JPH0489861A - One-pack grout composition - Google Patents

Abstract

PURPOSE:To obtain the title composition easy to fill or inject into cracks and gaps and improved in adhesiveness by mixing a polyether having terminal silyl ether groups, a curing catalyst, an organoalkoxysilane, a thixotropic agent, a filler, and a nonreactive diluent. CONSTITUTION:100 pts.wt. mixture comprising 100 pts.wt. polyether having terminal silyl ether groups, shown by the formula (wherein R is a 1-20C hydrocarbon group; X is alkoxy; (m)is 1 to 2; (n) is 1 to 300), 0.1-20 pts.wt. curing catalyst (e.g. tin octanoate), and 2-100 pts.wt. organoalkoxysilane is mixed with 0.1-200 pts.wt. thixotropic agent (e.g. hydrogenated castor oil), 0.1-200 pts.wt. filler (e.g. CaCO3), and a nonreactive diluent (e.g. dioctyl phthalate) in an amount of 0-200 pts.wt. based on 100 pts.wt. filler to give the title composition having a viscosity of 2,000 to 20,000 and a TI value of 3.0 or greater.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a one-component injection material composition used for repairing cracks, gaps, etc. occurring at joints in buildings, etc.

(Prior Art) Conventionally, as shown in FIGS. 1 and 2, sealant 4 filled in joints 1 between exterior wall members 3 of a building has been used.
When a gap 2a or a crack 2b occurs, the gap 2a and the crack 2b are repaired by the following three methods. In the figure, 3 is an outer wall member, and 13 is an uneven finishing coating material formed on the surface layer of the outer wall member 3.

The first method, as shown in FIG. 3, is to remove all the sealant 4 and backup material 5 from the joint 1 where the gap 2a has occurred. Next, after preparing the joint 1, as shown in FIG. 4, the method involves applying a primer 6 to the joint 1 and filling it with a new sealant 7 (refilling method). In the second method, as shown in Figure 5, after removing the cracked or peeled sealant,
Widen the joint (part A). After the joint is prepared, a primer 6 is applied to the widened joint and a new sealant 7 is filled (widening and refilling method). Furthermore, in the third method, first, the uneven finishing coating material 13 around the gap is cleaned. Next, a primer 6 is applied to this finishing coating material 13, and a bond breaker 8 is applied on this primer coating layer as shown in FIG.
Place and glue. Cover the bond breaker 8,
Furthermore, the gap 2a is covered with a sealant 9 so as to sufficiently adhere to the uneven finish coating material 13 (bridge method).

[Problem to be solved by the invention]

However, in the first refilling method among the above repair methods, the primer 6 used is compatible with both the wall surface forming the joint l, the sealant 4 remaining on the wall surface, and the sealant 7 to be filled. In many cases, the sealing material 7 has poor properties, and there is a problem in that the filled sealing material 7 peels off again, creating a gap. In addition, the second widening and refilling method widens the joints in the repaired area, which is a complicated work and impairs the aesthetic appearance of the building wall.

Furthermore, in the third bridge construction method, convex portions are formed by the sealing material 8 on the finishing coating material 13 of the building, so the aesthetic appearance of the building wall surface is greatly impaired.

Although it is possible to fill in the gaps and cracks using the conventional primer used in the above repair method, the above primer has a problem in workability.

That is, the primer has a low viscosity and drips from the injection part, making it impossible to actually use it.

This invention was made in view of the above circumstances, and it is possible to easily repair cracks and gaps that occur in joints, etc., and the filling injection work at that time is easy, and furthermore, it has excellent adhesive properties. The purpose of the present invention is to provide a liquid-type injection material composition.

[Means for Solving the Problem] In order to achieve the above object, the one-component injection material composition of the present invention contains the following components (A) to (C), (D) and (
A one-component injection material composition containing at least one of component E) as an essential component and component (F) as an optional component, having a viscosity of 2000 to 20000 cps and a TI value of 3.0.
The above configuration is adopted.

(A) Silyl ether group-terminated polyether.

(B) Curing catalyst.

(C) Organoalkoxysilane.

(D) Thixotropic agent.

(E) Filler.

(F) Non-reactive diluent.

[Effect]

That is, the present inventor has developed a liquid-type injection material composition that can be repaired by injecting and filling cracks and gaps in joints, has good injection-filling workability, and has excellent adhesive properties for injection-filling workability. I conducted a series of research to obtain this. As a result, a specific compound obtained by containing at least one of the above-mentioned silyl ether group-terminated polyether, curing catalyst, organoalkoxysilane, thixotropic agent, and filler as essential components, and adding a non-reactive diluent as an optional component. The present inventors have found that the desired objective can be achieved by using a composition having a viscosity and TI (thixotropic index) value within a range.

The one-component injection material composition of the present invention comprises a silyl ether group-terminated polyether (component A), a curing catalyst (component B),
An essential component consisting of an organoalkoxysilane (component C), one or both of a thixotropic agent (component D) and a filler (component E), and an optional non-reactive diluent (component F). It can be obtained using

The above silyl ether group-terminated polyether (component A) is
The base polymer of this liquid injection material composition includes, for example, a polymer having an alkoxysilyl group at the end and having the following structural formula in which the main chain is essentially a polyether.

Specifically, Kanejiki MS Polymer 15 manufactured by Kanebuchi Chemical Industry Co., Ltd.
A, Kaneki MS Polymer 20A, etc. are used. For example, in the Kaneka MS Polymer 20A, in the above structural formula, 1 to 2 methoxy groups are bonded to each silicon atom at both ends of the main chain.

In addition, the curing catalyst (component B), which is used as an essential component together with the above-mentioned silyl ether group-terminated polyether (component A), acts as a curing agent for the silyl ether group-terminated polyether (component A). , tin compounds such as tin octylate, dibutyltin dilaurate, dioctyltin maleate, diptyltin dioctoate, dibutyltin oxide, and dioctyltin oxide, titanate esters such as tetrabutoxytitanium and tetraisopropyloxytitanium, and amines. , used alone or in combination.

The amount of this curing catalyst (component B) is set within the range of 0.1 to 20 parts per 100 parts by weight (hereinafter abbreviated as "parts") of the silyl ether group-terminated polyether (component A). It is preferable to do so.

Next, the essential organoalkoxysilane (component C) used together with the silyl ether group-terminated polyether (component A) and the curing catalyst (component B) are as follows:
82NGHzC)IzCHzSi(OCH3)i.

HzNCHzCHJHCHzCHzCHzSi(OCH
:+)i.

CH3 HzNCHzCHzNHCHzCHzCHzSi (0
(Jh) 2(CJ sO) :+5iCH2CH2C
)I 2NHCHZCH2NHCH2CH2CH2S
i (QCzH9)3 and other amino group-substituted alkoxysilanes, CH2=CH5i (OCH) s , CH3C
H31(OCHzC)I3): 1st grade vinylsilane, CH3CHz=C-C-0(CHz)+5i(OCH:+)s
CH3 CHz=C-C-0-CHzCHz(JlzSi (O
CH2CH2OC)l:l) :+ etc. meta5i(OC
H:+)3. O Tesco rCflzCl(zSi(Q
C) an epoxysilane compound such as 13)i and H5
Examples include mercaptosilane compounds such as CHzCHzCHzSi (OCH3)3. These may be used alone or in combination.

By blending such organoalkoxysilane, the adhesiveness of the injection material composition is significantly improved, and it has strong adhesive strength not only to metals and stones, but also to plastics and wood. When a sealing material is used on the wall surface forming the joint, excellent adhesion is achieved on both the sealing material and the wall surface.

The amount of this organoalkoxysilane (component C) is:
The above silyl ether group-terminated polyether (component A) 10
It is preferable to set the ratio to 2 to 100 parts to 0 parts.

If the above-mentioned essential components (A-C components) are used alone, either the viscosity or drip resistance required for filling and injection will be lacking, so in addition to the above-mentioned A-C components, a thixotropic agent ( One or both of component D) and filler (component E) are used as essential components.

The thixotropic agent (component D) is hydrogenated castor oil.

Examples include amide wax, organic bentonite, and fumed silica. That is, when the viscosity of the obtained one-component injection material composition is low, by blending this thixotropic agent, the viscosity can be adjusted and dripping can be prevented.

In addition, the filler (E component) includes fine particulate materials such as calcium carbonate, kaolin talc, silica, aluminum silicate, zinc oxide, magnesium oxide, shirasu balloon, perlite, and plastic balloon, which may be used alone or in combination. used. These fillers not only act as fillers and thickeners, but also improve the modulus (tensile stress) after curing of the one-component injection composition of the present invention, increase the elongation rate, etc. Effects can be added.

The blending ratio of one or both of the thixotropic agent (component D) and the filler (component E) is preferably set within the range of 0.1 to 200 parts with respect to 100 parts of the AC components.

The optional non-reactive diluent (component F) used together with the above-mentioned essential components is the filler (
If component E) is used, the viscosity will be too high (20,000c).
ps may be exceeded.

Components used to suppress such high viscosity include, for example, phthalate esters such as dioctyl phthalate and butyl hensyl phthalate, chlorinated paraffin, epoxidized soybean oil, adipine, photoacid ester, and tricresyl≠- Examples include phosphoric acid esters such as sulfate, hensyl alcohol, and liquid petroleum resins, which may be used alone or in combination.

Among these, it is preferable to use one having a high boiling point and excellent compatibility with the silyl ether group-terminated polyether (component A), such as dioctyl phthalate.

The blending ratio of the above-mentioned optional non-reactive diluent (component F) is 0 to 200 parts per 100 parts of the filler (component E).
It is preferable to set it within the range of .

In addition to the above-mentioned essential and optional ingredients, the one-component injection material composition of the present invention may optionally contain colorants such as titanium oxide, carbon black, and pigments, anti-aging agents, ultraviolet absorbers, and antifoaming agents. Agents and the like may be added as appropriate.

The one-component injection composition of the present invention is produced, for example, as follows. That is, first, among the essential components, one or both of the silyl ether group-terminated polyether (component A), the thixotropic agent (component D), and the filler (component E) are mixed in a mixing container. Next, while heating the mixing container, the pressure inside the mixing container is reduced to dehydrate the mixture. After cooling, a curing catalyst (component B) and organoalkoxysilane (component C) are added thereto. At this time, if viscosity adjustment is necessary, it is produced by adding a non-reactive diluent (component F). The one-component injection material composition thus obtained is prepared in a substantially moisture-free state and then stored under sealed conditions. By storing in this way, the curing reaction of the composition does not proceed during the storage period, and by taking it out of the storage container and exposing it to the atmosphere,
By absorbing moisture in the atmosphere, the composition rapidly undergoes a curing reaction from the surface, becoming an elastic injection material.

The one-component injection material composition thus obtained must have a viscosity of 2,000 to 20,000 cps and a Tl value of 3.0 or more. That is, the viscosity is 2
If it is less than 000 cps fathom, liquid will drip, and on the contrary, if it is less than 20000 cps
When cps is exceeded, the extrudability of the injection material composition from the container filled with the injection material composition decreases, making it difficult to extrude the injection material composition from the container. Also, T
This is because if the l value is less than 3.0, liquid drips will occur if the viscosity is low. Note that the above Tl value is a value indicating the degree of resistance to dripping after application. The above viscosity was measured using a B-type rotational viscometer with a spindle of Nα3. This is a value obtained by measuring using Nα4 or Nα5, and the above Tl value is
This is the value obtained by dividing the viscosity at rpw+ by the viscosity at the rotational speed of 2 Orpm.

〔Effect of the invention〕

As described above, the one-component injection material composition of the present invention contains, as essential components, a silyl ether group-terminated polyether, a curing catalyst, an organoalkoxysilane, and one or both of a thixotropic agent and a filler. It has a viscosity within a specific range and is obtained by adding a non-reactive diluent as an optional component to the viscosity. Therefore, it can be easily injected into cracks (gap, fissures) generated at joints etc. using, for example, a syringe-like injector, and no liquid drips after injection. Moreover,
Good extrudability makes filling the injection material extremely easy.
It also has excellent adhesion to surrounding building components and various sealants. Therefore, cracks and the like can be repaired easily and quickly, and work efficiency is greatly improved.

Next, examples will be described together with comparative examples.

[Examples 1 to 5, Comparative Examples 1 to 5] The components shown in Table 1 below were mixed in the proportions shown in the table in a substantially moisture-free state to obtain - liquid injection material composition. I got something. In addition, the viscosity and Tl value of the above-mentioned liquid injection material composition were measured under the conditions shown above, and the results are also shown in the same table.

Using the one-component injection material compositions of Examples and Comparative Examples thus obtained, slump (sagging test),
An extrusion test and an adhesion test were conducted, and the results were summarized in the second section below.
Shown in the table. The slump, extrusion test and adhesion test were conducted as follows.

(Slump) Slate board (300m+X300++wnXthickness 5mm
) on top of the material (siding material, 300m+aX 5
0++oX thickness 12m1) 2 sheets with joint width 2.0 am
Then, stand the slate board so that the joints are vertical (up and down). In addition, a marked line should be drawn in advance at a location 50 m from the upper end of the joint. Next, a one-component injection material composition is injected into the gap up to 50 mm from the upper end of the joint using a syringe. Thirty minutes after injection and filling, the length (mm) of the liquid injection material composition hanging down from the above marked line was measured and evaluated. Note that the length of the injection material composition hanging down from the marked line is 0III1
1 is extremely good (◎), 1 to 31 II less than 11 is good (
○), less than 3 to 1 OIIn is slightly poor (△), 10iI
I11 or higher was judged as defective (×).

(Extrusion test) A syringe with a nozzle (needle) tip with an inner diameter of 1.8 mm and a capacity of 15 d is filled with a one-component injection material composition without entraining air, and the cylinder of the syringe is pushed to an inner volume of 10 mm. . Next, add 1 kgf/c-ffl to the above cylinder.
The time (seconds) required to extrude almost the entire amount of the one-component injection material composition in the syringe was measured and evaluated. It should be noted that the time required for extrusion of less than 15 seconds is considered extremely good (
◎), 15 seconds to less than 30 seconds is good (○), 30 seconds to less than 45 seconds is slightly poor (Δ), 45 seconds or more is poor (×)
And so.

(Adhesion test) Two members 10 as shown in FIGS. 7(A) and (B)
(Siding material, 50mm x 50mm x thickness 12mm)
Various sealants 11 (conforming to JIS A 5758) were filled in between so that the filling width was 10 mm, and after curing at 20°C4 relative humidity 60% for 14 days, the material was further cured at 30°C2 relative humidity 60%. It was cured for 14 days. Next, the interface between the member 10 and the sealant 11 was cut off using a cutter knife, so that the gap was 1 mm. Then, fill this gap with a one-component injection material composition.
A test specimen was prepared by curing for one day. This test specimen is called the Kiguchi test specimen. Further, as shown in FIGS. 8(A) and 8(B), after cutting off the central part of the sealing material 11 with a cutter knife so that the gap becomes III+,
The gap is filled with a one-component injection material composition (shaded area B),
A test specimen was prepared by curing at 20°C1 relative temperature 60% for 14 days. This specimen is called the central specimen. Furthermore, this central test specimen was used as a sunshine weather meter (WOM).
) for 500 hours. This is called a WOM test specimen. The above three types of test specimens (wood test specimen 7 central test specimen, WOM specimen) prepared in this manner were subjected to a tensile tester (manufactured by Orientic Co., Ltd., RTM-250) to examine the fracture state of each specimen. Ta. There are two types of failure states: CF (cohesive failure) where the liquid volume injection material composition or sealant has cohesive failure;
), and those with peeling between the liquid injection material composition and the component or the one-component injection material composition and the sealant were evaluated as 711. F
Re) was evaluated as poor adhesion and rated as 7.

(The following is a blank space) From the results in Table 2 above, Comparative Example 1 had extremely good extrudability, but had a large slump of 5, which was somewhat poor. In other words, a large slump means that when a composition is injected into a crack, not only will the composition sag, impairing the design, but also the injection material will be insufficient in some areas, making it impossible to repair the waterproof function.

Comparative Example 2 also had a slump of 131 m, which was extremely poor. Comparative Example 3 had a very good slump of 0, but the extrudability was poor at 32 seconds, which caused problems in workability. In addition, the adhesive property is also poor. Comparative Example 4 was also very good with zero slump, but the extrusion property was 64 seconds, which was extremely poor like Comparative Example 3. Furthermore, although the extrudability of Comparative Example 5 was good, the slump was 4, which was somewhat poor.

On the other hand, the example products had good slump and extrudability, and were also excellent in adhesive properties.

[Brief explanation of drawings]

Figure 1 is a cross-sectional view of a wall showing peeling that occurred at the joints of a building, Figure 2 is a cross-sectional view of a wall showing cracks that occurred at joints of a building, and Figure 3 is a view of the building before repair. Figure 4 is a cross-sectional view of the joints of a building repaired using the refilling method. Figure 5 is a cross-sectional view of the joints of a building repaired using the widening refilling method. The figure is a cross-sectional view showing the joints of a building repaired using the bridge construction method.
Figure (A) is a plan view showing the end test piece used for the adhesion test, Figure 7 (B) is its front view, Figure 8 (A) is a plan view showing the center test piece used for the adhesion test, FIG. 8(B) is its front view. Patent applicant Kanebo NSC Co., Ltd. Agent
Patent Attorney Yukihiko Nishifuji Figure 1 Figure 2 Figure 7 (A) 7th ft! 11 (8) Figure 5 Figure 8 (8)

Claims (1)

[Claims] (1) The following components (A) to (C), (D) and (E
A one-component injection material composition containing at least one of component (F) as an essential component and component (F) as an optional component, with a viscosity of 2,000 to 20,000 cps and a TI value of 3.0 or more. Characteristic one-component injection material composition. (A) Silyl ether group-terminated polyether. (B) Curing catalyst. (C) Organoalkoxysilane. (D) Thixotropic agent. (E) Filler. (F) Non-reactive diluent.