CN104987635A - Polyvinyl alcohol antibiosis packaging film and production method thereof - Google Patents
Polyvinyl alcohol antibiosis packaging film and production method thereof Download PDFInfo
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- CN104987635A CN104987635A CN201510255896.2A CN201510255896A CN104987635A CN 104987635 A CN104987635 A CN 104987635A CN 201510255896 A CN201510255896 A CN 201510255896A CN 104987635 A CN104987635 A CN 104987635A
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Abstract
The invention relates to a polyvinyl alcohol antibiosis packaging film. The film adopts polyvinyl alcohol resin as a base material and adopts glycerin, potassium sorbate and chitosan quaternary ammonium salt as modification agents, the modification agents also comprise nanometer montmorillonite, and the polyvinyl alcohol antibiosis packaging film is produced by mixing, by weight, 100 parts of the polyvinyl alcohol resin, 10 parts of glycerin, 1 part of montmorillonite, 1-3 parts of potassium sorbate and 1-2 parts of chitosan quaternary ammonium salt.
Description
Technical field
The invention belongs to film composite material technical field, be specifically related to a kind of preparation method of polyvinyl alcohol antimicrobial packaging film.
Background technology
Polyvinyl alcohol (PVA) is a class high molecular weight water soluble polymer, contains a large amount of hydrogen bond, so PVA molecule has the performance such as crystallinity, chemical stability, thermostability of height, have and apply very widely in its molecule with intermolecular.As wrapping material, because PVA film has good mechanical property, high oxygen barrier, the advantage such as toxicological harmless, biodegradable, is widely used in the various packing of product.At present, existing scholar prepares functional PVA film using PVA resin as base material both at home and abroad, and research was carried out to it, and prepare polyvinyl alcohol antibacterial film by adding potassium sorbate, calcium propionate etc., but because PVA molecule has very strong wetting ability, in the product that some moisture contents of packaging are higher, there is certain defect in the polyvinyl alcohol antibacterial film made; Limit its use range, there is the necessity improved further.
Summary of the invention
Object of the present invention: polyvinyl alcohol antimicrobial packaging film aiming to provide the certain water repelling property of a kind of tool and preparation method thereof, improves use properties and the scope of application of polyvinyl alcohol packing film.
For solving foregoing invention object, the present invention adopts following technical scheme:
This polyvinyl alcohol antimicrobial packaging film, with polyvinyl alcohol resin, glycerine, potassium sorbate, Quaternary Ammonium Salt of Chitosan for basic material, is characterized in that: be also added with nano imvite; And the proportions mixed glycerine 10 weight part according to the polyvinyl alcohol resin of every 100 weight parts, mix polynite 1 weight part, mix the ratio of potassium sorbate 1-3 part, mix Quaternary Ammonium Salt of Chitosan 1-2 part.
Potassium sorbate in described modified additive and Quaternary Ammonium Salt of Chitosan are pressed 1:1 compound proportion and are formed promoting agent combination, and directly join in modified additive with the ratio of 1 ?2 weight part and use.
The preparation method of described polyvinyl alcohol antimicrobial packaging film draws together following steps:
1), after first being cleaned in distilled water by polyvinyl alcohol resin particle, constant temperature blast drying oven is sent in 70 DEG C of dry 12h;
2) the dried PVA particle of 30g is accurately taken in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely to polyvinyl alcohol resin particle;
3) respectively to adding the polynite of different ratio, potassium sorbate and Quaternary Ammonium Salt of Chitosan in polyvinyl alcohol resin mother liquor, and constant temperature stirs 4h to MMT powder and promoting agent and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, prepares antimicrobial nano laminated film mother liquor;
4) use casting method dry 3h film forming at 60 DEG C, prepare modified Nano antimicrobial packaging film.
According to this polyvinyl alcohol antimicrobial packaging film that above technical scheme proposes, there is following beneficial effect:
The polyvinyl alcohol antimicrobial packaging film that the present invention proposes effectively can delay the oxidation of cold fresh meat and brown stain within the scope of 0-4 DEG C, can suppress its juice loss, play germicidal action simultaneously, effectively can extend the shelf lives of cold fresh meat product, reduce costs; And overcome traditional product directly interpolation or the change of product special flavour that the fresh-keeping mode such as dip-coating preservation agent causes, the problems such as the loss of nutritive substance and security reduction.
Accompanying drawing explanation
Fig. 1 is for carrying out pH Indexs measure curve obtained schematic diagram to cold fresh meat storage freshness;
Fig. 2 is for carrying out total volatile basic nitrogen Indexs measure curve obtained schematic diagram to cold fresh meat storage freshness.
Embodiment
The present invention is set forth further below in conjunction with embodiment.
This polyvinyl alcohol antimicrobial packaging film, with polyvinyl alcohol resin, glycerine, potassium sorbate, Quaternary Ammonium Salt of Chitosan for basic material, is characterized in that: be also added with nano imvite; And mix glycerine 10 weight part according to the polyvinyl alcohol resin of every 100 weight parts, mix polynite 1 weight part, mix potassium sorbate 1 ?3 parts ratio, mix Quaternary Ammonium Salt of Chitosan 1 ?the proportions of 2 parts.
Potassium sorbate in described modified additive and Quaternary Ammonium Salt of Chitosan also can form promoting agent combination by 1:1 compound proportion, and directly join in modified additive with the ratio of 1 ?2 weight part and use.
The preparation method of described polyvinyl alcohol antimicrobial packaging film draws together following steps:
1), after first being cleaned in distilled water by polyvinyl alcohol resin particle, constant temperature blast drying oven is sent in 70 DEG C of dry 12h;
2) the dried PVA particle of 30g is accurately taken in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely to polyvinyl alcohol resin particle;
3) respectively to adding the polynite of different ratio, potassium sorbate and Quaternary Ammonium Salt of Chitosan in polyvinyl alcohol resin mother liquor, and constant temperature stirs 4h to MMT powder and promoting agent and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, prepares antimicrobial nano laminated film mother liquor;
4) use casting method dry 3h film forming at 60 DEG C, prepare modified Nano antimicrobial packaging film.
The principle of this polyvinyl alcohol antimicrobial packaging film that the present invention proposes is as follows:
Because PVA molecule has very strong wetting ability, as wrapping material, traditional PVA film is when the product that packaging moisture content is high, and due to hygroscopic effect, its mechanical property obviously reduces, and easily occurs breakage, there is certain defect.
Polynite (MMT) is a kind of layered silicate, and skin has two-layer Si-O tetrahedron, and therebetween one deck AL-O-OH is octahedra, and each lamellar spacing is about 1nm, the about 100nm of length and width, can by polymkeric substance and monomer intercalation.DK4 type grade polymer nano imvite selects the montmorillonite mineral that white, electric density are moderate, through multistage purification, delaminate, the obtained large radius-thickness ratio montmorillonite of high purity, smectite content reaches 96-98%, for rice white powder, wafer mean thickness is less than 25nm, appropriate DK4 type MMT is intercalation in polymkeric substance, H key, Al-O key, Si-O key is closely formed with the hydroxyl in polyvinyl alcohol molecule structure, system is closely linked more, the PVA film hydrophilic made is weakened, and mechanical property strengthens.
Potassium sorbate, as a kind of unsaturated fatty acids, can participate in metabolism in human body, is finally broken down into carbonic acid gas and water, does not almost have toxicity.Again because potassium sorbate can mould fungus inhibition effectively, the activity of yeast and aerobic bacteria, can also prevent the harmful microbe Growth and reproductions such as Clostridium botulinum, staphylococcus, Salmonellas, so be widely used in food fresh keeping aspect.
Quaternary Ammonium Salt of Chitosan obtains by introducing quaternary ammonium salt group in chitosan molecule, this modified chitosan compares pure chitosan better water-soluble and germ resistance, under the same conditions, Quaternary Ammonium Salt of Chitosan compares pure chitosan has more excellent restraining effect to streptococcus aureus.
Beneficial effect: antistaling film of the present invention effectively can delay the oxidation of cold fresh meat and brown stain within the scope of 0-4 DEG C, its juice loss can be suppressed, play germicidal action simultaneously, effectively can extend the shelf lives of cold fresh meat product, reduce costs, and overcome traditional product directly interpolation or the change of product special flavour that the fresh-keeping mode such as dip-coating preservation agent causes, the problems such as the loss of nutritive substance and security reduction.
Embodiment 1
Composition of raw materials: by the mass percent relative to PVA, PVA, 10% glycerine, 1%DK4 type nano imvite, 1% potassium sorbate.
Preparation method comprises the following steps:
After being cleaned in distilled water by PVA particle, send into constant temperature blast drying oven in 70 DEG C of dry 12h.Accurately take the dried PVA particle of 30g in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h to PVA particle as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely.Again respectively to the DK4 type MMT and 1% potassium sorbate that add 1% in PVA mother liquor, and constant temperature stirs 4h to MMT powder and potassium sorbate and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, prepare antimicrobial nano laminated film mother liquor, use casting method dry 3h at 60 DEG C to obtain modified Nano packaging film A.
Embodiment 2
Composition of raw materials: by the mass percent relative to PVA, PVA, 10% glycerine, 1%DK4 type nano imvite, 2% potassium sorbate.
Preparation method comprises the following steps:
After being cleaned in distilled water by PVA particle, send into constant temperature blast drying oven in 70 DEG C of dry 12h.Accurately take the dried PVA particle of 30g in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h to PVA particle as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely.Again respectively to the DK4 type MMT and 2% potassium sorbate that add 1% in PVA mother liquor, and constant temperature stirs 4h to MMT powder and potassium sorbate and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, prepare antimicrobial nano laminated film mother liquor, use casting method dry 3h at 60 DEG C to obtain modified Nano packaging film B.
Embodiment 3
Composition of raw materials: by the mass percent relative to PVA, PVA, 10% glycerine, 1%DK4 type nano imvite, 3% potassium sorbate.
Preparation method comprises the following steps:
After being cleaned in distilled water by PVA particle, send into constant temperature blast drying oven in 70 DEG C of dry 12h.Accurately take the dried PVA particle of 30g in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h to PVA particle as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely.Again respectively to the DK4 type MMT and 3% potassium sorbate that add 1% in PVA mother liquor, and constant temperature stirs 4h to MMT powder and potassium sorbate and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, prepare antimicrobial nano laminated film mother liquor, use casting method dry 3h at 60 DEG C to obtain modified Nano packaging film C.
Embodiment 4
Composition of raw materials: by the mass percent relative to PVA, PVA, 10% glycerine, 1%DK4 type nano imvite, 1% Quaternary Ammonium Salt of Chitosan.
Preparation method comprises the following steps:
After being cleaned in distilled water by PVA particle, send into constant temperature blast drying oven in 70 DEG C of dry 12h.Accurately take the dried PVA particle of 30g in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h to PVA particle as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely.Again respectively to the DK4 type MMT and 1% Quaternary Ammonium Salt of Chitosan that add 1% in PVA mother liquor, and constant temperature stirs 4h to MMT powder and Quaternary Ammonium Salt of Chitosan and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, antimicrobial nano laminated film mother liquor, uses casting method dry 3h at 60 DEG C to obtain modified Nano packaging film D.
Embodiment 5
Composition of raw materials: by the mass percent relative to PVA, PVA, 10% glycerine, 1%DK4 type nano imvite, 2% Quaternary Ammonium Salt of Chitosan.
Preparation method comprises the following steps:
After being cleaned in distilled water by PVA particle, send into constant temperature blast drying oven in 70 DEG C of dry 12h.Accurately take the dried PVA particle of 30g in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h to PVA particle as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely.Again respectively to the DK4 type MMT and 2% Quaternary Ammonium Salt of Chitosan that add 1% in PVA mother liquor, and constant temperature stirs 4h to MMT powder and Quaternary Ammonium Salt of Chitosan and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, antimicrobial nano laminated film mother liquor, uses casting method dry 3h at 60 DEG C to obtain modified Nano packaging film E.
Embodiment 6
Composition of raw materials: by the mass percent relative to PVA, PVA, 10% glycerine, 1%DK4 type nano imvite, 1% potassium sorbate and Quaternary Ammonium Salt of Chitosan press the composite promoting agent of 1:1.
Preparation method comprises the following steps:
After being cleaned in distilled water by PVA particle, send into constant temperature blast drying oven in 70 DEG C of dry 12h.Accurately take the dried PVA particle of 30g in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h to PVA particle as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely.Again respectively to add in PVA mother liquor 1% DK4 type MMT and potassium sorbate and Quaternary Ammonium Salt of Chitosan by the composite promoting agent of 1:1, and constant temperature stirs 4h to MMT powder and promoting agent and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, antimicrobial nano laminated film mother liquor, uses casting method dry 3h at 60 DEG C to obtain modified Nano packaging film F.
Embodiment 7
Composition of raw materials: by the mass percent relative to PVA, PVA, 10% glycerine, 1%DK4 type nano imvite, 2% potassium sorbate and Quaternary Ammonium Salt of Chitosan press the composite promoting agent of 1:1.
Preparation method comprises the following steps:
After being cleaned in distilled water by PVA particle, send into constant temperature blast drying oven in 70 DEG C of dry 12h.Accurately take the dried PVA particle of 30g in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h to PVA particle as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely.Again respectively to add in PVA mother liquor 2% DK4 type MMT and potassium sorbate and Quaternary Ammonium Salt of Chitosan by the composite promoting agent of 1:1, and constant temperature stirs 4h to MMT powder and promoting agent and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, antimicrobial nano laminated film mother liquor, uses casting method dry 3h at 60 DEG C to obtain modified Nano packaging film G.
Embodiment 8 (comparative group)
Composition of raw materials: by the mass percent relative to PVA, PVA, 1% glycerine, 1%DK4 type nano imvite.
Preparation method comprises the following steps:
After being cleaned in distilled water by PVA particle, send into constant temperature blast drying oven in 70 DEG C of dry 12h.Accurately take the dried PVA particle of 30g in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, and the glycerine adding massfraction 1% stirs 2h to PVA particle as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely.Again respectively to the DK4 type MMT adding 1% in PVA mother liquor, and constant temperature stirring 4h to MMT powder and PVA solution merge evenly at 95 DEG C, degassed 1h under-0.1MPa, prepare polyvinyl alcohol/imvite modified nano compound film mother liquor, use casting method dry 3h at 60 DEG C to obtain modified Nano packaging film H.
Storage index of fish freshness detects
Cold fresh meat A, cold fresh meat B, cold fresh meat C, cold fresh meat D, cold fresh meat E, cold fresh meat F, cold fresh meat G, cold fresh meat H (control group) are respectively the test group after adopting the preservative film A-H in embodiment 1-8 to pack and control group.Have detected pH and the total volatile basic nitrogen (TVB-N) of test group and control group after storage 2d, 4d, 6d, 8d, 10d respectively.Experimental result following (shown in accompanying drawing 1):
In figure:
As shown in Figure 1 at the storage initial stage, may be because pork does not freeze, the respiratory activity of meat tissue cell is active makes Body development glycolysis and ATP in muscle decompose, produce the acidic substance such as lactic acid, phosphoric acid respectively, cause meat sample pH to reduce gradually, along with the prolongation of storage time, due to the effect of the protease of endogenous proteinase in meat and microorganism secretion, degraded muscle protein is many skins and amino acid, and discharges basic group, thus the pH value of meat is gone up.In the detection period of 10 days, along with the prolongation of time, G group pH value is minimum, and change is more steady.And other group pH value generally will lower than the control group H (shown in accompanying drawing 2) not adding promoting agent.In figure:
Total volatile basic nitrogen belongs to protein breakdown products, and the content of these degradation productions and the freshness of animal food have obvious corresponding relation, so index can evaluate the freshness of animal food.As shown in the figure, along with the prolongation of storage time, the TVB-N value of all samples is in the trend risen, and its reason is that in meat, protein is broken down into the nitrogenous substances such as ammonia and amine for TVB-N changing conditions.At first 4 days of storage, each group difference was little, but along with the prolongation experimental group TVB-N of time will far below control group, in experimental group, G class value is minimum, and other groups TVB-N value is generally higher than the control group H not adding promoting agent, and this is consistent with the detected result of pH.
Claims (3)
1. a polyvinyl alcohol antimicrobial packaging film take polyvinyl alcohol resin as base material, with glycerine, potassium sorbate, Quaternary Ammonium Salt of Chitosan for modified additive, it is characterized in that: in the mixture in described modified additive, be also added with nano imvite; And polyvinyl alcohol antimicrobial packaging film mixes glycerine 10 weight part according to the polyvinyl alcohol resin of every 100 weight parts, mix polynite 1 weight part, mix potassium sorbate 1 ?3 parts ratio, mix Quaternary Ammonium Salt of Chitosan 1 ?the preparation of 2 parts.
2. a kind of polyvinyl alcohol antimicrobial packaging film as claimed in claim 1, it is characterized in that: the potassium sorbate in described modified additive and Quaternary Ammonium Salt of Chitosan form promoting agent combination by 1:1 compound proportion, and directly join in modified additive with the ratio of 1 ?2 weight part and use.
3. a kind of polyvinyl alcohol antimicrobial packaging film as claimed in claim 1, its preparation method draws together following steps:
1), after first being cleaned in distilled water by polyvinyl alcohol resin particle, constant temperature blast drying oven is sent in 70 DEG C of dry 12h;
2) the dried PVA particle of 30g is accurately taken in 270mL deionized water, at 25 DEG C, constant temperature stirs swelling 2h, with the mass percent of PVA, the glycerine adding massfraction 10% stirs 2h as softening agent constant temperature at 95 DEG C and melts obtained PVA mother liquor completely to polyvinyl alcohol resin particle;
3) respectively to adding the polynite of different ratio, potassium sorbate and Quaternary Ammonium Salt of Chitosan in polyvinyl alcohol resin mother liquor, and constant temperature stirs 4h to MMT powder and promoting agent and PVA solution merges evenly at 95 DEG C, degassed 1h under-0.1MPa, prepares antimicrobial nano laminated film mother liquor;
4) use casting method dry 3h film forming at 60 DEG C, prepare modified Nano antimicrobial packaging film.
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| CN105295118A (en) * | 2015-11-25 | 2016-02-03 | 合肥工业大学 | Active packaging film for food and preparation method thereof |
| CN106751619A (en) * | 2016-12-21 | 2017-05-31 | 淮南市润吉生态农业有限公司 | A kind of lentinus edodes strain stick with sterilization and anticorrosion effect exempts to cut water-retaining film and preparation method thereof |
| CN106832828A (en) * | 2016-12-21 | 2017-06-13 | 淮南市润吉生态农业有限公司 | A kind of lentinus edodes strain stick containing oleic acid modified kaolin exempts to cut water-retaining film and preparation method thereof |
| CN108129783A (en) * | 2017-12-25 | 2018-06-08 | 安徽省临泉县万隆塑料包装有限公司 | A kind of high-performance is packed for laminated film |
| CN108690305A (en) * | 2018-05-30 | 2018-10-23 | 安徽农业大学 | A kind of preparation method of high-performance organic-inorganic composite membrane |
| WO2018201616A1 (en) * | 2017-05-02 | 2018-11-08 | 上海海洋大学 | Method for use in preparing intelligent chromogenic antibacterial anti-oxidation protective film |
| CN109337157A (en) * | 2018-08-20 | 2019-02-15 | 蚌埠市维光塑胶制品有限公司 | A kind of antibacterial food freshness protection package |
| CN110016161A (en) * | 2019-04-18 | 2019-07-16 | 刘杰 | A kind of Wholly-degradable material and preparation method for shopping bag, mulch and awning film |
| CN111057336A (en) * | 2019-12-30 | 2020-04-24 | 武汉轻工大学 | Composite film for food and preparation method thereof |
| CN114957748A (en) * | 2022-05-21 | 2022-08-30 | 敖媛 | Antibacterial food packaging film and preparation method thereof |
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| CN105295118A (en) * | 2015-11-25 | 2016-02-03 | 合肥工业大学 | Active packaging film for food and preparation method thereof |
| CN106751619A (en) * | 2016-12-21 | 2017-05-31 | 淮南市润吉生态农业有限公司 | A kind of lentinus edodes strain stick with sterilization and anticorrosion effect exempts to cut water-retaining film and preparation method thereof |
| CN106832828A (en) * | 2016-12-21 | 2017-06-13 | 淮南市润吉生态农业有限公司 | A kind of lentinus edodes strain stick containing oleic acid modified kaolin exempts to cut water-retaining film and preparation method thereof |
| WO2018201616A1 (en) * | 2017-05-02 | 2018-11-08 | 上海海洋大学 | Method for use in preparing intelligent chromogenic antibacterial anti-oxidation protective film |
| CN108129783A (en) * | 2017-12-25 | 2018-06-08 | 安徽省临泉县万隆塑料包装有限公司 | A kind of high-performance is packed for laminated film |
| CN108690305A (en) * | 2018-05-30 | 2018-10-23 | 安徽农业大学 | A kind of preparation method of high-performance organic-inorganic composite membrane |
| CN109337157A (en) * | 2018-08-20 | 2019-02-15 | 蚌埠市维光塑胶制品有限公司 | A kind of antibacterial food freshness protection package |
| CN110016161A (en) * | 2019-04-18 | 2019-07-16 | 刘杰 | A kind of Wholly-degradable material and preparation method for shopping bag, mulch and awning film |
| CN111057336A (en) * | 2019-12-30 | 2020-04-24 | 武汉轻工大学 | Composite film for food and preparation method thereof |
| CN111057336B (en) * | 2019-12-30 | 2023-02-03 | 武汉轻工大学 | Composite film for food and preparation method thereof |
| CN114957748A (en) * | 2022-05-21 | 2022-08-30 | 敖媛 | Antibacterial food packaging film and preparation method thereof |
| CN114957748B (en) * | 2022-05-21 | 2023-12-08 | 深圳市聚亿新材料科技股份有限公司 | Antibacterial food packaging film and preparation method thereof |
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