CN103707609B - Temp-sensitive, slow-releasing gas phase preservation compound film of a kind of bakery product and preparation method thereof - Google Patents
Temp-sensitive, slow-releasing gas phase preservation compound film of a kind of bakery product and preparation method thereof Download PDFInfo
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Abstract
Temp-sensitive, slow-releasing gas phase preservation compound film that the invention discloses a kind of bakery product and preparation method thereof, comprises the steps: that, by polycaprolactone and 4,4 '-methyl diphenylene diisocyanate, reacts 1-2h at 70-90 DEG C; Add BDO and 4 again, 4 '-methyl diphenylene diisocyanate also reacts 1.5-2.5h at 70-90 DEG C, obtains temperature sensitive polyurethane solutions; The solid content controlling temperature sensitive polyurethane solutions controls as 12-25wt%, and above-mentioned solution is placed in polytetrafluoroethylene (PTFE) to be become in template, volatilizes DMF solvent, obtained temperature sensitive polyurethane film; This film applies antiseptic, then adopts hot press to bond film and high barrier polymer material, obtained preservation compound film.Composite membrane of the present invention, by changing the release of the fresh-keeping composition of variable temperature control gas phase, while the good fresh-keeping effect of maintenance, reduces the use amount of anticorrisive agent and antioxidant in bakery product, extended shelf-life more than one times.
Description
Technical field
The present invention relates to intelligent packaging for foodstuff membrane preparation technology, relate generally to a kind of temp-sensitive, slow-releasing gas phase preservation compound film for bakery product and preparation method thereof.
Background technology
Being packaged in and providing protection to food, prevent food to be subject to the pollution of external microbe or other material, prevent or reduce Food Oxidation and there is irreplaceable effect other reaction aspect, is the important means of food preservation.Traditional food packaging material mainly through passive obstruct gas, water and microorganism etc. through and reach the object of taste of guaranteeing the quality.But along with the raising of people's living standard, to fresh, the demand of healthy food also increases day by day, the storage of food, and long-distance consuming etc. propose new challenge to packaging material.
Active packing can regulate the environment residing for packaged food and then better preserve food, becomes the study hotspot of domestic and international food circle.In active packing, antimicrobial packaging is in the packing container of sealing, enclose the parcel of energy delivery of antimicrobials or utilize the packaging material of energy delivery of antimicrobials to carry out connection with wrapping of piece, reaching Antimicrobial preservative object, enable packed article be able to a kind of packing technique of long period preservation.The microorganism of food surface is one of principal element affecting Food Shelf-life and security, and in order to suppress the growth of spoilage organisms in food, adopt antibiotic packaging material, it can kill or suppress the microorganism on food surface in processing, accumulating and processing procedure.Therefore, antimicrobial packaging can extend shelf life and the security of food effectively.After using antibiotic packaging material, a large amount of anticorrisive agents need not be added as conventional procedure in food processing and production process, effectively prevent the Excess free enthalpy of anticorrisive agent, using and packing two flow processs and unite two into one simultaneously by anticorrisive agent, also greatly simplify processing technology.Therefore, antibiotic packaging material is just towards safety, efficiently future development.
Intellectual material to environment can perception, can respond, and there is the functions such as function ability of discovery, detection, process.As temperature sensitive polymer, ionic strength responsive polymer etc.In environment-responsive polymeric system, temperature sensitive polymer due to variations in temperature be easy to control, and temperature is the most widely used stimulus signal, because variations in temperature easily causes quality deterioration and the microbial reproduction of food, so temperature sensitive polymer represents huge application prospect in the intelligent packaging for foodstuff controlled release preservation technique that exploitation is new.
Baked goods, its complex manufacturing technology, formula are unique, moisture and the more high reason of fat content, easily produce Oxidation of Fat and Oils, mouldy, spoiled, the not easily problem such as preservation in high temperature and high humidity environment.Microorganism, through the high-temperature baking of more than 200 DEG C, can all kill by bakery product.But, due to misoperation in the cooling and technology of the package of bakery product, form the microbial contamination of food, in transport and storage (especially temperature is within the scope of 30-50 DEG C), as easy as rolling off a logly cause microbial reproduction and Food Oxidation, make food quality generation deterioration and the phenomenon such as mouldy.In addition, at shorter or microbial growth initial stage time of the contaminated food products of microorganism, more easily killed by antistaling agent.
In order to prevent mouldy, the spoiled and growth of microorganism of baked goods, most manufacturing enterprises adopt methods such as adding antioxidant, anticorrisive agent and deoxidier to extend storage life.Due to the condition harsher (at low pH and non high temperature) that current most anticorrisive agent uses, and baked goods is close to neutral and hot conditions use, has that corrosion-resistanting fresh-keeping effect is undesirable, poor stability, residual quantity are high and the problem such as security.And the problems such as deoxidier method exists that packing cost is high, sanitary condition strict, gas leakage.Therefore, anticorrosion and additive security in baked goods production process, high efficiency, stability and the problem such as long-lasting, become the bottleneck of restriction bakery product industry development.
Summary of the invention
The present invention is directed to baked goods perishable, shelf-life short and antioxidant, anticorrisive agent easily exceeds standard and the problem such as use safety, from food additives safety and fresh-keeping long-lasting, adopt release internal layer and the outer field composite membrane of high barrier of preparing temperature-sensing property, and combination has volatile high-performance bio Antibacterial Constituents and natural, gas phase release and Co ntrolled release are carried out to biological preservation active component, prevent high oil, the oxidation of the baked goods of high-moisture and the product such as mouldy shoddy, to ensure peculiar flavour and the edible quality of baked goods, reach the long-term slow releasing of the fresh-keeping active component of volatility and extend the object of bakery product shelf-life.
The object of the invention is achieved through the following technical solutions:
A preparation method for the temp-sensitive, slow-releasing gas phase preservation compound film of bakery product, comprises the steps:
(1) by polycaprolactone (PCL), 4,4 '-methyl diphenylene diisocyanate (MDI) is dissolved in DMF solvent, at 70-90 DEG C, react 1-2h; Then in said mixture, add BDO (BDO) and 4,4 '-methyl diphenylene diisocyanate (MDI) also reacts 1.5-2.5h at 70-90 DEG C, obtains temperature sensitive polyurethane solutions; In above-mentioned reaction system, the mol ratio of-NCO and-OH group controls as 1:1, and add DMF to regulate reaction system viscosity, the solid content of temperature sensitive polyurethane solutions controls as 12-25wt%, then above-mentioned solution being placed in polytetrafluoroethylene (PTFE) becomes in template, DMF solvent is volatilized, obtained temperature sensitive polyurethane film at 60-90 DEG C;
(2) on obtained temperature sensitive polyurethane film, coat film weighs volatile antiseptic of 1%-5%, adopts hot press to bond the temperature sensitive polyurethane film after process and high barrier polymer material, obtained temp-sensitive, slow-releasing gas phase preservation compound film.
In described polycaprolactone and system total 4, the mol ratio of 4 '-methyl diphenylene diisocyanate is 1:(1.5 ~ 2.5).
The weight average molecular weight of described polycaprolactone is 3000-8000.
The solid content of described temperature sensitive polyurethane solutions first controls as 25-50wt%; Be allocated as 12-25wt% further again.
Described antiseptic is one or more in carvacrol, cinnamic acid and caryophyllus oil.
Described high barrier polymer material is nylon.
The temperature that step (2) adopts hot press to carry out bonding is 90-150 DEG C, and pressure is 0.1MPa-0.3MPa, and the time is 2-5s.
Compared with prior art, the present invention has following beneficial effect:
(1) according to bakery product in the present invention in cooling and packing stage secondary pollution feature and microorganism easily grows in 30-50 DEG C characteristic, by the control such as the structure to temperature sensitive polyurethane flexible segment, chain length, soft section and hard section ratio, regulate its phase transition temperature of soft section, design switch temperature is the temperature-responsive polyurethane cellular material of 35-55 DEG C, the microbial contamination of bakery product initial stage and easily cause in the temperature range of food deterioration, the volatile fresh-keeping active component of controlled release, reaches optimal anti-staling effect.
(2) the present invention has prepared the temp-sensitive, slow-releasing gas phase preservation compound film at 35-55 DEG C with Co ntrolled release function by MULTILAYER COMPOSITE technology.This composite membrane is three-decker, and a internal layer controlled release material is the temperature sensitive polyurethane film with temperature-responsive; B intermediate layer adopts volatile natural antibacterial active component; C skin adopts high barrier polymer material.When food is cooled to 30-50 DEG C, becomes in the aperture of the temperature sensitive polyurethane cellular material of composite packaging film inner layer large, discharge the fresh-keeping active component of gas phase at short notice fast, at the initial stage that bakery product pollutes, kill the microorganism of pollution as much as possible.Meanwhile, while the good fresh-keeping effect of maintenance, the use of anticorrisive agent, deoxidier in bakery product is decreased.
(3) adopt release internal layer and the outer field composite membrane of high barrier of preparing temperature-sensing property, pack with original bakery product and contrast, obviously more effectively can suppress growth of microorganism, thus reach the object extending the bakery product shelf-life.
Accompanying drawing explanation
Fig. 1 is the process chart of the inventive method;
The switch temperature of Fig. 2 embodiment 4 (PCL3000, carvacrol);
The switch temperature of Fig. 3 embodiment 4 (PCL4000, carvacrol);
The switch temperature of Fig. 4 embodiment 4 (PCL8000, carvacrol);
Rate of perviousness under Fig. 5 gas phase preservation compound film different temperatures;
Fig. 6 composite membrane antiseptic release rate figure.
Detailed description of the invention
Embodiment 1
By 1mol polycaprolactone (PCL, Mw=3000), 2mol4,4 '-methyl diphenylene diisocyanate (MDI), DMF (DMF) solvent of 700g, reacts 1.5h at 70 DEG C, forms soft section of phase.Then BDO and MDI adding metering reacts 1.5h and forms hard section at 70 DEG C, and soft or hard section alternately forms block polymer; In course of reaction, the mol ratio keeping-NCO and-OH group is 1:1, and regulate the viscosity change in reaction system with DMF, temperature sensitive polyurethane solutions solid content controls as 25wt%.Being adjusted to solid content with DMF further is again 15wt%, being placed in polytetrafluoroethylene (PTFE) becomes in template, volatilize DMF solvent at 60 DEG C, obtained temperature sensitive polyurethane film, on obtained polyurethane film, it brushing is the antiseptic (carvacrol) that film weighs 2%, adopt hot press to bond the polyurethane film after process and nylon, temperature is 90 DEG C, and pressure is 0.2MPa, time is 2s, the obtained anticorrosion composite membrane of temperature sensitive type.
Embodiment 2
By 2mol polycaprolactone (PCL, Mw=4000), 3.5mol4,4 '-methyl diphenylene diisocyanate (MDI), DMF (DMF) solvent of 1200g, reacts 1h at 75 DEG C, forms soft section of phase.Then BDO and MDI adding metering reacts 1.5h and forms hard section at 80 DEG C, and soft or hard section alternately forms block polymer; In course of reaction, the mol ratio keeping-NCO and-OH group is 1:1, and regulate the viscosity change in reaction system with DMF, temperature sensitive polyurethane solutions solid content controls as 45wt%.Being adjusted to solid content with DMF further is again 25wt%, being placed in polytetrafluoroethylene (PTFE) becomes in template, volatilize DMF solvent at 75 DEG C, obtained temperature sensitive polyurethane film, on obtained polyurethane film, it brushing is the antiseptic (cinnamic acid) that film weighs 2%, adopt hot press to bond the polyurethane film after process and nylon, temperature is 90 DEG C, and pressure is 0.15MPa, time is 3s, the obtained anticorrosion composite membrane of temperature sensitive type.
Embodiment 3
By 0.2mol polycaprolactone (PCL, Mw=8000), 0.5mol4,4 '-methyl diphenylene diisocyanate (MDI), DMF (DMF) solvent of 400g, reacts 2h at 80 DEG C, forms soft section of phase.Then BDO and MDI adding metering reacts 2h and forms hard section at 80 DEG C, and soft or hard section alternately forms block polymer; In course of reaction, the mol ratio keeping-NCO and-OH group is 1:1, and regulate the viscosity change in reaction system with DMF, temperature sensitive polyurethane solutions solid content controls as 30wt%.Being adjusted to solid content with DMF further is again 20wt%, being placed in polytetrafluoroethylene (PTFE) becomes in template, volatilize DMF solvent at 70 DEG C, obtained temperature sensitive polyurethane film, on obtained polyurethane film, antiseptic (1% carvacrol+1% cinnamic acid) in brushing, adopt hot press to bond the polyurethane film after process and nylon, temperature is 120 DEG C, and pressure is 0.1MPa, time is 2s, the obtained anticorrosion composite membrane of temperature sensitive type.
Embodiment 4
Add 0.1mol polycaprolactone (PCL, get Mw=3000,4000,8000 respectively) and 0.2mol 4,4 '-methyl diphenylene diisocyanate (MDI), add the N of 100g, dinethylformamide (DMF) solvent, at 80 DEG C, react 1.5h, form soft section of phase.Then BDO and MDI adding metering reacts 2h and forms hard section at 80 DEG C, and soft or hard section alternately forms block polymer; In course of reaction, the mol ratio keeping-NCO and-OH group is 1:1, and regulate the viscosity change in reaction system with DMF, temperature sensitive polyurethane solutions solid content controls as 30wt%.Being adjusted to solid content with DMF further is again 15wt%, being placed in polytetrafluoroethylene (PTFE) becomes in template, volatilize DMF solvent at 70 DEG C, obtained temperature sensitive polyurethane film, on obtained polyurethane film, it brushing is the antiseptic (carvacrol or cinnamic acid) of 2%, adopt hot press to bond the polyurethane film after process and nylon, temperature is 90 DEG C, and pressure is 0.15MPa, time is 4s, the obtained anticorrosion composite membrane of temperature sensitive type.
Embodiment 5
Add 4 of 0.1mol polycaprolactone (PCL gets Mw=4000) and 0.2mol, 4 '-methyl diphenylene diisocyanate (MDI), add the N of 200g, dinethylformamide (DMF) solvent, reacts 2h at 80 DEG C, forms soft section of phase.Then BDO and MDI adding metering reacts 2h and forms hard section at 80 DEG C, and soft or hard section alternately forms block polymer; In course of reaction, the mol ratio keeping-NCO and-OH group is 1:1, and regulate the viscosity change in reaction system with DMF, temperature sensitive polyurethane solutions solid content controls as 30wt%.Being adjusted to solid content with DMF further is again 20wt%, being placed in polytetrafluoroethylene (PTFE) becomes in template, volatilize DMF solvent at 75 DEG C, obtained temperature sensitive polyurethane film, on obtained polyurethane film, antiseptic (carvacrol or cinnamic acid in brushing, be respectively film and weigh 2%, 3%, 4%, 5%), adopt hot press to bond the polyurethane film after process and nylon, temperature is 90 DEG C, pressure is 0.2MPa, and the time is that 3s obtains the anticorrosion composite membrane of temperature sensitive type.
Implementation result
1) TSPU switch temperature measures
The switch temperature of temp-sensitive, slow-releasing gas phase preservation compound film adopts differential scanning calorimeter to carry out analytical test.Experiment condition: nitrogen atmosphere, sample film quality is 5-10mg, and temperature range is-50-250 DEG C, and heating rate is 10 DEG C/min.
Measure the switch temperature of temperature sensitive temp-sensitive, slow-releasing gas phase preservation compound film obtained in embodiment 4.From Fig. 2, Fig. 3, Fig. 4, the switch temperature of composite membrane is respectively 46.3 DEG C, 53.9 DEG C and 47.9 DEG C, has successfully been prepared the temp-sensitive, slow-releasing gas phase preservation compound film at 30-55 DEG C with Co ntrolled release function by MULTILAYER COMPOSITE technology.
2) permeability measures (temperature-responsive)
Test according to ASTME standard (the transmission of water vapor standard method of test of material).The anhydrous CaCl of metering is inserted in identical beaker
2then embodiment 1 composite membrane is covered rim of a cup, thing is tamping in case can exchange with sealing compound, then moisture vapor transmission cup being put people's constant humidity is 50%, constant pressure is in the incubator of 1atm, probe temperature is set as 15 DEG C, 25 DEG C, 35 DEG C, 45 DEG C, 55 DEG C, 65 DEG C respectively, measures the change of moisture vapor transmission cup weight after 24h.
Rate of perviousness can adopt its rate of perviousness of formula that formula can be adopted to calculate, and (unit is g ˙ m
-2˙ 24h):
Wherein, a
1-a
2, be the change (g) of quality in moisture vapor transmission cup;
S: the area (m of moisture vapor transmission cup
2).
As seen from Figure 5, along with the rising of temperature, composite membrane rate of perviousness has rising by a relatively large margin, and wherein from 35 DEG C, the slope of curve obviously becomes large, and rate of perviousness has a distinct increment, and after 55 DEG C, rate of perviousness declines to some extent.This is because composite membrane becomes large in 35-55 DEG C of its aperture at the temperature sensitive polyurethane cellular material of composite packaging film inner layer, gas permeation can be made at short notice greatly to increase, thus reach and can control diactinic object by control temperature.
3) release performance measures
Composite membrane is prepared by condition described in embodiment 5, antiseptic and concentration is regulated to be 2%, 3%, 4%, 5%, prepared composite membrane mass change is measured with analytical precision balances every 3 days, measure the release rate of antiseptic with this, the measurement result of Co ntrolled release antibacterial activity packaging material release rate is as shown in table 3.The computing formula of release rate is:
Release rate=(m
1-m
2)/m
0
In formula, m
1---initial packaging bag quality; m
2---the packaging bag quality after volatilization; m
0---antiseptic quality initial in packaging bag (can by m
1the concentration being multiplied by antiseptic is tried to achieve).
As shown in Figure 6, the rate of release of every 3 days of temp-sensitive, slow-releasing gas phase preservation compound film is 0.6 ~ 2.2%, along with the interpolation of variable concentrations antiseptic, the rate of release difference to some extent of obtained temp-sensitive, slow-releasing gas phase preservation compound film, the temp-sensitive, slow-releasing gas phase preservation compound film sustained release performance wherein adding 3 ~ 4% antiseptics is relatively excellent.
4) fresh-keeping effect measures
Temp-sensitive, slow-releasing gas phase preservation compound film obtained under embodiment 4 different condition is carried out bacteriostatic experiment respectively.Antibacterial film being cut into diameter is that the sequin of 0.5cm is some, puts into containing 10 after high-temperature steam sterilization
7~ 10
8the test panel central authorities of bacterium colony, 24h cultivated by incubator Escherichia coli, hay bacillus being placed in 36 DEG C ± 1 DEG C, and 72h cultivated by incubator mould being placed in 28 ± 1 DEG C.Repeating test 3 times, averages, and evaluates the size of antibacterial activity by comparing inhibition zone size.
The antibacterial loop diameter (mm) of table 1 composite membrane
As can be seen from Table 1, the composite membrane that with the addition of antiseptic all has obvious inhibitory action to Escherichia coli, hay bacillus, mould.The anticorrosion composite membrane that with the addition of carvacrol is all very strong to the inhibitory action of three kinds of bacterium, and load cinnamic acid sustained-release antibacterial film takes second place; Antiseptic can discharge at composite membrane, produces obvious inhibitory action to microorganism.Meanwhile, in compound, the molecular weight of polyalcohol can't have a significant impact the inhibitory action of antiseptic.
5) for the performance measurement of preservation bakery product
The warm temp-sensitive, slow-releasing gas phase preservation compound film that embodiment 1,2,3 is obtained respectively carries out bakery product keeping property mensuration.The bread that anticorrisive agent is not added in fresh cleaning by aseptic working platform loads composite membrane, and after heat-sealing, 48h cultivated by the incubator being placed in 36 DEG C ± 1 DEG C, measures that bread is initial, the total number of bacteria of ordinary packing bread, composite film packaging bread and Escherichia coli sum.
Table 2 bread keeping property is tested
Can be obtained by table 2, ordinary packing and composite membrane all can meet the preservation requirement of bread, GB20981-2007 requires total number of bacteria≤1500CFU/g in bread, Escherichia coli≤30MPN/100g, meet food preservation sanitary standard, and contrast ordinary packing mode, more effectively suppress growth of microorganism situation, extend the shelf life.
Claims (8)
1. a preparation method for the temp-sensitive, slow-releasing gas phase preservation compound film of bakery product, is characterized in that, comprise the steps:
(1) by polycaprolactone, 4,4 '-methyl diphenylene diisocyanate is dissolved in DMF solvent, at 70-90 DEG C, react 1-2h; Then in said mixture, add BDO and 4,4 '-methyl diphenylene diisocyanate also reacts 1.5-2.5h at 70-90 DEG C, obtains temperature sensitive polyurethane solutions; In above-mentioned reaction system, the mol ratio of-NCO and-OH group controls as 1:1, and add DMF to regulate reaction system viscosity, the solid content of temperature sensitive polyurethane solutions controls as 12-25wt%, then above-mentioned solution being placed in polytetrafluoroethylene (PTFE) becomes in template, DMF solvent is volatilized, obtained temperature sensitive polyurethane film at 60-90 DEG C;
(2) on obtained temperature sensitive polyurethane film, coat film weighs volatile antiseptic of 1%-5%, adopts hot press to bond the temperature sensitive polyurethane film after process and high barrier polymer material, obtained temp-sensitive, slow-releasing gas phase preservation compound film.
2. preparation method according to claim 1, is characterized in that, in described polycaprolactone and system total 4, the mol ratio of 4 '-methyl diphenylene diisocyanate is 1:(1.5 ~ 2.5).
3. preparation method according to claim 2, is characterized in that, the weight average molecular weight of described polycaprolactone is 3000-8000.
4. the preparation method according to claim 1 or 2 or 3, is characterized in that, the solid content of described temperature sensitive polyurethane solutions first controls as 25-50wt%; Be allocated as 12-25wt% further again.
5. the preparation method according to claim 1 or 2 or 3, is characterized in that, described antiseptic is one or more in carvacrol, cinnamic acid and caryophyllus oil.
6. the preparation method according to claim 1 or 2 or 3, is characterized in that, described high barrier polymer material is nylon.
7. the preparation method according to claim 1 or 2 or 3, is characterized in that, the temperature that step (2) adopts hot press to carry out bonding is 90-150 DEG C, and pressure is 0.1MPa-0.3MPa, and the time is 2-5s.
8. the temp-sensitive, slow-releasing gas phase preservation compound film prepared of claim 1 ~ 7 any one method.
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| CN107379703B (en) * | 2017-07-21 | 2019-04-19 | 上海海洋大学 | A kind of control release type active packing film and preparation method thereof |
| CN108912627A (en) * | 2018-05-30 | 2018-11-30 | 苏州汉德瑞生物工程有限公司 | A kind of degradable controlled release antibiotic food packaging and preparation method |
| CN110724295B (en) * | 2019-10-27 | 2021-08-24 | 江南大学 | Temperature-sensitive polyurethane gas-phase controlled-release antioxidant composite membrane and preparation method thereof |
| CN112167250A (en) * | 2020-10-13 | 2021-01-05 | 重庆中邦药业（集团）有限公司 | Temperature-sensitive type cyflumetofen capsule sustained release agent and preparation method thereof |
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