JPH06298968A - Method for removing gel substances - Google Patents

Abstract

PURPOSE:To perform efficient and complete removal of gels from jigs or the like for plastic lens by dipping the bodies the gels stick to in a surfactant, then in an alkali solution. CONSTITUTION:Plastics, glass or metal bodies which gels or cross-linked by- products such as organosilicon compound of the formula (R<1>, R<2> are alkyl, alkenyl, aryl, halogen; R<3> is 1-8C alkyl, alkoxyalkyl, acyl, phenyl; a, b are 0, 1) and/or its hydrolyzate are soaked in an anionic or other surfactant solution 11, then in an alkaline solution such as a sodium hydroxide solution 12.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for removing an unnecessary hardened material adhered to an object.

[0002]

2. Description of the Related Art The process of coating a surface of an object with a curable substance to improve its functionality and performance has been performed for a long time.

Among them, an optical member made of a synthetic resin such as a plastic lens has many advantages such as light weight and easy workability, but has drawbacks such as being easily scratched. Therefore, these advantages are used to cover the drawbacks. Therefore, in order to achieve higher performance, it is indispensable to perform a surface treatment for forming a cured film or vapor deposition film of an organic compound on the surface.

However, when such a surface treatment is performed,
The jig that holds the object to be treated cannot avoid adhesion of the cured product such as the cured film or vapor deposition film at the same time as the held object. Removing the cured product has become an important issue.

Conventionally, as a method of removing such a cured product, a method of immersing an object to which the cured product adheres in an aqueous alkaline solution, as disclosed in JP-A-62-117668, or JP-A-62. There is known a method of immersing in an alkaline aqueous solution containing a surfactant as disclosed in JP-A-149380.

[0006]

However, the method of immersing in an alkaline aqueous solution, which is disclosed in JP-A-62-117668, is disclosed in JP-A-62-149380. It has a defect that the curing to remove is low and it takes a long time to completely remove it.

Further, the method of immersing in an alkaline aqueous solution containing a surfactant, which is disclosed in Japanese Patent Laid-Open No. 62-149380, removes more than the case of using only the alkaline aqueous solution. It is highly effective and has the advantage that the cured product can be completely removed in a short time. However, according to the experiments by the present inventor, this method efficiently and completely removes a cured product in a short time in the case of an object having a relatively simple outer shape such as a plastic lens that does not have extreme irregularities. However, like the holding jig used for surface treatment of plastic lenses as shown in Fig. 1,
It has been found that in the case of an object having a complicated outer shape having an extremely bent portion or a joint portion, the cured product adhered to the recessed portion of the bent portion or the gap between the joint portions cannot be completely removed. .

The present invention is intended to solve such a problem, and its purpose is to adhere to an object in order to effectively use resources, reduce cost, and achieve high quality and high yield. It is to provide a method for efficiently and completely removing unnecessary cured products.

[0009]

The method for removing a cured product according to the present invention is characterized in that an object to which a cured product adheres is dipped in a surfactant solution and then dipped in an alkaline solution.

The cured product has at least the following A and B:
It is characterized by including a cured film formed by curing a composition comprising the components.

A An organosilicon compound represented by the following general formula (1) and / or a hydrolyzate thereof.

R ¹ _a R ² _b Si (OR ³ ) _4-ab (1) (wherein R ¹ and R ² are each an alkyl group, an alkenyl group, an aryl group, or a halogen group, Glycidoxy group,
A hydrocarbon group having an epoxy group, an amino group, a mercapto group, a methacryloxy group or a cyano group, R ³ is an alkyl group having 1 to 8 carbon atoms, an alkoxyalkyl group, an acyl group, a phenyl group, an allylalkyl group, a and b
Is 0 or 1.)

B Curable organic compound.

A typical representative example of the organosilicon compound represented by the general formula (1) is methyl silicate,
Ethyl silicate, n-propyl silicate, i-propyl silicate, n-butyl silicate, sec-butyl silicate, t-butyl silicate, tetraacetoxysilane, methyltrimethoxysilane, methyltriethoxysilane, methyltrimethoxyethoxysilane, methyltri Acetoxysilane, methyltributoxysilane, methyltripropoxysilane, methyltriamyloxysilane,
Methyltriphenoxysilane, methyltribenzyloxysilane, methyltriphenethyloxysilane, glycidoxymethyltrimethoxysilane, glycidoxymethyltriethoxysilane, α-glycidoxyethyltrimethoxysilane, α-glycidoxyethyltri Ethoxysilane, β-glycidoxyethyltrimethoxysilane, β-
Glycidoxyethyltriethoxysilane, α-glycidoxypropyltrimethoxysilane, α-glycidoxypropyltriethoxysilane, β-glycidoxypropyltrimethoxysilane, β-glycidoxypropyltriethoxysilane, γ- Glycidoxypropyltrimethoxysilane, γ-glycidoxypropyltriethoxysilane, γ-glycidoxypropyltripropoxysilane,
γ-glycidoxypropyltributoxysilane, γ-glycidoxypropyltrimethoxyethoxysilane, γ-
Glycidoxypropyltriphenoxysilane, α-glycidoxybutyltrimethoxysilane, α-glycidoxybutyltriethoxysilane, β-glycidoxybutyltrimethoxysilane, β-glycidoxybutyltriethoxysilane, γ- Glycidoxybutyltrimethoxysilane, γ-glycidoxybutyltriethoxysilane, δ-
Glycidoxybutyltrimethoxysilane, δ-glycidoxybutyltriethoxysilane, (3,4-epoxycyclohexyl) methyltrimethoxysilane, (3,4-
Epoxycyclohexyl) methyltriethoxysilane,
β- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, β- (3,4-epoxycyclohexyl) ethyltriethoxysilane, β- (3,4-epoxycyclohexyl) ethyltripropoxysilane, β-
(3,4-Epoxycyclohexyl) ethyltributoxysilane, β- (3,4-epoxycyclohexyl) ethyltrimethoxyethoxysilane, β- (3,4-epoxycyclohexyl) ethyltriphenoxysilane, γ
-(3,4-epoxycyclohexyl) propyltrimethoxysilane, γ- (3,4-epoxycyclohexyl) propyltriethoxysilane, δ- (3,4-epoxycyclohexyl) propyltrimethoxysilane, δ
-(3,4-epoxycyclohexyl) propyltriethoxysilane, glycidoxymethylmethyldimethoxysilane, glycidoxymethylmethyldiethoxysilane, α
-Glycidoxyethylmethyldimethoxysilane, α-glycidoxyethylmethyldiethoxysilane, β-glycidoxyethylmethyldimethoxysilane, β-glycidoxyethylmethyldiethoxysilane, α-glycidoxypropylmethyldimethoxysilane , Α-glycidoxypropylmethyldiethoxysilane, β-glycidoxypropylmethyldiethoxysilane, γ-glycidoxypropylmethyldimethoxysilane, γ-glycidoxypropylmethyldiethoxysilane, γ-glycidoxypropyl Methyldipropoxysilane, γ-glycidoxypropylmethyldibutoxysilane, γ-glycidoxypropylmethyldimethoxyethoxysilane, γ-glycidoxypropylmethyldiphenoxysilane, γ-glycidoxypropylethyldimethoxysilane, γ -Glycidoxypropylethyldiethoxysilane, γ-glycidoxypropylvinyldimethoxysilane, γ-glycidoxypropylvinyldiethoxysilane, γ-glycidoxypropylphenyldimethoxysilane, γ-glycidoxypropylphenyldiethoxysilane Silane, ethyltrimethoxysilane, ethyltriethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltriacetoxysilane,
Vinyltrimethoxyethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, phenyltriacetoxysilane, γ-chloropropyltrimethoxysilane, γ-chloropropyltriethoxysilane, γ-
Chloropropyltriacetoxysilane, 3,3,3-chloropropyltrimethoxysilane, γ-methacryloxypropyltrimethoxysilane, γ-mercaptopropyltrimethoxysilane, γ-mercaptopropyltriethoxysilane, β-cyanoethyltriethoxysilane,
Chloromethyltrimethoxysilane, chlorotrimethyltriethoxysilane, N- (β-aminoethyl) γ-aminopropyltrimethoxysilane, N- (β-aminoethyl) γ-aminopropylmethyldimethoxysilane, γ-
Aminopropyltrimethoxysilane, γ-aminopropylmethyldimethoxysilane, N- (β-aminoethyl)
γ-aminopropyltriethoxysilane, N- (β-aminoethyl) γ-aminopropylmethyldiethoxysilane, dimethyldimethoxysilane, phenylmethyldimethoxysilane, dimethyldiethoxysilane, phenylmethyldiethoxysilane, γ-chloropropylmethyl Dimethoxysilane, γ-chloropropylmethyldiethoxysilane, dimethyldiacetoxysilane, γ-methacryloxypropylmethyldimethoxysilane, γ-methacryloxypropylmethyldiethoxysilane, γ-mercaptopropylmethyldimethoxysilane, γ-mercaptopropylmethyldi Examples thereof include ethoxysilane, methylvinyldimethoxysilane, and methylvinyldiethoxysilane.

These organosilicon compounds may be used alone or in combination of two or more.

As the curable organic compound as the component B, bisphenol A type epoxy resin, bisphenol F type epoxy resin, aliphatic epoxy resin, brominated epoxy resin, glycidyl ester type epoxy resin, shrimp bis type epoxy resin, phthal There is no particular limitation as long as it is curable, such as epoxy resin such as acid glycidyl ester type epoxy resin, polyvinyl butyral, polyvinyl alcohol, celluloses, melamine resin, acrylic resin, polyurethane resin and the like.

In addition, there is no problem even if finely divided inorganic substances, which are commonly used for the purpose of improving the surface hardness, are added to the cured film. Here, the fine particle inorganic material has an average particle diameter of about 1 to 300 mμ, preferably 5
Examples include fine particles of metal oxides such as silicon, aluminum, titanium, zirconium, antimony, cerium, and tin having a particle size of ˜100 mμ.

Various curing catalysts can be used for these cured coatings for the purpose of accelerating the curing, curing at a low temperature and the like when forming the coatings. The curing catalyst used is experimentally determined according to the composition of the cured film, the film thickness, the curing conditions, the type of object forming the cured film, and the like.

The method for coating the effect coating on the object is not particularly limited, but usually in a liquid composition which is a precursor of a cured product,
It is carried out by immersing the object held in a suitable holding jig and then heating and hardening it.

On the other hand, the surfactant solution in the present invention is preferably an aqueous solution in which one or more of anionic, nonionic and cationic surfactants are dissolved.
The concentration of the surfactant is 0.1 to 0.1 in terms of treatment effect.
The range of 10 wt% is preferable.

Specific examples of the alkaline solution include lithium hydroxide, sodium hydroxide, potassium hydroxide, calcium hydroxide and ammonia. The type of the alkaline solution should be experimentally determined according to the composition of the effect coating, the film thickness, and the type of the object, but an alkali metal hydroxide salt is particularly preferable from the viewpoint of the strength of the alkali, the odor, and the like. Further, the concentration of the alkaline solution is preferably in the range of 2 to 40 wt% from the viewpoint of shortening the processing time, extending the life of the solution, and the like.

Further, the dipping time and the dipping temperature of each solution should be determined experimentally, but both are usually carried out for 1 minute to 3 hours in the range of 20 ° C to 90 ° C. At the same time, ultrasonic vibration may be applied to shorten the immersion time.

INDUSTRIAL APPLICABILITY The present invention is applied to an object having a complicated outer shape such as a holding jig used for holding a hard coat cured film on an optical lens, particularly a plastic spectacle lens. When it is applied to the removal of a cured product, a remarkable effect can be obtained, but it is not particularly limited to this. For example, when reproducing an optical lens having a mistake in the coating process of a hard coat or an antireflection film. , Is similarly applicable for the purpose of removing unnecessary cured products from an object.

[0024]

According to the present invention, by first immersing an object in a surfactant solution, the surfactant solution is sufficiently permeated to the extreme bends on the surface of the object or the gaps between the joints, The wettability of the cured product on the surface is improved. After that, by immersing it in an alkaline solution, the contact and reaction between the alkaline solution and the cured product are promoted, and the cured product is chemically dissolved.
The action and effect of the alkaline solution to be removed is improved. In addition, since the surface property of the object is improved by the surfactant, it is possible to easily and sufficiently penetrate into extremely small bends and small gaps in the joint that cannot be penetrated only with an alkaline solution, and the complicated external shape Even in the case of an object having the above, the cured product can be effectively removed.

In this case, the application of ultrasonic vibration during the immersion of the object is extremely effective in order to make the penetration of the surfactant solution and the alkaline solution into the details of the object more sufficient.

[0026]

EXAMPLES The present invention will now be described in detail based on examples, but the present invention is not limited thereto.

(Example 1) Preparation of hard coat liquid: 219 parts by weight of γ-glycidoxypropyritrimethoxysilane, isopropanol-dispersed koidal silica (Catalyst Chemical Co., Ltd., trade name "OSC")
AL-1432 ") 111 parts by weight and isopropanol 491 parts by weight were added dropwise to 60 parts by weight of 0.05N hydrochloric acid to carry out hydrolysis.
After aging at 24 ° C. for 24 hours, 112 parts by weight of propylene glycol diglycidyl ether (manufactured by Nagase & Co., Ltd., trade name “Denacol EX911”) and 7 parts by weight of magnesium perchlorate were added and stirred to homogenize. The flow control agent L-7604 was added to this to prepare a hard coat solution.

A plastic lens 1 made of diethylene glycol bis (allyl carbonate) held by a holding jig as shown in FIG. 1 is dipped in the hard coating solution thus prepared and gradually pulled up at a speed of 250 mm / min. While being held by the holding jig, it was heated and cured at 70 ° C. for 180 minutes.

In FIG. 1, reference numerals 2 and 5 represent the framework of the holding jig, and the plastic lens 1 is fixed by the lower fixed blade 3 and the side fixed blade 4 as shown in FIG. Also,
2 is a partially enlarged cross-sectional view of FIG. 1. As shown in FIG. 2, the lower fixed wing 3 (similarly to the side fixed wing 4 although not shown) has a wedge-shaped concave portion at the tip end thereof so that the plastic lens 1
Holding

By the above process, the hard coat hardened film adhered to the entire surface of the holding jig was removed by the method shown in FIG.

In FIG. 3, a surfactant tank (first tank)
11 is a nonionic surfactant (Yuken Industry Co., Ltd.)
Manufactured by the company, "Alnion L-61") containing a 1 wt% aqueous solution, and the alkaline solution tank (second tank) 12 contains 5
Contains a wt% KOH aqueous solution. Both tanks are equipped with an ultrasonic oscillator 10 and a heating device 13. The holding jig 6 to which the hard coat hardened film is attached is first dipped in the first tank 11 and subjected to ultrasonic vibration at 45 ° C. for 2 minutes and then pulled up, and then dipped in the second tank 12 and at 60 ° C. for 10 minutes. Ultrasonic vibration was applied for a minute and then pulled up.

No cured product adhered to the obtained holding jig, and it was clean enough to be used for coating and curing a hard coat on another plastic lens as it is.

(Embodiment 2) A holding jig to which a cured product is attached by the same process as in Embodiment 1 is used in the same manner as in FIG. 3 of Embodiment 1, except that the surfactant in the first tank 11 is used. Nonionic surfactant (manufactured by Pretec Co., Ltd., trade name)
The cured product was removed under the same conditions except that # PS-19 ″) was used.

No cured product was attached to the obtained holding jig, and it was clean enough to be used for coating and curing a hard coat on another plastic lens as it is.

(Embodiment 3) A holding jig to which a cured product is attached by the same process as in Embodiment 1 is used in the same manner as in FIG. 3 of Embodiment 1, except that the surfactant in the first tank 11 is used. The cured product was removed under the same conditions, except that the nonionic-anionic surfactant (trade name “CLEAN ACE”, sold by Inei Morieido) was used.

No cured product adhered to the obtained holding jig, and it was clean enough to be used for coating and curing a hard coat on another plastic lens as it is.

(Embodiment 4) A holding jig to which a cured product is attached by the same process as in Embodiment 1 is used in the same manner as in FIG. 3 of Embodiment 1, except that the alkali solution in the second tank 12 is 10 wt. The cured product was removed under the same conditions except that the aqueous NaOH solution was replaced.

No cured product was attached to the obtained holding jig, and it was clean enough to be used for coating and curing a hard coat on another plastic lens as it is.

(Comparative Example 1) A holding jig having a cured product adhered thereto by the same process as in Example 1 was used as a nonionic surfactant (Yuken Kogyo KK, trade name "Arnion L-6").
1 ″) was immersed in a 5 wt% KOH aqueous solution containing 1 wt% and ultrasonic vibration was applied at 60 ° C. for 10 minutes.

Although most of the hardened material adhered to the obtained holding jig was removed, the bottom fixed portion 3 of the lower fixing blade 3 and the side fixing blade 4 and the holding treatment as shown in FIG. The cured product remained on the joints with the skeletons 2 and 5 of the ingredient and could not be used as it was.

[0041]

As described above, according to the present invention, an article to which a cured product is attached is dipped in a surfactant solution and then immersed in an alkaline solution to efficiently and completely remove the cured article attached to the object. Can be removed. Therefore, it is possible to completely clean objects such as expensive and complicated jigs that are repeatedly used, so that high quality and high yield can be realized, effective use of resources and cost reduction are possible. Has the effect.

[Brief description of drawings]

FIG. 1 is a front view showing an example of a plastic lens holding jig according to the present invention.

2 is a partially enlarged sectional view of FIG.

FIG. 3 is a configuration diagram showing an example of a cured product removing method according to the present invention.

[Explanation of symbols]

 1 plastic lens 2 skeleton of holding jig 3 lower fixed wing 4 side fixed wing 5 skeleton of holding jig 6 holding jig 10 ultrasonic oscillator 11 surfactant tank (first tank) 12 alkaline solution tank (second Tank) 13 heating device

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁵ Identification code Office reference number FI technical display area // B29K 83:00

Claims (6)

[Claims] 1. A method for removing a cured product, which comprises immersing an object to which a cured product is attached in a surfactant solution and then immersing it in an alkaline solution. 2. The cured product removing method according to claim 1, wherein the cured product comprises a cured coating film obtained by curing a composition comprising at least the following components A and B. A An organosilicon compound represented by the following general formula (1) and / or a hydrolyzate thereof. R ¹ _a R ² _b Si (OR ³ ) _4-ab ... (1) (wherein R ¹ and R ² are each an alkyl group, an alkenyl group, an aryl group, or a halogen group, a glycidoxy group,
A hydrocarbon group having an epoxy group, an amino group, a mercapto group, a methacryloxy group or a cyano group, R ³ is an alkyl group having 1 to 8 carbon atoms, an alkoxyalkyl group, an acyl group, a phenyl group, an allylalkyl group, a and b
Is 0 or 1.) B Curable organic compound. 3. The method for removing a cured product according to claim 1, wherein the alkaline solution is an aqueous solution of an alkali metal hydroxide. 4. The method for removing a cured product according to claim 1, wherein the object is plastic, glass or metal. 5. The cured product removing method according to claim 4, wherein the object is a holding jig for holding the optical member during surface treatment of the optical member. 6. The method for removing a cured product according to claim 1, wherein the method is immersed in a surfactant solution and / or an alkaline solution while applying ultrasonic vibration.