CN107057616B - The preparation method of composited aluminum and plastic decking adhesive layer resin - Google Patents
The preparation method of composited aluminum and plastic decking adhesive layer resin Download PDFInfo
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- CN107057616B CN107057616B CN201710244038.7A CN201710244038A CN107057616B CN 107057616 B CN107057616 B CN 107057616B CN 201710244038 A CN201710244038 A CN 201710244038A CN 107057616 B CN107057616 B CN 107057616B
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- plastic decking
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/06—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Sealing Material Composition (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to a kind of composited aluminum and plastic decking preparation methods of adhesive layer resin, the following steps are included: each raw material weight number ratio are as follows: 100 parts of polyethylene, 1-2 parts of maleic anhydride, 0.5-1.0 parts of acrylic acid, 0.03-0.05 parts of initiator, 0.3-0.5 parts of antioxidant, hinder crosslinking agent 0.05-0.1 parts, 1.0-2.0 parts of paraffin oil, 0.3-1.0 parts of lithium diatomaceous earth；Above-mentioned raw materials are sent into extruder fusion-grafting after mixing, then are made after cooling, drying, granulation.Low, environmentally friendly, preparation the adhesive layer resin mechanical strength of the method for the present invention simple process, production cost is excellent, has excellent peel strength and heat sealing strength using it as the composited aluminum and plastic decking of adhesive layer, is conducive to composited aluminum and plastic decking recycling.
Description
Technical field
The present invention relates to resin art, the preparation method of specifically a kind of composited aluminum and plastic decking adhesive layer resin.
Background technique
Composited aluminum and plastic decking abbreviation aluminium-plastic panel refers to that using plastics as sandwich layer, single or double bonds the composite board of aluminium, and
In product surface coated with decorative and protective coating or film (being commonly referred to as coating if without especially indicating) as product
Decorative cover.Sandwich layer and the aluminium on two sides are bonded by adhesive layer resin, the performance of adhesive layer resin and composited aluminum and plastic decking
Property relationship is close, researcher wish adhesive layer resin not only and have better processing performance, heatproof weatherability, adhesive property,
Mechanical strength and heat sealing strength, it is also contemplated that resource reclaim problem.A kind of fire-proof aluminium plastic such as publication number 103992756 is compound
Plate Special-purpose macromolecule binding film and preparation method thereof, technical solution are low density polyethylene (LDPE) 80-100 parts, maleic anhydride (MAH)
5-10 parts, 5-10 parts of ethylene vinyl acetate (EVA), 0.05-0.1 parts of photoinitiator, 2-5 parts of styrene, triallyl different three
1-1.5 parts of polycyanate ester, four 0.1-0.3 parts of pentaerythritol ester of [(3,5- di-tert-butyl-hydroxy phenyl) propionic acid], solvent 8-15
Part, macromolecule felted-membrane is finally made.Macromolecule felted-membrane produced by the present invention can effectively improve flame retardant type polyvinyl plastic core
The peel strength of layer and aluminium sheet, expands the application range of aluminum-plastic composite board, can be widely used for advertising logo, fitting-up etc.
Field.The program is that adhesive film is made to generate stronger chemical interactions with metallic matrix by the way that chemical reaction occurs, and is unfavorable for aluminium
The later-stage secondary of plastic clad plate is processed, and does not utilize the recycling of resource.
CN104789168B discloses a kind of preparation method of composited aluminum and plastic decking adhesive resin composition, by certain matter
Measure number by ethylene-acrylic acid graft, terpene resin, rosin ester, cyanate, maleic anhydride imines, silicon powder, hindered phenol,
Atoleine and acetic acid collocation are blended the composited aluminum and plastic decking binder resin being prepared in 150-155 DEG C of heating, can have
There are good weatherability and persistence, adhesive strength reaches 7.5N/mm.The composited aluminum and plastic decking binder resin of the method preparation
In, cyanate improves production cost to human body nocuousness, the use of various kinds of resin by severe toxicity, phenols；The composited aluminum and plastic decking is viscous
Adhesive layer of the resin as aluminium-plastic tape is should to make the polarity group of resin and aluminum flake surface that chemistry occur by chemistry side
Reaction is unfavorable for the recycling of the composited aluminum and plastic decking in later period, reduces resource utilization, produces high risks to environment.
Therefore, it is desirable to develop the adhesive layer that a kind of properties are excellent, environmentally friendly, recycle conducive to composited aluminum and plastic decking
Resin.
Summary of the invention
The purpose of the present invention is to solve above-mentioned technical problem, provide a kind of simple process, production cost it is low, to environment
Friendly, preparation adhesive layer resin mechanical strength is excellent, has excellent removing strong using it as the composited aluminum and plastic decking of adhesive layer
Degree, heat sealing strength, water resistance and resistance to filling capacity are excellent, are conducive to the composited aluminum and plastic decking adhesive layer resin of secondary recovery processing
Preparation method.
In the preparation method, each raw material weight number ratio are as follows: 100 parts of polyethylene, 1-2 parts of maleic anhydride, acrylic acid
0.5-1.0 parts, 0.03-0.05 parts of initiator, 0.3-0.5 parts of antioxidant, crosslinking agent 0.05-0.1 parts is hindered, paraffin oil 1.0-
2.0 parts, 0.3-1.0 parts of lithium diatomaceous earth；Above-mentioned raw materials are sent into extruder fusion-grafting after mixing, then through cooling, drying, make
It is made after grain.
The polyethylene in linear low density polyethylene, high density polyethylene (HDPE) or low density polyethylene (LDPE) at least one
Kind.
The maleic anhydride is maleic anhydride.
The initiator is selected as cumyl peroxide and/or benzoyl peroxide；The resistance crosslinking agent is selected as in oneself
Amide and/or dimethylformamide.
The lithium diatomaceous earth additional amount is 0.6-0.8 parts.
In the fusion-grafting step, extruder is double screw extruder, and each section temperature is respectively set are as follows: an area
175 DEG C -180 DEG C, two 180 DEG C -185 DEG C of areas, three 190 DEG C -195 DEG C of areas, four 200 DEG C -205 DEG C of areas, five 190 DEG C -195 DEG C of areas,
185 DEG C -190 DEG C of head, 190 DEG C -195 DEG C of melt temperature, screw speed 25-40r/min.
For, there are problem, inventor joined lithium diatomaceous earth in the feed in background technique.Lithium diatomaceous earth is a kind of artificial conjunction
At product, be 2: 1 layered silicate structures, i.e., respectively have the silicon oxygen four of a shared oxygen atom on the octahedral both sides of magnesia
The magnesium courtyard of face body, part of divalent is replaced by monovalence lithium atom, makes particle surface with permanent negative electrical charge, preferred structure formula
It is [Mg for its structural formula5.34Li0.66Si8O20(OH)4]Na0.66Artificial synthesized lithium diatomaceous earth.In the present invention, in maleic anhydride
Lithium diatomaceous earth is introduced in fusion-grafting system, while lithium diatomaceous earth itself is in short range attraction and long-range repulsive force under effect, from
" reunion " effect that body can overcome nanoparticle strong, stable is dispersed in polycthylene grafted reaction melt；Lithium diatomaceous earth particle
Distinctive " card room " structure, on the one hand one-dimensional " nanoparticle " with polymolecularity has " quantum " effect, increases it
With the contact area of reaction melt, the activity of the graft reaction of raising improves the efficiency of initiation of initiator, improves maleic anhydride
Grafting rate, the special electronics cloud structure of another aspect lithium diatomaceous earth, flat crystal surface have 50-22mmol100g-1
Negative electrical charge, crystal edge have 4-5mmol100g-1Positive charge, can be with the acid in polycthylene grafted MAH reaction system
Anhydride group and carboxylic group generate electrostatic interaction, the distinctive card room structure of lithium diatomaceous earth, and the dispersibility with height makes lithium
The electrostatic interaction of diatomaceous earth and carboxyl point increases, and the physical crosslinking of system acts on enhancing, improves the mechanical strength of resin, and lithium algae
The hydroxyl isopolarity group that native surface has can also generate the effect of hydrogen bond with MAH, further improve the mechanical property of resin
Energy；And in the use of composited aluminum and plastic decking effect, acid anhydrides group is easy hydrolysis, can generate more free carboxyl, carboxyl
Generation further enhances electrostatic interaction intensity and hydrogen bond action；Furthermore special " card room " structure of lithium diatomaceous earth is formed by dynamic
State and orderly special physical crosslinking structure, make polar end (polarity, the polarity of acid anhydrides group of lithium diatomaceous earth itself) and non-pole
Property end (polyvinyl resin of main body) form orderly hierarchal arrangement structure, as adhesive layer resin, non-polar end energy
Enough non-polar ends with plate can be good at bonding since compatibility is good, and polar end can be with aluminium strip or aluminum flake surface
Polar functional group forms very strong interaction, enhances the adhesion strength of adhesive layer on the whole；The dynamic physics of lithium diatomaceous earth
Cross-linked structure does not influence the secondary operation between aluminium-plastic tape adhesive layer and aluminium flake, significantly improve the removing of adhesive layer with
Heat sealing strength, weatherability and excellent durability, to solve, chemical crosslinking in background technique is existing not to utilize resource reclaim
The problem of.Further, compared to 100 parts of polyethylene, the additive amount that 1-2 parts of maleic anhydride, lithium diatomaceous earth additional amount should be controlled strictly
System is more highly preferred to 0.6-0.8 parts at 0.3-1.0 parts, and to achieve the purpose that improve resin mechanical property, additional amount is excessive, nanometer
Particle aggregation reduces the mechanical strength of resin, and the very few adhesive strength that will cause binder resin reduces, and influences service performance.
Also, the purpose of co-monomer is added in order to improve MAH fusion-grafting speed in co-monomer acrylic acid used herein
The additive amount of rate, the co-monomer is controlled at 0.5-1.0 parts, excessively will cause co-monomer homopolymerization, its mechanical property is greatly reduced,
It is very few to will lead to the reduction of MAH grafting rate.Be added initiator effect be cause radical reaction, preferably cumyl peroxide and/
Or benzoyl peroxide, additive amount are 0.03-0.05 parts, it is excessively high excessively to will lead to free-radical contents, resin self cross-links degree liter
Height, it is very few to reduce fusion-grafting rate；It is to prevent resin from degrading that antioxidant action, which is added, preferably commercially available antioxidant 1010
Or commercially available antioxidant 215, additive amount are 0.3-0.5 parts, can excessively reduce free radical initiation grafting reaction rate, very few meeting
Resin is caused significantly to be degraded, mechanical property reduces.It is to inhibit resin self cross-links, preferably caprolactam that resistance crosslinking action, which is added,
And/or dimethylformamide, additive amount are 0.05-0.1 parts, can excessively reduce the efficiency of initiation of free radical, it is very few to will lead to tree
Rouge self-crosslinking；It is the dispersion in order to promote initiator Yu other auxiliary agents that paraffin oil effect, which is added, and additive amount is 1.0-2.0 parts, mistake
It will lead to the reduction of resin mechanical strength, very few to will lead to initiator and the dispersion of other auxiliary agents unevenly, graft reaction is unstable more.
All advantages of nontoxic raw materials of the present invention are easy to get, at low cost, harmless to environment and human body, as composited aluminum and plastic decking adhesive layer
Resin is in use, using lithium diatomaceous earth dynamic physical crosslinked polyethylene, maleic anhydride enhancing thickening principle, one side lithium diatomaceous earth and horse
Carry out anhydride group and generate very strong Physical interaction, the tensile strength of adhesive layer resin can be improved in dynamic crosslinking, another
Aspect lithium diatomaceous earth can form dynamic and orderly special physical crosslinking structure with resin itself in production and processing, use the tree
The peel strength of the composited aluminum and plastic decking of rouge is also significantly improved with heat sealing strength, is conducive to the secondary operation of composited aluminum and plastic decking, and resistance to
Aqueous up to 7.9, resistance to filling capacity is excellent, and properties are excellent, has significant economic significance and social effect.
Figure of description
Fig. 1 is present invention physical crosslinking structural schematic diagram.
Specific embodiment
Preparing for adhesive layer resin of the present invention is as follows:
The preparation of dry blend
By than weighing dispersing agent paraffin oil, lithium diatomaceous earth (being purchased from ROCKWOOD company, product type Laponite XLG)),
Initiator DCP (cumyl peroxide), co-monomer MAH (maleic anhydride) and AA (acrylic acid), resistance crosslinking agent CPL (acyl in oneself
Amine), antioxidant 1010 (four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters), by above-mentioned material stirring
It is uniformly dispersed to obtain reaction solution, reaction solution is then added to high-speed mixer high speed with PE and is uniformly mixed to obtain powder
Material, fusion-grafting.
The powder is added in double screw extruder and carries out fusion-grafting, double screw extruder each section temperature difference
Setting are as follows: 175 DEG C -180 DEG C of an area, two 180 DEG C -185 DEG C of areas, three 190 DEG C -195 DEG C of areas, four 200 DEG C -205 DEG C of areas, 5th area
190 DEG C -195 DEG C, 185 DEG C -190 DEG C of head, 190 DEG C -195 DEG C of melt temperature, screw speed 25-40r/min.The line of extrusion
Cooling water is cooling, forced air drying, is granulated.
1-6 of the embodiment of the present invention is prepared referring to the above method, wherein replaces with lithium diatomaceous earth in 1 raw material of comparative example
Lithium diatomaceous earth is not added in 2 raw material of comparative example, co-monomer is not added in 3 raw material of comparative example, design parameter is shown in Table 1 for montmorillonite.
Each material component (parts by weight) of table 1, embodiment 1-6 and comparative example 1-3
By adhesive layer resin made from embodiment 1-6 and comparative example 1-3, dumbbell shape batten is prepared in hot pressing, cold pressing
(width: 4.00 ± 0.05mm, 1.00 ± 0.05mm of thickness, original gauge length: 20 ± 0.05mm), is surveyed using universal tensile testing machine
Try the tensile strength and elongation at break of its dumbbell batten；By adhesive layer resin made from embodiment 1-6 and comparative example 1-3 with
The processing of aluminium flake thermal-adhering, 150 DEG C of temperature, pressure 275KPa, hot pressing time 10min, it is 150mm that length, which is prepared, and width is
The plastic-aluminum combined plate sample of 25.4mm, using universal tensile testing machine test its adhesive layer resin peel strength and heat seal it is strong
Degree；It is at 68 ± 1 DEG C that the plastic-aluminum combined plate sample prepared, which is placed directly in environment temperature, and standing time 168h observes aluminium
Delamination between band and plastic film；The plastic-aluminum combined plate sample prepared is immersed in the water that temperature is 68 ± 1 DEG C, leaching
Bubble time 168h detects its peel strength for soaked sample after testing again；Specifically it is shown in Table 2:
2 resin of table and composite plate performance
By upper table analysis combination Fig. 1 physical crosslinking structural schematic diagram it is found that with lithium diatomaceous earth addition, contain lithium diatomaceous earth
The tensile strength of adhesive layer resin improve, the removing of plate is also significantly improved with shear strength, experimental result explanation
The addition of lithium diatomaceous earth can be improved the mechanical strength of adhesive layer resin, show that dynamic physical cross-linked network can be in clad aluminum
It is formed in mould plate material, the addition of lithium diatomaceous earth enhances adhesive layer resin polarity, improves removing and the heat sealing strength of plate, improves
Water-fast, the resistance to filling capacity of plate.
Claims (5)
1. a kind of composited aluminum and plastic decking preparation method of adhesive layer resin, which is characterized in that each raw material weight number ratio are as follows: poly- second
100 parts of alkene, 1-2 parts of maleic anhydride, 0.5-1.0 parts of acrylic acid, 0.03-0.05 parts of initiator, 0.3-0.5 parts of antioxidant, resistance
0.05-0.1 parts of crosslinking agent, 1.0-2.0 parts of paraffin oil, 0.3-1.0 parts of lithium diatomaceous earth；Above-mentioned raw materials are sent into extrusion after mixing
Machine fusion-grafting, then be made after cooling, drying, granulation.
2. the composited aluminum and plastic decking as described in claim 1 preparation method of adhesive layer resin, which is characterized in that the poly- second
Alkene is selected from least one of linear low density polyethylene, high density polyethylene (HDPE) or low density polyethylene (LDPE).
3. the composited aluminum and plastic decking as described in claim 1 preparation method of adhesive layer resin, which is characterized in that the initiation
Cumyl peroxide and/or benzoyl peroxide are selected as in agent；The resistance crosslinking agent is selected as caprolactam and/or dimethyl formyl
Amine.
4. the composited aluminum and plastic decking as described in claim 1 preparation method of adhesive layer resin, which is characterized in that the lithium diatomaceous earth
Additional amount is 0.6-0.8 parts.
5. the preparation method of composited aluminum and plastic decking adhesive layer resin as described in claim any one of 1-4, which is characterized in that institute
It states in fusion-grafting step, extruder is double screw extruder, and each section temperature is respectively set are as follows: 175 DEG C -180 DEG C of an area,
Two 180 DEG C -185 DEG C of areas, three 190 DEG C -195 DEG C of areas, four 200 DEG C -205 DEG C of areas, five 190 DEG C -195 DEG C of areas, 185 DEG C -190 of head
DEG C, 190 DEG C -195 DEG C of melt temperature, screw speed 25-40r/min.
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| CN201710244038.7A CN107057616B (en) | 2017-04-14 | 2017-04-14 | The preparation method of composited aluminum and plastic decking adhesive layer resin |
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| CN201710244038.7A CN107057616B (en) | 2017-04-14 | 2017-04-14 | The preparation method of composited aluminum and plastic decking adhesive layer resin |
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| CN107057616B true CN107057616B (en) | 2019-02-12 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108047997A (en) * | 2017-12-26 | 2018-05-18 | 上海邦中新材料有限公司 | A kind of composited aluminum and plastic decking special bonding resin and preparation method thereof |
| CN112552845A (en) * | 2020-12-18 | 2021-03-26 | 溧阳市高邦电缆材料有限公司 | High-adhesion adhesive resin for aluminum-plastic composite belt and preparation method thereof |
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| CN102417561A (en) * | 2011-11-24 | 2012-04-18 | 上海日之升新技术发展有限公司 | Ultrahigh-fluidity propylene-based elastomer graft copolymer and preparation method thereof |
| CN102994025A (en) * | 2012-11-13 | 2013-03-27 | 上海工程技术大学 | Hot melt glue for aluminum-plastic composite panel and preparation method of hot melt glue |
| CN105440972A (en) * | 2015-07-31 | 2016-03-30 | 湖南工业大学 | Nano-compound biomass waterborne adhesive |
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2017
- 2017-04-14 CN CN201710244038.7A patent/CN107057616B/en active Active
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|---|---|---|---|---|
| CN102417561A (en) * | 2011-11-24 | 2012-04-18 | 上海日之升新技术发展有限公司 | Ultrahigh-fluidity propylene-based elastomer graft copolymer and preparation method thereof |
| CN102994025A (en) * | 2012-11-13 | 2013-03-27 | 上海工程技术大学 | Hot melt glue for aluminum-plastic composite panel and preparation method of hot melt glue |
| CN105440972A (en) * | 2015-07-31 | 2016-03-30 | 湖南工业大学 | Nano-compound biomass waterborne adhesive |
Non-Patent Citations (1)
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| 核壳型载药微球的制备及其释药性能研究;聂光庭，段泰炜，容建华;《功能材料》;20130228;第44卷(第2期);221-225 |
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