JPS60252657A - Easily-flowable moisture-curing one-pack resin composition - Google Patents

Abstract

PURPOSE:To obtain the titled composition storable for a long period causing little variation of fluidity and thixotropy, and applicable easily by extrusion, coating, etc. without causing sagging, by compounding a moisture-curing one-pack type resin with a specific surface-treated precipitated calcium carbonate filler and a liquid softener. CONSTITUTION:(A) 100pts.(wt.) of a moisture-curing one-pack type resin such as polyurethane resin, modified silicone resin, polysulfide resin, etc. is mixed with (B) 10-300pts. of a surface-treated precipitated calcium carbonate filler having an adsorbed moisture content of <=0.3% measured by the Karl Fischer method after drying at 105 deg.C for 2hr, and obtained by adding a drier to an aqueous suspension of precipitated calcium carbonate having a specific surface area of 5-40m<2>/g (by BET process) and prepared by chemical reaction in an aqueous phase before, during or after the surface-treatment of the calcium carbonate, and dehydrating, drying and pulverizing the suspension, and (C) 1-100pts. of a liquid softener such as ethyl acetate, acetone, xylene, etc. The mixing is carried out preferably by mixing the component A uniformly with the component C, and mixing the component B to the mixture.

Description

DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to free-flowing moisture-curing-forming resin compositions. More specifically, the present invention relates to a free-flowing moisture-curing-forming resin composition containing a surface-treated precipitated calcium carbonate filler having a BET specific surface area of 5 to 40 and an adsorbed moisture of 0.3 cm or less and a liquid softener.

"Prior Art" Conventional air-curing one-component resin compositions are widely used in civil engineering and construction sealants, flooring materials, waterproofing materials, adhesives, and the like.

Currently, polyurethane, modified silicone, polysulfide 9, silicone resin, and the like are used as base materials for moisture-curable original resin compositions. These resins are also used in 2-deep type resin compositions, but in the case of 2-deep type resin compositions, it is necessary to mix the two liquid components during construction.
It was damaged in handling.

There was a dark side.

One-component resin compositions are stored in sealed containers such as cartridges, polyvinyl chloride film packs, and cans, so there is no need to mix them during application, making the application process convenient and preferred in various fields. Its usage is increasing year by year.

These original resin compositions are particularly sensitive.

It is required that properties such as slump properties and dischargeability from a caulking gun or tube be excellent even after long-term storage. The fillers currently used in deep mold resin compositions are a combination of a thixotropic agent such as silicic anhydride and a so-called extender such as coarse dry cal, talc, or clay.

However, when silicic anhydride is used, the chicken and slump properties are improved, but it is difficult to adjust the viscosity, tends to become high, and has the disadvantage of poor extrusion flow from a corking gun or tube. There is a strong desire to eliminate such drawbacks.

"Structure of the Invention" The present invention is a moisture-curing deep-type resin (A), which has a BET specific surface area of 5 to 404 mm and has a Karl Fischer adsorbed moisture of 0.3% or less after drying at 105°C for 2 hours. The present invention provides a free-flowing, moisture-curing, deep resin composition comprising a surface-treated precipitated calcium carbonate filler (B) and a liquid softener (C).

The free-flowing, moisture-curing, deep resin composition of the present invention shows little change in fluidity and thixotropy during long-term storage, is easy to extrude and apply, and is easy to apply on inclined or vertical surfaces. does not occur.

The moisture-curable deep resin which is component (A) of the resin composition of the present invention is a combination of known organic diisocyanates 9 such as aliphatic diincyanates, araliphatic diisocyanates, alicyclic diisocyanates, aromatic diisocyanates and active hydrogen compounds 8 For example, a low molecular weight polyol with a molecular weight of 62 to 300, a low molecular weight polyamine with a molecular weight of 34 to 300, an alkanolamine with a molecular weight of 60 to 300, water, formic acid,
Polyurethane resin obtained by a known reaction with glycolic acid, modified silicone resin which is a polymer whose main chain is polyoxyalkylene and has an alkoxyl group at the end, and bis(ethyleneoxymethane) whose main chain contains a disulfide bond. Polysulfide resins are so-called polyalkylene polysulfides with reactive mercapto groups at the ends, and are represented by the general formula % (R = divalent aliphatic group whose carbon chain is interrupted by an oxygen atom). The main chain is diorganopolysiloxy with a hydroxyl group at the end, and the curing reaction mechanism expressed by the general formula is acetic acid type and oxime type.

This resin is commonly used as a base material for moisture-curable deep resin compositions such as alcohol-type, amine-type, and asibi-type silicone resins.

5 to 40 m/gO, which is a component of the resin composition of the present invention
A surface-treated precipitated calcium carbonate filler having a BET specific surface area and having a Karl Fischer adsorbed water content of 0.3% or less after drying at 105 DEG C. for 2 hours is described in detail in Japanese Patent Application No. 1983-17-21. This surface-treated precipitated calcium carbonate filler is obtained by adding a dryer to a precipitated calcium carbonate aqueous suspension having a BET specific surface area of 5 to 40 m/9 obtained by chemical reaction in an aqueous system before, during or after surface treatment. It is produced by dehydrating, drying, and powdering.

Examples of the liquid softener which is component (C) of the resin composition of the present invention include esters such as ethyl acetate and butyl acetate, ketones such as acetone and methyl ethyl ketone, and aromatic hydrocarbons such as toluene, xylene, and honey. , n-hexane, n-octane, and other aliphatic hydrocarbons, dinotyl phthalate, :) normal butyl phthalate, :) octyl phthalate, t(2-ethylhexyl) phthalate, butylbenzyl 7-thaleate, etc. 7-talic acid esters, di(2-ethylhexyl) adipate
Phthalate, sebacic acid: Aliphatic dibasic acid esters such as (2-ethylhexyl) phthalate.

Phosphate triesters, cricose esters.

Known plasticizers such as epoxy compounds and chlorinated paraffins are used.

The free-flowing, moisture-curing, deep-curing resin composition of the present invention is characterized by the above-mentioned (A
), (B) and (C) are uniformly mixed. Although the mixing order is not particularly limited, it is usually preferable to uniformly mix component (A) with component C), and then mix component (B) into the mixture.

The mixer can be a commonly used mixer such as a Niegoo, Preguu like a planetary mixer or Peicitrol.

The blending ratio of components (A), (B) and (C) is:

A: 100 parts by weight B: 10 to 300 parts by weight and C: 1 to too parts by weight.

If the amount of component (B) is less than 10 parts by weight, the resulting composition will have poor slump properties, and if it exceeds 300 parts by weight, extrudability will decrease.
It is preferably 10 to 300 parts by weight. (C)
The amounts of the components are not particularly limited and can be selected within the range of 1 to 100 parts by weight so as to obtain a resin composition with an appropriate viscosity.

The free-flowing moisture-curing liquid resin composition of the present invention may further contain a thixotropic agent, a dehydrating agent, a pigment, an adhesion promoter, and the like.

Next, in order to further clarify the features of the present invention, examples will be described.

Example 1 A free-flowing moisture-curable liquid resin composition was prepared by mixing each component in the following composition.

Composition Parts by weight Polyurethane resin 100 DOP 60 Xylene 10 Surface treated precipitated calcium carbonate filler 100 A planetary mixer was used for mixing, and first the polyurethane resin (amine equivalent 2700; Neo content 1.6 H), DOP and xylene were mixed in a planetary mixer. - A resin composition was obtained by mixing in a mixer and then adding and mixing a calcium carbonate filler.The composition thus obtained was stored at 60°C for 4 days and then its extrudability and slump property were tested. The results are shown in Table 1.

The surface-treated precipitated calcium carbonate filler used in Example 1 was prepared as follows: While stirring a precipitated calcium carbonate aqueous suspension having a BET specific surface area of 36 at a concentration of 10% by weight and a temperature of 25°C. , aluminum sulfate aqueous solution 3 with a concentration of 10% by weight
Then, 8 ml of an aqueous solution of sodium oleate having a concentration of 10% by weight and a temperature of 90° C. was added, and the mixture was further stirred for 15 minutes. This calcium carbonate suspension was press-dehydrated, dried and pulverized to give about 10 kg.

Comparative Examples 1, 2 and 3 (B) In place of the surface-treated precipitated calcium carbonate filler according to the present invention, heavy charcoal calcium (trade name: Whiten P-
30, manufactured by Toyo Fine Chemical Co., Ltd.; Comparative Example 1), talc (trade name: Crown Talc SC1, manufactured by Matsumura Sangyo Co., Ltd.; Comparative Example 2), and silicic anhydride (trade name: Aerosil 2001, manufactured by Nippon Aerosil Co., Ltd.; Comparative Example 3). A resin composition was obtained in the same manner as in Example 1 except that the same amount was used. In addition, in Comparative Examples 2 and 3, 6 parts by weight of silicic anhydride was added to each. The test results of the obtained composition are shown in Table 1.

Example 2 A resin composition was obtained in the same manner as in Example 1, except that 30 parts of the surface-treated precipitated calcium carbonate filler of the present invention was used as component (B). The test results for this composition are shown in Table 1.

Comparative Examples 4 and 5 (B) 8 parts by weight (Comparative Example 4) and 350 parts by weight (
Comparative Example 5) A resin composition was obtained in the same manner as in Example 1 except for using the following. The test results for these compositions are shown in Table 1.

Example 3 A free-flowing moisture-curing liquid-type side fat composition was prepared by mixing each component in the following composition.

Modified silicone resin 1100-D OP 25 Surface treated precipitated calcium carbonate filler 100% Product name:
Kaneka MS Polymer 2OA, manufactured by Kanekabuchi Chemical Industry Co., Ltd.

The test results of the obtained monofat composition are shown in Table 1.

Comparative Examples 6 and 7 However, commercially available precipitated calcium carbonate (Comparative Example 6) and heavy carbonate calcium (Comparative Example 7) were used as ingredients instead of the surface-treated precipitated carbonate carbonate filler of the present invention, and the other components were as in Example A resin composition was obtained in the same manner as in Example 3. In Comparative Example 7, 5 parts by weight of silicic anhydride was also added. The test results of the obtained composition are shown in Table 1.

Slump C◎ ○ ◎ × ○ ○ × ◎ Go to Ch.
○* Test method for “building sealant” JIS A 5
758, the extrudability of the resin composition was evaluated by the discharge amount. Measurement temperature: 25°C.

※※ Evaluation of slump property is as follows: ◎Very good, ○Good, △Slightly poor, X poor. - "Effects of the Invention" From the results in Table 1, it is clear that the resin composition according to the present invention has excellent extrudability and slump properties even after being stored at 60° C. for 4 days.

On the other hand, it can be seen that the comparative examples only satisfy either extrudability or slump properties, and are poor in practical use.

(3 others) Procedural Amendment July 1980 Mr. Commissioner of the Patent Office (Mr. Patent Office Examiner) 1. Indication of the case 1982 Patent Application No. 108647 2. Name of the invention Easy-flowing moisture curing - Deep Resin Composition 3, Relationship with the Amended Person's Case Name of Patent Applicant Shiroishi Chuo Research Institute Co., Ltd. Kasumigaseki Building Post Office P.O. Box No. 49 Eiko Patent Office Telephone (581)-9601 (Representative) Statement of Specification The column "Detailed Description of the Invention" shall be amended as follows.

0 On page 6, line 7 of the specification bundle, "Corking" is corrected to "Caulking".

0 On page 4, line 1 of the specification, "who" is corrected to "who".

O In the second line from the bottom of page 4 of the specification, “interrupted” is replaced with “
It may be interrupted.''

O In the 7th negative line of the specification, "Basitrol" is corrected to "Paintroll".

Page 4 of the O specification, lines 8 to 17, “(B) Component...
......The test results are shown in Table 1. ” to “(B
) As a substitute for the surface-treated precipitated calcium carbonate filler according to the present invention, commercially available precipitated calcium carbonate (trade name: Hakuenka DD, Shiroishi Kogyo Membrane; Comparative Example 1) heavy calcium carbonate (part name: Whiten P -60, manufactured by Toyo Fine Chemical Co., Ltd.; Comparative Example 2), and Merck (trade name: Crown Talc SC1, manufactured by Matsumura Sanraisha; Comparative Example 6) were used,
A resin composition was obtained in the same manner as in Example 1 in other respects. In addition, in Comparative Examples 2 and 6, 6 parts by weight of silicic anhydride (trade name: Aerosil 200, manufactured by Nippon Aerosil Co., Ltd.) were added. The test results of the obtained composition are shown in Table 1. ” he corrected.

0 In the 6th line from the bottom of page 10 of the specification, after "resin composition" add "60C'T! After storage for 14 days".

0 Specification, page 10, line 1, P, P base carbon awakening, Σ”Lm, completed 6 years ago, C1 year old man ψ Sanba Utsushiuha”, written on the page - 1゜0 Specification No. 10 2nd line of the page, lateralize ``heavy carbonate'' as ``heavy calcium carbonate'' 1, 0 2nd line from the bottom of page 11 of the specification, delete ``4 days''.

Claims (1)

[Claims] 1. Moisture curing-liquid resin, (B) 5-40 B of 4
A free-flowing moisture-curing material consisting of a surface-treated precipitated calcium carbonate filler having an ET specific surface area and a Karl Fischer adsorbed moisture of 0.3'A or less after drying at 105°C for 2 hours, and (C) a liquid softener. Original resin composition. 2. 10 parts by weight of component (B) per 100 parts by weight of component (A)
300 parts by weight and 1 to 100 parts by weight of component (C).