KR101224972B1 - Primer composition for non-slip rubber and adhesion method of non-slip rubber by using the same - Google Patents
Primer composition for non-slip rubber and adhesion method of non-slip rubber by using the same Download PDFInfo
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Abstract
The present invention is a pretreatment agent composition for non-slip rubber comprising a polychlorinated polyolefin graft polymer, an acid, a thermoplastic polyurethane resin, and an adhesion promoter and a solvent for improving adhesion and wettability thereof, and adhesion of the non-slip rubber using the same. The method relates to a aging step performed in the conventional bonding process of a conventional non-slip rubber when the non-slip rubber, in particular butyl rubber, is adhered using the pre-treatment agent composition for the non-slip rubber according to the present invention. The advantage is that by excluding the process, the process is simplified to increase productivity, reduce manufacturing cost, and improve adhesion.
Description
The present invention relates to a pretreatment agent composition for non-slip rubber and a method for adhering to non-slip rubber using the same, and more particularly, in a conventional conventional non-slip rubber adhering process when adhering rubber requiring non-slip property. The present invention relates to a method for adhering a non-slip rubber pre-treatment composition and an non-slip rubber using the same, which simplifies the process by excluding the aging process, the secondary adhesive treatment process, and the like, thereby improving productivity.
In general, rubber is classified into natural rubber and synthetic rubber, and is a polymer material having elasticity mainly composed of isoprene. On the other hand, raw rubber itself is soft, especially sensitive to temperature changes, and becomes sticky at high temperatures, and loses its elasticity at low temperatures. In order to stably use the rubber, vulcanization technology and filling technology have been developed. As a result, it has strong and good properties and is currently used in many applications.
On the other hand, the rubber is used butyl rubber containing a butyl group, especially for rubbers that require high friction force, that is, non-slip properties depending on the purpose of use, such as safety shoes, fishing shoes, hiking boots, non-slip floor mats It is used for various demands.
As described above, in the conventional bonding method for butyl rubber having non-slip characteristics, as shown in FIG. 1, the surface of the rubber is ground and buffed (S1) and impregnated in a washing solvent to form an aromatic or the like. After washing with polar solvent (S2), drying at room temperature for 1 hour (S3), using a rubber surface treatment agent, primer treatment (S4) and drying (S5), etc. After applying the primary adhesive (S6) using, and then dried (S7) by the same method as the above-mentioned drying (S5) method, aged at room temperature for 3-6 hours (S8), and a polyurethane adhesive The secondary adhesive is applied (S9) and dried (S10) to bond the non-slip rubber with the shoe parts.
However, in the conventional rubber bonding method to the butyl rubber as described above, the primary adhesive treatment (S6) after the primer treatment (S4) to the butyl rubber, and then dried, after the aging treatment (S8) and then repeated again secondary As the adhesive treatment (S9) is carried out, the bonding process is very complicated, not only the production speed and workability are lowered, but also the bonding is unstable due to the aging process (S8).
In order to solve the problems as described above, the applicant of the present invention has previously filed a patent application for adhesion reinforcing primer composition (Patent Publication No. 10-2010-0078473).
The primer composition for adhesion reinforcement previously filed by the applicant of the present invention, 5 to 15 parts by weight of the polyolefin resin, 3 to 10 parts by weight of the adhesion promoter, 0.2 to 2 parts by weight of the silane coupling agent based on 100 parts by weight of the thermoplastic polyurethane resin And a primer composition consisting of 600 to 2,000 parts by weight of 3 to 6 kinds of mixed solvents including methyl ethyl ketone, normal hexane, cyclohexane, and the like, wherein the thermoplastic polyurethane resin is used as a main component to give the primer inherent physical properties. Adhesion to the hard-adhesive synthetic resin was improved by using chlorinated polyolefin resin, adhesion promoter, silane coupling agent to improve the strength, and three low-toxic organic solvents to improve initial contact, wettability, and solubility of the primer.
However, the prior art has improved the adhesion to the hard-adhesive synthetic resin, but when applied to the 'butyl rubber' in the state excluding the aging process, the adhesion was still unreliable.
Therefore, in order to solve the above problems, the present invention uses an chlorinated polyolefin graft polymer, an acid, a thermoplastic polyurethane resin as a main component for the non-slip rubber made of an adhesion promoter and a mixed solvent for improving adhesion and wettability thereto By using the pretreatment composition, the productivity is improved by simplifying the process by eliminating the aging process, the secondary adhesive treatment process, etc. which are performed in the conventional non-slip rubber bonding process in the process of bonding the non-slip rubber, especially butyl rubber, An object of the present invention is to provide a pre-treatment agent composition for non-slip rubber and a method for adhering non-slip rubber using the same.
In the pretreatment composition for non-slip rubber, the present invention comprises 1.5 to 3 parts by weight of olefin chloride graft polymer, 0.5 to 1.5 parts by weight of acid, 0.5 to 1.5 parts by weight of thermoplastic polyurethane resin, and 0.5 to 1.0 parts by weight of adhesion promoter. And a pre-treatment agent composition for non-slip rubber, comprising 93 to 97 parts by weight of a mixed solvent, as a means for solving the problem.
And the non-slip rubber pretreatment composition is preferably 3 to 7% by weight of the total solid content.
On the other hand, the olefin chloride graphite polymer is formed by graft polymerization of 50 to 100 parts by weight of a non-functional acrylic monomer with respect to 100 parts by weight of a polyolefin resin having a chloride degree of 10 to 50% by weight and a softening point of 40 to 120 ° C. .
Moreover, it is preferable to use the said acidic acid individually or in combination of 2 or more types among carboxylic acid, hydrochloric acid, oxalic acid, malic acid, benzoic acid, sulfuric acid, amino acid, citric acid, ascorbic acid, nitric acid, and acetic acid.
Moreover, it is preferable to use the said adhesion promoter individually or in combination of 2 or more types from a silane coupling agent, a titanate coupling agent, and an organic phosphate adhesion promoter.
Moreover, it is preferable to use together the 3 or more types of the said solvent in methylcyclohexane, methyl ethyl ketone, cyclohexane, acetone, ethyl acetate, cyclohexanol, isosropanol, n-propanol, and ethanol.
And the present invention buffing the non-slip rubber (A1) and then impregnated in the cleaning agent (A2), after drying the non-slip rubber taken out from the cleaning agent (A3), using the pre-treatment composition for non-slip rubber according to the invention Another method of adhering the non-slip rubber is characterized by adhering the adhered surface of the non-slip rubber (A4), drying (A5), and then applying the adhesive to the non-slip rubber with the shoe parts. It is to solve the problem.
Aging process of the conventional non-slip rubber during the bonding of the non-slip rubber, in particular butyl rubber, using the pre-treatment composition for non-slip rubber excellent in adhesion and wettability characteristics according to the present invention, secondary It is an advantage that the process is simplified by excluding the adhesive treatment process, thereby increasing productivity, reducing manufacturing cost, and improving adhesion.
1 is a block diagram showing a conventional bonding process for non-slip rubber
Figure 2 is a block diagram showing the bonding process using a pre-treatment agent composition for non-slip rubber according to an embodiment of the present invention
The present invention for achieving the above effect relates to a pre-treatment agent composition for non-slip rubber and a method for manufacturing the same, and only a portion necessary for understanding the technical configuration of the present invention is described, the description of the other parts are the gist of the present invention. Note that it will be omitted so as not to scatter.
Hereinafter, the pre-treatment composition for non-slip rubber according to the present invention will be described in detail.
In the pretreatment composition for non-slip rubber, the present invention comprises 1.5 to 3 parts by weight of olefin chloride graft polymer, 0.5 to 1.5 parts by weight of acid, 0.5 to 1.5 parts by weight of thermoplastic polyurethane resin, and 0.5 to 1.0 parts by weight of adhesion promoter. And 93 to 97 parts by weight of a mixed solvent.
And the non-slip rubber pretreatment composition is preferably 3 to 7% by weight of the total solid content.
The chlorinated polyolefin graft polymer used in the present invention is used to impart the surface adhesion of the non-slip rubber, and the amount of the chlorinated polyolefin graft polymer is preferably used in the range of 1.5 to 3 parts by weight. If the content is less than 1.5 parts by weight, the adhesion may be lowered. If the content is more than 3 parts by weight, the wettability of the butyl rubber may be degraded, and the solubility in the solvent may be reduced.
According to a preferred embodiment, the chlorinated polyolefin graft polymer is a non-functional acrylic monomer with respect to 100 parts by weight of the chloride polyolefin resin such as polypropylene chloride or polyethylene chloride having a chloride degree of 10 to 50% by weight and a softening point of 40 to 120 ℃ When the graft polymerization is performed using 50 to 100 parts by weight, when the amount of the non-functional acrylic monomer is less than 50 parts by weight, there is a problem in that the adhesion of the pretreatment agent is not improved. The interfacial cohesion may be lowered.
In addition, as said nonfunctional acryl-type monomer, ethyl acrylate, butyl methacrylate, and methyl methacrylate can be used individually or in combination of 2 or more types.
In the graft polymerization, methyl ethyl ketone or the like diluted with benzoyl peroxide as a reaction initiator may be used.
In addition, the acid used in the present invention is used within the range of 0.5 to 1.5 parts by weight. When the amount of the acid is less than 0.5 parts by weight, the surface wettability of the non-slip rubber may be lowered. When the amount of the acid is more than 1.5 parts by weight, the cohesive force of the pretreatment agent may be lowered as the amount of the low molecular weight composition increases.
On the other hand, acidic acids can be used alone or in combination of two or more of carboxylic acid, hydrochloric acid, oxalic acid, malic acid, benzoic acid, sulfuric acid, amino acid, citric acid, ascorbic acid, nitric acid, acetic acid and the like.
The thermoplastic polyurethane resin used in the present invention is used to improve adhesive strength, aging resistance, and cohesion of the pretreatment agent, and is preferably used within a range of 0.5 to 1.5 parts by weight. If the amount of the thermoplastic polyurethane resin is less than 0.5 parts by weight, cohesive force may be lowered. If the amount of the thermoplastic polyurethane resin is greater than 1.5 parts by weight, the solubility in the solvent may be lowered and the viscosity of the pretreatment agent may increase, resulting in poor workability. This can be
On the other hand, the thermoplastic polyurethane resin used in the invention can be used all polyester, polyether, polycaprolactone.
The adhesion promoter used in the present invention is used for improving compatibility with the adhesive and reinforcing the adhesive strength, and it is preferable to use within the range of 0.5 to 1 parts by weight. If the amount is less than 0.5 parts by weight, the compatibility with the adhesive may be lowered. If the amount is more than 1 part by weight, the price increases due to the use of expensive adhesive promoters, so it is not valid in consideration of the increase in the effect of the increase. The low molecular weight may act as an adhesion barrier, resulting in a decrease in adhesion. As the adhesion promoter of the present invention, a silane coupling agent, a titanate coupling agent, an organic phosphate adhesion promoter, or the like may be used alone or in combination of two or more thereof.
The solvent used in the present invention is used for dissolving the composition and improving the wettability of the adherend, but is preferably used within the range of 93 to 97 parts by weight. If the amount is less than 93 parts by weight, the dissolution of the composition and the wettability of the adherend may be lowered, and if it exceeds 97 parts by weight, there is a problem of reducing the amount of the other composition.
On the other hand, it is preferable to select and use 3 or more types of methylcyclohexane, methyl ethyl ketone, cyclohexane, acetone, ethyl acetate, cyclohexanol, isosropanol, n-propanol, and ethanol.
The solvent used in the present invention is preferably used while adjusting the total solid content of the pretreatment composition mixture to be 3 to 7% by weight, and the solvent is used alone or the total solid content is less than the range defined above. If there is a possibility that the efficiency of the pretreatment agent coating workability may be lowered, and if the total solid content exceeds the above-defined range, the storage stability and solubility are inferior. In the present invention, the term "total solids" refers to a compound in which the organic matter contained in the pretreatment composition is dissolved.
On the other hand, it is preferable to use a pretreatment agent having the above-described components mixed with an isocyanate-based curing agent in order to increase the cohesive force in use and improve the adhesion.
On the other hand, the amount of the curing agent is preferably used 2 to 4 parts by weight with respect to 100 parts by weight of the pretreatment composition, if the amount is less than 2 parts by weight, there is a fear that the adhesive force is lowered, if it exceeds 4 parts by weight There is a fear that the speed of use increases and the usage time of the pretreatment agent is too short.
Hereinafter, the method for adhering the non-slip rubber using the pre-treatment agent composition for the non-slip rubber according to the present invention will be described in detail with reference to FIG. 2.
After buffing the non-slip rubber (A1) and then impregnating the detergent (A2), drying the non-slip rubber taken out from the detergent (A3), and then using the pretreatment composition for the non-slip rubber according to the present invention, the non-slip rubber It is characterized in that the non-slip rubber is adhered to the shoe parts through a process of applying (A4), drying (A5) and then applying an adhesive.
When described in detail for each process in the bonding method, the buffing (A1) is deposited by a conventional method using a grinder, etc. in order to facilitate the adhesion surface of the non-slip rubber with other shoe parts material It is a process to roughen the surface. Subsequently, the cleaning agent impregnation (A2) is a process for removing foreign matters and the like adhered to the adhered surface of the non-slip rubber, and typically uses a mixture of organic solvents such as methyl ethyl ketone. And the dry (A3) impregnated non-slip rubber is removed from the cleaning agent and then carried out by a conventional method in a process for removing the organic solvent adhered to the surface of the non-slip rubber at room temperature or 70 ℃. After the pretreatment treatment (A4) is applied to the adhered surface of the non-slip rubber using the pre-treatment agent composition for non-slip rubber according to the present invention and then dried (A5) by the same method as the above-mentioned drying (A3), According to a conventional method, adhesive treatment (A6) is performed using adhesives, such as a polyurethane system.
As such, the present invention is a conventional conventional non-slip rubber, as shown in Figure 1, when the non-slip rubber, in particular butyl rubber when using the pre-treatment agent composition for the non-slip rubber composed of the components as described above in detail Simplify the process by eliminating the aging process, secondary adhesive treatment process, etc. performed in the bonding process of the increase the productivity and reduce the manufacturing cost. In addition, the pre-treatment agent composition for non-slip rubber according to the present invention is characterized in that it is possible to improve the adhesion of the non-slip rubber by excellent properties of adhesion and wettability.
Hereinafter, the present invention will be described in detail with reference to Examples. However, the present invention is not necessarily limited to the following Examples.
1. Preparation of Chlorinated Polyolefin Graft Polymers
100 parts by weight of polychlorinated polyolefin resin (Superchlon 360, NIPPON PAPER CHEMICALS) and 50 parts by weight of methyl methacrylate were added 1000 parts by weight of methyl ethyl ketone to a 500 ml reactor equipped with a reflux condenser, a stirrer, a thermometer and a nitrogen injection device. Then, the mixture was stirred at 70 ° C. for 1 hour at a stirring speed of 75 rpm. Next, 1 part by weight of benzoyl peroxide, a reaction initiator, was diluted in 100 parts by weight of methyl ethyl ketone, and then charged in units of 1 hour over 4 times, and the temperature was raised to 75 ° C. to maintain a stirring speed of 70 rpm. To prepare a chlorinated polyolefin graft polymer.
2. Preparation of pretreatment composition for non-slip rubber
(Example 1)
1.5 parts by weight of chlorinated polyolefin graft polymer, 0.8 parts by weight of acetic acid (Samcheon Chemical), 0.5 parts by weight of thermoplastic polyurethane resin (Pearstic 45 / 40-19, Merquinsa) in a mixed container with temperature control and speed control 0.7 parts by weight of an adhesion promoter (KBM-403, Shin Etsu) was added thereto, followed by 48.0 parts by weight of methyl ethyl ketone, 19.4 parts by weight of normal hexane, and 29.1 parts by weight of cyclohexane (a ratio of about 50:20:30). A pretreatment composition for non-slip rubber having a total solid content of 3% by weight of the mixed solution dissolved by stirring for 6 hours at a temperature of 45 ° C. was prepared.
(Example 2)
3 parts by weight of chlorinated polyolefin graft polymer, 1.5 parts by weight of acetic acid (Samcheon Chemical), 1.5 parts by weight of thermoplastic polyurethane resin (Pearstic 45 / 40-19, Merquinsa) and an adhesion promoter (KBM-403, Shin Etsu) 1 part by weight of methyl ethyl ketone 46.5 parts by weight, normal hexane 18.6 parts by weight, cyclohexane 27.9 parts by weight (in a ratio of about 50:20:30) was added in combination with the same method as in Example 1 A pretreatment composition for slip rubber is prepared.
(Example 3)
2 parts by weight of chlorinated polyolefin graft polymer, 0.7 parts by weight of acetic acid (Samcheon Chemical), 0.8 parts by weight of thermoplastic polyurethane resin (Pearstic 45 / 40-19, Merquinsa) and an adhesion promoter (KBM-403, Shin Etsu) added 0.8 parts by weight of methyl ethyl ketone, 47.85 parts by weight of normal hexane, 19.14 parts by weight of normal hexane, 28.71 parts by weight of cyclohexane (approximately 50:20:30 ratio), and the same method as in Example 1 A pretreatment composition for slip rubber is prepared.
(Comparative Example 1)
0.5 parts by weight of chlorinated polyolefin graft polymer, 1.5 parts by weight of thermoplastic polyurethane resin (Pearstic 45 / 40-19, Merquinsa), and 1 part by weight of an adhesion promoter (KBM-403, Shin Etsu), followed by 48.25 parts by weight of methyl ethyl ketone. , 19.6 parts by weight of normal hexane and 29.15 parts by weight of cyclohexane (a ratio of about 50:20:30) were used in combination to prepare a pre-treatment composition for non-slip rubber in the same manner as in Example 1.
(Comparative Example 2)
1.5 parts by weight of chlorinated polyolefin graft polymer, 1.5 parts by weight of thermoplastic polyurethane resin (Pearstic 45 / 40-19, Merquinsa) were added 1.5 parts by weight of adhesion promoter (KBM-403, Shin Etsu), and 46.75 parts by weight of methyl ethyl ketone. , 19.7 parts by weight of normal hexane and 29.05 parts by weight of cyclohexane (in a ratio of about 50:20:30) were used in combination to prepare a pretreatment composition for non-slip rubber in the same manner as in Example 1.
(Comparative Example 3)
A conventional non-slip rubber adhesive product was used. Specifically, PR-305 (Hwaseung T & C) was used as the CR-based pretreatment agent, and HRF-E (Hwaseung T & C) was applied to A-340 (Hwaseung T & C) as the CR-based adhesive. An adhesive added with 5wt% was used.
The composition table of the said Examples 1-3 and Comparative Examples 1-3 was shown in [Table 1] below.
Chlorinated Polyolefin Graft Polymers
1.5
3
2
0.5
1.5
Conventional
Non-slip rubber
Adhesive
product
Note 1) Acetic Acid: Samcheon Chemical
Note 2) Pearstic 40 / 40-19: Merquinsa
Note 3) KBM-403: Shin Etsu
3. Evaluation of Pretreatment Composition for Non-slip Rubber
Examples 1 to 3 and Comparative Examples 1 and 2 were applied to the non-slip rubber sheet according to the contents described below in the non-slip rubber sheet according to the method shown in FIG. The ethylene vinyl acetate specimens were bonded to each other, and Comparative Example 3 was conventionally treated with primers on the non-slip rubber sheet by a method as shown in FIG. 1 and then bonded with ethylene vinyl acetate specimens using a polyurethane-based adhesive. After that, the results are shown in the following [Table 2].
end. Specimen Fabrication with Pretreatment Composition
The ethylenevinylacetate specimens of 25 × 100 mm are washed with polar solvents, dried and then coated with D-ply P-6-2 (Henkel Technology) and dried at 60 ° C. for 2 minutes. The dried specimens were UV irradiated.
After that, as shown in Figure 2, the non-slip rubber sheet is also prepared in a size of 25 × 100mm buffing (A1), then washed (A2), dried (A3) and then the line according to the above Examples and Comparative Examples 3 wt% of a rubber pretreatment agent (DRF, Henkel Technology) was added to the treatment composition, followed by coating (A4) and drying (A5) at 60 ° C for 5 minutes.
Next, the adhesive was applied to each of the two adherends above (A6), dried at 60 ° C. for 5 minutes, and then bonded to each other by pressing at a load of about 10 kg. At this time, five test specimens used in the same test was used.
I. Initial Adhesion Evaluation
The prepared adhesive specimen was left at room temperature for 30 minutes, and then peeled at a tensile speed of 100 mm / min using a universal tensile tester to measure adhesive strength.
All. State Adhesion Evaluation
The prepared adhesive specimen was left at room temperature for 24 hours, and then peeled at a tensile speed of 100 mm / min using a universal tensile tester (UTM) to measure adhesive strength.
la. Heat resistance evaluation
After the prepared adhesive specimens were allowed to stand at room temperature for 24 hours, the distances were measured after standing for 30 minutes at a load of 1 kg at 90 ° C.
(kg f / cm)
(kg f / cm)
(mm)
(min)
As shown in Table 2, Examples 1 to 3 of the present invention was evaluated to have a good adhesive strength, in particular, excellent state adhesive strength compared to Comparative Examples 1 to 3.
In addition, the adhesion time was significantly reduced compared to Comparative Example 3, the adhesion was also excellent.
As described above, the pre-treatment agent composition for non-slip rubber according to the present invention and a manufacturing method thereof have been described through the above-described preferred embodiments, and the superiority thereof has been confirmed, but those skilled in the art will appreciate the present invention described in the following claims. It will be understood that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention.
A1: Buffing A2: Washing
A4: pretreatment treatment A6: adhesive treatment
Claims (7)
1.5 to 3 parts by weight of olefin chloride graft polymer, 0.5 to 1.5 parts by weight of acid, 0.5 to 1.5 parts by weight of thermoplastic polyurethane resin, 0.5 to 1.0 parts by weight of adhesion promoter and 93 to 97 parts by weight of mixed solvent,
The acid,
Pretreatment composition for non-slip rubber, characterized in that it is used alone or in combination of two or more of carboxylic acid, hydrochloric acid, oxalic acid, malic acid, benzoic acid, sulfuric acid, amino acid, citric acid, ascorbic acid, nitric acid, acetic acid.
The non-slip rubber pre-treatment composition is a non-slip rubber pre-treatment composition, characterized in that the total solid content of 3 to 7% by weight.
The olefin chloride graphite polymer,
50 to 100 parts by weight of a non-functional acrylic monomer is graft-polymerized with respect to 100 parts by weight of a polyolefin chloride having a chloride degree of 10 to 50% by weight and a softening point of 40 to 120 ° C.
The adhesion promoter,
Pre-treatment agent composition for non-slip rubber, characterized in that used alone or in combination of two or more of the silane coupling agent, titanate coupling agent, organic phosphate-based adhesion promoter
The solvent,
Pretreatment agent for non-slip rubber, characterized in that it is used in combination of three or more of methylcyclohexane, methyl ethyl ketone, cyclohexane, acetone, ethyl acetate, cyclohexanol, isosropanol, n-propanol, ethanol Composition
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6048610A (en) | 1997-10-31 | 2000-04-11 | Intertape Polymer Group, Inc. | Primer coating for polyolefin-backed tapes |
| JP2004210894A (en) | 2002-12-27 | 2004-07-29 | Yokohama Rubber Co Ltd:The | Primer composition |
| KR20090035625A (en) * | 2006-08-31 | 2009-04-09 | 피피지 인더스트리즈 오하이오 인코포레이티드 | Universal primer |
| KR20100078473A (en) * | 2008-12-30 | 2010-07-08 | 한국신발피혁연구소 | Primer composition for improved adhesion |
-
2010
- 2010-12-16 KR KR1020100128771A patent/KR101224972B1/en active IP Right Grant
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6048610A (en) | 1997-10-31 | 2000-04-11 | Intertape Polymer Group, Inc. | Primer coating for polyolefin-backed tapes |
| JP2004210894A (en) | 2002-12-27 | 2004-07-29 | Yokohama Rubber Co Ltd:The | Primer composition |
| KR20090035625A (en) * | 2006-08-31 | 2009-04-09 | 피피지 인더스트리즈 오하이오 인코포레이티드 | Universal primer |
| KR20100078473A (en) * | 2008-12-30 | 2010-07-08 | 한국신발피혁연구소 | Primer composition for improved adhesion |
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