 DEG C of baking oven, and maleylation lignin sulfonic acid is made；
(2) preparation of cloves extracting solution-garlic oil-beta cyclodextrin antibacterial inclusion compound:
Deionized water is added into 10-20 parts of beta cyclodextrins, saturated solution is made, it is molten that dehydrated alcohol is added into 2-3 portions of garlic oils
Solution, then mixes it in saturated solution for being added drop-wise to beta cyclodextrin with cloves extracting solution, is 500W, includes temperature in inclusion power
Inclusion 1-2h is carried out under the conditions of 30-33 DEG C of degree, and crystallisation by cooling, vacuum filtration is washed 3-5 times with dehydrated alcohol, dry antibacterial
Inclusion compound；
(3) preparation of antimicrobial preservative film:
By 90-110 parts of polyadipate-butylene terephthalates, 27-33 parts of polycaprolactone master batches respectively in 60-63 DEG C and 30-
It in 33 DEG C of vacuum ovens after dry 20-24h, is mixed with resulting material in (1), (2), injects twin-screw extrusion casting machine
Group, extrusion obtain 50 μm of thickness of blending antibacterial preservative film.
2. according to claim 1 a kind of antimicrobial preservative film is prepared with cloves extracting solution-garlic oil-beta cyclodextrin clathrate
Method, which is characterized in that the preparation of cloves extracting solution in step (2):
Cloves is dried at 60-63 DEG C, crushes, cross 40 meshes, the extraction of 10 times of volumes is added into 20-25 parts of cloves powder
The ethyl alcohol of solvent 95%, the ultrasonic wave assisted extraction 1-2h at 50-53 DEG C, is concentrated under reduced pressure after filtering, and cloves extracting solution is made.
3. according to claim 1 a kind of antimicrobial preservative film is prepared with cloves extracting solution-garlic oil-beta cyclodextrin clathrate
Method, which is characterized in that in step (3) extrusion temperature be 170-190 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811144031.9A CN109401220A (en) | 2018-09-29 | 2018-09-29 | A method of antimicrobial preservative film is prepared with cloves extracting solution-garlic oil-beta cyclodextrin clathrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811144031.9A CN109401220A (en) | 2018-09-29 | 2018-09-29 | A method of antimicrobial preservative film is prepared with cloves extracting solution-garlic oil-beta cyclodextrin clathrate |
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| CN109401220A true CN109401220A (en) | 2019-03-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113956638A (en) * | 2021-11-25 | 2022-01-21 | 宁波嘉信化工实业有限公司 | Polycaprolactone composite material and preparation method thereof |
| CN117441878A (en) * | 2023-12-07 | 2024-01-26 | 北方民族大学 | Modified starch emulsifier and preparation method thereof |
-
2018
- 2018-09-29 CN CN201811144031.9A patent/CN109401220A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113956638A (en) * | 2021-11-25 | 2022-01-21 | 宁波嘉信化工实业有限公司 | Polycaprolactone composite material and preparation method thereof |
| CN117441878A (en) * | 2023-12-07 | 2024-01-26 | 北方民族大学 | Modified starch emulsifier and preparation method thereof |
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