CN104449533A - Reactive polyurethane hot melt adhesive for electronic appliance and preparing method thereof - Google Patents
Reactive polyurethane hot melt adhesive for electronic appliance and preparing method thereof Download PDFInfo
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Abstract
The invention discloses a reactive polyurethane hot melt adhesive for an electronic appliance and a preparing method of the reactive polyurethane hot melt adhesive. The hot melt adhesive comprises, by weight, polyester polyol, isocyanate, tackifying resin, an adhesion promoter, a catalyst and antioxidant. The polyester polyol and the tackifying resin are placed in a reaction kettle for heating, stirred, dehydrated in a vacuum mode and then cooled, polyisocyanate is added, the prepolymerization reaction is carried out under protection of nitrogen, the adhesion promoter, the catalyst and the antioxidant of the measured amount are sequentially added after the reaction and mixed evenly, vacuum defoamation is carried out finally, discharge, sealing and packaging are carried out, and the reactive polyurethane hot melt adhesive for the electronic appliance is prepared. The hot melt adhesive has high initial adhesion, high curing speed and high in final strength, can be used for bonding various base materials such as PC, PBT, PET, PVC, PMMA, Al and inorganic glass, and can be widely used for fixing and bonding of various parts in the industry of electronic appliances.
Description
Technical field
The invention belongs to reaction type polyurethane hot-melt adhesive technical field, specifically, the present invention relates to a kind of electronic apparatus reaction type polyurethane hot-melt adhesive and preparation method thereof.
Background technology
Reaction type polyurethane hot-melt adhesive (PUR) generally makes base-material with NCO end group performed polymer, is equipped with tackifying resin, oxidation inhibitor, catalyzer, filler etc. formulated.Time bonding, tackiness agent heating and melting fluidly applies applying glue, and after two kinds of clung body laminatings, glue-line cooling cohesion obtains initial bonding force at once; Active NCO group afterwards in glue-line is reacted with the moisture of the moisture in air, adherend surface adsorption and active hydrogen group again, produces chemical crosslinking cure, generates the high molecular polymer with Gao Juli, bounding force, thermotolerance etc. are significantly improved.Its existing hot melt adhesive is solvent-free, tack is high, assembling time locate the characteristics such as rapid, the performance such as water-fast, the heatproof of responding property sizing agent, resistance to creep, moisture-proof and media-resistant again.
PUR has environmental protection, elastic adhesive, cure shrinkage are little, applied widely; Higher initial bond strenght can be reached in short period of time, be particularly suitable for the bonding of precision components in the pipelining production of electronic enterprises.But due to technical elements, current domestic Jin You minority enterprise can produce PUR product, and mostly there is the problems such as low, the resistance to environmental resistance of bonding strength is poor, curing speed is slow, is difficult to meet the demand of domestic high-grade client at electronic enterprises.
Summary of the invention
Based on this, in order to overcome the defect of above-mentioned prior art, the invention provides a kind of electronic apparatus reaction type polyurethane hot-melt adhesive and preparation method thereof, be characterized in the solidification of this reaction type polyurethane hot-melt adhesive rapidly, initial adhesive strength is high, have good cementability to base materials such as plastics, metal, glass, resistance to environmental resistance is excellent.
In order to realize foregoing invention object, this invention takes following technical scheme:
A kind of electronic apparatus reaction type polyurethane hot-melt adhesive, described hot melt adhesive is made up of the raw material of following weight part:
Polyester polyol 100 parts, isocyanic ester 10 ~ 30 parts, tackifying resin 10 ~ 20 parts, adhesion promotor 1 ~ 3 part, catalyzer 0.1 ~ 0.5 part, 1 ~ 2 part, oxidation inhibitor.
Wherein in some embodiments, described hot melt adhesive is made up of the raw material of following weight part:
Polyester polyol 100 parts, isocyanic ester 23.5 parts, tackifying resin 20 parts, adhesion promotor 1.8 parts, catalyzer 0.15 part, 2 parts, oxidation inhibitor.
Wherein in some embodiments, described polyester polyol is the poly-hexanodioic acid-1 of number-average molecular weight 1000 ~ 6000,4-butanediol ester glycol, poly-hexanodioic acid-1,6-hexylene glycol esterdiol, polydiethylene glycol adipate glycol, poly-phthalic acid-1, one or more in 4-butanediol ester glycol, poly-carbonic acid-1,6-hexylene glycol esterdiol.
Wherein in some embodiments, described isocyanic ester is 4,4 '-diphenylmethanediisocyanate or MDI-50.
Wherein in some embodiments, described tackifying resin is one or more in Gum Rosin, hydrogenated rosin resin, petroleum resin, terpine resin.
Wherein in some embodiments, described adhesion promotor is one or more in 3-mercaptopropyl trimethoxysilane, 3-sulfo-capryloyl-1-propyl-triethoxysilicane, 3-isocyanic ester propyl-triethoxysilicane, 3-isocyanic ester propyl trimethoxy silicane, 3-[3-(trimethoxysilyl) propyl group] isocyanuric acid ester, 3-glycidyl ether oxygen propyl trimethoxy silicane, 3-glycidoxypropyltrietandysilane andysilane.
Wherein in some embodiments, described catalyzer is one or more in dibutyl tin laurate, triethylenediamine, dimorpholine base Anaesthetie Ether.
Wherein in some embodiments, described oxidation inhibitor is 2,6-di-tert-butyl methyl phenol, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid positive octadecanol ester, three (2.4-di-tert-butyl-phenyl) phosphorous acid ester, one or more in two (3,5-di-tert-butyl-hydroxy phenyl) thioether.
Present invention also offers the preparation method of above-mentioned electronic apparatus reaction type polyurethane hot-melt adhesive, take following technical scheme:
A preparation method for electronic apparatus reaction type polyurethane hot-melt adhesive, comprises the following steps:
(1), by polyester polyol, tackifying resin drop in reactor, be heated to 110 ~ 130 DEG C, under agitation vacuum hydro-extraction 1.5 ~ 2.5 hours, vacuum tightness is-0.095 ~ 0.05MPa;
(2), be cooled to 80 ~ 90 DEG C, drop into isocyanic ester, at N
2in 75 ~ 85 DEG C of stirring reactions 1 ~ 3 hour under protection;
(3) adhesion promotor, catalyzer, antioxidant is added, successively, at N
2in 75 ~ 85 DEG C of stirring reactions 0.5 ~ 2 hour under protection;
(4), be warming up to 110 ~ 140 DEG C, be evacuated to bubble-free and occur, discharging, to obtain final product.
Electronic apparatus reaction type polyurethane hot-melt adhesive of the present invention, selects the polyester polyol of high crystalline to prepare performed polymer, can shorten the open hour of prepared hot melt adhesive and improve its initial bonding strength; Select to add appropriate tackifying resin, when hot melt adhesive cools, hot melt adhesive cohesion can be accelerated, be conducive to the initial bonding strength improving hot melt adhesive; Select to add appropriate adhesion promotor, the alkoxyl group utilizing it subsidiary and bonding substrate surface form hydrogen bond or chemical reaction occur, and can improve hot melt adhesive to the sticking power of bonding base material and bonding rear resistance to environmental resistance.Compared with prior art, the present invention has following beneficial effect:
1, reaction type polyurethane hot-melt adhesive of the present invention, has the features such as initial bonding strength is strong, curing speed fast, finally bonding strength is high, and resistance to environmental resistance is excellent, is particularly suitable for electronic enterprises precision components production line balance, has good market outlook; For single-component mist-solidifying adhesive for polyurethane, belong to solvent-free environment-protection sizing agent industry, can be used for the bonding of the base materials such as electronic enterprises plastics, glass, metal;
2, the preparation technology of reaction type polyurethane hot-melt adhesive of the present invention is simple, easily operates, is easy to industrialization.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
In following examples, the raw material used is commercially available.
Embodiment 1
The reaction type polyurethane hot-melt adhesive of the present embodiment is made up of the raw material of following weight part:
The preparation method of the reaction type polyurethane hot-melt adhesive of the present embodiment, comprises the following steps:
(1), by 100 parts by weight average molecular weights be 2000 poly-hexanodioic acid-1,4-butanediol ester glycol (PBA), 15 weight part Gum Rosins drop in reactor, be heated to 120 DEG C, under agitation vacuum hydro-extraction 2 hours, vacuum tightness is 0.03MPa;
(2), be then cooled to 80 DEG C, drop into the mixture (MDI-50) of 25 weight part 2,4-diphenylmethanediisocyanates and 4,4'-diphenylmethanediisocyanate, at N
2in 82 DEG C of stirring reactions 2 hours under protection;
(3), finally 1.5 weight part 3-[3-(trimethoxysilyl) propyl group] isocyanuric acid ester is added successively, 0.5 weight part 3-glycidyl ether oxygen propyl trimethoxy silicane, 0.2 weight part dibutyl tin laurate, 1.2 weight part BHTs are at N
2in 82 DEG C of stirring reactions 1.5 hours under protection;
(4), be warming up to 125 DEG C, be evacuated to bubble-free and occur, then discharging, packs, and obtained electronic apparatus reaction type polyurethane hot-melt adhesive, places stand-by.
Embodiment 2
The reaction type polyurethane hot-melt adhesive of the present embodiment is made up of the raw material of following weight part:
The preparation method of the reaction type polyurethane hot-melt adhesive of the present embodiment, comprises the following steps:
(1), by 100 parts by weight average molecular weights be 3000 poly-hexanodioic acid-1,6-hexylene glycol esterdiol (PHA), 12 weight part terpine resins drop in reactor, be heated to 125 DEG C, under agitation vacuum hydro-extraction 2.2 hours, vacuum tightness is-0.055MPa;
(2), be then cooled to 88 DEG C, drop into 16.5 weight part MDI-50, at N
2in 85 DEG C of stirring reactions 1.5 hours under protection;
(3), finally add 2.0 weight part 3-isocyanic ester propyl trimethoxy silicanes successively, 0.15 weight part dibutyl tin laurate, 1.5 weight part β-positive octadecanol ester of (3,5-di-tert-butyl-hydroxy phenyl) propionic acid is at N
2in 85 DEG C of stirring reactions 1 hour under protection;
(4), be warming up to 130 DEG C, be evacuated to bubble-free and occur, then discharging, packs, and obtained electronic apparatus reaction type polyurethane hot-melt adhesive, places stand-by.
Embodiment 3
The reaction type polyurethane hot-melt adhesive of the present embodiment is made up of the raw material of following weight part:
The preparation method of the reaction type polyurethane hot-melt adhesive of the present embodiment, comprises the following steps:
(1), by 30 parts by weight average molecular weights be 5500 poly-carbonic acid-1,6-hexylene glycol esterdiol, 70 parts by weight average molecular weights be 1500 PBA, 20 weight part petroleum resin drop in reactors, be heated to 128 DEG C, under agitation vacuum hydro-extraction 2.4 hours, vacuum tightness is-0.025MPa;
(2), be then cooled to 80 DEG C, drop into the mixture (MDI-50) of 23.5 weight part 2,4-diphenylmethanediisocyanates and 4,4'-diphenylmethanediisocyanate, at N
2in 83 DEG C of stirring reactions 2.5 hours under protection;
(3), finally 1 weight part 3-isocyanic ester propyl trimethoxy silicane is added successively, 0.8 weight part 3-[3-(trimethoxysilyl) propyl group] isocyanuric acid ester, 0.05 weight part dibutyl tin laurate, 0.1 weight part 2,2-dimorpholine base Anaesthetie Ether, two (3, the 5-di-tert-butyl-hydroxy phenyl) thioether of 2 weight parts is at N
2in 83 DEG C of stirring reactions 1.6 hours under protection;
(4), be warming up to 135 DEG C, be evacuated to bubble-free and occur, then discharging, packs, obtained electronic apparatus reaction type polyurethane hot-melt adhesive.
Embodiment 4
The reaction type polyurethane hot-melt adhesive of the present embodiment is made up of the raw material of following weight part:
The preparation method of the reaction type polyurethane hot-melt adhesive of the present embodiment, comprises the following steps:
(1), by 50 parts by weight average molecular weights be 2500 poly-phthalic acid-1,4-butanediol ester glycol, 50 parts by weight average molecular weights be 2000 polydiethylene glycol adipate glycol, 15 parts by weight of hydrogenated Gum Rosins drop in reactors, be heated to 118 DEG C, under agitation vacuum hydro-extraction 2.5 hours, vacuum tightness is-0.015MPa;
(2), be then cooled to 80 DEG C, drop into the mixture (MDI-50) of 22 weight part 2,4-diphenylmethanediisocyanates and 4,4'-diphenylmethanediisocyanate, at N
2in 78 DEG C of stirring reactions 2.8 hours under protection;
(3), finally 1.2 weight part 3-isocyanic ester propyl trimethoxy silicanes are added successively, 0.6 weight part 3-glycidoxypropyltrietandysilane andysilane, 0.1 weight part dibutyl tin laurate, 0.1 weight part 2,2-dimorpholine base Anaesthetie Ether, 1.8 weight part β-positive octadecanol ester of (3,5-di-tert-butyl-hydroxy phenyl) propionic acid is at N
2in 78 DEG C of stirring reactions 1.7 hours under protection;
(4), be warming up to 127 DEG C, be evacuated to bubble-free and occur, then discharging, packs, obtained electronic apparatus reaction type polyurethane hot-melt adhesive.
Comparative example 1
Except not containing 1.2 weight part 3-isocyanic ester propyl trimethoxy silicanes, outside 0.6 weight part 3-glycidoxypropyltrietandysilane andysilane, other raw materials are all identical with embodiment 4, and preparation method is also identical with embodiment 4.
The electronic apparatus reaction type polyurethane hot-melt adhesive that Example 1 ~ 4 and comparative example 1 obtain, melting viscosity is tested by GB/T 10247-2008, the open hour are tested by ASTM 4497-2004, by GB/T528-2009 test tensile strength, tensile shear strength is tested by GB/T 7124-2008, by GB/T7124-2008 test hot and humid (sample is tested place 72 hours under the condition of 85 DEG C/95%RH after), thermal shock (sample be positioned over be set to 1 hour 85 DEG C, then 1 hour thermal shock test chamber of-40 DEG C was tested after 72 hours) tensile shear strength of sample afterwards, test result is as shown in table 1.
The reaction type polyurethane hot-melt adhesive correlated performance test result of table 1 embodiment
As can be seen from the performance comparison of embodiment in table 14 with comparative example 1, add adhesion promotor 3-isocyanic ester propyl trimethoxy silicane and 3-glycidoxypropyltrietandysilane andysilane, hot melt adhesive can be significantly improved to substrate bonding intensity and high-temp resisting high-humidity resisting, thermal shock performance.It is low that reaction type polyurethane hot-melt adhesive prepared by the embodiment of the present invention 1 ~ 4 has melting viscosity, curing speed is fast, to Al, PC, PBT, PET, ABS, PVC, PMMA, there is good adhesiveproperties, and under standing the condition of hot and humid, thermal shock, bonding strength change is little, wherein, the over-all properties of the reaction type polyurethane hot-melt adhesive of embodiment 3 is the most excellent.Reaction type polyurethane hot-melt adhesive prepared by embodiment 1 ~ 4 can be widely used in the fixing, bonding of the various component of electronic enterprises.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. an electronic apparatus reaction type polyurethane hot-melt adhesive, is characterized in that, described hot melt adhesive is made up of the raw material of following weight part:
Polyester polyol 100 parts, isocyanic ester 10 ~ 30 parts, tackifying resin 10 ~ 20 parts, adhesion promotor 1 ~ 3 part, catalyzer 0.1 ~ 0.5 part, 1 ~ 2 part, oxidation inhibitor.
2. electronic apparatus reaction type polyurethane hot-melt adhesive according to claim 1, is characterized in that, described hot melt adhesive is made up of the raw material of following weight part:
Polyester polyol 100 parts, isocyanic ester 23.5 parts, tackifying resin 20 parts, adhesion promotor 1.8 parts, catalyzer 0.15 part, 2 parts, oxidation inhibitor.
3. electronic apparatus reaction type polyurethane hot-melt adhesive according to claim 1 and 2, it is characterized in that, described polyester polyol is the poly-hexanodioic acid-1 of number-average molecular weight 1000 ~ 6000,4-butanediol ester glycol, poly-hexanodioic acid-1,6-hexylene glycol esterdiol, polydiethylene glycol adipate glycol, poly-phthalic acid-1, one or more in 4-butanediol ester glycol, poly-carbonic acid-1,6-hexylene glycol esterdiol.
4. electronic apparatus reaction type polyurethane hot-melt adhesive according to claim 1 and 2, is characterized in that, described isocyanic ester is 4,4 '-diphenylmethanediisocyanate or MDI-50.
5. electronic apparatus reaction type polyurethane hot-melt adhesive according to claim 1 and 2, is characterized in that, described tackifying resin is one or more in Gum Rosin, hydrogenated rosin resin, petroleum resin, terpine resin.
6. electronic apparatus reaction type polyurethane hot-melt adhesive according to claim 1 and 2; it is characterized in that, described adhesion promotor is one or more in 3-mercaptopropyl trimethoxysilane, 3-sulfo-capryloyl-1-propyl-triethoxysilicane, 3-isocyanic ester propyl-triethoxysilicane, 3-isocyanic ester propyl trimethoxy silicane, 3-[3-(trimethoxysilyl) propyl group] isocyanuric acid ester, 3-glycidyl ether oxygen propyl trimethoxy silicane, 3-glycidoxypropyltrietandysilane andysilane.
7. electronic apparatus reaction type polyurethane hot-melt adhesive according to claim 1 and 2, is characterized in that, described catalyzer is one or more in dibutyl tin laurate, triethylenediamine, dimorpholine base Anaesthetie Ether.
8. electronic apparatus reaction type polyurethane hot-melt adhesive according to claim 1 and 2, it is characterized in that, described oxidation inhibitor is 2,6-di-tert-butyl methyl phenol, four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid positive octadecanol ester, three (2.4-di-tert-butyl-phenyl) phosphorous acid ester, one or more in two (3,5-di-tert-butyl-hydroxy phenyl) thioether.
9. the preparation method of the electronic apparatus reaction type polyurethane hot-melt adhesive described in any one of claim 1 ~ 8, is characterized in that, comprise the following steps:
(1), by polyester polyol, tackifying resin drop in reactor, be heated to 110 ~ 130 DEG C, under agitation vacuum hydro-extraction 1.5 ~ 2.5 hours, vacuum tightness is-0.095 ~ 0.05MPa;
(2), be cooled to 80 ~ 90 DEG C, drop into isocyanic ester, at N
2in 75 ~ 85 DEG C of stirring reactions 1 ~ 3 hour under protection;
(3) adhesion promotor, catalyzer, antioxidant is added, successively, at N
2in 75 ~ 85 DEG C of stirring reactions 0.5 ~ 2 hour under protection;
(4), be warming up to 110 ~ 140 DEG C, be evacuated to bubble-free and occur, discharging, to obtain final product.
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Application publication date: 20150325 |