CN105131896A - Method for preparing polyurethane hot melt adhesive capable of achieving quick positioning - Google Patents
Method for preparing polyurethane hot melt adhesive capable of achieving quick positioning Download PDFInfo
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Abstract
The invention relates to a method for preparing polyurethane hot melt adhesive capable of achieving quick positioning. The preparing method includes the steps that 1, reactive tackifier and hydrogenated bisphenol A are added into a reaction still, dehydration is conducted for 2 hours at the temperature of 110 DEG C and the pressure intensity of -0.095 MPa, the mixture is cooled to 70 DEG C, a catalyst and polyisocyanate are added, stirring is conducted at the rotation speed of 400-700 r/min, a reaction is conducted for 1-3 hours at the temperature of 70 DEG C-80 DEG C, then a silane modifier is added, a reaction is conducted for 2-5 hours at the temperature of 70 DEG C-80 DEG C, and modified prepolymer at the sending end of silane is obtained; 2, dehydration is conducted on polyester polyol, polyether polyol and acrylic resin for 2 hours at the temperature of 120 DEG C and the pressure intensity of -0.095 MPa, after dehydration is conducted, the polyisocyanate is added, stirring is conducted at the rotation speed of 400-700 r/min, a reaction is conducted for 1-3 hours at the temperature of 100 DEG C-120 DEG C, then the prepared modified prepolymer at the sending end of the silane, antioxygen and the catalyst are added, the temperature is raised to 110 DEG C, vacuumizing is conducted till the pressure intensity is below -0.095 MPa, air bubble removing is conducted for 30 minutes, discharging and sealed packing are conducted, and the polyurethane hot melt adhesive capable of achieving quick positioning is obtained.
Description
Technical field
The present invention relates to a kind of preparation method realizing the polyurethane hot melt of quick position, belong to chemical sizing agent field.
Background technology
Current, in the streamline link that touch-screen encapsulation manufactures, very urgent to the requirement of enhancing productivity.Traditional hot melt adhesive is generally used to position encapsulation at present.Because traditional hot melt adhesive initial bonding strength is low, setting time is long, and bonding strength is low, and its initial fix undercapacity 0.1MPa of 5 minutes, therefore must carry out pressurize by fixer, to meet the quality of pressing.The requirement of encapsulation laminating can be met in order to ensure device, generally the time of pressurize needs more than 2 hours, seriously constrain the production efficiency that touch-screen encapsulation manufactures, and pressurize utensil is a lot, waste a large amount of resources and space, improve the cost of manufacture.Meanwhile, because the shortcoming that traditional hot-melt adhesive bonding strength is low, the bonding strength of 24 hours, less than 4.0MPa, causes product scrap rate high.Therefore, research and develop a kind of quick position packaged material, become the active demand in this field.
Research and development quick position packaged material develops rapidly abroad, and dominant company comprises Henkel, Fuller, 3M company etc.China's starting is more late, and research and development institution is less, mainly comprises Darbond Technology Co., Ltd., Yantai etc.Therefore the research and development of quick position packaged material, market potential is huge.
Summary of the invention
In order to solve the initial adhesive strength that polyurethane hot melt in prior art exists low, cannot quick position, cold-and-heat resistent impact property is poor, salt spray resistance is poor, loss of properties on aging and the low weakness of bonding strength, the invention provides a kind of polyurethane hot melt realizing quick position and preparation method thereof, its polyurethane hot melt prepared is single-component mist-solidifying polyurethane adhesive, belong to solvent-free environment-protection sizing agent industry, be suitable for the bonding of plastics and various metals base material.
The present invention relates to a kind of polyurethane hot melt realizing quick position, possesses high tack, after applying glue, the bonding strength of 5min is higher than 0.5MPa, quick position can be realized, then this material is by after fixing generation crosslinking reaction, thus improves bulk strength, thermotolerance, the water-fast and chemical resistance of material.
The polyurethane hot melt realizing quick position of the present invention can embody several large advantage: the snappiness that (1) is good and bonding strength, the impact of the expansion coefficient difference between differing materials can be overcome, stress distribution is even, thus encapsulates dissimilar base material; (2) initial adhesive strength is high: after applying glue, the bonding strength of 5min is higher than 0.5MPa; (3) open hour are short: be less than 3min; (4) viscosity is low easy to operate: 100 DEG C of melting viscosities are lower than 8Pa.S; (5) Heat stability is good: 120 DEG C of heating 5 hours viscosity lift-off values are lower than 30%; (6) resistance to drop performance is good: cylinder falls higher than 300 times; (7) final strength is high: PC with PET material bonding strength higher than 7MPa.
The mechanism that polyurethane hot melt of the present invention can realize quick position is: adopt xylene formaldehyde resin and special acrylic acid resin as composite modifier, the two plays synergy, produces the effect that one-plus-one is greater than two.Adopt acrylic resin be the resin with particular molecule functional structure, its active function groups can with isocyanic ester generation graft polymerization reaction, effectively improve the crystallinity of hot melt adhesive, thus realize fast positioning function.The xylene formaldehyde resin adopted is as high-effective viscosity agent, participate in isocyanate reaction, improve the initial bond strenght of hot melt adhesive, thus realize the function of quick position, xylene formaldehyde resin is as toughner simultaneously, effectively improves the snappiness of product, shock resistance and water-fast ageing-resistant performance.In addition, silicone hybrid isocyanate groups generation moisture curing crosslinking reaction, generates the fine and close build macromole of obdurability, thus obtains final high strength.
Technical scheme of the present invention is as follows: a kind of preparation method realizing the polyurethane hot melt of quick position, and preparation process is:
A. by reactive tackifier 5 ~ 20 parts, Hydrogenated Bisphenol A meter 1 ~ 8 part adds in reactor, in 110 DEG C ,-0.095MPa dewaters 2h, be cooled to 70 DEG C, add catalyzer 0.01 ~ 0.05 part, polyisocyanates 10 ~ 45 parts, stirred with the rotating speed of 400 ~ 700 revs/min, in 70 DEG C ~ 80 DEG C reactions 1 ~ 3 hour.Add silane modifier 20 ~ 30 parts again, in 70 DEG C ~ 80 DEG C reactions 2 ~ 5 hours, obtained Silante terminated modification performed polymer, Hydrogenated Bisphenol A can give the skeleton rigid structure of sizing agent, improves bonding strength and shock resistance.
B. by polyester polyol 40 ~ 65 parts, polyether glycol 15 ~ 35 parts, acrylic resin 10 ~ 30 parts is in 120 DEG C,-0.095MPa carries out dehydration 2h, after dehydration, add polyisocyanates 12 ~ 35 parts, stir with the rotating speed of 400 ~ 700 revs/min, react 1 ~ 3 hour at 100 DEG C ~ 120 DEG C, add Silante terminated modification performed polymer 5 ~ 25 parts prepared by this step a again, 0.02 part ~ 1 part, oxidation inhibitor, catalyzer 0.001 ~ 0.1 part, be warmed up to 110 DEG C, be evacuated to below-0.095MPa, remove bubble 30min, discharging, airtight package, the polyurethane hot melt of obtained quick position.
On the basis of technique scheme, the present invention can also do following improvement:
Further, polyisocyanates in described step a and b is tolylene diisocyanate (TDI-80, TDI-100), ditan-4,4 ＇-vulcabond (MDI), HDI (HDI), an xylylene diisocyanate (M-XDI), polymethine polyphenyl polyisocyanate (PAPI), triphenylmethane triisocyanate (TTI), 2, at least one in 4-toluene diisocyanate trimer, HDI tripolymer, 1,5-naphthalene diisocyanate, hydrogenation TDI, hydrogenation MDI.Be preferably the mixture of one or more in commercially available tolylene diisocyanate TDI-80, TDI-100 and HDI tripolymer DesmodurN3300 of commercially available 4, the 4' diphenylmethanediisocyanate MDI of Yantai Wan Hua limited-liability company, Bayer A.G.
Further, in described step a, reactive tackifier are xylene formaldehyde resin.The preferred trade mark is commodity " Nikanol " resin by name of Mitsubishi gas companies market.
The beneficial effect of above-mentioned further scheme is adopted to be containing hydroxyl, ehter bond isoreactivity group in xylene formaldehyde resin molecular structure, more than 80% is had for dimethylbenzene methyne structure in molecular composition, self there are good toughness group and water resistance, its active o content 9 ~ 12%, hydroxyl value 4.5%.The present invention's choosing uses it as tackifier and toughner, participate in isocyanate reaction, improve the initial bond strenght of hot melt adhesive, thus realize the function of quick position, also effectively improve the snappiness of product, final bonding strength, shock resistance and water-fast ageing-resistant performance simultaneously.
Further, the catalyzer in described step a and b is at least one in dibutyl tin laurate, stannous octoate, lead octoate 36, triethylamine, triethylenediamine, cobalt octoate, iron octoate, zinc naphthenate, tetrabutyl titanate, dimorpholine base Anaesthetie Ether (DMDEE).
Further, in described step a, silane modifier is one or more in organosilane Y9669, KH550, KH560, A189 of Buddhist santonin company.
The beneficial effect of above-mentioned further scheme is adopted to be, adopt silane hybrid polyurethane technology, in molecular structure, distinctive silicone-type group can generate three dimensional structure, make polymkeric substance development in tridimensional network after reaction chain extension, the longer molecular chain of resistance to lotus can be caused, give the unit elongation that sizing agent is longer, higher tear strength, tensile strength and stripping strength, and better sticking power.
Further, in described step b polyether glycol be molecular weight 1000 ~ 4000 Polyoxypropylene diol, polyoxytrimethylene-ethylene oxide dibasic alcohol, PTMG, polycaprolactone glycol, one in polycarbonate diol, be preferably one or both the mixture in commercially available PTMG2000, PTMG3000, PPG204, PPG210, PPG220.
Further, in described step b, polyester polyol is hexanodioic acid and 1,4-butyleneglycol, neopentyl glycol, ethylene glycol, glycol ether and 1, at least one dibasic alcohol in 6-hexylene glycol is polymerized, described polyhexamethylene adipate glycol is preferably the commercially available XCP-3000H of Jiangsu Xu Chuan chemical company, its hydroxyl value is 35 ~ 39mgKOH/g, acid number is 0.1 ~ 0.8mgKOH/g, described poly-hexanodioic acid-1,4-butanediol ester glycol is preferably the commercially available POL-356T of Qingdao New Yutian Chemical Co., Ltd., its hydroxyl value is 53 ~ 59mgKOH/g, and acid number is 0.1 ~ 0.8mgKOH/g.
The beneficial effect of above-mentioned further scheme is adopted to be that the polyvalent alcohol that the present invention adopts is mixed by multiple crystallinity or amorphism polyvalent alcohol and forms, and the amount increasing crystallinity polyvalent alcohol can improve initial strength, but crystallinity is excessive, glue-line is fine and close, steam can be hindered to enter, curing speed is slowed down; The amount increasing amorphism polyvalent alcohol can extend the open hour, but initial strength can reduce.Therefore the consumption balancing various polyvalent alcohol is needed, to obtaining good performance.
Further, acrylic resin in described step b, is specially the one in DB256, DB66, DB68 that Yantai federal corporate produces.
The beneficial effect of above-mentioned further scheme is adopted to be, the acrylic resin that the present invention adopts Yantai federal corporate to produce is the resin of the particular molecule functional structure with unknown concrete structure, its active function groups can with isocyanic ester generation graft polymerization reaction, effectively improve the crystallinity of hot melt adhesive, thus realize fast positioning function.
Further, in described step b, oxidation inhibitor is at least one in commercially available antioxidant 264, antioxidant 1010, antioxidant 1076.
The beneficial effect of above-mentioned further scheme is adopted to be that oxidation inhibitor can improve the ageing resistance of sizing agent.
During use, first open heating system, temperature is set to 100 ~ 160 DEG C, and with glue rifle gluing, pressing as early as possible within the open hour, room temperature can reach final strength in 7 days.
The present invention is that the initial bond strenght that polyurethane hot melt in prior art exists is low, shock resistance is poor, water resistance is poor in order to solve, loss of properties on aging and the slow weakness of curing speed, a kind of preparation method realizing the polyurethane hot melt of quick position is provided, belong to solvent-free environment-protection sizing agent industry, obtained polyurethane hot melt can meet the compound sticking of plastics and various metals base material, brings great improvement to polyurethane adhesive performance.
Polyurethane hot melt prepared by the present invention, there is good initial strength, efficient positioning function fast can be realized, and its bonding strength, snappiness, shock resistance, water-fast, ageing-resistant performance and curing speed are all very excellent, there is great raising than current similar sizing agent on the market, the rigors in the high-end manufacture field such as mobile phone, communication equipment can be met.
Embodiment
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Raw material in following examples is parts by weight; Polyether glycol PPG210, polyether glycol PPG220, polyether glycol PPG204 are that Plant of Tianjin Petrochemical Company three factory is commercially available; Polyester polyol POL-356T is that Qingdao New Yutian Chemical Co., Ltd. is commercially available, and its hydroxyl value is 53 ~ 59mgKOH/g, and acid number is 0.1 ~ 0.8mgKOH/g; Polyester polyol XCP-3000H is that Jiangsu Xu Chuan chemical company is commercially available, and its hydroxyl value is 35 ~ 39mgKOH/g, and acid number is 0.1 ~ 0.8mgKOH/g; Reactive tackifier " Nikanol " resin is Mitsubishi gas companies market; 4,4' diphenylmethanediisocyanate MDI is that Yantai Wan Hua limited-liability company is commercially available; Tolylene diisocyanate TDI80, TDI-100, DesmodurN3300 are that Bayer A.G is commercially available; At least one in DB256, DB66, DB68 that acrylic resin produces for Yantai federal corporate.
Embodiment 1:1) by reactive plasticizer " Nikanol " resin 5 parts, Hydrogenated Bisphenol A meter 8 parts adds in reactor, in 110 DEG C ,-0.095MPa dewaters 2h, be cooled to 70 DEG C, add dibutyl tin laurate 0.01 part, Germany Baeyer DesmodurN3300 counted 10 parts, stirs with the rotating speed of 400 revs/min, in 70 DEG C of reactions 3 hours.Add silane modifier Y9669 again and count 20 parts, in 70 DEG C of reactions 5 hours, obtained Silante terminated modification performed polymer.
2) polyester polyol XCP-3000H is counted 65 parts, polyether glycol PPG220 counts 15 parts, acrylic resin DB256 counts 30 parts in 120 DEG C,-0.095MPa carries out dehydration 2h, after dehydration, add 4, 4' diphenylmethanediisocyanate MDI-100 counts 35 parts, stir with the rotating speed of 700 revs/min, react 1 hour at 120 DEG C, add Silante terminated modification performed polymer 5 parts prepared by this step a again, antioxidant 264 agent 1.0 parts, dimorpholine base Anaesthetie Ether (DMDEE) 0.1 part, be warmed up to 110 DEG C, be evacuated to below-0.095MPa, remove bubble 30min, discharging, airtight package, the polyurethane hot melt of obtained quick position.
Embodiment 2:1) by reactive plasticizer " Nikanol " resin 20 parts, Hydrogenated Bisphenol A meter 1 part adds in reactor, in 110 DEG C ,-0.095MPa dewaters 2h, be cooled to 70 DEG C, add stannous octoate 0.05 part, 2,4 toluene diisocyanate tripolymer meter 45 parts, stir with the rotating speed of 700 revs/min, in 80 DEG C of reactions 1 hour.Add silane modifier A189 again and count 30 parts, in 80 DEG C of reactions 2 hours, obtained Silante terminated modification performed polymer.
2) polyester polyol POL-356T is counted 40 parts, polyether glycol PPG204 counts 35 parts, acrylic resin DB66 counts 10 parts in 120 DEG C,-0.095MPa carries out dehydration 2h, after dehydration, add 4, 4' diphenylmethanediisocyanate MDI-100 counts 9 parts, tolylene diisocyanate TDI-100 counts 3 parts, stir with the rotating speed of 400 revs/min, react 3 hours at 100 DEG C, add Silante terminated modification performed polymer 25 parts prepared by this step a again, antioxidant 1010 meter 0.02 part, triethylenediamine 0.001 part, be warmed up to 110 DEG C, be evacuated to below-0.095MPa, remove bubble 30min, discharging, airtight package, the polyurethane hot melt of obtained quick position.
Embodiment 3:1) by reactive plasticizer " Nikanol " resin 13 parts, Hydrogenated Bisphenol A meter 4 parts adds in reactor, in 110 DEG C ,-0.095MPa dewaters 2h, be cooled to 70 DEG C, add dibutyl tin laurate 0.04 part, triphenylmethane triisocyanate (TTI) counted 30 parts, stirs with the rotating speed of 550 revs/min, in 75 DEG C of reactions 2 hours.Add silane modifier KH-550 again and count 26 parts, in 75 DEG C of reactions 3.5 hours, obtained Silante terminated modification performed polymer.
2) polyester polyol XCP-3000H is counted 33 parts, polyester polyol POL-356T counts 20 parts, polyether glycol PPG210 counts 25 parts, acrylic resin DB68 counts 20 parts in 120 DEG C,-0.095MPa carries out dehydration 2h, after dehydration, add 4, 4' diphenylmethanediisocyanate MDI counts 14 parts, tolylene diisocyanate TDI100 counts 5 parts, stir with the rotating speed of 550 revs/min, react 2 hours at 110 DEG C, add Silante terminated modification performed polymer 15 parts prepared by this step a again, antioxidant 1076 meter 0.05 part, dimorpholine base Anaesthetie Ether (DMDEE) 0.04 part, triethylenediamine 0.01 part, be warmed up to 110 DEG C, be evacuated to below-0.095MPa, remove bubble 30min, discharging, airtight package, the polyurethane hot melt of obtained quick position.
When the hot melt adhesive that above embodiment 1 to embodiment 3 obtains uses, first open heating system, temperature is set to 70 ~ 120 DEG C, with glue rifle gluing.Initial strength is tested by after 5min after applying glue, and final strength is tested after placing 7 days after applying glue.General self-vulcanizing can reach maximum intensity in 7 days.
Comparative example: the formula and processing technology of conventional wet curing PUR glue is as follows: polyether glycol PPG210 is counted 20 parts, polyester polyol POL-356T counts 45 parts and adds in reactor, stir with the rotating speed of 500 revs/min, vacuum hydro-extraction 2 hours at 120 DEG C, vacuum tightness remains on-0.09MPa.Then be cooled to 80 DEG C, limit is stirred and is counted 15 parts all over adding 4,4' diphenylmethanediisocyanate MDI, then slowly heats up, and control temperature is at 80 DEG C, and inflated with nitrogen protection simultaneously, reacts 2.5 hours.After analysis NCO% content to be sampled reaches design load, then add terpenes tackifying resin 15 parts, catalyst dibutyltin dilaurylate 0.1 part and triethylene diamine 0.4 part.Be be evacuated to bubble-free under the condition of 110 DEG C to occur in temperature, then discharging, airtight package, places stand-by.This glue, when technique uses, first opens heating system, and temperature is set to 100 ~ 130 DEG C, and with glue rifle gluing, gluing process is guaranteed to complete within the open hour, then is carried out in accordance with regulations test.Initial strength is tested after placing 5min after gluing, and final strength is tested after placing 7 days after gluing.General self-vulcanizing can reach maximum intensity in 7 days.
Polyurethane hot melt polyurethane hot melt obtained for above-described embodiment 1 ~ 3 and comparative example prepared carries out initial shear strength, initial bonding strength, tensile strength, elongation at break, final shearing resistance, final stripping strength, thermal shock, SaltSprayTest and two 85 aging rear tests by tackiness agent touchstone, and data results is as shown in table 1, table 2, table 3.Wherein characterize the ability of quick position with the numerical value of the gluing initial shear strength of 5 minutes and initial bonding strength, this is that core of the present invention considers index.In addition, snappiness of the present invention, bonding strength, shock resistance are characterized by the numerical value of the tensile strength of table 2, elongation at break, final shearing resistance, final stripping strength, thermal shock respectively; Salt spray resistance and heat aging property are characterized by the numerical value of table 3 test item.
Table 1 embodiment and comparative example's initial strength (quick position ability) test comparison
Table 2 embodiment contrasts with comparative example's measuring mechanical property
Table 3 embodiment and the water-fast ageing-resistant performance test comparison of comparative example
As can be seen from above-mentioned table 1-3, embodiment 1 ~ 3 shows with the performance test analysis of comparative example, and polyurethane hot melt prepared by the present invention has efficient positioning performance fast.Meanwhile, this glue has good bonding strength and excellent snappiness, cold-and-heat resistent impact and salt spray resistance ageing-resistant performance.So, provided by the present invention have polyurethane hot melt, the strict demand of the manufacture such as mobile phone, communication equipment field needs quick position, high-adhesive-strength can be met, can greatly enhance productivity, reduce manufacturing cost, the core competitiveness promoting domestic polyurethane hot melt is had important practical significance.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. can realize a preparation method for the polyurethane hot melt of quick position, it is characterized in that preparation process is:
A. by reactive tackifier 5 ~ 20 weight part, Hydrogenated Bisphenol A meter 1 ~ 8 weight part adds in reactor, in 110 DEG C ,-0.095MPa dewaters 2h, be cooled to 70 DEG C, add catalyzer 0.01 ~ 0.05 weight part, polyisocyanates 10 ~ 45 weight part, stir with the rotating speed of 400 ~ 700 revs/min, in 70 DEG C ~ 80 DEG C reactions 1 ~ 3 hour, then add silane modifier 20 ~ 30 weight part, in 70 DEG C ~ 80 DEG C reactions 2 ~ 5 hours, obtained Silante terminated modification performed polymer;
B. by polyester polyol 40 ~ 65 weight part, polyether glycol 15 ~ 35 weight part, acrylic resin 10 ~ 30 weight part is in 120 DEG C,-0.095MPa carries out dehydration 2h, after dehydration, add polyisocyanates 12 ~ 35 weight part, stir with the rotating speed of 400 ~ 700 revs/min, react 1 ~ 3 hour at 100 DEG C ~ 120 DEG C, add Silante terminated modification performed polymer 5 ~ 25 weight part prepared by step a again, oxidation inhibitor 0.02 weight part ~ 1.0 weight part, catalyzer 0.001 ~ 0.1 weight part, be warmed up to 110 DEG C, be evacuated to below-0.095MPa, remove bubble 30min, discharging, airtight package, the polyurethane hot melt of obtained quick position.
2. the polyurethane hot melt realizing quick position according to claim 1, is characterized in that, in described step a, reactive tackifier are xylene formaldehyde resin.
3. the preparation method realizing the polyurethane hot melt of quick position according to claim 1, the catalyzer that it is characterized in that in described step a and b is the one in dibutyl tin laurate, stannous octoate, lead octoate 36, triethylamine, triethylenediamine, cobalt octoate, zinc naphthenate, tetrabutyl titanate, dimorpholine base Anaesthetie Ether.
4. the preparation method realizing the polyurethane hot melt of quick position according to claim 1, it is characterized in that the polyisocyanates in described step a and b is tolylene diisocyanate, ditan-4,4 ＇-vulcabond, HDI, 1, one in 5-naphthalene diisocyanate, an xylylene diisocyanate, polymethine polyphenyl polyisocyanate, 2,4 toluene diisocyanate tripolymer, HDI tripolymer, hydrogenation TDI, hydrogenation MDI.
5. the polyurethane hot melt realizing quick position according to claim 1, is characterized in that, in described step a, silane modifier is one or more in organosilane Y9669, KH550, KH560, A189.
6. the preparation method realizing the polyurethane hot melt of quick position according to claim 1, it is characterized in that polyether glycol in described step b be molecular weight 1000 ~ 4000 Polyoxypropylene diol, polyoxytrimethylene-ethylene oxide dibasic alcohol, PTMG, polycaprolactone glycol, one in polycarbonate diol.
7. the preparation method realizing the polyurethane hot melt of quick position according to claim 1, it is characterized in that in described step b, polyester polyol is hexanodioic acid and 1, at least one dibasic alcohol in 4-butyleneglycol, neopentyl glycol, ethylene glycol, glycol ether and 1,6-hexylene glycol is polymerized.
8. the preparation method realizing the polyurethane hot melt of quick position according to claim 1, is characterized in that the one in DB256, DB66, DB68 that acrylic resin in described step b produces for Yantai federal corporate.
9. the preparation method realizing the polyurethane hot melt of quick position according to claim 1, is characterized in that oxidation inhibitor in described step b is at least one in commercially available antioxidant 264, antioxidant 1010, antioxidant 1076.
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