JPH06313167A - Emulsion composition based on organosilicon compound - Google Patents
Emulsion composition based on organosilicon compoundInfo
- Publication number
- JPH06313167A JPH06313167A JP5123499A JP12349993A JPH06313167A JP H06313167 A JPH06313167 A JP H06313167A JP 5123499 A JP5123499 A JP 5123499A JP 12349993 A JP12349993 A JP 12349993A JP H06313167 A JPH06313167 A JP H06313167A
- Authority
- JP
- Japan
- Prior art keywords
- group
- water
- component
- emulsion composition
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/65—Water proofers or repellants
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00034—Physico-chemical characteristics of the mixtures
- C04B2111/00086—Mixtures with prolonged pot-life
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
- Aftertreatments Of Artificial And Natural Stones (AREA)
- Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は有機ケイ素化合物系エマ
ルジョン組成物に関する。詳しくは、貯蔵安定性に優
れ、かつ、コンクリート,モルタル,レンガ等の多孔質
な無機質基材(建材)に優れた撥水性を付与することの
できる有機ケイ素化合物系エマルジョン組成物に関す
る。TECHNICAL FIELD The present invention relates to an organosilicon compound emulsion composition. More specifically, the present invention relates to an organosilicon compound emulsion composition which has excellent storage stability and can impart excellent water repellency to a porous inorganic base material (building material) such as concrete, mortar and brick.
【0002】[0002]
【従来の技術とその問題点】オルガノアルコキシシラン
が、コンクリート,モルタル,レンガ等の多孔質な無機
質基材(建材)の撥水剤として有用であることは広く知
られている。このような撥水剤としては、通常、オルガ
ノアルコキシシランを種々の有機溶剤で希釈した有機溶
剤型の撥水剤が用いられていた。しかし、希釈剤として
使用されている有機溶剤は人体への毒性や引火の危険性
があり、また環境汚染を引き起こすため、希釈剤に水を
用いてオルガノアルコキシシランを乳化させたエマルジ
ョン型の撥水剤が検討されている。このような撥水剤と
して、例えば、HLBが4〜15のノニオン性界面活性
剤を用いてアルキルアルコキシシランを乳化させたエマ
ルジョン組成物(特公平3−13195号公報参照)や
ノニオン性界面活性剤とアニオン性界面活性剤を併用し
てアルキルアルコキシシランを乳化させたエマルジョン
組成物(特開平4−114979号公報参照)が提案さ
れている。しかし、これらの組成物は、経時的にアルキ
ルアルコキシシランと水とが分離しやすいため有機溶剤
型の撥水剤に比べて貯蔵安定性に劣るという欠点や、こ
れを多孔質な無機質基材(建材)に塗布した場合、その
基材内部は優れた撥水性を示すが、塗布表面の撥水性が
不十分であるという欠点があった。BACKGROUND OF THE INVENTION Organoalkoxysilanes are widely known to be useful as a water repellent agent for porous inorganic base materials (building materials) such as concrete, mortar and bricks. As such a water repellent, an organic solvent type water repellent obtained by diluting an organoalkoxysilane with various organic solvents has been usually used. However, the organic solvent used as a diluent has toxicity to human body and danger of ignition and causes environmental pollution.Therefore, an emulsion type water repellent obtained by emulsifying organoalkoxysilane with water as a diluent. Agents are under consideration. As such a water repellent, for example, an emulsion composition in which an alkylalkoxysilane is emulsified using a nonionic surfactant having an HLB of 4 to 15 (see Japanese Patent Publication No. 3-13195) and a nonionic surfactant. And an anionic surfactant are used together to emulsify an alkylalkoxysilane (see JP-A-4-114979). However, these compositions have a drawback that they are inferior in storage stability as compared with organic solvent-type water repellents because the alkylalkoxysilane and water are easily separated with time, and this is due to a porous inorganic substrate ( When applied to a building material), the inside of the base material exhibits excellent water repellency, but there is a drawback that the water repellency of the applied surface is insufficient.
【0003】[0003]
【発明が解決しようとする課題】本発明者らは上記欠点
を解消するため鋭意検討した結果、本発明に到達した。
すなわち、本発明の目的は、貯蔵安定性に優れ、かつ、
コンクリート,モルタル,レンガ等の多孔質な無機質基
材(建材)に優れた撥水性を付与することのできる有機
ケイ素化合物系エマルジョン組成物を提供することにあ
る。The present inventors have arrived at the present invention as a result of extensive studies to solve the above-mentioned drawbacks.
That is, the object of the present invention is excellent in storage stability, and
An object of the present invention is to provide an organosilicon compound emulsion composition capable of imparting excellent water repellency to a porous inorganic base material (building material) such as concrete, mortar, brick and the like.
【0004】[0004]
【課題を解決するための手段】 本発明は、(A)一般式:R1 aSi(OR2)4-a(式中、R1は炭素原子数が 1〜20の同種または異種の一価炭化水素基であり、R2は炭素原子数が1〜3 の一価炭化水素基であり、aは1または2である。)で表されるオルガノアルコ キシシラン 100重量部、 (B)ケイ素原子に結合した式:−R3−Si(R4)b(OR2)3-b(式中、R2 は炭素原子数が1〜3の一価炭化水素基であり、R3は二価炭化水素基であり、 R4は同種または異種の一価炭化水素基である。bは0,1または2である。) で表される有機基を1分子中に少なくとも1個有するオルガノシロキサン 1〜200重量部、 (C)アニオン性界面活性剤 本発明組成物を乳化 させるのに必要な量 および (D)水 からなることを特徴とする、有機ケイ素化合物系エマル
ジョン組成物に関する。Means for Solving the Problems The present invention provides (A) a general formula: R 1 a Si (OR 2 ) 4-a (wherein R 1 is the same or different one having 1 to 20 carbon atoms). A hydrocarbon group, R 2 is a monovalent hydrocarbon group having 1 to 3 carbon atoms, and a is 1 or 2) 100 parts by weight of organoalkoxysilane, (B) silicon bound to atoms formula: -R 3 -Si (R 4) b (OR 2) in 3-b (wherein, R 2 is a monovalent hydrocarbon group having 1 to 3 carbon atoms, R 3 is two Is a valent hydrocarbon group, R 4 is the same or different monovalent hydrocarbon group, and b is 0, 1 or 2.) An organosiloxane having at least one organic group represented by the formula 1 to 200 parts by weight, (C) anionic surfactant, and an amount necessary to emulsify the composition of the present invention and (D) water. And an organosilicon compound-based emulsion composition.
【0005】本発明の有機ケイ素化合物系エマルジョン
組成物について詳細に説明する。(A)成分のオルガノ
アルコキシシランは本発明組成物の主成分である。本成
分は分子量が小さいため、本発明組成物を多孔質な無機
質基材(建材)に塗布すると、その基材内部に浸透す
る。そしてその基材中に存在する水酸基と反応して基材
と結合することにより、基材内部に優れた撥水層を形成
する。上式中、R1は炭素原子数が1〜20の同種また
は異種の一価炭化水素基であり、具体的にはメチル基,
エチル基,プロピル基,tert-ブチル基,ペンチル基,
n−ヘキシル基,ヘプチル基,2−エチルヘキシル基,
オクチル基,ドデシル基,オクタデシル基等のアルキル
基;フェニル基,トリル基,キシリル基,ナフチル基等
のアリール基;ベンジル基,フェネチル基等のアラルキ
ル基;フロロメチル基,3,3,3-トリフルオロプロピル
基,3,3,4,4,5,5-ヘプタフルオロペンチル基,ジフルオ
ロモノクロルプロピル基等の置換アルキル基が例示され
る。これらの中でも炭素原子数が4〜10のアルキル基
が好ましい。これは、炭素原子数が4未満であると疎水
性成分であるアルキル鎖が短くなるため撥水性が不十分
になり易く、一方、炭素原子数が10を越えると分子量
が大きくなって多孔質な無機質基材(建材)内部への浸
透性が低下し易くなることがあるためである。R2は炭
素原子数が1〜3の一価炭化水素基であり、具体的には
メチル基,エチル基,プロピル基が例示される。aは1
または2である。本成分としては、1種類のオルガノア
ルコキシシランを単独で使用してもよく、必要に応じて
2種類以上のオルガノアルコキシシランを混合して使用
してもよい。The organosilicon compound emulsion composition of the present invention will be described in detail. The organoalkoxysilane as the component (A) is the main component of the composition of the present invention. Since this component has a small molecular weight, when the composition of the present invention is applied to a porous inorganic base material (building material), it penetrates into the base material. Then, by reacting with the hydroxyl group existing in the base material and binding with the base material, an excellent water-repellent layer is formed inside the base material. In the above formula, R 1 is the same or different monovalent hydrocarbon group having 1 to 20 carbon atoms, specifically, a methyl group,
Ethyl group, propyl group, tert-butyl group, pentyl group,
n-hexyl group, heptyl group, 2-ethylhexyl group,
Alkyl group such as octyl group, dodecyl group, octadecyl group; aryl group such as phenyl group, tolyl group, xylyl group, naphthyl group; aralkyl group such as benzyl group, phenethyl group; fluoromethyl group, 3,3,3-trifluoro group Substituted alkyl groups such as propyl group, 3,3,4,4,5,5-heptafluoropentyl group and difluoromonochloropropyl group are exemplified. Among these, an alkyl group having 4 to 10 carbon atoms is preferable. This is because if the number of carbon atoms is less than 4, the alkyl chain, which is a hydrophobic component, becomes short and water repellency tends to be insufficient. On the other hand, if the number of carbon atoms exceeds 10, the molecular weight becomes large and it becomes porous. This is because the permeability to the inside of the inorganic base material (building material) is likely to decrease. R 2 is a monovalent hydrocarbon group having 1 to 3 carbon atoms, and specific examples thereof include a methyl group, an ethyl group and a propyl group. a is 1
Or 2. As this component, one kind of organoalkoxysilane may be used alone, or two or more kinds of organoalkoxysilane may be mixed and used if necessary.
【0006】(B)成分のオルガノシロキサンは(A)
成分の乳化安定性を向上させるための成分である。ま
た、本成分は(A)成分に比べて分子量が大きいため、
本発明組成物を多孔質な無機質基材(建材)に塗布する
と、塗布表面に残存し易く、そのため塗布表面に優れた
撥水層を形成する。このような本成分は、ケイ素原子に
結合した式:−R3−Si(R4)b(OR2)3-bで表さ
れる有機基を1分子中に少なくとも1個有する。ここ
で、式中、R2は前記と同様である。R3は二価炭化水素
基であり、具体的にはエチレン基,n−プロピレン基,
イソプロピレン基,イソブチレン基等のアルキレン基が
例示され、これらの中でもエチレン基が代表的である。
R4は同種または異種の一価炭化水素基であり、具体的
にはメチル基,エチル基,プロピル基,オクチル基,デ
シル基,ドデシル基等のアルキル基;フェニル基,ナフ
チル基,トリル基等のアリール基;2-フェニルエチル
基,2-フェニルプロピル基等のアラルキル基;3,3,3-ト
リフルオロプロピル基等のハロゲン化アルキル基が例示
される。bは0,1または2であるが、好ましくは0ま
たは1である。上式で表される有機基の結合位置として
は、分子鎖末端のみ,側鎖のみ,または分子鎖末端と側
鎖の両方が挙げられる。また、本成分中の上式で表され
る有機基以外の基としては、同種または異種の一価炭化
水素基が好ましいが、さらに好ましくはメチル基と炭素
原子数が4以上のアルキル基の組合せである。本成分は
直鎖状であることが好ましいが、分岐状や環状であって
もよい。本成分は単独重合体でもよく、また、ブロック
共重合体やランダム共重合体でもよい。本成分として
は、例えば、式:The organosiloxane of component (B) is (A)
It is a component for improving the emulsion stability of the component. In addition, since this component has a larger molecular weight than the component (A),
When the composition of the present invention is applied to a porous inorganic base material (building material), it tends to remain on the applied surface, so that an excellent water-repellent layer is formed on the applied surface. Such a component has at least one organic group represented by the formula: —R 3 —Si (R 4 ) b (OR 2 ) 3-b bonded to a silicon atom in one molecule. Here, in the formula, R 2 is the same as described above. R 3 is a divalent hydrocarbon group, specifically, ethylene group, n-propylene group,
Examples of the alkylene group include an isopropylene group and an isobutylene group, and of these, an ethylene group is typical.
R 4 is the same or different monovalent hydrocarbon group, specifically, an alkyl group such as methyl group, ethyl group, propyl group, octyl group, decyl group, dodecyl group; phenyl group, naphthyl group, tolyl group, etc. And an aralkyl group such as a 2-phenylethyl group and a 2-phenylpropyl group; and a halogenated alkyl group such as a 3,3,3-trifluoropropyl group. b is 0, 1 or 2, but is preferably 0 or 1. The bonding position of the organic group represented by the above formula includes only the molecular chain end, the side chain only, or both the molecular chain end and the side chain. Further, as the group other than the organic group represented by the above formula in this component, the same or different monovalent hydrocarbon groups are preferable, and more preferably a combination of a methyl group and an alkyl group having 4 or more carbon atoms. Is. This component is preferably linear, but may be branched or cyclic. This component may be a homopolymer, or may be a block copolymer or a random copolymer. As this component, for example, the formula:
【化1】 (式中、mおよびnは0〜50の範囲の数である。)で
表されるオルガノシロキサンが挙げられる。なお、上式
中、m+nは0〜50の範囲であることが好ましい。こ
れは、m+nが50を越えると多孔質な無機質基材(建
材)内部への浸透性が低下して、塗布表面に多量の本成
分が残存し易くなる。その結果、塗布表面の色が濃くな
り、濡れたような外観を呈することがあるためである。
本成分の配合量は(A)成分100重量部に対して1〜
200重量部の範囲であり、好ましくは10〜100重
量部の範囲である。これは、1重量部未満では本発明組
成物の貯蔵安定性が低下し、さらに塗布表面の撥水性が
不十分になるためであり、また、200重量部を越える
と本成分に対する(A)成分の割合が小さくなって本発
明組成物の多孔質な無機質基材(建材)内部への浸透量
が減少し、基材内部の撥水性が不十分になるためであ
る。[Chemical 1] (In the formula, m and n are numbers in the range of 0 to 50). In the above formula, m + n is preferably in the range of 0-50. This is because when m + n exceeds 50, the permeability into the porous inorganic base material (building material) decreases, and a large amount of this component tends to remain on the coated surface. As a result, the color of the applied surface becomes dark and the appearance may be wet.
The blending amount of this component is 1 to 100 parts by weight of the component (A).
It is in the range of 200 parts by weight, and preferably in the range of 10 to 100 parts by weight. This is because if the amount is less than 1 part by weight, the storage stability of the composition of the present invention is lowered and the water repellency of the coated surface becomes insufficient, and if it exceeds 200 parts by weight, the component (A) relative to this component is used. This is because the ratio of (3) becomes small and the amount of the composition of the present invention penetrating into the porous inorganic base material (building material) decreases, resulting in insufficient water repellency inside the base material.
【0007】(C)成分のアニオン性界面活性剤は
(A)成分および(B)成分を乳化するための成分であ
る。本成分の具体例としては、オクチルベンゼンスルホ
ン酸,ドデシルベンゼンスルホン酸,セチルベンゼンス
ルホン酸等のアルキルベンゼンスルホン酸;高級アルコ
ール硫酸エステル;ポリオキシエチレンアルキルエーテ
ル硫酸エステル;ポリオキシエチレンアルキルフェニル
エーテル硫酸エステル;アルキルナフチルスルホン酸等
のナトリウム塩,カリウム塩,リチウム塩またはアミン
塩が挙げられる。本成分の配合量は本発明組成物を乳化
させることができる量であればよく、その種類により異
なるが、通常は(A)成分と(B)成分の合計量100
重量部に対して0.1〜50重量部の範囲であり、好ま
しくは0.1〜10重量部の範囲である。The component (C) anionic surfactant is a component for emulsifying the component (A) and the component (B). Specific examples of this component include alkylbenzenesulfonic acids such as octylbenzenesulfonic acid, dodecylbenzenesulfonic acid and cetylbenzenesulfonic acid; higher alcohol sulfuric acid ester; polyoxyethylene alkyl ether sulfuric acid ester; polyoxyethylene alkylphenyl ether sulfuric acid ester; Examples thereof include sodium salt, potassium salt, lithium salt or amine salt of alkylnaphthyl sulfonic acid and the like. The blending amount of this component may be any amount as long as it can emulsify the composition of the present invention, and it varies depending on the type, but usually the total amount of the (A) component and the (B) component is 100.
It is in the range of 0.1 to 50 parts by weight, and preferably in the range of 0.1 to 10 parts by weight, based on parts by weight.
【0008】(D)成分の水は(A)成分および(B)
成分の分散媒である。本成分の配合量は本発明組成物が
O/W型のエマルジョンとなる量であれば特に限定され
ないが、(A)成分と(B)成分の合計濃度が5〜60
重量%となるような量であることが好ましく、より好ま
しくは10〜50重量%となるような量である。The component (D) water is composed of the components (A) and (B).
It is a dispersion medium for the components. The blending amount of this component is not particularly limited as long as the composition of the present invention is an O / W type emulsion, but the total concentration of the (A) component and the (B) component is 5 to 60.
The amount is preferably such that the amount is 10% by weight, more preferably 10 to 50% by weight.
【0009】本発明組成物は上記した(A)成分〜
(D)成分からなるものであるが、これに有機ケイ素化
合物系エマルジョン組成物の添加剤として公知である他
の成分を添加配合することは、本発明の目的を損なわな
い限り差し支えない。このような添加剤として、例え
ば、ノニオン性界面活性剤やpH調節剤が挙げられる。
ノニオン性界面活性剤としては、ポリオキシエチレンア
ルキルエーテル類,ポリオキシエチレンアルキルフェニ
ルエーテル類,ポリオキシエチレンアルキルエステル
類,ポリオキシエチレンソルビタンアルキルエステル
類,ソルビタンアルキルエステル類,ポリエチレングラ
イコール,ポリプロピレングライコールが例示される。
このようなノニオン性界面活性剤を本発明組成物に添加
配合した場合、本発明組成物の貯蔵安定性がさらに向上
することがある。また、本発明組成物においては、その
pHを調節するためにpH調節剤を使用することができ
る。本発明組成物のpHは通常6〜8の範囲であり、好
ましくは6〜7の範囲である。これは、pHがこの範囲
より外れると(A)成分および(B)成分の加水分解反
応や縮合反応が起こり易くなる。その結果、(A)成分
および(B)成分の分子量が大きくなり、多孔質な無機
質基材(建材)内部への浸透性が低下することがあるた
めである。pH調節剤の具体例としては、水酸化ナトリ
ウム,水酸化カリウム,アンモニア,各種アミン類,炭
酸水素ナトリウム,オレイン酸ナトリウムが挙げられ
る。その他の添加剤としては、鉄,亜鉛,チタン,錫,
コバルト等の有機金属化合物;ポリエステル樹脂,アク
リル樹脂等の合成樹脂;スチレン・ブタジエン共重合体
ゴム,天然ゴム等のゴムラテックス;防錆剤;防腐剤;
着色剤が挙げられる。The composition of the present invention comprises the above-mentioned component (A)
Although it is composed of the component (D), addition of other components known as an additive of the organosilicon compound emulsion composition may be added thereto, as long as the object of the present invention is not impaired. Examples of such additives include nonionic surfactants and pH adjusters.
Examples of nonionic surfactants include polyoxyethylene alkyl ethers, polyoxyethylene alkyl phenyl ethers, polyoxyethylene alkyl esters, polyoxyethylene sorbitan alkyl esters, sorbitan alkyl esters, polyethylene glycol, and polypropylene glycol. Is exemplified.
When such a nonionic surfactant is added to the composition of the present invention, the storage stability of the composition of the present invention may be further improved. Further, in the composition of the present invention, a pH adjusting agent can be used to adjust the pH. The pH of the composition of the present invention is usually in the range of 6 to 8, preferably 6 to 7. This is because when the pH is out of this range, the hydrolysis reaction and the condensation reaction of the component (A) and the component (B) are likely to occur. As a result, the molecular weights of the component (A) and the component (B) increase, and the permeability to the inside of the porous inorganic base material (building material) may decrease. Specific examples of the pH adjusting agent include sodium hydroxide, potassium hydroxide, ammonia, various amines, sodium hydrogen carbonate, and sodium oleate. Other additives include iron, zinc, titanium, tin,
Organometallic compounds such as cobalt; synthetic resins such as polyester resins and acrylic resins; rubber latex such as styrene / butadiene copolymer rubber and natural rubber; rust preventives; antiseptic;
Colorants can be mentioned.
【0010】本発明組成物は従来周知のエマルジョンの
製造方法に使用される生産手段を使用して容易に製造す
ることができる。例えば、(A)成分,(B)成分,
(C)成分および(D)成分を攪拌バネにより混合し、
これをホモミキサー,ラインミル,ホモジナイザー等の
乳化機を用いて乳化することにより製造することができ
る。また、(A)成分および(B)成分をそれぞれ
(C)成分および(D)成分で乳化した後、これらのエ
マルジョンを混合することにより製造することができ
る。The composition of the present invention can be easily produced by using the production means used in the conventional production method of emulsion. For example, (A) component, (B) component,
The components (C) and (D) are mixed by a stirring spring,
This can be produced by emulsifying with an emulsifying machine such as a homomixer, a line mill, a homogenizer. Further, it can be produced by emulsifying the component (A) and the component (B) with the component (C) and the component (D), respectively, and then mixing these emulsions.
【0011】本発明組成物は、これをスプレー塗布,ロ
ール塗布,はけ塗り等の方法によりコンクリート,モル
タル,レンガ等の多孔質な無機質基材(建材)に塗布す
ることができる。The composition of the present invention can be applied to a porous inorganic base material (building material) such as concrete, mortar and bricks by a method such as spray coating, roll coating and brush coating.
【0012】以上のような本発明組成物は(A)成分の
オルガノアルコキシシランと(B)成分のオルガノシロ
キサンを併用しているため、オルガノアルコキシシラン
を単独で使用した組成物に比べて乳化しやすく、貯蔵安
定性に優れている。また、本発明組成物をコンクリー
ト,モルタル,レンガ等の多孔質な無機質基材(建材)
に塗布すると、(A)成分のオルガノアルコキシシラン
がその基材内部に浸透し、基材と結合して内部に優れた
撥水層を形成し、また、(B)成分のオルガノシロキサ
ンが塗布表面に優れた撥水層を形成する。そのため、本
発明組成物を塗布した多孔質な無機質基材(建材)は撥
水性に優れ、特に表面の撥水性に優れている。さらに、
本発明組成物は長期間貯蔵後も優れた撥水性を保持する
ことができる。このような本発明組成物はコンクリー
ト,モルタル,レンガ等の多孔質な無機質基材(建材)
の撥水剤として極めて有用である。Since the composition of the present invention as described above uses the organoalkoxysilane of the component (A) and the organosiloxane of the component (B) in combination, it is more emulsified than the composition using the organoalkoxysilane alone. Easy and has excellent storage stability. In addition, the composition of the present invention may be used for porous inorganic base materials (building materials) such as concrete, mortar and bricks.
When applied to, the (A) component organoalkoxysilane penetrates into the inside of the base material and binds to the base material to form an excellent water repellent layer inside, and the (B) component organosiloxane is applied to the coated surface. An excellent water repellent layer is formed. Therefore, the porous inorganic base material (building material) coated with the composition of the present invention has excellent water repellency, and particularly excellent surface water repellency. further,
The composition of the present invention can retain excellent water repellency even after long-term storage. Such a composition of the present invention is a porous inorganic base material (building material) such as concrete, mortar and brick.
Is extremely useful as a water repellent.
【0013】[0013]
【実施例】本発明を実施例により詳細に説明する。実施
例中、粘度の値は25℃において測定した値である。部
は重量部を表し、%は重量%を表し、cSはセンチスト
ークスである。また、有機ケイ素化合物系エマルジョン
組成物の評価は次に示す試験方法によって行なった。 ○貯蔵安定性 エマルジョン組成物を100ccのガラス瓶に封入し
て、そのまま密封状態で室温にて3カ月間放置し、その
外観の変化を肉眼にて観察した。 良好:3カ月経過後も水層と油層の分離が認められなか
った。 不良:3カ月以内に水層と油層の分離が認められた。こ
の場合、水層と油層の分離が認められた日数を示した。 ○表面撥水性 セメント:砂:水の配合割合が1:2:0.6のモルタ
ルスラリーを100×100×16mmのステンレス製
型枠に打設し、2日後に脱型した。次いでこれを温度2
0℃、湿度85%の条件下で20日間養生させてモルタ
ル試験体を作成した。このモルタル試験体の表面にエマ
ルジョン組成物を塗布し(塗布量300g/m2)、次
いで温度20℃、湿度65%の条件下で7日間養生させ
てモルタル試験体を撥水処理した。この撥水処理された
モルタル試験体の表面の3箇所に約0.03gの水滴を
それぞれ滴下し、その水滴の形状変化を肉眼にて観察し
た。評価結果は次の5段階に分けて報告した。 ◎:10分後でも水滴は球状に保たれており、撥水性は
非常に良好であった。 ○:5分後に水滴は半球状に崩れたが、撥水性は良好で
あった。 △:3分後に水滴は崩れたが、モルタルに吸収されるま
でにはいたらず、撥水性はやや良好であった。 ×:1分後に水滴はモルタルに吸収され、撥水性は悪か
った。 ○吸水率 上記と同様の方法で撥水処理されたモルタル試験体を、
20℃の蒸留水中に24時間全面浸せきした。その後、
このモルタル試験体の重量増加量から吸水率(%)を求
めた。 吸水率(%)=(浸せき後の重量−浸せき前の重量)/
浸せき前の重量×100EXAMPLES The present invention will be described in detail with reference to Examples. In the examples, the viscosity value is a value measured at 25 ° C. Parts represent parts by weight,% represents% by weight and cS is centistokes. Further, the evaluation of the organosilicon compound emulsion composition was carried out by the following test method. ○ Storage stability The emulsion composition was enclosed in a 100 cc glass bottle, left in a sealed state at room temperature for 3 months, and the change in its appearance was observed with the naked eye. Good: No separation of the water layer and the oil layer was observed even after 3 months. Poor: Separation of water layer and oil layer was observed within 3 months. In this case, the number of days when separation of the water layer and the oil layer was observed was shown. ○ Surface water repellency A mortar slurry having a mixing ratio of cement: sand: water of 1: 2: 0.6 was cast into a stainless steel mold of 100 × 100 × 16 mm, and demolded after 2 days. Then add this to temperature 2
A mortar test body was prepared by curing for 20 days at 0 ° C. and a humidity of 85%. The emulsion composition was applied to the surface of this mortar test body (coating amount: 300 g / m 2 ), and then cured at a temperature of 20 ° C. and a humidity of 65% for 7 days to make the mortar test body water repellent. Approximately 0.03 g of water droplets were dropped on each of three points on the surface of the water-repellent treated mortar specimen, and the shape change of the water droplets was visually observed. The evaluation results are reported in the following five stages. A: Water droplets were kept spherical even after 10 minutes, and the water repellency was very good. ◯: Water repellency was good although the water droplets collapsed into a hemisphere after 5 minutes. (Triangle | delta): Although the water droplet collapsed after 3 minutes, it was not absorbed by the mortar and the water repellency was rather good. X: Water droplets were absorbed by the mortar after 1 minute and the water repellency was poor. ○ Water absorption rate A mortar test piece that has been subjected to water repellent treatment in the same manner as above is
The whole surface was soaked in distilled water at 20 ° C. for 24 hours. afterwards,
The water absorption rate (%) was determined from the weight increase of this mortar test body. Water absorption rate (%) = (weight after immersion-weight before immersion) /
Weight before immersion × 100
【0014】[0014]
【実施例1】n−ヘキシルトリエトキシシラン20部、
式:Example 1 20 parts of n-hexyltriethoxysilane,
formula:
【化2】 で表される粘度が21cSのオルガノシロキサン10
部、ポリオキシエチレン(2モル)ラウリルエーテル硫
酸ナトリウム0.5部、オレイン酸ナトリウム0.05部
およびイオン交換水69.45部を混合した。この混合
液をホモジナイザーに入れてこの中を300kg/cm
2の圧力で2回通過させて、pH6.9の乳白色の有機ケ
イ素化合物系エマルジョン組成物を得た。このエマルジ
ョン組成物の貯蔵安定性、表面撥水性および吸水率を測
定した。これらの測定結果を表1に示した。[Chemical 2] Organosiloxane 10 having a viscosity of 21 cS represented by
Parts, polyoxyethylene (2 mol) sodium lauryl ether sulfate 0.5 parts, sodium oleate 0.05 parts and ion-exchanged water 69.45 parts were mixed. Put this mixture in a homogenizer and add 300kg / cm
It was passed twice at a pressure of 2 to obtain a milky white organosilicon compound emulsion composition having a pH of 6.9. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0015】[0015]
【実施例2】実施例1において、ポリオキシエチレン
(2モル)ラウリルエーテル硫酸ナトリウム0.5部を
ラウリルスルホ酢酸ナトリウム0.3部に変え、オレイ
ン酸ナトリウムの配合量を0.02部とした以外は実施
例1と同様にして、pH6.5の乳白色の有機ケイ素化
合物系エマルジョン組成物を得た。このエマルジョン組
成物の貯蔵安定性、表面撥水性および吸水率を測定し
た。これらの測定結果を表1に示した。Example 2 In Example 1, 0.5 part of sodium polyoxyethylene (2 mol) lauryl ether sulfate was changed to 0.3 part of sodium lauryl sulfoacetate, and the content of sodium oleate was 0.02 part. A milky white organosilicon compound emulsion composition having a pH of 6.5 was obtained in the same manner as in Example 1 except for the above. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0016】[0016]
【実施例3】実施例1において、ポリオキシエチレン
(2モル)ラウリルエーテル硫酸ナトリウム0.5部を
N−ラウリルメチルタウリンナトリウム0.25部に変
え、オレイン酸ナトリウムの配合量を0.01部とした
以外は実施例1と同様にして、pH6.7の乳白色の有
機ケイ素化合物系エマルジョン組成物を得た。このエマ
ルジョン組成物の貯蔵安定性、表面撥水性および吸水率
を測定した。これらの測定結果を表1に示した。Example 3 In Example 1, 0.5 part of sodium polyoxyethylene (2 mol) lauryl ether sulfate was changed to 0.25 part of sodium N-laurylmethyl taurine, and the content of sodium oleate was 0.01 part. A milky white organosilicon compound emulsion composition having a pH of 6.7 was obtained in the same manner as in Example 1 except for the above. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0017】[0017]
【実施例4】実施例1において、ポリオキシエチレン
(2モル)ラウリルエーテル硫酸ナトリウム0.5部を
ポリオキシエチレン(2モル)ラウリルエーテル硫酸ナ
トリウム0.2部およびポリオキシエチレン(6モル)
ラウリルエーテル0.3部に変え、オレイン酸ナトリウ
ムの配合量を0.02部とした以外は実施例1と同様に
して、pH6.8の乳白色の有機ケイ素化合物系エマル
ジョン組成物を得た。このエマルジョン組成物の貯蔵安
定性、表面撥水性および吸水率を測定した。これらの測
定結果を表1に示した。Example 4 In Example 1, 0.5 part of sodium polyoxyethylene (2 mol) lauryl ether sulfate was added to 0.2 part of polyoxyethylene (2 mol) sodium lauryl ether sulfate and polyoxyethylene (6 mol).
A milky white organosilicon compound emulsion composition having a pH of 6.8 was obtained in the same manner as in Example 1 except that the content of sodium oleate was changed to 0.02 part instead of 0.3 part of lauryl ether. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0018】[0018]
【実施例5】実施例1において、粘度が21cSのオル
ガノシロキサンを式:Example 5 In Example 1, an organosiloxane having a viscosity of 21 cS was prepared by the formula:
【化3】 で表される粘度が7.5cSのジメチルシロキサン10
部に変えた以外は実施例1と同様にして、pH6.8の
乳白色の有機ケイ素化合物系エマルジョン組成物を得
た。このエマルジョン組成物の貯蔵安定性、表面撥水性
および吸水率を測定した。これらの測定結果を表1に示
した。[Chemical 3] Dimethylsiloxane 10 having a viscosity of 7.5 cS represented by
A milky white organosilicon compound emulsion composition having a pH of 6.8 was obtained in the same manner as in Example 1 except that the parts were changed. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0019】[0019]
【実施例6】n−ヘキシルトリエトキシシラン25部、
式:Example 6 25 parts of n-hexyltriethoxysilane,
formula:
【化4】 で表される粘度が7.5cSのジメチルシロキサン5
部、ラウリルスルホ酢酸ナトリウム0.3部、オレイン
酸ナトリウム0.02部およびイオン交換水69.68部
を混合した。この混合液をホモジナイザーに入れてこの
中を300kg/cm2の圧力で2回通過させて、pH
6.8の乳白色の有機ケイ素化合物系エマルジョン組成
物を得た。このエマルジョン組成物の貯蔵安定性、表面
撥水性および吸水率を測定した。これらの測定結果を表
1に示した。[Chemical 4] Dimethylsiloxane 5 with a viscosity of 7.5 cS
Parts, 0.3 parts of sodium lauryl sulfoacetate, 0.02 parts of sodium oleate and 69.68 parts of ion-exchanged water were mixed. The mixture was put in a homogenizer and passed through the homogenizer twice at a pressure of 300 kg / cm 2 to adjust the pH.
A milky white organosilicon compound emulsion composition of 6.8 was obtained. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0020】[0020]
【実施例7】実施例6において、n−ヘキシルトリエト
キシシランの配合量を15部とし、粘度が7.5cSの
ジオルガノシロキサンの配合量を15部とした以外は実
施例6と同様にして、pH6.8の乳白色の有機ケイ素
化合物系エマルジョン組成物を得た。このエマルジョン
組成物の貯蔵安定性、表面撥水性および吸水率を測定し
た。これらの測定結果を表1に示した。Example 7 Example 6 was repeated except that the amount of n-hexyltriethoxysilane was 15 parts and the amount of diorganosiloxane having a viscosity of 7.5 cS was 15 parts. A milky white organosilicon compound emulsion composition having a pH of 6.8 was obtained. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0021】[0021]
【比較例1】n−ヘキシルトリエトキシシラン30部、
ポリオキシエチレン(2モル)ラウリルエーテル硫酸ナ
トリウム0.5部、オレイン酸ナトリウム0.05部およ
びイオン交換水69.45部を混合した。この混合液を
ホモジナイザーに入れてこの中を300kg/cm2の
圧力で2回通過させて、pH6.8の乳白色のエマルジ
ョン組成物を得た。このエマルジョン組成物の貯蔵安定
性、表面撥水性および吸水率を測定した。これらの測定
結果を表1に示した。Comparative Example 1 30 parts of n-hexyltriethoxysilane,
Polyoxyethylene (2 mol) sodium lauryl ether sulfate 0.5 part, sodium oleate 0.05 part and ion-exchanged water 69.45 parts were mixed. This mixture was put into a homogenizer and passed through the homogenizer twice at a pressure of 300 kg / cm 2 , to obtain a milky white emulsion composition having a pH of 6.8. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0022】[0022]
【比較例2】n−ヘキシルトリエトキシシラン30部、
ポリオキシエチレン(6モル)ラウリルエーテル2部お
よびイオン交換水68部を混合した。この混合液をホモ
ジナイザーに入れてこの中を300kg/cm2の圧力
で2回通過させて、pH6.6の乳白色のエマルジョン
組成物を得た。このエマルジョン組成物の貯蔵安定性、
表面撥水性および吸水率を測定した。これらの測定結果
を表1に示した。Comparative Example 2 30 parts of n-hexyltriethoxysilane,
2 parts of polyoxyethylene (6 mol) lauryl ether and 68 parts of ion-exchanged water were mixed. This mixed solution was put into a homogenizer and passed through the homogenizer twice at a pressure of 300 kg / cm 2 , to obtain a milky white emulsion composition having a pH of 6.6. Storage stability of this emulsion composition,
Surface water repellency and water absorption were measured. The results of these measurements are shown in Table 1.
【0023】[0023]
【比較例3】n−ヘキシルトリエトキシシラン30部、
ポリオキシエチレン(2モル)ラウリルエーテル2部お
よびイオン交換水68部を混合した。この混合液をホモ
ジナイザーに入れてこの中を300kg/cm2の圧力
で2回通過させて、乳白色のエマルジョン組成物を得
た。このエマルジョン組成物の貯蔵安定性、表面撥水性
および吸水率を測定した。これらの測定結果を表1に示
した。Comparative Example 3 30 parts of n-hexyltriethoxysilane,
2 parts of polyoxyethylene (2 mol) lauryl ether and 68 parts of ion-exchanged water were mixed. This mixed solution was put in a homogenizer and passed through the homogenizer twice at a pressure of 300 kg / cm 2 , to obtain a milky white emulsion composition. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0024】[0024]
【比較例4】n−ヘキシルトリエトキシシラン30部、
ポリオキシエチレン(2モル)ラウリルエーテル硫酸ナ
トリウム0.2部、ポリオキシエチレン(6モル)ラウ
リルエーテル0.3部、オレイン酸ナトリウム0.02部
およびイオン交換水69.48部を混合した。この混合
液をホモジナイザーに入れてこの中を300kg/cm
2の圧力で2回通過させて、pH6.7の乳白色のエマル
ジョン組成物を得た。このエマルジョン組成物の貯蔵安
定性、表面撥水性および吸水率を測定した。これらの測
定結果を表1に示した。Comparative Example 4 30 parts of n-hexyltriethoxysilane,
0.2 parts of sodium polyoxyethylene (2 mol) lauryl ether sulfate, 0.3 parts of polyoxyethylene (6 mol) lauryl ether, 0.02 part of sodium oleate and 69.48 parts of ion-exchanged water were mixed. Put this mixture in a homogenizer and add 300kg / cm
Two passes at a pressure of 2 gave a milky white emulsion composition with a pH of 6.7. The storage stability, surface water repellency and water absorption of this emulsion composition were measured. The results of these measurements are shown in Table 1.
【0025】[0025]
【表1】 [Table 1]
【0026】[0026]
【発明の効果】本発明の有機ケイ素化合物系エマルジョ
ン組成物は(A)成分〜(D)成分からなり、特に
(A)成分のオルガノアルコキシシランと(B)成分の
オルガノシロキサンを含有しているので、貯蔵安定性に
優れ、かつ、これをコンクリート,モルタル,レンガ等
の多孔質な無機質基材(建材)に塗布した場合には、こ
れらの多孔質な無機質基材(建材)に優れた撥水性を付
与することができるという特徴を有する。The organosilicon compound emulsion composition of the present invention comprises the components (A) to (D), and particularly contains the organoalkoxysilane (A) and the organosiloxane (B). Therefore, when it is applied to porous inorganic base materials (building materials) such as concrete, mortar, bricks, etc., it has excellent storage stability and excellent repellent properties for these porous inorganic base materials (building materials). It has a feature that it can be rendered water-based.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 小名 功 千葉県市原市千種海岸2番2 東レ・ダウ コーニング・シリコーン株式会社研究開発 本部内 ─────────────────────────────────────────────────── ─── Continued Front Page (72) Inventor Isao Ona 2-2 Chikusaigan, Ichihara, Chiba Toray Dow Corning Silicone Co., Ltd.
Claims (3)
4-a(式中、R1は炭素原子数が1〜20の同種または異
種の一価炭化水素基であり、R2は炭素原子数が1〜3
の一価炭化水素基であり、aは1または2である。)で
表されるオルガノアルコキシシラン
100重量部、 (B)ケイ素原子に結合した式:−R3−Si(R4)b(OR2)3-b(式中、R2 は炭素原子数が1〜3の一価炭化水素基であり、R3は二価炭化水素基であり、 R4は同種または異種の一価炭化水素基である。bは0,1または2である。) で表される有機基を1分子中に少なくとも1個有するオルガノシロキサン 1〜200重量部、 (C)アニオン性界面活性剤 本発明組成物を乳化 させるのに必要な量 および (D)水 からなることを特徴とする、有機ケイ素化合物系エマル
ジョン組成物。1. (A) General formula: R 1 a Si (OR 2 ).
4-a (In the formula, R 1 is the same or different monovalent hydrocarbon group having 1 to 20 carbon atoms, and R 2 is 1 to 3 carbon atoms.
Is a monovalent hydrocarbon group, and a is 1 or 2. ) Organoalkoxysilane represented by
100 parts by weight, (B) wherein bonded to a silicon atom: -R 3 -Si (R 4) b (OR 2) 3-b ( wherein, R 2 is a monovalent hydrocarbon having 1 to 3 carbon atoms Group, R 3 is a divalent hydrocarbon group, R 4 is a monovalent hydrocarbon group of the same type or a different type, and b is 0, 1 or 2. 1 molecule of an organic group represented by 1 to 200 parts by weight of organosiloxane having at least one of them, (C) anionic surfactant, an amount necessary for emulsifying the composition of the present invention, and (D) water, an organosilicon compound Emulsion composition.
シランである、請求項1記載の有機ケイ素化合物系エマ
ルジョン組成物。2. The organosilicon compound emulsion composition according to claim 1, wherein the component (A) is n-hexyltriethoxysilane.
求項1記載の有機ケイ素化合物系エマルジョン組成物。3. The organosilicon compound emulsion composition according to claim 1, which is a water-repellent agent for porous inorganic substrates.
Priority Applications (1)
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JP12349993A JP3403217B2 (en) | 1993-04-27 | 1993-04-27 | Organosilicon compound emulsion composition |
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JP12349993A JP3403217B2 (en) | 1993-04-27 | 1993-04-27 | Organosilicon compound emulsion composition |
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JPH06313167A true JPH06313167A (en) | 1994-11-08 |
JP3403217B2 JP3403217B2 (en) | 2003-05-06 |
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