CN104293275B - Uvioresistant digestion resistant adhesive and its preparation method and application - Google Patents
Uvioresistant digestion resistant adhesive and its preparation method and application Download PDFInfo
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Abstract
The present invention discloses a kind of uvioresistant digestion resistant adhesive and its preparation method and application, and uvioresistant digestion resistant adhesive is applied to the composite membrane of resistance to boiling, bag, includes the component of following parts by weight：The parts by weight of PEPA 28 42；The parts by weight of isocyanates 46；The parts by weight of titanium dioxide 36；The parts by weight of silica 37；The parts by weight of organo silane coupling agent 0.5 1；With the parts by weight of ethyl acetate 40 62.The composite membrane of resistance to boiling prepared therefrom, bag have anti-ultraviolet function, improve opacity and barrier, and the shelf-life of its packaged food is longer；Its technological process of production is short, and production cost sticks the agent complex pocket of resistance to boiling compared to traditional high temperature resistant two-component polyurethane adhesive can decline 20% or so.
Description
Technical field
The present invention relates to the composite membrane of resistance to boiling, bag technique field, a kind of specifically disclosed uvioresistant digestion resistant gluing
Agent and its preparation method and application.
Background technology
With China's expanding economy, the prosperity of tourist industry, the emergence of golden week economy, demand of the people to instant food
It is increasing.The instant food such as foods packed in carton containers and high-temperature cooking food, it is not only numerous in variety, and also quantity required is huge.It is large quantities of high
Barrier, high impact properties, thermophilic digestion resistance, the food packaging items of resistance to medium arise at the historic moment, so as to ensure that conveniently
The fresh and nutrition of food, extends the shelf-life of instant food, is the optimal packaging material of foods packed in carton containers.
High-temperature retort bag is a kind of composite plastic film bag that can be heated, and it has Can container and resistance to boiling water
The advantage of both polybags.Food can remain untouched in bag, by high temperature (typically at 120~135 DEG C) sterilization processing, take out
Just edible.The food of high temperature sterilization such as uses Trend of High Obstructive Materials Ordnance Engineering College, and not only the storage shelf-life is longer at normal temperatures, and
Transport, storage sells all very convenient, is especially suitable for the consumption demand of modern society.
High-performance barrier film or high-barrier packaging are widely used in food service industry.The main bag of film class high-barrier packaging
Include following several classes：
(1) PVA is coated with high-isolation film
PVA coating high-isolation films are to be coated on the PVA that with the addition of nano-inorganic substance after polyethylene film through printing, again
Conjunction is formed, on the premise of cost is not increased substantially, and solves current three-layer polyethylene co-extrusion packing film barrier property poor
Technical bottleneck, PVA coating high-isolation film pushed market to comprehensively.
(2) PVDC (polyvinylidene chloride)
PVDC resins, frequently as composite or monomer material and coextruded film piece, are packed using most high barriers
Material, wherein PVDC coated films usage amount are especially more.
(3) EVOH (ethylene/vinyl alcohol copolymer)
EVOH is always to apply most high barrier materials.
(4) nylon based packaging material
" nylon 6 " is used before nylon based packaging material always.
(5) inorganic oxide plating film
On the film of other base materials plating SiOx (silica) afterwards obtained so-called plating film increasingly by market
Pay attention to, in addition to silica plated film, also aluminum oxide evaporated film.
At present, the retort pouch overwhelming majority in the world is manufactured with dry type composite algorithm, and few in number can also use nothing
Solvent composite algorithm or coextrusion composite algorithm go manufacture.The compound quality of dry type is than solvent-free compound high, the arrangement group of material
It is also more reasonable and extensive than what coextrusion was combined to close, and is also more trusted using upper.For example, patent CN103273724A discloses one kind
The processing method for obstructing boiling type packaging film, comprises the following steps：A, get the raw materials ready：Get out binding agent and need the packaging of processing
Film base material；B, gluing are combined：Gluing cable roll or glue spreader in glue application device are utilized in bag using common glue application device
Binding agent on the film base material table even Tu in face is filled, then is formed coated basement membrane again with another basement membrane pressure viscosity by composite press roller
Close film；C, curing：Composite membrane is inserted in 40-60 degrees Celsius of curing chamber 72-168 hours；D, making finished product：After curing
Obtained barrier boiling type packaging film composite membrane finished product, by above-mentioned barrier boiling type packaging film by being obtained after cutting or bag
To barrier boiling type packaging film wound membrane or barrier boiling type packaging film sack.Patent CN103879125A discloses thermophilic digestion
The solvent-free complex method and its set composite of composite membrane, bag, the complex method are that the first film is pre-processed, and are mounted in
Moved towards on first unwinding device and by Film laminated through guide roller；It is combined through glue spreading apparatus drying and composite part；By
Two films on the second unwinding device and are moved towards through guide roller by Film laminated；Adjust glue spreading apparatus enters glue amount, progress
Production；Finally wound, cured and cooled down again.The set composite includes rack-mounted first unwinding device, gluing
Device, the second unwinding device, compound hot drum, wrap-up and carry-over pinch rolls；And for adding adding for adhesive to glue spreading apparatus
Glue bucket.
Generally, the compound manufacturing process of dry type comprises the following steps：
It is selection first.To be gone to determine according to the final use of retort pouch using which base material, how combined, which kind of is used
Ink and adhesive.
Then, in concrete operations, the technological parameter of technique list is followed, the line number and site including glue spreader are deep
Degree, the concentration of operation glue, the temperature of each bringing-up section of drying tunnel, the size of blow rate required rim of the mouth exhaust air rate, the height of starting up speed, also
There are unwinding tension, drying tunnel tension force, the control of winding tension, the surface temperature of composite steel roll and composite pressure etc..
3rd, in specific composition operation, some adhesive suppliers are required two layers of (PET/AL or OPA/ for the first time
AL the curing room that 50~55 DEG C are first dropped it off after) getting well again goes to place after 4h or 12h, then carries out second of third layer (PET/
AL/CPP or PET/AL/OPA) it is compound, this process will be had each time by be combined, but also have much that gluing punishment can be with a gas
Breathe out into two layers of ground, three layers of even four layers of whole it is good again after, the curing chamber for being just put into 50~55 DEG C goes to allow it to cure.
4th is curing.Temperature and the time of curing on curing, typically require at 50~55 DEG C holding 48h with
On, best 72h, but also the requirement of some adhesive is put 15~7 days.
5th is detection bag.After compound is cured, the compound fastness and residual solvent amount of interlayer, data are first detected
Reach after requirement, can just take out bag of taking away.
The national standard that high-temperature retort bag is used is GB10004-1998《The composite membrane of resistance to boiling, bag》, the material knot of product
Structure include bis- layers of PET/CPP, PA/CPP transparent type and tri- layers of PET/AL/CPP, PA/AL/CPP opaque type and
The transparent type that tri- layers of PET/PA/CPP, also this three major types of tetra- layers of PET/AL/PA/CPP opaque type.
Digestion resistant adhesive technology is also constantly developed, and such as patent CN1232851A discloses polyurethane high temperature
Retort pouch composite dry adhesive, the component of the component of its product by weight is：Diethylene glycol (DEG) 13.64~18.6%；Decanedioic acid
23.26~25.73%；1,2- propane diols 2.06~2.94%；M-phthalic acid 6~5.43%；Diphenylmethane diisocyanate
Ester 3.86~5.74%；Ethyl acetate 48.71~44.03%.It is double that patent CN1629245A discloses a kind of boiling resistant polyurethane
Component adhesive, including mass percentage content are 50-90% host and 10-50% curing agent；Described host is by (A)
The PEPA composition that the polyester ether polylol and (B) hydroxyl value that hydroxyl value is 10-30mgKOH/g are 30-100mgKOH/g；It is described
Curing agent be polyisocyanate prepolymers.Patent CN103666344A discloses a kind of digestion resistant composite soft packaging film and used
The preparation method of adhesive, first by gamma-aminopropyl-triethoxy-silane to Nano-meter SiO_22Carry out surface graft modification；Add
Polyisocyanates and oligomer polyol, add hydrophilic chain extender reaction and obtain base polyurethane prepolymer for use as；Use modified Nano
SiO2It is modifies to polyurethane prepolymer；Add hydroxy acryl acid ester end-blocking；Carry out neutralizing after cooling disperseing, obtain modified water-soluble and gather
Urethane hybrid emulsions；Using dispersion as seed emulsion and macromolecule emulsifier, fluorinated acrylate and initiator are added, is led to
Cross seeded emulsion polymerization and prepare multiple modified aqueous polyurethane complex emulsions；Thickener and defoamer are added to the complex emulsions,
Obtain multiple modified aqueous polyurethane composite gel stick.But, adopt and use the high barrier materials such as Tu (boiling) films or pure aluminum foil, its
Raw material processing process length, cost are high, according to the retort pouch of pure aluminum foil technique productions, it is impossible to use microwave stove heat.
The content of the invention
It is an object of the invention to provide a kind of uvioresistant digestion resistant adhesive, it can be applied to resistance to boiling and be combined
Film, bag, it not only possesses resistance to elevated temperatures, also with anti-ultraviolet function, improves opacity and the barrier of high-temperature retort bag
Property.
It is another object of the present invention to provide a kind of method for preparing uvioresistant digestion resistant adhesive, its work
Skill flow is short, and production cost is low.
A further object of the present invention be to provide a kind of uvioresistant digestion resistant adhesive the composite membrane of resistance to boiling,
Application in bag.
The present invention provides a kind of uvioresistant digestion resistant adhesive, it is adaptable to the composite membrane of resistance to boiling, bag, including as follows
The component of parts by weight：PEPA 28-42 parts by weight；Isocyanates 4-6 parts by weight；Titanium dioxide 3-6 parts by weight；Titanium dioxide
Silicon 3-7 parts by weight；Organo silane coupling agent 0.5-1 parts by weight；With ethyl acetate 40-62 parts by weight.
PEPA is matrix resin, and isocyanates makees curing agent, and being added with for inorganic filler is beneficial to improve thermally-stabilised
Property, barrier, opacity, organo silane coupling agent can strengthen the coefficient of elasticity of glue.Wherein, the addition of inorganic filler is not
It is easily excessive, it otherwise can cause the degradation of peel strength.The present invention adds appropriate silica on the basis of titanium dioxide
There is humidification to peel strength, to realize cooperative effect.
Preferably, described PEPA is selected from the PEPA that hydroxyl value is 20-90mgKOH/g, its solid content is
65-72%, viscosity is 3000-8000mPas；For 28-42 parts by weight, such as 28,29,30,31,32,33,34,35,36,37,
38th, 39,40,41 or 42 parts by weight, it is preferred that be 28-38 parts by weight, such as 28.5,29.5,30.5,31.5,32.5,33.5,
34.5th, 36.5,37.5 parts by weight, it is further preferred that being 28-32 parts by weight, but are also not necessarily limited to this.
PEPA, organic matter is typically to be contracted by Dicarboxylic Acids (acid anhydrides or ester) and polyalcohol (including glycol)
Close (or ester exchange) or formed by lactone with polymerization.Binary acid have phthalic acid or phthalate anhydride or its ester, oneself two
Acid, halo phthalic acid etc..Polyalcohol has ethylene glycol, propane diols, diglycol, trimethylolpropane, pentaerythrite etc..
The PEPA of different cultivars is because species is different or preparation technology is different, and property is also different, for PEPA
Important several indexs are hydroxyl value, acid number, moisture, viscosity, molecular weight, density and colourity etc..The spy of PEPA
Property and purposes：The PAUR ester group more because intramolecular contains, amino isopolarity group, cohesive strength and adhesive force
By force, with higher intensity, wearability.
Preferably, described isocyanates is selected from toluene di-isocyanate(TDI), di-isocyanate and two benzaldehyde methane cyanic acid
One or more in ester, its solid content is 75 ± 2%, viscosity 1000-3000mPas, is 4-6 parts by weight, such as 4,4.5,5,
5.5th, 6 parts by weight, preferably 4-5.5 parts by weight, it is further preferred for 4-5 parts by weight, but it is also not necessarily limited to this.
Isocyanates be widely used in rigid foam, RIM (resin injection moulding) elastomer, TPUE,
The fields such as coating, bonding agent, elastomer and construction material.In the present invention, preferably toluene di-isocyanate(TDI), two isocyanic acids
One or more in ester and two benzaldehyde methane cyanates.
Preferably, described organo silane coupling agent is preferably γ-(2,3- glycidoxy) propyl trimethoxy silicane.
Described organo silane coupling agent be 0.5-1 parts by weight, such as 0.5,0.6,0.7,0.8,0.9,1 parts by weight, further preferably
For 0.5-0.8 parts by weight.γ-(2,3- glycidoxy) propyl trimethoxy silicane, alias is silane coupler KH-560；
Silane coupling A -187；3- glycydoxy trimethoxy silanes；γ-(oxygen of 2,3- epoxies third) propyl group trimethoxy
Base silane；Silane coupler YDH-560；(3- oxiranyhnethoxies propyl group) trimethoxy silane；Coupling agent 560；Coupling agent-
560；γ-glycidyl-oxygen propyl-trimethoxysilane；3-glycydoxy trimethoxy silane.
The present invention also provides the method for preparing above-mentioned uvioresistant digestion resistant adhesive, comprises the steps：
Step 1, dilution is configured：The titanium dioxide of selected parts by weight, silica are added in ethyl acetate, stirring
Uniformly obtained dilution is standby；
Step 2, matrix resin dissolves：The PEPA of selected parts by weight stirring and dissolving in ethyl acetate, and add
Dilution stirs made from step 1；
Step 3, the isocyanates for selecting parts by weight is added in the mixed liquor of step 2, stirs, and uvioresistant is made
Digestion resistant adhesive.
The present invention provides application of the above-mentioned uvioresistant digestion resistant adhesive in the composite membrane of resistance to boiling, bag.
The present invention provides a kind of composite membrane of resistance to boiling, bag, including high-isolation film and above-mentioned uvioresistant high temperature resistant are steamed
Adhesive is boiled, described high-isolation film can be two layers, such as：PA/PE or PA/RCPP, PET/PE or PET/
RCPP；It can also be three layers, four layers, such as：PET/PA/PE, PET/PA/RCPP, etc..
The present invention provides the above-mentioned composite membrane of resistance to boiling, the preparation method of bag, comprises the following steps：
Step 1, get the raw materials ready：Above-mentioned uvioresistant digestion resistant adhesive is prepared, suitable height is selected according to functional analysis
Barrier film,
Step 2, gluing is combined：Above-mentioned uvioresistant digestion resistant adhesive is evenly applied to by height by glue application device
On barrier film, and it is combined；Wherein, resin added control is in 3.5-5g/m2；
Step 3, cure：Composite membrane inserts curing chamber curing, and the composite membrane of resistance to boiling, bag is made；Wherein, curing temperature is controlled
At 55-60 DEG C, the curing time was controlled at 72-96 hours.
Beneficial effects of the present invention have：
1st, the uvioresistant digestion resistant adhesive composite membrane of resistance to boiling of the invention, bag have anti-ultraviolet function,
The opacity and barrier of high-temperature retort bag are improved, the shelf-life of its packaged food is longer.
2nd, the uvioresistant digestion resistant adhesive composite membrane of resistance to boiling of the invention, bag the technological process of production it is short, it is raw
Production cost sticks the agent complex pocket of resistance to boiling compared to traditional high temperature resistant two-component polyurethane adhesive can decline 20% or so.
Embodiment
This hair can be further well understood by the specific embodiment and comparing embodiment of invention now given below
It is bright, but they are not limitation of the invention.It is use not have the part described in detail in specific embodiment and comparing embodiment
What prior art, known technology means and professional standard were obtained.
Unless otherwise indicated, the percentage employed in the present invention is percetage by weight.
Embodiment 1
With reference to the recipe ingredient and the technological parameter of table 2 of table 1, the composite membrane of resistance to boiling, bag are prepared as follows：
(1) uvioresistant digestion resistant adhesive is prepared：
Recipe ingredient in reference table 1 is got the raw materials ready：The parts by weight of PEPA 28；The parts by weight of isocyanates 4；Titanium dioxide
The parts by weight of titanium 3；The parts by weight of silica 7；The parts by weight of organo silane coupling agent 0.5；With the parts by weight of ethyl acetate 40.
Aforementioned body resin and curing agent can be purchased from Chinese Neweast Printing Ink Co., Ltd., the limited public affairs of Henkel share
Take charge of, the producer such as Beijing Gao Meng new materials limited company two-component solvent polyurethane composite adhesive series, wherein, mainly
Component PEPA, the physical parameter control of isocyanates refer to table 3.
The first step：It is standby that titanium dioxide, silica add ethyl acetate to stir again；
Second step：PEPA (host) plus ethyl acetate add the dilution of first step after stirring, stir
Mix uniform and then add isocyanates (curing agent), stir standby.
(2) composite membrane of resistance to boiling, bag：
Above-mentioned uvioresistant digestion resistant adhesive is prepared, suitable high-isolation film is selected according to functional analysis；
Above-mentioned uvioresistant digestion resistant adhesive is evenly applied on high-isolation film by glue application device, gone forward side by side
Row is compound；Wherein, resin added control is in 3.5g/m2；
Composite membrane inserts curing chamber curing, and curing temperature control is at 55 DEG C, and the curing time was controlled at 72 hours, is made resistance to and steams
Boil composite membrane, bag.
The formula rate of table 1
The technological parameter of table 2
The physical parameter of the key component of table 3
Embodiment 2
The implementation process of the embodiment is substantially the same manner as Example 1, and the adjustment of its recipe ingredient and technological parameter is referring to table 1
With table 2.
Embodiment 3
The implementation process of the embodiment is substantially the same manner as Example 1, and the adjustment of its recipe ingredient and technological parameter is referring to table 1
With table 2.
Embodiment 4
The implementation process of the embodiment is substantially the same manner as Example 1, and the adjustment of its recipe ingredient and technological parameter is referring to table 1
With table 2.
Comparative example 1
The implementation process of the comparative example is substantially the same manner as Example 3, its recipe ingredient, component physical parameter and technological parameter
Adjustment referring to Tables 1 and 2, the main proportion relation of two kinds of filler components of adjustment on formula, the physical parameter of key component
Change is mainly hydroxyl value, viscosity etc., main resin added control parameter in technique.
Comparative example 2
The implementation process of the comparative example is substantially the same manner as Example 4, formula rate, component physical parameter and technological parameter
Adjustment refers to the filler systems that main adjustment filler on table 1, table 2, formula is adjusted to one pack system, the physical parameter of key component
Change is mainly hydroxyl value, viscosity etc., the control parameter of main curing step in technique.
Comparative example 3
The gluing agent prescription of the comparative example sticks agent using high temperature resistant two-component polyurethane adhesive commonly used in the prior art, such as
Referenced patent CN1629245A is prepared from.
Table 4 gives the composite membrane of resistance to boiling made from embodiment 1 to 4 and comparative example 1 to 3, bag the performance test results.Its
In, peel strength be 121 DEG C of boilings before, the peel strength after boiling, determined using standard GB/T/T10004-2008 methods,
Wherein peel strength requirement be：For PET/PA material structures, peel strength >=3.5N/15mm before boiling, the stripping after boiling
From intensity >=2.8N/15mm；For PA/RCPP material structures, peel strength >=5N/15mm before boiling, the stripping after boiling
Intensity >=4N/15mm.
The composite membrane of resistance to boiling of table 4, bag performance test
Application study
The complex pocket of resistance to boiling made from prior art and the technology of the present invention is applied to packaging for foodstuff, what will be commonly used is resistance to
High temperature two-component polyurethane adhesive sticks the agent complex pocket of resistance to boiling and destroyed with the uvioresistant high-temperature Resistance Adhesives complex pocket of resistance to boiling
Property Experimental comparison.Specifically：
Variety selection corn is tested, reason has three：1st, there is wide market, as long as outlet at present, domestic market is dived
Power is big.2nd, corn is health product, and is safe, strong on practical significance in process without any additive
Health product.3rd, the product preserves nondiscolouring in 1 year, never degenerated after high temperature sterilization under normal temperature.
Experiment condition：The product is placed in natural environment, through Exposure to Sunlight, wind and rain are beaten after (121 DEG C) sterilizations of high temperature.
Experimental quantities：Each 50.
Experimental result：Such as following table.
Using the uvioresistant high-temperature Resistance Adhesives complex pocket of resistance to boiling of the present invention, packing cost can decline 20% or so.
Above disclosed is only the preferred embodiments of the present invention, can not limit the right of the present invention with this certainly
Scope, therefore the equivalent variations made according to scope of the present invention patent, still belong to the scope that the present invention is covered.
Claims (7)
1. a kind of uvioresistant digestion resistant adhesive, it is adaptable to the composite membrane of resistance to boiling, bag, it is characterised in that：Including as follows
The component of parts by weight：PEPA 28-42 parts by weight；Isocyanates 4-6 parts by weight；Titanium dioxide 3-6 parts by weight；Titanium dioxide
Silicon 3-7 parts by weight；Organo silane coupling agent 0.5-1 parts by weight；With ethyl acetate 40-62 parts by weight；Wherein, described polyester is more
First alcohol is selected from the PEPA that hydroxyl value is 20-90mgKOH/g, and its viscosity is 3000-8000mPas, described isocyanates choosing
From the isocyanates that viscosity is 1000-3000mPas.
2. uvioresistant digestion resistant adhesive according to claim 1, it is characterised in that：Described organosilan is even
Connection agent is γ-(2,3- glycidoxies) propyl trimethoxy silicane.
3. a kind of method for preparing uvioresistant digestion resistant adhesive according to claim 1 or 2, its feature exists
In：Comprise the following steps：
Step 1, dilution is configured：The titanium dioxide of selected parts by weight, silica are added in ethyl acetate, stirred
Dilution is made standby；
Step 2, matrix resin dissolves：The PEPA of selected parts by weight stirring and dissolving in ethyl acetate, and add step 1
Obtained dilution stirs；
Step 3, the isocyanates for selecting parts by weight is added in the mixed liquor of step 2, stirs, and the resistance to height of uvioresistant is made
Warm boiling adhesive.
4. uvioresistant digestion resistant adhesive according to claim 1 or 2 or side according to claim 3
Application of the uvioresistant digestion resistant adhesive that method is prepared in the composite membrane of resistance to boiling, bag.
5. a kind of composite membrane of resistance to boiling, bag, including high-isolation film and the resistance to height of uvioresistant according to claim 1 or 2
Warm boiling adhesive, described high-isolation film is PA/PE, PA/RCPP, PET/PE, PET/RCPP, PET/PA/PE, PET/
PA/RCPP。
6. a kind of method for preparing the composite membrane of resistance to boiling according to claim 5, bag, it is characterised in that：Including following step
Suddenly：
Step 1, get the raw materials ready：Uvioresistant digestion resistant adhesive according to claim 1 or 2 is prepared, according to function point
The suitable high-isolation film of analysis selection；
Step 2, gluing is combined：Above-mentioned uvioresistant digestion resistant adhesive is evenly applied to by high-barrier by glue application device
On film, and it is combined；Wherein, resin added control is in 3.5-5g/m2；
Step 3, cure：Composite membrane inserts curing chamber curing, and the composite membrane of resistance to boiling, bag is made；Wherein, curing temperature control exists
55-60 DEG C, the curing time was controlled at 72-96 hours.
What 7. the composite membrane of resistance to boiling according to claim 5, bag or method according to claim 6 were prepared
The application of the composite membrane of resistance to boiling, bag in packaging for foodstuff.
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| CN201410624526.7A CN104293275B (en) | 2014-11-06 | 2014-11-06 | Uvioresistant digestion resistant adhesive and its preparation method and application |
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| CN105082708A (en) * | 2015-08-10 | 2015-11-25 | 漳州市芳远印务有限公司 | Manufacturing method for compound packaging film resistant to high-temperature steaming and boiling |
| CN106905904A (en) * | 2015-12-22 | 2017-06-30 | 北京奥托米特电子有限公司 | Digestion resistant adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103660437A (en) * | 2013-12-05 | 2014-03-26 | 广东挚信彩印有限公司 | Nanometer impermeable boiling bag, and nano-binder and making method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103660437A (en) * | 2013-12-05 | 2014-03-26 | 广东挚信彩印有限公司 | Nanometer impermeable boiling bag, and nano-binder and making method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 耐蒸煮软包装用聚氨酯胶黏剂的研制;陈晓东等;《化学与黏合》;20091231;第31卷(第2期);第67-70页 * |
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