WO2021006593A1 - 기능성 핫멜트 점착제의 제조방법 및 그에 따른 기능성 핫멜트 점착제 - Google Patents
기능성 핫멜트 점착제의 제조방법 및 그에 따른 기능성 핫멜트 점착제 Download PDFInfo
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- WO2021006593A1 WO2021006593A1 PCT/KR2020/008838 KR2020008838W WO2021006593A1 WO 2021006593 A1 WO2021006593 A1 WO 2021006593A1 KR 2020008838 W KR2020008838 W KR 2020008838W WO 2021006593 A1 WO2021006593 A1 WO 2021006593A1
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- melt adhesive
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/416—Additional features of adhesives in the form of films or foils characterized by the presence of essential components use of irradiation
Definitions
- the present invention relates to a method for producing a functional acrylic hot-melt adhesive in a solid state that does not contain a volatile organic solvent and an unreacted monomer, and a pressure-sensitive adhesive therefrom.
- solvent-free bulk-type acrylic adhesives have many restrictions on the use of solid-type functional additives because of dispersion problems, unlike organic solvent-type products.
- the additive when the additive is to be accompanied by a quantitatively uniform dispersion, there are many problems in that the additive is not mixed and separated or precipitated in the main curing process.
- functional additives are affected by the final target physical properties by the profile of the thermal energy (minimum/maximum temperature, residence time and rise/fall degree, etc.) activated or applied by heat.In particular, the uniformity before melting of the hot melt resin It is important to ensure sufficient uniformity for this as it helps to realize stable physical properties only when secured.
- the selected CBA is the melting temperature range of the hot melt resin (unnecessary side reactions such as decomposition and oxidation by heat of the resin).
- the CBA touches the molten resin having a temperature above a certain temperature and the stirring equipment such as an extruder, it is activated by the thermal energy applied from the surrounding area and gases such as CO 2 or nitrogen Therefore, when CBA is reacted and activated on the surface and the periphery of the resin, it is difficult to inject the generated gas into the interior as desired, as the thickness of the finished product is thicker than the amount used. Therefore, there is a difficult problem in producing low-density products through even dispersion of the generated gas.
- Korean Patent Publication No. 10-2007-0041896 relates to an ultraviolet-curable hot-melt adhesive composition and adhesive tape comprising a hot-melt adhesive component, a photopolymerization initiator and a photocrosslinking agent, and the hot-melt adhesive component is styrene- Isoprene-styrene block copolymer, styrene-1,4-butadiene-styrene block copolymer, or styrene-1,2-butadiene-1,4-butadiene-styrene block copolymer.
- Korean Patent Laid-Open Publication No. 10-2018-0130522 is a hot-melt adhesive composition that can be hot melted by heat melting at a relatively low temperature, and has excellent adhesion, holding power and tack, and a point using the adhesive composition. Commencing adhesive products.
- the above patents are somewhat limited in that they cannot provide a fundamental solution to the problem of uniformly dispersing additives and CBA. Accordingly, the present invention has completed the present invention in order to solve the above-described problems and at the same time provide improved physical properties.
- Patent Document 1 Korean Registered Patent Publication No. 10-2007-0041896 (2007.04.20)
- Patent Document 2 Korean Patent Publication No. 10-2018-0130522 (2018.12.07)
- An object of the present invention is to solve all of the above-described problems.
- Another object of the present invention is to expose a PVC substrate or an oil additive to the surface when affixed to a soft PVC substrate or a substrate containing an excessive amount of oil-based additives including chlorinated rubber (CR) and chlorinated polyolefin (CPO) as functional additives. It prevents the adhesion of the adhesive layer due to the movement of plasticizers or other additives on the substrate and provides a function of preventing corrosion of the metal surface when attached to the metal substrate.
- CR chlorinated rubber
- CPO chlorinated polyolefin
- the characteristic configuration of the present invention is as follows.
- a hot melt adhesive prepared by the above manufacturing method is provided.
- the movement of plasticizers or other additives to the material surface It provides an effect of preventing the adhesion of the adhesive layer.
- FIG. 1 is a finished product film pouch according to the present invention, showing a film pouch type when a large amount of heat is generated during polymerization.
- FIG. 2 is a finished product film pouch according to the present invention, showing a film pouch type when stability is ensured due to low possibility of exothermic reaction during polymerization.
- FIG. 3 is a finished product film pouch according to the present invention, showing a film pouch type when stability is ensured during polymerization.
- FIG 4 shows the sealing sequence of the film pouch according to the present invention.
- Figure 5 shows an overall manufacturing equipment for manufacturing the pressure-sensitive adhesive according to the present invention.
- the following steps may be additionally provided.
- the step of removing volatiles by stirring the acrylic monomer mixture in step (a) under an inert gas or vacuum atmosphere is provided.
- the acrylic monomer mixture is stirred under an inert gas before performing the prepolymerization reaction, and the volatility of alcohols, liquid alkanes, and derivatives thereof can be removed by applying a vacuum of 1000 mbar or less.
- volatile matter may be removed while applying vacuum even in the resin sufficiently melted by heat of 150°C or higher.
- the final hot-melt adhesive is a pressure-sensitive adhesive having a minimum of VOC (Volatile Organic Compounds) content, and the purity of the solid content is preferably 99.99% or more.
- the ultraviolet irradiation of step (e) is divided into at least three times to set the ultraviolet (UV) intensity, and irradiation is provided.
- the setting is provided in a Low-Medium-High formula. That is, in order to remove unreacted acrylic monomers and oligomers, the intensity of ultraviolet (UV) energy applied during polymerization of the pouch sealed in step (e), which is the main curing step, is increased step by step with an intensity step of at least three steps or more.
- the energy can be provided by increasing the energy by at least 50% or more of the intensity of the ultraviolet rays irradiated in the previous step.
- the ultraviolet energy irradiated at the last stage can be provided as the maximum intensity that can be realized by the facility.
- a vacuum is applied to the sufficiently melted resin by heat of 150° C. or higher to remove monomers and oligomers located on the surface and inside.
- the ultraviolet intensity is increased three or more times as described above, the unreacted monomer is removed and the chemical blowing agent (CBA) increases the temperature in stages evenly inside the resin, so that the size and dispersion uniformity of the foaming gas is increased. And it can provide an advantage in bubble stability. Therefore, compared with the known technology, the amount of the chemical blowing agent to be introduced can be reduced, and the efficiency can be improved through the uniformity of bubble dispersion and generated bubble size.
- CBA chemical blowing agent
- the prepolymerization reaction it is possible to cure by using heat or ultraviolet rays.
- the acrylic monomer mixture in step (a) is methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate, carboxyl ethyl acrylate, n-octyl acrylate, 2-ethyl It provides at least one or more selected from hexyl acrylate, isooctyl acrylate, hydroxypropyl acrylate, lauryl acrylate, isobornyl acrylate, methyl methacrylate, acrylic acid and methacrylic acid. Further, in this case, the viscosity of the acrylic monomer mixture is 1 cps or less.
- the initiator of step (a) may include a thermal initiator by heat and a photoinitiator by ultraviolet rays.
- the thermal initiator is cyclic peroxide, diacyl peroxide, dialkyl peroxide, hydroperoxide, peroxycarbonate, peroxydicarbonate, peroxyester, ketone peroxide, and the azo compound is 2,2' -Azobisisobutylonitrile, at least any selected from 2,2'-azobis(2,4-dimethyl-pentanenitrile), 2,2'-azobis-(2-methylbutyronitrile) Provide more than one.
- the initiator is benzophenone, hexaalkylditine, 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)-butanone-1, 2,2- Dimethoxy-1,2-diphenylethan-1-one, bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide, 2-hydroxy-2-methyl-1-phenyl-1propenone and methyl It provides at least one or more selected from benzoyl formate.
- the heat and photoinitiator Based on 100 parts by weight of the acrylic monomer, the heat and photoinitiator provides 0.01 to 5 parts by weight. If the initiator is less than 0.01, the initiation efficiency is lowered, and if it exceeds 5 parts by weight, the above range is preferable because temperature control during the reaction is problematic.
- the thermal initiator preferably 0.01 to 1 parts by weight may be provided with respect to 100 parts by weight of the acrylic monomer, and 0.01 to 0.2 parts by weight may be provided with respect to 100 parts by weight of the acrylic monomer in the case of the photoinitiator.
- the provided light source may be provided with a wavelength of 320 to 385 nm (area A) by UV.
- area A area A
- the chain transfer agent in step (a) is ascorbic acid, benzoquinone, butylhydroxyanisole (BHA), butylhydroxytoluene (BHT), 2,2-diphenyl-1- Picrylhydride (DPPH), isooctylthioglycolate, n-butylmercaptan, Galvanoxyl, nitrobenzene, a-tocopherol, phenyl-at-butylnitrogen (2,2,6,6-tetramethylpiperidine It provides at least any one or more selected from -1-yl)oxyl (TEMPO) and triphenyl verdazil.
- BHA butylhydroxyanisole
- BHT butylhydroxytoluene
- DPPH 2,2-diphenyl-1- Picrylhydride
- isooctylthioglycolate n-butylmercaptan
- Galvanoxyl nitrobenzene
- phenyl-at-butylnitrogen 2,2,
- the chain transfer agent it may be provided for controlling the molecular weight, and 0.01 to 2 parts by weight may be provided based on 100 parts by weight of the acrylic monomer mixture.
- the more flexible and low melting temperature pressure-sensitive adhesive resin is made the greater the amount of the chain transfer agent is added and used, and the amount used can be adjusted if necessary.
- the photocuring agent in step (a) is hydroxycyclohexyl phenyl ketone, 2,2-dimethoxy2-phenyl, acetophetone, benzophenone, phenyl-2-hydroxy-2- It provides at least any one or more selected from propyl ketone and azo-bisbenzophenol.
- the photocuring agent can be provided for post-curing purposes by providing a UV lamp having a relatively high energy, for example, a high-pressure mercury lamp of 200W or more, a metal halide lamp, and a high-power LED according to the final purpose.
- 0.05 to 5 parts by weight of a photocuring agent is provided based on 100 parts by weight of the acrylic monomer mixture.
- the hydrocarbon-based resin of step (a) includes at least one selected from C5 aliphatic resin and C9 aromatic resin, and terpene-phenol, polyterpene, and styrene as terpene-based resin Provides containing at least one or more selected from terpenes.
- the tackifier is, for example, a hydrocarbon-based petroleum resin, such as C5 aliphatic resin, C9 aromatic resin, hydrogenated petroleum resin, styrene-terpene resin, phenolic resin, Polymethylstyrene resin, ketonealdehyde resin, xylene formaldehyde resin, cashew oil-modified phenolic resin, rubber, resin emulsion may be provided, but is not limited thereto.
- a hydrocarbon-based petroleum resin such as C5 aliphatic resin, C9 aromatic resin, hydrogenated petroleum resin, styrene-terpene resin, phenolic resin, Polymethylstyrene resin, ketonealdehyde resin, xylene formaldehyde resin, cashew oil-modified phenolic resin, rubber, resin emulsion may be provided, but is not limited thereto.
- a terpene-based resin may be provided, and for example, a terpene resin, a terpene-phenol resin, a terpene-styrene resin, and a terpene-phenolic resin may be provided.
- the viscosity of the acrylic syrup prepared by the prepolymerization in step (a) is 100 to 10,000 cps.
- agitation is performed so that it can sufficiently contact air in the atmosphere after the reaction.
- a method for producing a functional hot melt adhesive comprising. That is, by providing a syrup in which the functional acrylate is uniformly dispersed by further including at least one or more selected from urethane acrylate, epoxy acrylate and silicone acrylate as a functional acrylate in the acrylic syrup having a viscosity of 100 to 10,000 cps. As a result, it can help to improve the target properties of the final product.
- step (b) micronizing of a chemical blowing agent, chlorinated rubber (CR) and chlorinated polyolefin (CPO) as functional additives; is provided.
- the average diameter size of the functional additive is 0.5 to 50 ⁇ m by the micronization in step (b) is provided.
- Micronization can be done by using a ball mill or a homogenizer to make a fine powder form advantageous for dispersion.
- the size of the powder is preferably made as small as possible, and the average particle size is preferably 50 ⁇ m or less.
- Chlorinated rubber and chlorinated polyolefin prevent corrosion of metal surfaces and prevent plasticizers from moving in case of concern about delamination due to migration of plasticizers in PVC over time on the soft PVC surface. It provides the function of maintaining the attachment performance for a long period without phenomenon.
- this functional additive is not mixed with most solvent-free acrylic solutions (a mixture of monomers, oligomers, and polymers having a certain viscosity), it cannot be used in general UV-curable acrylic adhesives.
- the present invention provides a prepolymerized acrylic syrup having a certain level of viscosity.
- the viscosity of acrylic syrup above a certain level makes it possible to evenly disperse CR or CPO processed into fine powder in the solution, and since this dispersion state is maintained for a certain time or longer, it is injected and sealed in a film pouch of a certain size. If the solidification operation is performed within the time that the dispersed state is maintained, a solid acrylic hot melt resin in which the solid additives are uniformly and stably dispersed can be provided. Compared with the product obtained through the conventional extrusion hot melt process, the obtained hot melt resin can obtain a finished product in which the additive is stably dispersed, and by the heat applied during the process, CR and CPO can achieve an improved dispersion state with the acrylic resin. Will have.
- a PVC substrate or a substrate containing an excess oil type oil type, for example, an oil type dispersion stabilizer, a detachable release agent after the plastic casting process
- oil type for example, an oil type dispersion stabilizer, a detachable release agent after the plastic casting process
- additives materials in which the phenomenon of migration of this oil type additive to the surface occurs
- step (c) stirring the mixed resin added to the acrylic syrup stirred in step (a) with the micronized functional additive under an inert gas; is provided.
- the functional additive in the form of fine powder is added to the acrylic syrup having a viscosity of 100 to 10,000 cps, and sufficiently stirred to achieve a uniform dispersion. Stirring is preferably carried out under nitrogen or an inert gas in order to prevent contact with oxygen. Thereafter, a syrup in which the additives are uniformly dispersed by sufficiently stirring is provided, and the sedimentation of the additives is slowed by the viscosity, and the dispersed state can be maintained for a certain time. In this case, it goes without saying that the amount of functional additives added can be adjusted as needed.
- functional additives are characterized by melting at a certain temperature because their main component is a thermoplastic resin such as rubber or polyolefin, and they are well mixed with the acrylic resin during the extrusion process without a separate phase separation phenomenon.
- (d) injecting a quantity of the stirred mixed resin into a film pouch for sealing; is provided.
- the film pouch including mixed resin is well sealed and sealed so that outside air and water in the tank do not enter the pouch.
- the film pouch may be provided in an amount of 5 to 100 g, a size of 3 to 10 cm, and a length of 3 to 15 cm, but is not limited thereto.
- the film pouch as a finished product is shown in FIGS. 1 to 3.
- 1 to 3 show the shape of a finished pouch, and the type can be distinguished according to the reactivity of the contents.
- a film pouch type when a large amount of heat is generated during polymerization. This is a case where a large amount of heat may be generated during the polymerization reaction, and the initiator of the polymerization reaction is activated by heat. In order to prevent accidents and secure safety, it is desirable to reduce the size of the pouch and manufacture it in one or two lines at the same time.
- a square or similar plastic bag type may be provided with a size of 1 to 10 cm in width and length, respectively.
- a film pouch type is shown when stability is ensured due to low possibility of exothermic reaction during polymerization.
- the amount of the reaction solution is significantly reduced and there is no possibility of a rapid exothermic reaction, and stability is secured to a certain extent, it can be produced and provided by increasing it to 4 or 8 lines.
- the ratio of width and height is usually 1:2, and from 1 to 8 lines per size is provided to be selected and used according to the purpose and capacity.
- the polymer resin provided as the film pouch should stably maintain a film state without side reactions with a general-purpose acrylic monomer, and should be capable of sealing through melting at a certain temperature.
- the film should not be deformed or damaged by heat generated during the polymerization reaction, and it should be mixed with acrylic resin in the final melt extrusion process. Therefore, the polymer resin provided as the film pouch of step (d) may be provided with polyethylene, ethylene vinyl acetate, and polyolefin elastomer as described above, and a thermoplastic type hydrocarbon C5, C9-based tackifier that can transmit ultraviolet rays, and Mixtures of these, perfen-based resins, modified resins, and the like may be included.
- these pouches alone or containing a mixture are processed into a film shape and used, and the processed film must not be dissolved in water and acrylic monomers or oligomers, and at least 10% of ultraviolet rays at a thickness of 10 ⁇ m to 1.0mm It must have the penetration ability of area A. In some cases, it should be able to transmit at least 10% of the ultraviolet rays B and C regions (180 nm to 300 nm).
- step (d) 50 to 1,000 parts by weight of the mixed resin to be injected is provided based on 10 parts by weight of the film pouch in step (d).
- side reactions such as sulfur change caused by oxygen must be removed from the mixed resin injected as much as possible to prevent side reactions such as sulfur change caused by oxygen, and inert gas such as nitrogen is purged during stirring after a certain ratio of composition work is completed. It must be sufficiently stirred to prevent side reactions of the initiator by oxygen.
- the sealing order is as follows. First, in the original state of the film, it is folded once in the horizontal direction and sealed, and the first solution is injected into a pouch with an open upper part, and then sealed in the vertical direction. Next, after sealing, inject the second solution into the open upper part and seal it in the vertical direction again. Repeat this process to perform continuous work. The procedure for this is shown in FIG. 4.
- (e) polymerizing and curing the sealed pouch by irradiating ultraviolet rays in water at 10 to 30° C.; is provided.
- the mixed syrup injected into the film pouch undergoes polymerization and curing by irradiating the light of the A region with a wavelength of 320 to 385 nm of ultraviolet rays.
- the pouch film is damaged due to the polymerization exothermic reaction of the acrylic resin and the heat of the functional additive.
- the sealed pouch stays in water having a temperature of room temperature or lower and the reaction proceeds.
- the main curing reaction through polymerization of the mixed syrup on the film pouch it is limited to polymerization by ultraviolet (UV) in water in order to secure stability by controlling the exothermic reaction that may occur rapidly.
- UV ultraviolet
- a post-curing reaction by heat of less than 100°C may be selectively involved. This is applied when the finished hot melt resin is a dark color that absorbs light, for example, black or dark gray, and it is difficult to transmit light smoothly because it contains an excessive amount of additives.
- an additional polymerization reaction by heat may be performed for the purpose of removing unreacted monomers or oligomers.
- the reaction may proceed while passing through a water bath set to a temperature condition of at least three steps or more.
- the temperature of water is prepared by dividing into three steps according to the activation temperature of the initiator for thermal reaction.
- the first section provides at least 10°C lower than the reaction activation temperature, and the second section provides +10°C to the activation temperature.
- the third section is set again at least 5°C and at most 15°C lower than the activation temperature of the initiator, and if necessary, it is desirable to install an additional cooling water tank to prevent a situation in which a rapid exothermic reaction may occur. .
- the temperature of the water is 10 to 30°C as purified water, and preferably 23 to 27°C at room temperature may be provided.
- the polymerization reaction is promoted by heating the water to raise the temperature, and the temperature can be adjusted as needed.
- the water contained in the tank is heated to a certain temperature, and the temperature is controlled by dividing it into at least 3 steps, and the tank in the same section can have a maximum deviation of ⁇ 1.5°C.
- the temperature of water is set to 35 to 100°C, and it is placed from a low temperature to a high temperature.
- the UV used is in the A region (320 to 365 nm wavelength) and the intensity of light is in the range of 0.1 to 20 mW/cm 2 .
- a UV V range (380 to 440 nm) may be provided to promote reaction and improve efficiency, and in this case, the intensity of light is 1 to 20 mW/cm 2 .
- the amount of the thermal initiator to be added may be included in a small amount and 0.001 to 2.0 parts by weight based on 100 parts by weight of the acrylic monomer, and the amount to be added is determined based on the molar concentration as necessary.
- the brightness of the first section is set low in the range of 1 to 25% to prevent rapid reaction and at the same time Provides to obtain macromolecules.
- the second and third UV oven sections increase the brightness step by step and provide the polymer to be converted to more than 99.9% after passing through the last section.
- FIG. 5 The overall manufacturing equipment in which the adhesive according to the present invention is manufactured is shown in FIG. 5.
- Acrylic syrup and functional additives are put into the film through the input part and sealed by heat, and are put into the water tank along the guide roll and can be moved in the water tank.
- UV irradiation is possible through an ultraviolet lamp on the top of the tank, and polymerization and curing proceeds by this light, and liquid acrylic syrup and functional additives having a viscosity similar to water are solidified.
- the reaction proceeds.
- the water tank can be heated as needed, an additional water tank for additional cooling can be added at the end of the water tank, and the pouch of the finished product can be layered at the last step.
- compressed air may be provided or a simple squeezer may be installed to remove moisture and stacked on the storage container.
- a water tank for cooling may be provided in the section at which the polymerization reaction ends for stability and uniformity in the polymerization and curing reaction by irradiation with ultraviolet rays of the step (d).
- the film pouch when producing a pouch made by an exothermic reaction, the film pouch must be immersed in water at least 5cm, and a sufficient amount of oxygen is secured using compressed air at the top of the water tank, so that an initiator when the artificial reaction is terminated for safety purposes. Radicals generated by activation of the lamp and sufficient oxidation are made to terminate the reaction.
- a hot melt adhesive prepared by the above manufacturing method is provided, and a functional hot melt adhesive including a functional additive uniformly dispersed therein can be provided.
- the hot-melt pressure-sensitive adhesive according to the present invention has an active chemical blowing agent (CBA) that is stably and evenly dispersed in the resin, causing uniform foaming inside the resin by constant thermal energy applied during the extrusion process of the hot-melt resin.
- CBA active chemical blowing agent
- a target low-density adhesive or foamed resin body can be produced.
- the amount of CBA used can be reduced.
- chlorinated rubber (CR) or chlorinated polyolefin (CPO) is uniformly included in the adhesive resin, soft PVC (PVC containing a certain amount of plasticizer) or a substrate containing an excessive amount of oil type additives (this oil type additive migrates to the surface).
- PVC chlorinated rubber
- CPO chlorinated polyolefin
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Claims (16)
- (a) 아크릴 모노머 혼합액 100 중량부에 대하여, 개시제 0.01 내지 5 중량부, 연쇄이동제 0.01 내지 2 중량부, 광경화제 0.05 내지 5 중량부 및 점착부여제 5 내지 50 중량부를 투입하여, 열 또는 자외선을 조사하고, 예비중합반응으로 아크릴시럽을 제조하여 상온에서 교반하는 단계;(b) 기능성 첨가제로 화학발포제, 염소화 고무 및 염소화 폴리올레핀을 미분화하는 단계;(c) 상기 미분화된 기능성 첨가제를 (a)단계에서 교반한 아크릴 시럽에 투입한 혼합수지를 불활성 기체 하에서 교반하는 단계;(d) 상기 교반한 혼합수지를 필름파우치에 정량을 주입하여 실링하는 단계; 및(e) 상기 실링한 파우치를 10 내지 30℃의 수중에서 자외선을 조사하여 중합 및 경화하는 단계;를 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (a)단계의 아크릴 모노머 혼합액을 불활성 기체 또는 진공 분위기 하에서 교반을 통하여 휘발분을 제거하는 단계;를 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (e)단계의 자외선 조사는 적어도 3회 이상으로 나눠서 자외선(UV) 강도를 설정(Low-Medium-High식으로)하여, 조사하는 것으로 자외선 세기를 단계적으로 증가하는 것인 기능성 핫멜트 점착제의 제조방법.
- 제 3 항에 있어서,상기 자외선 세기를 단계적으로 증가하는 것은 전 단계 에너지의 50% 이상을 증가하는 것인 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (a)단계의 아크릴 모노머 혼합액은 메틸아크릴레이트, 에틸아크릴레이트, 프로필아크릴레이트, 부틸아크릴레이트, 카르복실에틸아크릴레이트, n-옥틸아크릴레이트, 2-에틸헥실아크릴레이트, 아이소옥틸아크릴레이트, 하이드록시프로필아크릴레이트, 라우릴아크릴레이트, 아이소보닐아크릴레이트, 메틸메타크릴레이트, 아크릴산 및 메타크릴산에서 선택되는 적어도 어느 하나 이상을 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (a)단계의 아크릴 모노머 혼합액의 100 중량부에 대하여, 우레탄아크릴레이트, 에폭시아크릴레이트 및 실리콘아크릴레이트에서 선택되는 적어도 어느 하나 이상을 1 내지 40 중량부 더 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (a)단계의 개시제는 과산화물 및 아조계 화합물인 열개시제이고,과산화물은 사이클릭 퍼옥사이드, 디아실 퍼옥사이드, 디알킬 퍼옥사이드, 하이드로퍼옥사이드, 퍼옥시카보네이트, 퍼옥시디카보네이트, 퍼옥시에스테르, 케톤 퍼옥사이드이고,아조계 화합물은 2,2'-아조비시소부틸로니트릴, 2,2'-아조비스(2,4-디메틸-펜테인나이트릴), 2,2'-아조비스-(2-메틸부티로나이트릴)에서 선택되는 적어도 어느 하나 이상을 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (a)단계의 개시제는 광개시제이고, 벤조페논, 헥사알킬디틴, 2-벤질-2-디메틸아미노-1-(4-몰포리노페닐)-부타논-1, 2,2-디메톡시-1,2-디페닐에탄-1-온, 비스(2,4,6-트리메틸벤조일)-페닐포스핀옥사이드, 2-하이드록시-2-메틸-1-페닐-1프로페논 및 메틸벤조일포메이트에서 선택되는 적어도 어느 하나 이상을 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (a)단계의 연쇄이동제는 아스코르브산, 벤조퀴논, 부틸하이드록시아니솔(BHA), 부틸하이드록시톨루엔(BHT), 2,2-디페닐-1-피크릴하이드(DPPH), 아 이소옥틸티오글리코레이트, n-부틸메르캅탄, 갈비녹실(Galvanoxyl), 니트로벤젠, a-토코페롤, 페닐-a-t-부틸니트로겐 (2,2,6,6-테트라메틸피페리딘-1-일)옥실(TEMPO) 및 트리페닐베르다질에서 선택되는 적어도 어느 하나 이상을 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (a)단계의 광경화제는 하이드록시 사이클로헥실 페닐 케톤, 2,2-디메톡시2-페닐, 아세토페톤, 벤조페논, 페닐-2-히드록시-2-프로필케톤 및 아조-비스벤조페놀에서 선택되는 적어도 어느 하나 이상을 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (a)단계의 점착부여제는 하이드로카본계 수지로 C5 지방족 수지 및 C9 방향족 수지에서 선택된 적어도 어느 어느 하나 이상을 포함하고,테르펜계 수지로 테르펜-페놀, 폴리테르펜 및 스티렌화 테르펜에서 선택되는 적어도 어느 하나 이상을 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (a)단계의 아크릴시럽의 점도는 100 내지 10,000cps인 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (b)단계의 미분화에 의하여 기능성 첨가제의 평균직경크기는 0.5 내지 50㎛인 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (d)단계의 필름파우치로 제공되는 수지는 폴리에틸렌, 에틸렌비닐아세테이트, 폴리올레핀일라스토머, 테르펜 및 하이드로카본(C5/C9)수지에서 적어도 어느 하나 이상의 포함하는 기능성 핫멜트 점착제의 제조방법.
- 제 1 항에 있어서,상기 (d)단계의 필름파우치 질량 10 중량부에 대하여, 주입되는 혼합수지는 50 내지 1,000 중량부인 기능성 핫멜트 점착제의 제조방법.
- 제 1 항 내지 제 15 항에 어느 한 항에 따른 방법으로 제조된 핫멜트 점착제.
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CN115975103A (zh) * | 2023-02-07 | 2023-04-18 | 太仓斯迪克新材料科技有限公司 | 无硅转移的非硅离型剂、应用及制备方法 |
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