JP5309453B2 - Cleaning agent and cleaning method using the cleaning agent - Google Patents

Description

  The present invention mainly relates to a cleaning agent that can be used for removing a cured product of a moisture-curable hot melt composition, and a cleaning method using the same. More specifically, the present invention relates to a cleaning agent that can be used for cleaning various supply devices used when applying a moisture-curable hot melt composition to various substrates, and a cleaning method thereof.

  Hot melt adhesives generally have excellent properties such as instantaneous adhesiveness, and thus have been used in large amounts in various applications such as bookbinding, packaging, and woodworking in recent years.

  Since the hot melt adhesive is usually in a very viscous liquid or solid state at room temperature, an adhesive supply device generally called a hot melt applicator is used when the adhesive is used in the above-mentioned applications. It is necessary to heat and melt the adhesive and adjust it to a desired heat melt viscosity suitable for coating.

  The hot-melt applicator used for application of the hot-melt adhesive is usually a hot-melt adhesive inlet, a melting tank for heating and melting the charged hot-melt adhesive, and hot-melt hot-melt bonding In many cases, it is composed of a discharge port for coating the agent and a hose portion for transferring the adhesive from the melting tank to the discharge port.

  In particular, when a moisture curable hot melt adhesive is used as the hot melt adhesive, the above equipment generally has a melting point from the viewpoint of preventing the moisture curable hot melt adhesive from coming into contact with moisture and curing. Equipment for replacing the air in the tank with nitrogen gas or carbon dioxide gas constantly or periodically may be required.

  However, even if it has a replacement facility as described above, the moisture inside the hot melt applicator cannot be completely eliminated with such a facility alone, so the moisture curing of the adhesive inside the applicator is still possible. It was difficult to suppress the level to a sufficient level.

  In addition, since the moisture-curable hot melt adhesive may gradually cure due to the influence of heat, the air inside the hot melt applicator can be sufficiently replaced with nitrogen gas or the like by the replacement equipment. When the applicator is used for a long period of time, the cured product of the adhesive may adhere to the wall surface of the melting tank or the like inside the melting tank or the transfer hose.

  If a cured product of the adhesive or the like is fixed inside the hot melt applicator, the heat-cured moisture-curing hot melt adhesive cannot be efficiently transferred to the coating device, and the adhesive particles or flakes The cured product or gelled product may be applied to the substrate together with the heat-cured moisture-curing hot-melt adhesive, which may cause poor adhesion or poor appearance of laminates such as cosmetic products There is. For this reason, there has been a demand from the industry to study a cleaning agent and a cleaning method that can efficiently remove the adhered adhesive remaining inside the applicator and the like.

  For example, a method using a treatment agent having a functional group capable of reacting with an isocyanate group of a moisture curable hot melt adhesive and containing a compound such as alcohol, primary or secondary amine, or carboxylic acid as a main component (for example, , Patent Document 1), and a method of replacing the moisture-curing hot melt adhesive inside the applicator with a specific non-reactive hot melt adhesive is known (for example, see Patent Document 2).

  However, in any of the above methods, it has been difficult to efficiently remove the moisture-curable hot melt adhesive and its cured product fixed inside the applicator to a sufficient level.

JP-A-7-197006 JP 2001-129477 A

The problem to be solved by the present invention is to efficiently remove the moisture curable hot melt composition fixed in the moisture curable hot melt composition supply apparatus and the cured product thereof to a practically sufficient level. It is to provide a possible cleaning agent and a cleaning method using the same.
Further, the problem to be solved by the present invention is to provide a method for efficiently applying a moisture curable hot melt composition onto a substrate using a supply device for the moisture curable hot melt composition washed by the above method. It is to be.

  As a result of intensive studies to solve the above problems, the present inventors have efficiently used a moisture-curable polyurethane composition and its cured product when a specific polyester compound that has been conventionally known as a plasticizer is used. It was found that it can be removed to a sufficient level.

  That is, this invention relates to the cleaning agent characterized by including the compound (A) shown by the following general formula (I).

(In general formula (I), R ₁ and R ₅ are butyl groups, R ₂ and R ₄ are ethylene groups, R ₃ is a butylene group, and n is 2.)
Further, the present invention, by contacting the site where the cured product of the moisture curable hot melt composition is fixed and the cleaning agent heated at a temperature equal to or higher than the softening point of the moisture curable hot melt composition, The present invention relates to a cleaning method, wherein the fixed cured product is removed from the portion.

  The present invention also provides a moisture curable hot melt composition supply device that supplies the cleaning agent heated at a temperature equal to or higher than the softening point of the moisture curable hot melt composition, and constitutes the supply device. The present invention relates to a method for cleaning a supply device, in which the cured product is released from the inner wall of the flow path by circulating in the flow path of the curable hot melt composition.

  Further, the present invention, by contacting the site where the cured product of the moisture curable hot melt composition is fixed and the cleaning agent heated at a temperature equal to or higher than the softening point of the moisture curable hot melt composition, The present invention relates to a method of removing the fixed cured product from the site, then supplying a moisture-curable hot melt composition, and applying the moisture-curable hot melt composition in a heated and melted state onto a substrate.

  Further, the present invention supplies the cleaning agent heated at a temperature equal to or higher than the softening point of the moisture curable hot melt composition to a moisture curable hot melt composition supply device, and constitutes the supply device. After the cured product is released from the inner wall of the flow path by circulating in the flow path of the moisture curable hot melt composition, the cleaning agent is discharged from the supply device, and then to the supply device. The present invention relates to a method for supplying a moisture-curable hot melt composition and applying the moisture-curable hot melt composition in a heated and melted state on a substrate.

  Further, the present invention supplies the cleaning agent heated at a temperature equal to or higher than the softening point of the moisture curable hot melt composition to a moisture curable hot melt composition supply device, and constitutes the supply device. After the cured product is released from the inner wall of the flow path by circulating in the flow path of the moisture curable hot melt composition, the cleaning agent is discharged from the supply device, and then to the supply device. Supplying the moisture-curing hot melt composition in a heated and melted state, and filtering the moisture-curing hot melt composition in a heat-melting state filtered using a filter made of fired metal fibers having a filtration accuracy of 40 to 80 μm on a substrate It is related with the method of apply | coating to.

  The cleaning agent of the present invention contains the compound (A) represented by the following general formula (I) and, if necessary, other various additives.

(In the general formula (I), R ₁ And R ₅ Is a butyl group, R ₂ And R ₄ Is ethylene group, R ₃ Is a butylene group and n is 2. )

  The cleaning agent may be solid or liquid at room temperature, but is solid at room temperature, but is preferably melted by heating because it is easy to handle.

The compound (A) or a heated melt thereof easily dissolves the moisture-curing hot melt composition in a heat-melted state, and also swells the cured product of the moisture-curing hot melt composition, thereby fixing the fixing site. Can be liberated from In particular, it is preferable to use a compound having a solubility parameter in the range of 8.5 to 9.9 as the compound (A) because the moisture-curable hot melt composition in a heat-melted state is easily dissolved.
The solubility parameter is a value calculated by the Small formula (the following formula 1).

SP = dΣG / M (1)
Here, SP is a solubility parameter, M is a unit molecular weight, d is a density (g / cm ³ ), and G is a constant specific to an atomic group or a functional group.

As the compound (A), any compound can be used as long as it satisfies the general formula (I), but R ₁ and R ₅ in the general formula (I) are each independently 1 to 8 carbon atoms. R ₂ and R ₄ are each independently an aliphatic alkylene group having 1 to 4 carbon atoms, R ₃ is an aliphatic alkylene group having 1 to 10 carbon atoms, and Preferably, n is an integer of 1 to 4, R ₁ and R ₅ are butyl groups, R ₂ and R ₄ are ethylene groups, R ₃ is a butylene group, and n is 2 is more preferable, and specifically, di-monobutylethyl glycol adipate is particularly preferable because of its excellent cleaning effect.

  In addition, it is preferable to use a compound having a molecular weight of 500 or less as the compound (A) because the cured product of the moisture-curable hot melt composition is easily swelled and easily released from the fixing site.

  The said compound (A) can be manufactured by esterifying the dicarboxylic acid and the polyether polyol by which the hydroxyl group of one terminal was blocked by a well-known and usual method.

  As the dicarboxylic acid, for example, adipic acid, sebacic acid and the like can be used, and among them, the use of adipic acid is relatively inexpensive and easily available, and the solubility of the resulting compound (A) This is preferable because the parameters can be easily adjusted.

Examples of the polyether polyol in which the hydroxyl group at one end is blocked include hydroxyl groups at one end such as ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, propylene glycol, dipropylene glycol, and tripropylene glycol. A monoalkylene glycol monoalkyl ether or polyalkylene glycol polyalkyl ether blocked with an alkyl group such as a group or an ethyl group can be used, and among them, the hydroxyl group at one end of diethylene glycol is a methyl group or an ethyl group, or It is preferable to use diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether or the like blocked with a butyl group, The use of Riwake diethylene glycol monobutyl ether is easily swelled a cured product of the moisture-curing hot-melt composition, and preferred because of its excellent washability.

  The cleaning agent of the present invention preferably contains a crystalline polymer, if necessary, in addition to the compound (A).

  The crystalline polymer is a polymer having a crystalline segment in the molecule, and specifically includes a polyester resin, a polyurethane resin, a polyamide resin, a polyacetal resin, and a polyethylene resin having a crystalline segment in the molecule. Polyalkylene resins such as polypropylene resins can be used. Among these, linear aliphatic polyester resins, linear aliphatic polyether resins having 4 or more carbon atoms, linear aliphatic polycarbonate resins, and linear urethane resins having the same structure as the above resins are used. It is preferable to use, and it is more preferable to use polycaprolactone. By using the crystalline polymer, the compatibility between the compound (A) and the moisture-curable hot melt composition can be improved, and the used cleaning agent discharged from the supply device after cleaning and the inside of the device Since the moisture-curable hot melt composition removed from can be made into a solid state, it is possible to easily handle the discharged matter.

  The crystalline polymer is preferably used in a range where the cleaning agent of the present invention is in a solid state at room temperature, and specifically, it is preferably used in a range of 1 to 50% by mass with respect to the total amount of the cleaning agent. .

  Moreover, it is preferable that the cleaning agent of this invention contains the wax which has active hydrogen as needed other than the said compound (A).

  The wax having active hydrogen reacts with an isocyanate group or silyl group that contributes to the moisture curing reaction of the moisture curable hot melt composition, and stops or suppresses the progress of the moisture curing reaction of the composition remaining inside the apparatus. can do. Moreover, the cleaning agent of the present invention containing waxes having active hydrogen is used to solidify the used cleaning agent discharged from the supply device after cleaning and the moisture-curable hot melt composition removed from the inside of the device. Therefore, it is possible to facilitate the handling of such effluent.

  As the wax having active hydrogen, for example, a solid higher alcohol or hydroxycarboxylic acid can be used.

  As the higher alcohol, for example, stearyl alcohol can be used, and as the hydroxycarboxylic acid, for example, hydroxystearic acid can be used, but it is preferable to use hydroxystearic acid.

  The wax having active hydrogen is preferably used in a range where the cleaning agent of the present invention is in a solid state at ordinary temperature, and specifically, used in a range of 1 to 50% by mass with respect to the total amount of the cleaning agent. It is preferable.

  In addition, the cleaning agent of the present invention is preferably used for cleaning a cured product of a moisture curable polyurethane hot melt composition fixed inside a supply device or the like.

Next, a cleaning method using the cleaning agent of the present invention will be described.
The cleaning method of the present invention involves dissolving or swelling the composition or the cured product by bringing the moisture-curing hot melt composition or a portion to which the cured product is fixed into contact with the heated cleaning agent of the present invention. It is a method of releasing from the fixing site.

  The heating temperature of the cleaning agent of the present invention is preferably about the softening temperature of the moisture curable hot melt composition, and more specifically in the range of 80 to 150 ° C. Since the cleaning agent adjusted to such a temperature easily penetrates into the cured product of the moisture curable hot melt composition and swells it, a further excellent cleaning effect can be exhibited.

  More specifically, the contact is performed by immersing a moisture-curing hot melt composition or a portion where the cured product is fixed in a liquid detergent, or applying a liquid detergent to the portion. Etc. The contact is preferably about 5 minutes to 8 hours.

Hereinafter, the cleaning method using the cleaning agent of the present invention will be described with specific examples.
First, a method for cleaning a two-roll type roll coater, which is known as a general coating apparatus for a moisture-curable hot melt composition, will be described.

  First, the softening temperature of the moisture-curable hot melt composition, specifically, a solid cleaning agent is placed on a roll whose temperature is adjusted to about 80 to 150 ° C., and heated and melted on the roll surface. The cleaning agent in a heated and melted state is brought into contact, or a liquid cleaning agent that has been heated and melted in advance is brought into contact with the roll surface. In that case, it is preferable to make this cleaning agent contact the whole roll surface by rotating a roll.

  Secondly, the cured product of the moisture-curable hot melt composition and the heat-cured moisture-cured hot melt composition are released from the roll surface, or the moisture-cured hot-melt composition is dissolved in the cleaning agent of the present invention. After confirmation, the cleaning agent is removed from the roll surface.

  The removal can be performed by increasing the distance between the two rolls or changing the rotation direction of the rolls as appropriate.

  By repeating the above steps about 2 to 3 times, it is possible to remove the moisture-curable hot melt composition fixed to the roll surface constituting the roll coater and the cured product in a short time.

  Next, a cleaning method for a die coater known as a general coating apparatus for a moisture-curable hot melt composition will be described.

  As a method for cleaning the die coater, for example, a part of the die coater to which the composition and the cured product are fixed is immersed in a cleaning agent in a heated and melted state heated to about the softening temperature of the moisture-curable hot melt composition. There is a way. The cured product of the moisture curable hot melt composition is particularly likely to adhere to the opening of the die coater (the discharge portion of the moisture curable hot melt composition).

  Therefore, the cured product of the composition adhering to the opening is applied onto the base material together with the composition in a heated and melted state, and as a result, it may cause poor appearance of the resulting cosmetic product or the like. .

  Therefore, when the die coater is cleaned, it is preferable that the opening is sufficiently immersed in the cleaning agent.

  Further, the die coater usually keeps the hot melt applicator and its opening in a sealed state from the viewpoint of suppressing the curing of the moisture curable hot melt composition remaining in the die coater. As a method for sealing, there is a method in which the opening of the die coater is sealed using a non-breathable adhesive sheet or the like.

  However, in the said method, when peeling an adhesive sheet from the opening part, an adhesive remains in the said opening part, As a result, a coating defect may be caused.

  On the other hand, if the method of completely immersing the opening of the die coater in the cleaning agent, there is an advantage that not only the opening can be cleaned but also the inside of the die coater can be maintained without using an adhesive sheet. .

  Next, a hot melt composition supply device such as a hot melt applicator, particularly, a method for cleaning a melting tank constituting the hot melt composition supplying device will be described.

  First, after the moisture curable hot melt composition remaining inside the melting tank constituting the supply device is discharged to some extent, the cleaning agent of the present invention is heated to a temperature equal to or higher than the softening point of the moisture curable hot melt composition. It puts in the melting tank adjusted to 150 degreeC. At that time, the cleaning agent may be in a solid state or heated and melted.

In the case of cleaning only in the melting tank, it can be cleaned by leaving the cured product of the moisture curable hot melt composition fixed in the melting tank sufficiently immersed in the cleaning agent for about 30 minutes to 8 hours. It is.
On the other hand, when the inside of the flow path of the moisture curable hot melt composition such as a pump, a hose, and a discharge port is cleaned simultaneously as well as the melting tank constituting the supply device, the moisture curable hot melt composition A method in which the cleaning agent heated at a temperature equal to or higher than the softening point is circulated in the flow path constituting the supply device is preferable from the viewpoint of reducing the amount of the cleaning agent used.

  The circulation time varies depending on the size of the supply device to be cleaned and the degree of contamination, but is preferably about 30 minutes to 8 hours.

  By the above method, the moisture-curable hot melt composition remaining inside the supply device is dissolved in the cleaning agent and can be easily removed from the inside of the device.

  In addition, since the cured product of the moisture-curable hot melt composition that has been fixed inside the supply device swells by the cleaning agent, for example, a cleaning agent having a relatively high viscosity, which is different from the cleaning agent of the present invention, or a hot By separately charging, circulating, and discharging the melt composition, etc., it can be easily released from the inner wall of the apparatus.

  If it is supply apparatuses, such as a hot-melt applicator wash | cleaned by the said method, a moisture hardening type hot-melt composition can be efficiently apply | coated on various base materials.

  The cleaning method of the present invention can be applied to cleaning of supply devices such as a slit coater, a die coater, a nozzle gun, and a spray gun in addition to the supply device.

  The apparatus for supplying a moisture-curable hot melt composition cleaned by the cleaning method of the present invention can be used for manufacturing a laminated body, for example, a decorative product, which requires a good surface appearance, for example. it can.

  At that time, one of the cured products of the moisture curable hot melt composition released by the cleaning agent when applying the moisture curable hot melt composition on various substrates using the supply device cleaned by the above method. The part may be supplied to the application surface. Since the cured product impairs the smoothness of the coated surface, for example, it may cause a defective surface appearance, a convex surface defect, or a linear uncoated defect of a decorative product obtained by applying decorative paper on a substrate. There is.

  As a method for solving the above problem, for example, a method of applying the moisture-curable hot melt composition heated and melted on a substrate through a filter can be mentioned.

  As the filter, it is preferable to use a non-woven filter obtained by firing a felt laminate made of metal fibers or a fired metal fiber filter such as a wire mesh made of fired metal fibers because the pressure loss is low. In particular, it is more preferable to use a non-woven filter obtained by firing a felt laminate made of metal fibers from the viewpoint of improving filtration accuracy.

  The fired metal fiber filter is obtained by firing a nonwoven fabric made of metal fibers having a diameter of several microns, and can collect solid contents such as particles in contact with the pores in the filter. .

  The metal composing the metal fired fiber filter may be any metal that does not corrode or peel off. For example, nickel such as nickel, stainless steel, or Hastelloy (registered trademark of Haynes), which is industrially available. An alloy is mentioned.

  The filtration accuracy (pore diameter) of the metal fired fiber filter is preferably 80 μm or less from the viewpoint of fine particle removal rate, and more preferably in the range of 40 to 80 μm from the viewpoint of ensuring high filtration accuracy.

  As the fired metal filter, for example, Fuji metal fiber manufactured by Fuji Filter Co., Ltd. or metal fiber manufactured by Nichidai Filter Co., Ltd. can be used.

[Measuring method of melt viscosity]
Using an ICI type cone plate type rotational viscometer (cone diameter: φ19.5 mm, cone angle: 2.0 °), a melt viscosity (mPa at 125 ° C.) of a moisture curable hot melt adhesive described later or a cleaning agent described later. -S) was measured.

[Preparation example of moisture-curing hot melt adhesive]
Obtained by reacting 500 parts by weight of a polyester polyol having a number average molecular weight of 3000 obtained by reacting adipic acid and 1,6-hexanediol in a 1 liter four-necked flask, neopentyl glycol and terephthalic acid. 250 parts by mass of the polyester polyol having a number average molecular weight of 1000 and 250 parts by mass of a polyester polyol having a number average molecular weight of 3500 obtained by reacting sebacic acid with 1,6-hexanediol were heated to 120 ° C. under reduced pressure. And dehydrated to a moisture content of 0.05% by mass.

  Next, after cooling the four-necked flask to 70 ° C., 207 parts by mass of 4,4′-diphenylmethane diisocyanate was added, and then the temperature was raised to 90 ° C., and the reaction was continued for 3 hours until the isocyanate group content became constant. As a result, a urethane prepolymer was obtained.

  0.15 parts by mass of the obtained urethane prepolymer, 2,2′-dimorpholinodiethyl ether (trade name: U-CAT 2041, manufactured by San Apro Corporation), and 0.05 part by mass of methanesulfonic acid By mixing and stirring until uniform, a moisture-curable hot melt composition was obtained. The resulting moisture-curable hot melt composition had a melt viscosity of 11000 mPa · s, and the isocyanate group content measured by an appropriate method was 2.1% by mass.

Example 1
[Preparation of cleaning agent 1]
In a 2 liter four-necked flask, 300 parts by mass of adipic acid and 750 parts by mass of diethylene glycol monobutyl ether were added and heated to 200 ° C. with stirring, and then 0.0005 parts by mass of p-toluenesulfonic acid was further added. It was. Subsequently, the detergent 1 was obtained by making it esterify for 2 hours, refluxing under reduced pressure. The boiling point of the cleaning agent 1 was 300 ° C., and the viscosity at 23 ° C. was a liquid of 100 mPa · s.

(Example 2)
[Preparation of cleaning agent 2]
In a 2-liter four-necked flask, 800 parts by mass of the cleaning agent 1, 100 parts by mass of 12-hydroxystearic acid, and Placcel H1 which is a polycaprolactone polymer (manufactured by Daicel Chemical Industries, Ltd., number average molecular weight 10,000) 50 parts by mass was mixed, heated at 120 ° C. for 1 hour, and uniformly dissolved to obtain cleaning agent 2. The cleaning agent 2 was pasty at 23 ° C.

(Comparative Example 1)
[Preparation of cleaning agent 3]
In a 2 liter four-necked flask, 900 parts by weight of polyethylene wax (“VESTOWAX A118” manufactured by Degussa Japan Co., Ltd.) and 100 parts by weight of stearyl alcohol are heated at 140 ° C. for 1 hour and uniformly dissolved, thereby cleaning. 3 was obtained. The cleaning agent 3 was solid at 23 ° C.

(Comparative Example 2)
[Preparation of cleaning agent 4]
700 parts by mass of terephthalic acid and 350 parts by mass of butyl alcohol were placed in a 2 liter four-necked flask, heated to 200 ° C. with stirring, and 0.0005 parts by mass of p-toluenesulfonic acid was added. Detergent 4 was obtained by carrying out esterification reaction for 2 hours while refluxing under reduced pressure. The boiling point of the cleaning agent 4 was a pale yellow liquid at 23 ° C.

(Example 3) Cleaning of roll coater The roll surface temperature of a triple hot melt roll coater (manufactured by Matsushita Kogyo Co., Ltd.) having an effective width of 400 mm is set to 115 ° C., and 0.5 kg of the moisture curable hot melt adhesive is added. I put it in.

Next, 40 g / m ^{2 of the} moisture-curing hot melt adhesive was applied to the surface of a medium density fiber board (abbreviated as MDF; width: 300 mm, length: 1800 mm, thickness: 2.5 mm) at a speed of 20 m / min. Then, a decorative sheet was obtained by laminating a decorative sheet (width: 300 mm, thickness: 160 μm, length: 300 m roll shape) made of olefin on the coated surface using a roll press.

  After the above operation was completed, a large amount of the moisture curable hot melt adhesive and a cured product of the moisture curable hot melt adhesive were fixed on the end of the roll on the roll coater.

  Therefore, 50 g of the cleaning agent 1 is put on a roll coater adjusted to 115 ° C., and the roll coating machine is rotated, so that the cleaning agent 1 is added to the fixed portion of the cured product of the moisture-curable hot melt adhesive. When contacted for a minute, the moisture-curable hot melt adhesive fixed on the roll coater was released.

  The mixture of the cleaning agent 1 and the moisture curable hot melt adhesive released from the roll coater is removed from the roll coater, and 50 g of the cleaning agent 1 is again put on the roll coater and the roll coater is left for 5 minutes. After rotating, the cleaning agent 1 was removed from the roll coater.

  After removal, the moisture-curing hot melt adhesive partially remaining on the surface of the roll coater was wiped off with a waste cloth, and the cleaning operation was completed. On the surface of the roll coater after washing, no adhesion of the moisture curable hot melt adhesive and its cured product was observed at all.

Example 4
The roll coater was cleaned in the same manner as in Example 3 except that the cleaning agent 2 was used instead of the cleaning agent 1.

When the cleaning agent 1 is used, if the cleaning agent 1 partially remaining on the roll surface is not wiped off with a waste cloth or the like, the moisture curable hot melt adhesive is used when the roll coater is reused the next day. However, if the cleaning agent 2 is used, the next day roll coater can be used without wiping off the cleaning agent 2 partially remaining on the roll surface after cleaning. In the reuse, the hardened moisture-curing hot melt adhesive was hardly on the roll surface.
In addition, when the cleaning agent 2 is used, the mixture of the cleaning agent 2 and the moisture-curing hot melt adhesive peeled off from the roll coater is solidified by cooling. It was easy.

(Comparative Example 3)
The roll coater was cleaned in the same manner as in Example 3 except that the cleaning agent 3 was used instead of the cleaning agent 1.

  In the cleaning agent 3, the moisture curable hot melt adhesive fixed to the roll surface and the cured product thereof could not be dissolved or released. Although the cleaning was repeated three times using the cleaning agent 3, the moisture curable hot melt adhesive and its cured product were still fixed on the roll surface.

(Example 5) Cleaning of parts In the 1500 parts by mass of the cleaning agent 2 heated to 150 ° C., the moisture-curing hot melt adhesive, the filter to which the cured product is fixed, and the connection fitting between the melting tank and the heat hose are heated to 150 ° C. It was immersed in and maintained for 2 hours, and it was confirmed visually that the moisture-curing hot melt adhesive and its cured product that had been fixed to the filter and the connection fitting were completely removed.

(Comparative Example 4) Cleaning of parts The moisture-curable hot melt adhesive and the filter and the metal fitting to which the cured product was fixed were immersed in 500 parts by mass of acetone and heated at 50 ° C for 2 hours. The moisture-curing hot melt adhesive and its cured product were still adhered to the surface of the connection fitting.

(Comparative Example 5) Cleaning of parts The moisture-curable hot-melt adhesive and the filter and the metal fitting to which the cured product was fixed were combined with 500 parts by mass of Hysol SAS (Shin Nippon Oil Co., Ltd., high-boiling aromatic hydrocarbons). Although it was immersed in the compound) and heated at 150 ° C. for 2 hours, the moisture-curable hot-melt adhesive and its cured product were still adhered to the surface of the filter and the connection fitting.

(Example 6) Laminator cleaning A polyurethane resin laminator “Laminator PL-” manufactured by Marunaka Corp. equipped with a melting device “MC-8” manufactured by Nordson and a die coater “BC-51” manufactured by Nordson. 300 PUR / M "(with an effective width of 400 mm and a Φ20 mm * 100 mm 200 mesh in-line filter. Melting tank, hose part and die coater temperature condition: 120 ° C.) A moisture-curing hot melt adhesive is applied on a decorative sheet made of olefin (width: 300 mm, thickness: 160 μm, length: 300 m roll shape) to a thickness of 50 μm at a coating speed of 10 m / min. Next, a medium density fiber board (abbreviated as MDF. Next: 3) 00 mm, length: 1800 mm, thickness: 2.5 mm) were pasted together to produce a decorative member.

  After producing 10 decorative products by the above method, the temperature of the melting device, the hose portion, and the die coater constituting the polyurethane resin laminator is returned to room temperature, and aluminum tape (made by Nitoms, 50 μm thick) is opened at the die coater opening. Soft aluminum foil / adhesive) was applied and allowed to stand for 20 hours in a state where the intrusion of air into the laminator was blocked.

  The production of the decorative member and the leaving in a state where the intrusion of air is blocked is a one-day operation, and after performing this for five days, the two-day leaving in the same state as the above-mentioned leaving is regarded as one cycle. When this was done for 4 cycles, the laminator was washed. A large amount of the moisture-curing hot melt adhesive and its cured product adhered to the inner wall of the laminator before cleaning.

  7 kg of the cleaning agent 1 was put into the laminator in which the temperature of the melting device, the hose portion and the die coater was set to 150 ° C. It was set so that the cleaning agent 1 discharged from the die coater returned to the melting tank again and circulated in the laminator. In addition, the cleaning agent 1 discharged from the die coater is mixed with a moisture curable hot melt adhesive and a cured product thereof. In order to prevent them from circulating inside the apparatus, A 200 mesh wire mesh was placed between the hose connecting the melting tank.

After carrying out circulating cleaning for 2 hours at the maximum capacity of the laminator (pump rotation speed 80 rpm), the cleaning agent 1 and the like were discharged, and the molten tank wall of the laminator cured the swollen moisture-curing hot melt adhesive. Things remained.
Since the cured product of the swollen moisture curable hot melt adhesive can be easily peeled off, by removing the cured product using a vacuum cleaner or the like, the moisture curable hot melt adhesive in the laminator and Most of the cured product could be removed.

(Example 7)
Metal fiber (made by Nitadai Filter Co., Ltd., trade name 40AL3, filtration product) made of a non-woven sintered body composed of metal fibers in micron units between the melting tank constituting the laminator washed by the above method and the die coater. Using a laminator provided with a filtration device having an accuracy of 40 μm) as a filtration element, a cosmetic product was produced in the same manner as described above. In that case, since the hardened | cured material etc. hardly exist in the application surface of the moisture hardening type hot-melt-adhesive apply | coated on the decorative sheet, the cosmetics production member excellent in surface smoothness was able to be manufactured.

(Comparative Example 6)
A laminator is produced in the same manner as in Example 6 except that 8 kg of benzoate plasticizer Monosizer PB-3 (manufactured by Dainippon Ink & Chemicals, Inc., SP value: 9.9) is used instead of the cleaning agent 1 Was washed.

  However, the cured product of the moisture curable hot melt adhesive is still adhered to the inner wall of the laminator and cannot be easily removed.

Claims (7)

It contains a compound (A) represented by the following general formula (I) heated at a temperature equal to or higher than the softening point of the moisture curable hot melt composition and a portion where the cured product of the moisture curable hot melt composition is fixed. A cleaning method, wherein the fixed cured product is removed from the site by contacting with a cleaning agent .

(In general formula (I), R ₁ and R ₅ are each independently an alkyl group, R ₂ , R ₃ and R ₄ are each independently an alkylene group, and n is an integer of 1 to 4.) R in the general formula (I) ₁ And R ₅ Are each independently an aliphatic alkyl group having 1 to 8 carbon atoms, and R ₂ And R ₄ Are each independently an aliphatic alkylene group having 1 to 4 carbon atoms, and R ₃ The washing | cleaning method of Claim 1 using the cleaning agent whose is a C1-C10 aliphatic alkylene group and n is an integer of 1-4. Detergent containing a compound (A) represented by the following general formula (I) heated at a temperature equal to or higher than the softening point of the moisture curable hot melt composition in a moisture curable hot melt composition supply device The cleaning method of the supply apparatus is made to release the cured product from the inner wall of the flow path by circulating the inside of the flow path of the moisture curable hot melt composition constituting the supply apparatus.

(In general formula (I), R ₁ and R ₅ are each independently an alkyl group, R ₂ , R ₃ and R ₄ are each independently an alkylene group, and n is an integer of 1 to 4.) The cleaning method according to any one of claims 1 to 3, wherein a heating temperature of the cleaning agent is in a range of 130 ° C to 150 ° C. It contains a compound (A) represented by the following general formula (I) heated at a temperature equal to or higher than the softening point of the moisture curable hot melt composition and a portion where the cured product of the moisture curable hot melt composition is fixed. The fixed cured product is removed from the site by contacting with the cleaning agent, and then a moisture curable hot melt composition is supplied, and the moisture curable hot melt composition in a heated and melted state is used as a base. Method to apply on the material.

(In general formula (I), R ₁ and R ₅ are each independently an alkyl group, R ₂ , R ₃ and R ₄ are each independently an alkylene group, and n is an integer of 1 to 4.) Cleaning comprising a moisture curable hot melt composition supply apparatus containing a compound (A) represented by the following general formula (I) heated at a temperature equal to or higher than a softening point of the moisture curable hot melt composition: Supplying the agent and circulating the inside of the flow path of the moisture curable hot melt composition constituting the supply device to release the cured product from the inner wall of the flow channel, and then supplying the cleaning agent to the supply device. The moisture curable hot melt composition is then supplied to the supply device, and the moisture curable hot melt composition in a heated and melted state is applied onto a substrate.

(In general formula (I), R ₁ and R ₅ are each independently an alkyl group, R ₂ , R ₃ and R ₄ are each independently an alkylene group, and n is an integer of 1 to 4.) Cleaning comprising a moisture curable hot melt composition supply apparatus containing a compound (A) represented by the following general formula (I) heated at a temperature equal to or higher than a softening point of the moisture curable hot melt composition: Supplying the agent and circulating the inside of the flow path of the moisture curable hot melt composition constituting the supply device to release the cured product from the inner wall of the flow channel, and then supplying the cleaning agent to the supply device. The moisture curable hot melt in a heated and melted state is then supplied to the supply device and filtered using a filter made of fired metal fibers having a filtration accuracy of 40 to 80 μm. A method of applying the composition onto a substrate.

(In general formula (I), R ₁ and R ₅ are each independently an alkyl group, R ₂ , R ₃ and R ₄ are each independently an alkylene group, and n is an integer of 1 to 4.)