CN1550534A - Method for preparing emulsion adhesive and its use - Google Patents

Method for preparing emulsion adhesive and its use Download PDF

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Publication number
CN1550534A
CN1550534A CNA2004100423178A CN200410042317A CN1550534A CN 1550534 A CN1550534 A CN 1550534A CN A2004100423178 A CNA2004100423178 A CN A2004100423178A CN 200410042317 A CN200410042317 A CN 200410042317A CN 1550534 A CN1550534 A CN 1550534A
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emulsion
application
methyl
defoamer
high speed
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CN1261517C (en
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角善男
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Toyo Ink Mfg Co Ltd
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Toyo Ink Mfg Co Ltd
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Abstract

The method for producing an emulsion type pressure-sensitive adhesive having 40-1,000 mPa*s of viscosity, comprises a continuous dispersing process of an acrylic copolymer emulsion mainly comprising an alkyl (meth)acrylate and an antifoaming agent by using a high speed rotating shear type stirrer having stirring blades and fixed rings. The pressure-sensitive adhesive product comprises a pressure-sensitive adhesive layer composed of the obtained emulsion type pressure-sensitive adhesive.

Description

The manufacture method of Emulsion Adhesive and application thereof
Technical field
The present invention relates to be applicable to adhesive label and paste manufacture method and the application thereof that band waits the Emulsion Adhesive of the tackiness agent of pasting goods.Particularly relate to and be applicable to that high-speed production is pasted the manufacture method of the Emulsion Adhesive of goods by the body material of pasting goods is carried out the high speed application.
Background technology
In recent years, low price trend in the world is to the raising and the rationalization of productivity and reduce cost and propose very high request, is the high speed that advances adhesion application processing as a countermeasure of pasting goods manufacturing firm.Up to now, paste in Japan in the manufacturing of goods, though in most cases be that people require to carry out application than its higher speed with the mode goodsization of about 100~200 meters/minute application speed application tackiness agents.
Paste the goods producer and will carry out the high speed application of tackiness agent, must suitably adjust the form, particularly viscosity of tackiness agent and viscosity so that adapt to this high speed application.Under the occasion with existing application speed (100~200 meters/minute) application, can use industrial coating machine, unicoater, reverse coating machine, be applicable to the viscosity of the tackiness agent of these coating machines, can adjust to about thousands of~20,000 mPas as coating machine.On the other hand, under the occasion with the application speed application more than 200 meters/minute, the coating machine that can adapt to the high speed application, can use box gravure coating machine, scraper plate coating machine, curtain formula coating machine etc., according to the principle of its application mode, in tens of~hundreds of mPas left and right sides scope that the viscosity of tackiness agent is preferably in.
Yet, make and can directly use existing device, have tens of~such low viscosity of hundreds of mPas simultaneously, the Emulsion Adhesive that coating performance is good is because following various reasons but very difficult.
That is to say, Emulsion Adhesive, except directly application on the body materials such as paper and plastics film, often adopt transfer printing as demoulding processing and application carry out application on the stickup face of release liner of silicone resin, allocate tensio-active agent therein in order to reduce surface tension as far as possible under this occasion.And the resin emulsion of Emulsion Adhesive, owing to adopt the emulsion polymerization manufactured, adopt tensio-active agent as this emulsifying agent.
Therefore, Emulsion Adhesive is owing to contain the exhibiting high surface promoting agent, thus adjust to low viscosity with the occasion that adapts to the high speed application under, than more be easy to generate bubble in the past, this can produce harmful effect to the high speed coating performance.The bubble that produces of the bubble of the inclusion of air coating machine head that produces during application and circulation time particularly, will destroy the smoothness of application face, perhaps under serious occasion, will become the reason that forms pin hole (pin hole), flake (eye hole) and shrinkage cavity (cissing or repellence).So-called shrinkage cavity is meant and produces circular and oval-shaped not application part on a part is filmed.
As this foaming countermeasure and the general method that adopts is to use the stronger defoamer of froth breaking ability.As the stronger defoamer of this froth breaking ability, use the polysiloxane series defoamer of allocating hydrophobicity silicon oxide and mineral oil in case of necessity into.Yet, though this defoamer froth breaking ability is strong, but be difficult in the system of being dispersed in (whole tackiness agent), under the situation that defoamer exists with big particle diameter, form the high hydrophobic part of concentration in the part, this becomes the starting point of shrinkage cavity often.
And the manufacturing process of Emulsion Adhesive in the past is, adds matrix polymer, adds defoamer while stirring, with in the ammoniacal liquor with after add sanitas successively, give tackifying resin and wetting agent etc., adjust with tackifier at last; For making its viscosity realize lowering viscousity, when additional water is diluted operation for this reason, adopt the method for the amount of control tackifier.Though yet adopt this mode can obtain required viscosity, it is bad only to adopt this measure defoamer to disperse, and can produce shrinkage cavity during application.Even like this, in the industry manufacturing still of aqueous binder, also must have various agitating vanes such as blade, water screw, screw blade, anchor shape blade, turbine blade, large-scale blade usually, and flow deflector (baffle in case of necessity, interceptor, flow-disturbing rod) etc., no matter use which kind of equipment, for the strong polysiloxane defoamers of above-mentioned froth breaking power is disperseed equably, also must have shearing force to a certain degree.At this moment, though because for the high tackiness agent of making in the past of viscosity need apply sufficient shearing force, but under the occasion of the low tackiness agent of viscosity if can not obtain to disperse necessary shearing force, defoamer is produced disperse bad.Viscosity height described here is meant the viscosity about thousands of~20,000 mPas, the low viscosity that is meant about tens of~hundreds of mPas of described viscosity.
For example for the polysiloxane series defoamer, can control balance between defoaming and the dispersiveness by the molecular weight that changes polysiloxane.When molecular weight increased, defoaming increased and dispersiveness reduces, otherwise will show opposite behavior when molecular weight reduces.The producer of nearly all defoamer can produce the goods of various grades according to user's practical purpose.Here, the inventor etc. produce shrinkage cavity during for fear of the application of tackiness agent high speed and have allocated the polysiloxane series defoamer of dispersed good grade into, make still with traditional intermittent type and carried out research trial, but do not obtain the target defoaming, and then studied the defoamer of each manufacturer, between defoaming and dispersiveness, do not obtain required balance yet.
On the other hand, though considered that in case the method for dilute with water again after adjusting to high viscosity and defoamer fully being disperseed, the final nonvolatile component of goods reduces under this occasion.The price of tackiness agent rises if nonvolatile component reduces then, and this is inconsistent again with the requirement of carrying out the high speed application for reducing cost of pasting product manufacturer.
Summary of the invention
So the object of the invention is to provide a kind of manufacturing to be suitable for the high speed application and has the method for the tackiness agent of good wettability, utilize tackiness agent that this method obtains and the stickup goods that use this tackiness agent.
The present invention relates to the manufacture method that a kind of viscosity is the Emulsion Adhesive of 40~1000mPas, has the high speed rotating shear-type stirrer of agitating vane and set collar comprising use, to (methyl) alkyl acrylate being the propylene series copolymer emulsion of main component and the operation that defoamer carries out dispersion treatment continuously.Adopt the present invention, can make the beautiful specification of high speed coating machine reach lowering viscousity, can be with the high productivity a large amount of high comprehensive performance that wettabilities and defoaming take into account, Emulsion Adhesives made on technical scale with good coating performance.
Another aspect of the present invention relates to the Emulsion Adhesive that the manufacture method of the Emulsion Adhesive that utilizes the invention described above obtains.
The stickup goods that include the binder layer that the Emulsion Adhesive by the invention described above forms that relate in one aspect to again of the present invention.
Description of drawings
Fig. 1 is the part stereographic map that schematically illustrates an example of the agitating vane of high speed rotating shear-type stirrer and set collar.
Fig. 2 (a) schematically illustrates the cross-section side view of dispersion treatment with an example of device, and Fig. 2 (b) is along the sectional view of cross hatching B-B among Fig. 2 (a).
Embodiment
The propylene series copolymer emulsion that this Emulsion Adhesive (being designated hereinafter simply as " tackiness agent ") uses, with (methyl) alkyl acrylate as main component.In this specification sheets, described (methyl) vinylformic acid be meant methacrylic acid and vinylformic acid the two.
This propylene series copolymer emulsion can adopt known method in water medium, is that the monomer mixture of main component carries out free-radical emulsion polymerization and makes at an easy rate by means made from (methyl) alkyl acrylate.In letex polymerization, can also add chain-transfer agent or softening agent in case of necessity.
In the above-mentioned multipolymer, as (methyl) alkyl acrylate that the monomer main component is used, can enumerate (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) vinylformic acid n-propyl, (methyl) isopropyl acrylate, (methyl) n-butyl acrylate, (methyl) isobutyl acrylate, (methyl) Ethyl acrylate, (methyl) cyclohexyl acrylate, (methyl) 2-EHA, (methyl) vinylformic acid n-octyl, (methyl) Isooctyl acrylate monomer, (methyl) vinylformic acid ester in the positive ninth of the ten Heavenly Stems, (methyl) vinylformic acid ester in the different ninth of the ten Heavenly Stems, (methyl) decyl acrylate and (methyl) lauryl acrylate etc.These can also be used in combination except that independent use.In these materials, special preferred alkyl carbonatoms is (methyl) alkyl acrylate of 4~12.
(methyl) alkyl acrylate (calculating with its resultant when several are shared) preferably accounts for about 70~99.5 weight % in 100 weight % multipolymers.
As can with other monomers of (methyl) alkyl acrylate copolymer, can enumerate vinyl monomer, for example (methyl) vinyl cyanide, alpha-chloro (methyl) vinyl cyanide etc. contain the vinyl monomer of cyano group; Vinyl aromatic monomers such as vinylbenzene, alpha-methyl styrene, Vinyl toluene; Unsaturated carboxylic acids such as (methyl) vinylformic acid, Ba Dousuan, TRANSCINNAMIC ACID, methylene-succinic acid, fumaric acid, toxilic acid; Unsaturated dicarboxylic acid mono alkyl esters such as methylene-succinic acid mono ethyl ester, fumaric acid mono, butyl maleate; (methyl) vinylformic acid 2-hydroxy methacrylate, (methyl) vinylformic acid 2-hydroxyl butyl ester, (methyl) vinylformic acid hydroxy propyl ester, 2-hydroxyl-3-phenoxy propyl (methyl) acrylate, glycerine (methyl) acrylate, polyethyleneglycol (methyl) acrylate, polypropylene glycol list (methyl) acrylate and polyethylene glycol-propylene glycol list (methyl) acrylate etc. contain the vinyl monomer of hydroxyl; Ethene such as acrylamide, Methacrylamide, N-methylol-acrylamide are unsaturated carboxylic acid acid amides and N substituent thereof; Unsaturated alcohols such as allyl alcohol.In addition, can also use (methyl) glycidyl acrylate, vinyl acetate, vinylchlorid, vinylidene chloride etc. as copolymer composition.
Copolymer emulsion can carry out the alkali neutralization in order to improve its stability, for example neutralizes with ammoniacal liquor.
The solids content of copolymer emulsion considers to be preferably 40~70 weight % from coating.Coating described here is meant the application face that can obtain not having indentation and shrinkage cavity on the edge, described indentation (retraction) is meant the application part at the film two ends, originally be coated with the center side that holding position is shifted to film from what coating was supplied with in coating outlet, cause coating area to reduce, the thickness of application end increases.
As defoamer can enumerate the polysiloxane series defoamer, mineral oil is defoamer and nonionic surface active agent, wherein from the preferred use polysiloxane series of the strong viewpoint of froth breaking power defoamer.As the polysiloxane series defoamer, can use defoamer with polydimethyl sily oxide structure etc.Can also use the polysiloxane series defoamer that is mixed with hydrophobicity silicon oxide and mineral wet goods in case of necessity, the commodity that the commercially available product of these defoamers for example preferably use to finish Migong, Cook department (PVC Star Network ケ ミ-society) are called the BYK-011,018,019,020,021,022,023,024,025,028,034,038,044,088,094,1610 and 1615 etc. of BYK series; The SN デ Off オ マ-223 of the SN moral Buddhist sign indicating number (デ Off オ マ-) of the severe company of Sang Nuopu (サ Application ノ プ コ society) series, 245,247,250,364,375,382,440,483,485,554 and 777 etc.; The promise of the promise general severe (ノ プ コ) of the severe company of Sang Nuopu (サ Application ノ プ コ society) series general severe 8034,8034-L, 267-A and DF-122 etc.
The use level of defoamer the viewpoint of shrinkage cavity occurs from avoiding application face, preferably accounts for 0.01~1.5 weight part in 100 weight part copolymer emulsions.
Except aforesaid propylene based copolymer emulsion and defoamer,, can also allocate the Synergist S-421 95 of employed kind and quantity in the adhesive field in case of necessity in the tackiness agent in order to give as desired physical properties of the Emulsion Adhesive of target product and performance.As the Synergist S-421 95 that can add, tackifier are for example arranged, give sticky agent, linking agent, sanitas, pigment and wetting agent etc.
As the gradation composition of dispersion treatment tackiness agent (promptly, propylene series copolymer emulsion and defoamer and other compositions in case of necessity) stirrer of usefulness, can use to have high speed rotating shear-type stirrer agitating wing and set collar (being designated hereinafter simply as " stirrer ").The invention is characterized in that using this stirrer is with continous way rather than the above-mentioned gradation composition of intermittent type dispersion treatment.That is to say that employed device not only makes the agitating vane high speed rotating, and by making up with set collar, powerful shearing action and the surging force of utilizing the gap between agitating wing and set collar to produce can improve fluidic micronize effect.
Shown in an example illustrated in figures 1 and 2, stirrer 100 has the steel basin cylindraceous 10 that supply-pipe 11 is connected with outlet pipe 12, has agitating wing 1 and set collar 2 in steel basin 10 inside.
Agitating wing 1 is fixed on the lower end of the turning axle 3 that utilizes motor 4 rotations that are arranged on top, makes it with high speed rotating.The speed of rotation of agitating wing 1 is fully disperseed in order to make defoamer, more than preferred 15 meter per seconds of circumferential speed, more preferably about 20~40 meter per seconds.Perhaps preferably with the above high speed rotating of 1500rpm.As agitating wing, can adopt the various agitating vanes of arbitrary shapes such as oar blade type blade, screw blade, screw blade, anchor shape blade, turbine blade, large-scale blade, there is no particular restriction for the number of blade.
Set collar (stator) 2 has the spoiler effect, prevents to produce excessive hole near the periphery of agitating wing 1, prevents that the hole from causing axial flow.But for making the agitating wing high speed rotating, residual in the small gap between agitating wing and set collar have a suitable hole, to apply surging force.Its result can produce powerful rotational shear effect and surging force in the gap of agitating wing and set collar, convection cell produces the micronize effect, can carry out stable dispersion treatment whereby.
As shown in the figure, preferably agitating wing 1 is designed slightly littler, be located at the inboard of set collar 2 than set collar 2 diameters.Specifically, if an example will be shown, then preferably make the internal diameter of set collar 2 be about 20 centimetres, and the external diameter of agitating wing is slightly littler than it, the gap of the two (leading section of agitating wing and the distance between the set collar) is 0.2 millimeter.
As shown in Figure 1, the shape that is provided with a plurality of holes both can be made in the top of set collar 2, also can make the tubular shape of atresia, and there is no particular restriction.Though figure does not go out, except that set collar 2, garden for example moving up and down disk shaped part can also be set on the turning axle of the top of set collar.
The gradation composition of tackiness agent is supplied with steel basin 10 continuously by the supply-pipe of stirrer 100, discharges to the outside from outlet pipe through after the dispersion treatment.Can carry out the dispersion treatment of gradation composition so continuously.Not with intermittent mode but, can suppress the generation of bubble by carrying out the dispersion treatment of continous way.At this moment, both each gradation composition can be supplied with steel basin 10 respectively successively, the form with the mixture (composition) of gradation composition after also can mixing in other stills of preparing burden etc. is supplied with.
In preferred embodiment, before carrying out dispersion treatment, carry out pre-dispersed in advance to each gradation composition with above-mentioned stirrer 100.Carrying out when pre-dispersed, preferably as shown in Figure 2, can be by the supply-pipe 11 of stirrer 100, carrying out with in pipeline and the batching still 20 that stirrer 100 is connected by pump 24.Can adopt any method to carry out at batching pre-dispersed in the still 20, there is no particular restriction to it.For example, can use inside to have the batching still as shown in the figure of agitating vane 22 and bar-shaped baffle plate (choked flow rod) 23, supply with each gradation composition from the supply-pipe 21 of batching still 20, and carry out suitable stirring.Because there is no particular restriction to the structure of the batching still of this pre-dispersed usefulness, thereby for example can adopt and only be provided with agitating vane and unbaffled batching still.
For example as shown in Figure 2, also can connect, the treatment solution after stirrer 100 dispersion treatment is returned in the batching still 20 once more, while use pump 24 to make the treatment solution circulation carry out dispersion treatment by still 20 that the outlet pipe 12 of stirrer 100 is prepared burden therewith.That is to say,, can constantly carry out the continous way processing under the round-robin situation by on the external circulation line of batching still stirrer being set in pipeline.
As the typical equipments of high speed rotating shear-type stirrer, can enumerate the even line of flow machine of T.K. (ホ モ ミ Star Network ラ イ Application Off ロ-) (special machine Chemical Co., Ltd make), card Pitot dragon (キ ヤ PVC ト ロ Application) (Pacific Machinery ﹠ Engineering Co., Ltd.'s manufacturing), E Balamailuda (エ バ ラ マ イ Le ダ-) (Ebara Corporation's manufacturing), colloidal mill (refreshing steel パ Application テ Star Network Co., Ltd. make), Tuo Luneiduo (ト Le ネ-De) (shallow field ironworker Co., Ltd. make), Xia Luote colloidal mill (manufacturing of ケ ミ コ ロ イ De ラ ボ ラ De リ Co., Ltd.) and the Li Akuda of De Si Baku (デ イ ス パ Star Network-リ ア Network -) (manufacturing of IKA-WERKEGMBH Co., Ltd.) etc.
The dispersion state of defoamer, except that stirring velocity owing to also depend on churning time, so, suitably adjust churning time preferably according to the composition of kind, quantity and the gradation composition mixture of defoamer etc.Like this, also can make the tackiness agent that can form the application face that does not have shrinkage cavity even carry out the high speed application.That is to say, the churning time till the tackiness agent that can obtain to form the application face that does not have shrinkage cavity, because of the composition of the mixture of kind, quantity and the gradation composition of defoamer different.Under the inadequate situation of churning time,,, will form the application face that does not have shrinkage cavity sometime in case proceed stirring though produce shrinkage cavity when the application because of the defoamer dispersion medium is bad.Surpass this and make constantly under the long situation of churning time, the mixture of gradation composition and the consistency between the defoamer rise, though there is not shrinkage cavity to be easy to generate bubble, coating performance are had a negative impact.Therefore, importantly should conscientious at any time sampling in the process that stirs with stirrer, the method for utilizing aftermentioned to determine, when not producing shrinkage cavity on the application face as the terminal point that stirs, the stirring that after this no longer exceeds needs.
The viscosity of the tackiness agent of manufacturing is preferably 40~1000mPas, more preferably 50~500mPas, preferred especially 150~300mPas.This viscosity is that to adopt BL type rotational viscosimeter be to survey periodic value under 60/ minute the condition at the revolution of #2 rotor.The viscosity of resultant tackiness agent among the present invention, with carry out pre-dispersed occasion under the viscosity of pre-dispersed thing equate substantially.When therefore making,, just can control the viscosity of end article tackiness agent in the viscosity of carrying out passing through under the pre-dispersed occasion the pre-dispersed thing of adjustment.
The solids content of tackiness agent is preferably 40~70 weight %.This solids content is lower than under the situation of 40 weight %, and the drying property after the application is poor, might become the reason that shrinkage cavity occurs.
With the Emulsion Adhesive that the present invention obtains, coating performance is good, is suitable for the high speed application, can not produce shrinkage cavities such as pin hole and flake when the high speed application, can form the good application face of smoothness.And, the Emulsion Adhesive that utilizes the present invention to obtain by employing, can be under higher application speed than the past, make at an easy rate with the speed of application in the past under the stickup goods that obtain have the stickup goods of equal bond properties, the productivity of pasting goods is significantly improved.
The stickup goods that the present invention relates to are the goods that form the binder layer of being made up of the above-mentioned Emulsion Adhesive that obtains.
There is no particular restriction to its structure, for example, can enumerate the stickup sheet material that stacks gradually release liner, binder layer and body material as a preferred embodiment.
There is no particular restriction for release liner and body material.Known interleaving paper or the stripping film that the coating stripper forms on paper such as good quality paper or plastic film can be used as release liner, known body materials such as high-quality paper, enamelled paper, cast-coated paper, polyester film, polyethylene film, polypropylene screen can be used as body material.
There is not special restriction though paste the manufacture method of sheet material yet, but because binder layer forms used Emulsion Adhesive is the aforesaid tackiness agent that is suitable for the high speed application, so preferred for example box gravure coating machine, reverse coating machine and the curtain formula coating machine etc. of using carry out application with the application speed more than 200 meters/minute.Specifically, for example adopt application tackiness agent on release liner, the method that after the drying body material is layered in utilization pressurization transfer printing application on the resulting binder layer can obtain well.The glue spread of tackiness agent in dry weight be preferably 5~50 the gram/square metre, more preferably 10~25 the gram/square metre.Preferred 5~25 microns of the thickness of binder layer when drying.
Below, utilize embodiment and reference examples that the present invention more specifically is described, but following examples only are one embodiment of the present invention, the present invention is not subjected to its a bit restriction.
As the shrinkage cavity and the blistered evaluation of the project of representing coating performance, according to following test method.
At first, blistered evaluation is described.
Use the surge pump " プ ロ Port Application " of upright adroit Co., Ltd. altogether, getting 400 gram tackiness agents prevents in 500 milliliters of cups, heat to 40 ℃, with the flow of 600 ml/min and 0.5 kilogram/square centimeter ejection pressure, in the bubblement of circulation after 1 hour under 4 centimetres of height of falls, represent with the bubbled area percent of covering of liquid level.Consider the influence to coating performance, preferred area percent is no more than 60%.
Secondly, the evaluation of shrinkage cavity is described.
With manual liquid feeder coating adhesive on the PET film of 2mil (milliinch), represent with the number of shrinkage cavity.
Embodiment 1
Use has the reaction vessel of stirrer, reflux cooling device, temperature-control device, nitrogen ingress pipe and dropping groove, and having made with (methyl) alkyl acrylate in such a way is the copolymer emulsion of main component.At first with 47 weight parts (following brief note is done " part ") 2-EHA, 47 parts of butyl acrylates, 4 parts of methyl methacrylates, 2 parts of vinylformic acid, calculate as in the reactive ammonia and 2 parts of (solids content) " KH-10 " (Di-ichi Kogyo Seiyaku Co., Ltd.'s manufacturings) of using of type anionic emulsifier and 0.3 part (solids content) " ニ ユ-コ-Le 1860 " of using as non-reacted nonionic surfactant (Japanese emulsifying agent Co., Ltd. manufacturing) with respect to 100 parts of whole these monomers, and 21 parts of deionized waters add respectively in the dropping groove, make the emulsifying agent solids content reach 76 weight %, emulsification in dripping groove.In reactor, add 17 parts of deionized waters, under nitrogen atmosphere, stir, make the temperature in the container be warming up to 80 ℃, add 0.15 part 3% Potassium Persulphate according to solid content meter.Begin to drip the emulsion in the dropping groove after the above-mentioned pre-emulsification after 5 minutes, meanwhile in 4 hours, drip 0.45 part of (solids content) 3% persulfate aqueous solution.After drip stopping, kept 30 minutes down, make in 30 minutes then that temperature reaches 60~65 ℃ in the container, in 30 minutes, divide and add 0.14 part of tertbutyl peroxide and 0.2 part of rongalite three times at 80 ℃.And then 1 hour postcooling of slaking while stirring with the ammoniacal liquor neutralization, has obtained copolymer emulsion to room temperature.The solids content of resulting emulsion is 60 weight %, and median size is 400 nanometers.
With 7540 kilograms of this copolymer emulsions, add as shown in Figure 2 the even line of flow machine of T.K. (ホ モ ミ Star Network ラ イ Application Off ロ-) that special machine Chemical Co., Ltd is made be arranged in the pipeline, be equipped with agitating vane and choked flow rod 10,000 (10,000) rise in the batching still, begin to stir (pre-dispersed) with agitating vane with 30rpm speed.Secondly, add 850 kilograms of ion exchanged waters and 4 kilograms of defoamers " BYK025 " (PVC Star Network ケ ミ-Co., Ltd. makes), after with ammoniacal liquor pH being adjusted to 7.5, add 13 kilograms of sanitass " レ バ Na Star Network ス AM-100 " (prosperous flourish KCC makes) successively, give sticky agent " E-720 " (waste river KCC make) and 35 kilograms of wetting agents " ペ レ Star Network ス OTP " (Kao Corp's manufacturing) for 890 kilograms, add 20 kilograms of tackifier " ア デ カ ノ-Le UH-420 " (manufacturing of rising sun electrochemical Co., Ltd.) at last, the emulsion viscosity that obtains is adjusted to 250mPas.
After confirming that viscosity falls in the specification, agitating vane in the batching still is rotated with 30rpm, make of the circumferential speed running of the agitating vane of the even line of flow machine of T.K. (ホ モ ミ Star Network ラ イ Application Off ロ-) on one side, make emulsion continue circulation and carry out dispersion treatment continuously with 30 meter per seconds.The moment through 3 hours dispersion treatment terminates as the required stir process of application face that obtains not have shrinkage cavity, and the filtration treatment thing takes out tackiness agent.Tackiness agent in the batching still when handling termination is in and does not almost have blistered state.
Reference examples 1
In the foregoing description 1, after batching was carried out in the still pre-dispersed and adjusted the viscosity of emulsion, (ホ モ ミ Star Network ラ イ Application Off ロ-) stirred without the even line of flow machine of T.K., filtered, and took out tackiness agent.The tackiness agent of this moment is in and does not almost have blistered state.
Reference examples 2
Same with the foregoing description 1, in the batching still, obtained through pre-dispersed emulsion, from wherein taking out about 1500 kilograms, immigration has in 2000 liters of batching stills of agitating vane.With whipping appts as shown in Figure 1 with agitating wing and the set collar that is positioned at its outside, sling to be immersed in and make it not contact agitating vane in the emulsion from the top of batching still, make agitating vane and agitating wing respectively with 30rpm and the rotation of 30 meter per second clock circumferential speeds, stir emulsion with intermittent mode.
Below, same with the foregoing description 1, sampling in per 30 minutes is once and carried out dispersion treatment.After handling through 3 hours and 3.5 hours, owing to do not find that the shrinkage cavity number improves, so stopped stir process.On the adhesive surface when handle stopping in the batching still, on surface owing to produced bubble as the tiny ice cream, so foaming is not estimated later on.
Shrinkage cavity and blistered evaluation result for resulting tackiness agent are shown in table 1.
Table 1
Embodiment 1 Reference examples 1 Reference examples 2
The pre-dispersed back stir process time Continous way stirred 3 hours 0 hour Intermittent type stirred 3 hours
Shrinkage cavity number (individual) ??0 ??9~15 ??3~6
Bubble: bubble area percentage ratio (%) ??20~30 ??10~15 ??-
In sum, it is investigated the bright good application face that has obtained not having shrinkage cavity in an embodiment.In contrast to this, it is many only to have carried out in the pre-dispersed reference examples 1 shrinkage cavity, and it is very many to have carried out with intermittent mode bubbling in the reference examples 2 of dispersion treatment.

Claims (5)

1. the manufacture method of an Emulsion Adhesive, it is characterized in that: the viscosity of this emulsion is 40~1000mPas, this method comprises uses the high speed rotating shear-type stirrer with agitating wing and set collar, to (methyl) alkyl acrylate being the propylene series copolymer emulsion of main component and the operation that defoamer carries out dispersion treatment continuously.
2. according to the manufacture method of the described Emulsion Adhesive of claim 1, it is characterized in that: also comprise described propylene series copolymer emulsion and defoamer are carried out pre-dispersed operation.
3. according to the manufacture method of claim 1 or 2 described Emulsion Adhesives, it is characterized in that: use agitating wing to be positioned at the high speed rotating shear-type stirrer of set collar inboard.
4. utilize the Emulsion Adhesive that the manufacture method of any one described Emulsion Adhesive obtains in the claim 1~3.
5. paste goods for one kind, it is characterized in that: comprise the binder layer that forms by the described Emulsion Adhesive of claim 4.
CN 200410042317 2003-05-16 2004-05-17 Method for preparing emulsion adhesive and its use Active CN1261517C (en)

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CN101235335B (en) * 2007-01-19 2015-01-28 雅富顿公司 High TBN / low phosphorus economic STUO lubricants
CN115433500A (en) * 2022-08-24 2022-12-06 广东弘方涂料有限公司 Epoxy anticorrosive primer and preparation method and application thereof

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WO2013146939A1 (en) * 2012-03-29 2013-10-03 リンテック株式会社 Re-peelable emulsion-based adhesive composition, re-peelable adhesive sheet, and method for manufacturing re-peelable adhesive sheet

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101235335B (en) * 2007-01-19 2015-01-28 雅富顿公司 High TBN / low phosphorus economic STUO lubricants
CN115433500A (en) * 2022-08-24 2022-12-06 广东弘方涂料有限公司 Epoxy anticorrosive primer and preparation method and application thereof

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