CN104559901B - A kind of two component adhesive and its preparation method and application - Google Patents
A kind of two component adhesive and its preparation method and application Download PDFInfo
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- CN104559901B CN104559901B CN201410833464.0A CN201410833464A CN104559901B CN 104559901 B CN104559901 B CN 104559901B CN 201410833464 A CN201410833464 A CN 201410833464A CN 104559901 B CN104559901 B CN 104559901B
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Abstract
The invention belongs to field of adhesive technology, be specifically related to a kind of two component adhesive and its preparation method and application；The present invention includes component A and the B component that weight ratio is 2～10:1, and described component A includes hydroxy resin 100 parts, Organic substance 3～40 parts, Heat Conduction Material 100～500 parts, deicer 1～20 parts, fire retardant 10～200 parts, thixotropic agent 0.1～10 parts, catalyst 0.01～10 parts and additive 0.1～10 parts；Described B component includes resin 100 parts containing isocyanate functional groups and dehydrant 1～10 parts；The present invention has relatively low curing shrinkage internal stress, and battery core, battery core protecting film have good adhesive force, and the heat that battery can be produced due to charge and discharge quickly discharges, and improves effect and the service life of battery.
Description
Technical field
The invention belongs to field of adhesive technology, be specifically related to a kind of two component adhesive and preparation method thereof and
Application.
Background technology
Lithium ion battery electric motor car is more efficient relative to traditional lead-acid battery, safe and environment-friendly, most important
It is that lithium electricity battery is the most durable so that electric motor car will not be heavy, the most attractive in appearance, thus increasingly obtains
Everybody favor.At present, the battery of lithium battery electrical automobile is to be combined by the least battery core, is to lean on
Mechanical means is fixed.Automobile has the biggest impulsive force in running, can cause electricity by mechanical means is fixing
Phase mutual friction between core and affect service life；Automobile occurs may cause hitting between battery core during violent collision
Power of hitting is too big and causes battery repid discharge accident to occur, as on fire from explosion.
Summary of the invention
In order to solve the problems referred to above, it is an object of the invention to provide a kind of two component adhesive；This adhesive
There is relatively low curing shrinkage internal stress, and battery core, battery core protecting film have good adhesive force, and can be battery
The heat produced due to charge and discharge quickly discharges, and improves effect and the service life of battery.
The two of the purpose of the present invention there is provided the preparation method of described two component adhesive.
The three of the purpose of the present invention there is provided the method for application of described two component adhesive.
The four of the purpose of the present invention there is provided the application of described two component adhesive.
The present invention is achieved through the following technical solutions:
A kind of two component adhesive, including the component A that viscosity is 10000～70000cps and viscosity be 150～
The B component of 10000cps, the weight ratio between described component A and B component is 2～10:1；Solidification (can
With cold curing, it is possible to be warmed to 40～100 DEG C of solidifications) afterwards heat conductivity be 0.4～2W/m.K, bonding
Intensity > 4MPa, anti-flammability is UL-94V0.
Described component A includes the following raw material calculated in parts by weight:
Wherein, described hydroxy resin is the resin of 100% solid content, and described Organic substance is vinyl silanes
Homopolymer and/or copolymer；
Described B component includes the following raw material calculated in parts by weight:
Resin containing isocyanate functional groups 100 parts
Dehydrant 1～10 parts；
The described resin containing isocyanate functional groups is HDI addition product, HDI performed polymer, XDI addition product, IPDI
Trimer, HDI biuret, HDI trimer, TDI-HDI mixing polymer, HDI-IPDI mixing poly
One or more mixing in body, TDI-TMP addition product, liquefied mdi, polymeric MDI.Wherein, mixed
Close the resin of multiple isocyanate functional groups, preferable hardening time, adhesion strength, heat resistance can be obtained.
The Desmodur VT66, Mondur 44 of the product of commercialization such as Bayer, Desmodur HZ1,
DesmodurRN, Desmodur XP2625, Desmodur 3200, Desmodur N100, Desmodur
N3300, Desmodur N3600, Desmodur N3800, Desmodur N3900, Desmodur 44P16,
Desmodur 44V20L, Desmodur 4470L, Desmodur E22, Desmodur PC；Japan three
Cosmonate LL, Cosmonate MR-200, the Cosmonate MR-400 of well KCC,
Tankenate L75, Tankenate D-170N, Tankenate D-177N, Tankenate D-102,
Tankenate D-204；The Wannate P-100, Wannate of Yantai Wanhua Polyurethane Co., Ltd
P-200, Wannate P-300, Wannate P-400, Wannate P-2025, Wannate 8001, Wannate
8020, Wannate 8319, Wannate 6110 etc..
It is preferred that described hydroxy resin is hydroxy polyethers resin, flame retardant polyether polyol, hydroxyl polyester tree
Fat, hydroxy polyethers ester resin, epoxy resin, epoxy polyurethane polyhydric alcohol oily, castor oil modified, hydroxyl third
One or more mixing in olefin(e) acid resin.The Sovermol 805 of the product of commercialization such as BASF,
Sovermol 815, Sovermol 819, Sovermol 750, Sovermol 860, Sovermol 920；Day
Uric H-52, Uric H-81, Uric H-102, the Uric H-420, Uric of this Itoh Oil Mfg
AC-006；The Acrol 1003 of Bayer, Acrol 1007, Acrol 1011, Acrol 1048, Acrol 1053,
Multranol 4034, Multranol 4050 etc..Wherein polyhydric alcohol is to use 2 functional groups, coordinates few
3 functional groups of amount and the polyhydric alcohol of 4 functional groups, to improve intensity and the temperature tolerance of adhesive.
It is preferred that described vinyl silanes be vinyltrimethoxy silane, VTES gather
In compound, 3-(triethoxy is silica-based) propyl methacrylate, 3-(triethoxy is silica-based) propyl acrylate
One or more mixing.In described VTES polymer, comonomer includes metering system
One or more mixing in acid esters, hydroxyl-metacrylate, acrylate, hydroxy acrylate.Poly-
Closing temperature and control at 100～150 DEG C, the response time is 3～6 hours, and the degree of polymerization is 3～15；Preferred polymeric
Temperature controls at 110～130 DEG C, and the response time is 4～5 hours, and the degree of polymerization is 7～10.Due to this type of
Organic substance contains hydroxyl and substantial amounts of alkoxyl, hydroxyl and firming agent reaction in adhesive solidification process, with
Time alkoxyl can react with base material, can improve and the adhesion strength of base material and temperature tolerance；Organic
Addition is the 3～40% of hydroxy resin total amount, preferably 5～10%.
It is preferred that described deicer is physics deicer and chemistry deicer compositions；Described chemistry deicer
For one or more in monocycle oxazolidine, dicyclo oxazolidine, sulfonyloxy methyl isocyanates, ethyl orthoformate
Mixing；Described physics deicer is calcium oxide, molecular sieve, anhydrous slufuric acid aluminum, the one in anhydrous calcium chloride
Or several mixing.Physics deicer and chemistry deicer with the use of, utilize chemistry deicer remove major part
Moisture, recycling physics deicer absorb remaining moisture.Addition is the 1～20% of hydroxy resin total amount,
It is preferably 3～10%.
It is preferred that described fire retardant is additive flame retardant and reactive flame retardant compositions；Described response type
Fire retardant is N, N-bis-(2-ethoxy) aminomethy-lenephosphonic acids diethylester, three (dipropylene glycol) Asia
Phosphate acid ester, N, N-bis-(2-ethoxy) aminomethy-lenephosphonic acids dimethyl ester, poly-organic phosphoric acid glycol, tetrabromo
One or more mixing in phthalic acid esterdiol, brominated chloropolyether polyhydric alcohol；Business-like Exolit
OP550, Exolit OP560, Levergard 4090N, Weston 430, Niax CS-22 etc..Described add
Adding type fire retardant is APP, tripolycyanamide, melamine salt, phosphate ester, aluminium hydroxide, hydroxide
One or more mixing in magnesium, Firebrake ZB, antimony oxide.The fire retardant of the present invention uses additive flame
Combustion agent and reactive flame retardant with the use of, at least contain the flame retardant polyether polyol of a kind of 2 functional groups, with
Improve intensity and the anti-flammability of adhesive.Flame retardant polyether polyol employing is phosphorous, halogen, antimony, nitrogen etc. are fire-retardant
The initiator of element forms with oxyalkylene ring-opening polymerisation, and the adhesive being made up of these polyethers has certain
Fire resistance.Compared with additive flame retardant, owing to flame retardant polyether polyol participates in reaction, stably combine
In polyurethane matrix, the intensity of adhesive will not be reduced, also will not separate out during life-time service and drop
Low flame retardancy energy.The addition of fire retardant is the 10～200% of hydroxy resin total amount, preferably 20～100%.
It is preferred that described thixotropic agent includes gas-phase silica, bentonite, lithium magnesium silicate, polyamide wax, hydrogen
Change one or more mixing in Oleum Ricini, modified urea；Addition is the 0.1～10% of hydroxy resin total amount,
It is preferably 2～7%.
It is preferred that described catalyst be tertiary amine, bridged piperazine derivatives, morpholine class, imdazole derivatives, organotin,
One or more mixing in carboxylic acid potassium class, titanate ester and rare earth；Catalyst is used for accelerating curing rate,
Shorten the response time, improve production efficiency, increase adhesion strength.Consumption is few, but effect is the biggest.Addition
For the 0.01～10% of hydroxy resin total amount, preferably 0.1～3%.
It is preferred that Heat Conduction Material be aluminium oxide, magnesium oxide, zinc oxide, aluminium nitride, boron nitride, carborundum,
One or more mixing in silicon dioxide, calcium carbonate.The Heat Conduction Material particle diameter that the present invention selects is from 0.1 micron
To 100 microns, grain shape includes spherical, hemispherical, lamellar, threadiness.In order to improve heat conductivility,
Need to add heat filling as far as possible, but the increase of the addition along with filler, viscosity can significantly increase, from
And affect the adhesion strength of workability and adhesive.Filler and spherical heat filling that surface processes are permissible
Improve addition and less to viscosity and performance impact；Aluminium nitride, boron nitride, carborundum, due to them certainly
The heat conductivity of body is high, adds less amount and can be obtained by higher heat conductivity.Ball-aluminium oxide and nitrogen
Change aluminum, boron nitride collocation uses, and can prepare the adhesive that adhesive property is good, heat conductivity is high.Heat conduction is filled out
Addition is hydroxy resin total amount the 100～500% of material, preferably 250～350%.
Described additive, any traditional additive can add this invention, including pigment, defoamer, dispersion
Agent, levelling agent, anti-settling agent etc., depend on the purposes of product.As pigment includes carbon black, titanium dioxide, phthalein is blue or green
Inorganic, the organic pigments such as indigo plant, for changing the color of adhesive.The consumption of additive is hydroxy resin total amount
0.1～10%, be preferably 1～5%.
The method preparing described two component adhesive:
(1), organic synthesis:
Propylene glycol monomethyl ether is added in reactor, adds oxazolidine, stir 1 hour under room temperature；Add described
The 30% of vinyl silanes total amount, limit stirring is warming up to 120～150 DEG C；Add thermal initiator isopropylbenzene peroxide
Change hydrogen, stir；Control reaction temperature, at 120～150 DEG C, dripped remaining in 3～6 hours
The vinyl silanes of 70%；When the viscosity of reactant reaches to be coated with four glasss 13～15 seconds, open vacuum and steam the third two
Alcohol methyl ether, prepares described Organic substance；
(2), the preparation procedure of component A is as follows:
Hydroxy resin is added in planetary mixer, adds Organic substance while stirring, add described deicer,
It is stirred at room temperature 30 minutes；Add Heat Conduction Material and fire retardant, high speed dispersion 60～180 minutes, evacuation
To-0.9MPa, control temperature 80～105 DEG C；Cooling causes temperature and is less than 80 DEG C, adds thixotropic agent, catalyst
Stir with additive；Vacuum defoamation 30 minutes；Filter and package, obtain described component A；
(3), the preparation procedure of B component is as follows:
Resin containing isocyanate functional groups is added in planetary mixer, adds dehydrant while stirring, in room
Temperature stirring 60 minutes；Vacuum defoamation 30 minutes；Filter and package and obtain described B component.
The method of application of described two component adhesive, battery core surface preparation-battery core surface apply described adhesive-
Battery core assembling-base plate applies described adhesive-base plate and installs-solidification.Typically there is PET protection film on battery core surface,
The method of pretreatment includes the methods such as solvent clean, plasma clean, ultraviolet rays cleaning；Battery core surface
Construction method can by hand, bi-component automatic dispensing machine；Battery core assembling fixture, from two adhesive surface sides
To the pressure that holding is certain；The construction method of base plate can by hand, bi-component automatic dispensing machine；Base plate is pacified
Dress can be fixed with fixture, it is possible to relies on the gravity of battery core to fix；The solidification of adhesive can be natural in room temperature
Solidification, it is possible to be heated up to 40～70 DEG C of solidifications.
The purposes of described two component adhesive, described adhesive is at automobile power cell module, transformator, electricity
The element of son assembles and uses in embedding；The present invention was used between battery core when batteries of electric automobile assembles
Bonding between bonding and battery core and base plate, replacement is mechanically fixed.
The present invention includes that component A that viscosity is 10000～70000cps and viscosity are 150～10000cps
B component, the weight ratio between described component A and B component is 2～10:1；This adhesive has relatively low consolidating
Change shrinkage stress, and battery core, battery core protecting film have good adhesive force, there is the flame retardant effect of excellence simultaneously,
The battery using adhesive to assemble, can slow down the friction between battery core, the impulsive force between buffering battery core.
Adhesive between battery core and base plate can quickly discharge the heat produced during battery impulse electricity, thus extends
The service life of battery, it is to avoid occur unexpected.Use the lithium battery for automobile power of the adhesive producing of the present invention
The performance of group can meet the code requirement of UN 38.3 " lithium metal battery and lithium battery group ".
Specific embodiment
Below in conjunction with detailed description of the invention, the present invention is described in further detail, to help art technology
Personnel understand the present invention.
MS-Plus is monocycle oxazolidine, and ALT-401 is dicyclo oxazolidine, and M-5 is aerosil.
The preparation of Organic substance A:
2000 grams of propylene glycol monomethyl ethers are added in reactor, adds 20 grams of oxazolidine, stir 1 under room temperature little
Time；Adding 480 grams of VTESs, 120 grams of Hydroxypropyl methacrylates, limit stirring is warming up to
110℃；Add 20 grams of isopropyl benzene hydroperoxides, stir；Control reaction temperature is at 130 DEG C, little 3
Time interior drip the mixed of remaining 1120 grams of VTESs and 280 grams of Hydroxypropyl methacrylates
Compound；When the viscosity of reactant reaches 13～15 seconds (being coated with four glasss), open vacuum and steam propylene glycol monomethyl ether.
Prepare Organic substance A.
The preparation of Organic substance B:
1200 grams of propylene glycol monomethyl ethers and 800 grams of butanol are added in reactor, adds 50 grams of oxazolidine, often
The lower stirring of temperature 1 hour；Add 360 grams of vinyltrimethoxy silanes, 120 grams of 3-(triethoxy is silica-based) third
Methyl acrylate and 120 grams of 2-(Acryloyloxy)ethanols, limit stirring is warming up to 110 DEG C；Add 30 grams of isopropyls
Benzene hydrogen peroxide, stirs；Control reaction temperature, at 140 DEG C, dripped remaining 840 in 4 hours
Gram VTES, 240 grams of 3-(triethoxy is silica-based) propyl methacrylate and 240 gram third
The mixture of olefin(e) acid hydroxyl ethyl ester；When the viscosity of reactant reaches 13～15 seconds (being coated with four glasss), open vacuum
Steam propylene glycol monomethyl ether and butanol.Prepare Organic substance B
Embodiment 1
The preparation of two component adhesive:
The preparation procedure of component A is as follows:
Sovermol 805, Uric-52, Acrol 1011 are added in planetary mixer, added while stirring
Organic substance A, stirs, and adds MS-plus, is stirred at room temperature 30 minutes；Addition ball-type aluminium oxide,
Aluminium hydroxide and OP550, high speed dispersion 120 minutes, it is evacuated to-0.9MPa, controls temperature 102 DEG C；
Cooling causes temperature and is less than 80 DEG C, adds M-5, butyl tin dilaurate, carbon black, stirs；Vacuum takes off
Steep 30 minutes；Filter and package.
The preparation procedure of B component is as follows:
Desmodur N3300 is added in planetary mixer, adds Cosmonate MR-200 while stirring,
Add ALT-401, be stirred at room temperature 60 minutes；Vacuum defoamation 30 minutes；Filter and package.
Embodiment 2
The preparation of two component adhesive:
The preparation procedure of component A is as follows:
Sovermol 805, Sovermol 750, Acrol 1011 are added in planetary mixer, and limit is stirred
Limit adds Organic substance B, stirs, and adds MS-plus, is stirred at room temperature 30 minutes；Add ball-type oxygen
Change aluminum, aluminium hydroxide and Weston 430, high speed dispersion 150 minutes, be evacuated to-0.9MPa, control
Temperature 94 DEG C；Cooling causes temperature and is less than 80 DEG C, adds M-5, triethanolamine, carbon black, stirs；Very
Empty deaeration 30 minutes；Filter and package.
The preparation procedure of B component is as follows:
Desmodur N3300 is added in planetary mixer, add while stirring Desmodur XP2625,
Wannate P-200, adds ALT-401, is stirred at room temperature 60 minutes；Vacuum defoamation 30 minutes；Filter
Packaging.
Embodiment 3
The preparation of two component adhesive:
The preparation procedure of component A is as follows:
Sovermol 750, Sovermol 860, Uric-52 add in planetary mixer, add while stirring
Enter Organic substance A, stir, add MS-plus, be stirred at room temperature 30 minutes；Addition ball-type aluminium oxide,
Aluminium hydroxide and Weston 430, high speed dispersion 150 minutes, it is evacuated to-0.9MPa, controls temperature 105 DEG C；
Cooling causes temperature and is less than 80 DEG C, adds M-5, butyl tin dilaurate, carbon black, stirs；Vacuum takes off
Steep 30 minutes；Filter and package.
The preparation procedure of B component is as follows:
Desmodur N3300 is added in planetary mixer, adds Cosmonate MR-200 while stirring,
Add ALT-401, be stirred at room temperature 60 minutes；Vacuum defoamation 30 minutes；Filter and package.
Embodiment 4
The preparation of two component adhesive:
The preparation procedure of component A is as follows:
Uric-52, Acrol 1011 being entered in planetary mixer, adds Organic substance B while stirring, stirring is all
Even, add MS-plus, be stirred at room temperature 30 minutes；Addition ball-type aluminium oxide, aluminium hydroxide and OP550,
Weston 430, high speed dispersion 60 minutes, it is evacuated to-0.9MPa, controls temperature 82 DEG C；Cooling causes temperature
Degree, less than 80 DEG C, adds M-5, butyl tin dilaurate, carbon black, stirs；Vacuum defoamation 30 minutes；
Filter and package.
The preparation procedure of B component is as follows:
Cosmonate MR-200 is added in planetary mixer, adds Wannate P-200 while stirring,
Add ALT-401, be stirred at room temperature 60 minutes；Vacuum defoamation 30 minutes；Filter and package.
Above-described embodiment, simply presently preferred embodiments of the present invention, be not used for limiting the scope of the present invention,
Therefore all with the feature described in the claims in the present invention and principle done equivalence change or modify, all should be included in
Within scope of the invention as claimed.
Above-described embodiment is mixed by following mass ratio, prepares various test sample, and condition of cure is 45C*3hrs
Hard DEG C, adhesion strength, heat conductivity and anti-flammability of+25C*72hrs. test test adhesive.
Claims (8)
1. a two component adhesive, it is characterised in that include component A that viscosity is 10000～70000cps and
Viscosity is the B component of 150～10000cps, the weight ratio between described component A and B component be 2～
10:1；
Described component A includes the following raw material calculated in parts by weight:
Wherein, described hydroxy resin is the resin of 100% solid content；
Described B component includes the following raw material calculated in parts by weight:
Resin containing isocyanate functional groups 100 parts
Dehydrant 1～10 parts；
The described resin containing isocyanate functional groups is HDI addition product, HDI performed polymer, XDI addition product, IPDI
Trimer, HDI biuret, HDI trimer, TDI-HDI mixing polymer, HDI-IPDI mixing poly
One or more mixing in body, TDI-TMP addition product, liquefied mdi, polymeric MDI；Described organic
Thing is the homopolymer of vinyl silanes.
2. two component adhesive as claimed in claim 1, it is characterised in that described hydroxy resin is hydroxy polyethers
Resin, flame retardant polyether polyol, hydroxy polyester resin, hydroxy polyethers ester resin, castor oil modified polyhydric alcohol,
One or more mixing in Hydroxylated acrylic resin.
3. as claimed in claim 1 two component adhesive, it is characterised in that described deicer be physics deicer and
Chemistry deicer compositions；Described chemistry deicer is that monocycle oxazolidine, dicyclo oxazolidine, sulfonyloxy methyl are different
One or more mixing in cyanate；Described physics deicer be calcium oxide, molecular sieve, anhydrous slufuric acid aluminum,
One or more mixing in anhydrous calcium chloride.
4. two component adhesive as claimed in claim 1, it is characterised in that described fire retardant is additive flame retardant
With reactive flame retardant compositions；Described reactive flame retardant is N, N-bis-(2-ethoxy) aminomethylene
Diethyl phosphonate, three (dipropylene glycol) sub-phosphate acid ester, N, N-bis-(2-ethoxy) aminomethylene
One or more mixing in dimethyl phosphonate, brominated chloropolyether polyhydric alcohol；Described additive flame retardant is
APP, tripolycyanamide, melamine salt, phosphate ester, aluminium hydroxide, magnesium hydroxide, Firebrake ZB,
One or more mixing in antimony oxide.
5. as claimed in claim 1 two component adhesive, it is characterised in that described thixotropic agent be gas-phase silica,
One or more mixing in bentonite, lithium magnesium silicate, polyamide wax, castor oil hydrogenated, modified urea；
Described catalyst is tertiary amine, bridged piperazine derivatives, morpholine class, imdazole derivatives, organotin, carboxylic acid potassium
One or more mixing in class, titanate ester and rare earth；
Described Heat Conduction Material be aluminium oxide, magnesium oxide, zinc oxide, aluminium nitride, boron nitride, carborundum, two
One or more mixing in silicon oxide, calcium carbonate.
6. the method for two component adhesive described in any one in preparation claim 1-5, it is characterised in that:
(1), organic synthesis:
Propylene glycol monomethyl ether is added in reactor, adds oxazolidine, stir 1 hour under room temperature；Add described
The 30% of vinyl silanes total amount, limit stirring is warming up to 120～150 DEG C；Add thermal initiator isopropylbenzene peroxide
Change hydrogen, stir；Control reaction temperature, at 120～150 DEG C, dripped remaining in 3～6 hours
The vinyl silanes of 70%；When the viscosity of reactant reaches to be coated with four glasss 13～15 seconds, open vacuum and steam the third two
Alcohol methyl ether, prepares described Organic substance；
(2), the preparation procedure of component A is as follows:
Hydroxy resin is added in planetary mixer, adds Organic substance while stirring, add described deicer,
It is stirred at room temperature 30 minutes；Add Heat Conduction Material and fire retardant, high speed dispersion 60～180 minutes, evacuation
To-0.9MPa, control temperature 80～105 DEG C；Cooling causes temperature and is less than 80 DEG C, adds thixotropic agent, catalysis
Agent and additive stir；Vacuum defoamation 30 minutes；Filter and package, obtain described component A；
(3), the preparation procedure of B component is as follows:
Resin containing isocyanate functional groups is added in planetary mixer, adds dehydrant while stirring, in room
Temperature stirring 60 minutes；Vacuum defoamation 30 minutes；Filter and package and obtain described B component.
7. the method for application of two component adhesive described in any one in claim 1-5, it is characterised in that: battery core
Surface preparation battery core surface applies described adhesive battery core assembling plate and applies at the bottom of described adhesive
Solidification installed by plate.
8. the purposes of two component adhesive described in any one in claim 1-5, it is characterised in that: described gluing
Agent assembles at the element of automobile power cell module, transformator, electronics and uses in embedding.
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| JPS61185520A (en) * | 1985-02-12 | 1986-08-19 | Kuraray Co Ltd | Production of polyester polyurethane |
| CN103045153B (en) * | 2012-11-20 | 2015-11-25 | 陈晴 | Bi-component polyurethane adhesive of a kind of resistance to acid liquid corrosion and its preparation method and application |
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