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JPH0791387B2 - Aqueous inorganic composition - Google Patents
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JPH0791387B2 - Aqueous inorganic composition - Google Patents

Aqueous inorganic composition

Info

Publication number
JPH0791387B2
JPH0791387B2 JP3069384A JP6938491A JPH0791387B2 JP H0791387 B2 JPH0791387 B2 JP H0791387B2 JP 3069384 A JP3069384 A JP 3069384A JP 6938491 A JP6938491 A JP 6938491A JP H0791387 B2 JPH0791387 B2 JP H0791387B2
Authority
JP
Japan
Prior art keywords
inorganic composition
aqueous inorganic
aqueous
alkaline
acid
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.)
Expired - Fee Related
Application number
JP3069384A
Other languages
Japanese (ja)
Other versions
JPH05306339A (en
Inventor
栄次 竹内
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
TEE ESU BII JUGEN
Original Assignee
TEE ESU BII JUGEN
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by TEE ESU BII JUGEN filed Critical TEE ESU BII JUGEN
Priority to JP3069384A priority Critical patent/JPH0791387B2/en
Publication of JPH05306339A publication Critical patent/JPH05306339A/en
Publication of JPH0791387B2 publication Critical patent/JPH0791387B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/006Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
    • C03C1/008Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route for the production of films or coatings

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Silicon Polymers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Paints Or Removers (AREA)

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、低温で被膜形成可能な
水性無機系組成物、さらに詳しくは、水性でありながら
これを塗布、乾燥した場合、沸騰水に十分の抵抗性をも
ち、硬く、撥水性のある被膜を形成し、したがって、建
材,電気機器などの各種のコーティング剤およびこれら
のコーティング剤に用いるバインダーとして有用な水性
無機系組成物に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an aqueous inorganic composition capable of forming a film at a low temperature, and more specifically, when it is applied while being aqueous, it has sufficient resistance to boiling water and is hard. The present invention relates to an aqueous inorganic composition which forms a water-repellent film and is therefore useful as various coating agents for building materials, electric appliances and the like and as a binder used for these coating agents.

【0002】[0002]

【従来の技術】従来、シラン化合物の加水分解・重縮合
反応は、低級アルコールの水溶液中で塩酸を触媒として
行われるている。低級アルコールは、シラン化合物の溶
剤として用いられているものであるが、この低級アルコ
ールとして最もよく使用されているのはメチルアルコー
ルである。
2. Description of the Related Art Conventionally, a hydrolysis / polycondensation reaction of a silane compound has been carried out in an aqueous solution of a lower alcohol using hydrochloric acid as a catalyst. The lower alcohol is used as a solvent for the silane compound, and the most commonly used lower alcohol is methyl alcohol.

【0003】[0003]

【発明が解決しようとする課題】しかし、メチルアルコ
ールは毒性が強く作業者に悪影響をもたらす溶剤である
ので、発明者はこれを解決すべく鋭意研究し、アルコー
ル類を用いずにシラン化合物を加水分解・重縮合する本
発明を完成するに至ったものである。
However, since methyl alcohol is a solvent that is highly toxic and has a bad effect on workers, the inventor has conducted diligent research to solve this, and hydrolyzes silane compounds without using alcohols. This has led to the completion of the present invention of decomposition and polycondensation.

【0004】[0004]

【課題を解決するための手段】すなわち、本発明は、水
系コロイダイルシリカの存在下で、特定の酸を触媒と
し、特定のシラン化合物を加水分解・重縮合させること
によって、上記の課題を解決したものである。
[Means for Solving the Problems] That is, the present invention solves the above problems by hydrolyzing and polycondensing a specific silane compound using a specific acid as a catalyst in the presence of aqueous colloidal silica. It was done.

【0005】ここで、加水分解・重縮合触媒としての特
定の酸としてはりん酸である。特定のシラン化合物とし
てはγ−グリシドキシプロピルトリメトキシシランとジ
メチルジメトキシシランの混合物であり、しかも、これ
らγ−グリシドキシプロピルトリメトキシシランとジメ
チルジメトキシシランの比率が重量比で85:15ない
し60:40、さらに好ましくは、80:20である。
Here, phosphoric acid is used as the specific acid as the hydrolysis / polycondensation catalyst. The specific silane compound is a mixture of γ-glycidoxypropyltrimethoxysilane and dimethyldimethoxysilane, and the ratio of these γ-glycidoxypropyltrimethoxysilane and dimethyldimethoxysilane is 85:15 by weight. 60:40, more preferably 80:20.

【0006】コロイダルシリカとしては、市販されてい
る各種の商品、例えば、日産化学工業株式会社製スノー
テックス20(20%,アルカリ性),スノーテックス
O(20%,酸性)、触媒化成工業株式会社製カタロイ
ドS−20L・S−20H(20%,アルカリ性),カ
タロイドS−30L・S−30H(30%,アルカリ
性),カタロイドSI−30・SI−350(30%,
アルカリ性),カタロイドSI−40・SI−45P・
SI−80(40%,アルカリ性),カタロイドSI−
50(50%,アルカリ性),カタロイドSI−SN
(20%,酸性),カタロイドSI−SA(30%,ア
ルカリ性),カタロイドSN−350(15%,酸
性)、日本化学工業株式会社製シリカドール−20(2
0%,アルカリ性),シリカドール−20A(20%,
酸性),シリカドール−20G(20%,アルカリ
性),シリカドール−20GA(20%,酸性),シリ
カドール−30(30%,アルカリ性),シリカドール
−40(40%,アルカリ性)などがそのまま、または
水で希釈して使用可能であるが、酸性タイプのコロイダ
ルシリカを用いた場合、生成する水性無機系組成物の透
明度が高いので特に好ましい。
As the colloidal silica, various commercially available products, for example, Snowtex 20 (20%, alkaline), Snowtex O (20%, acidic) manufactured by Nissan Chemical Industry Co., Ltd., manufactured by Catalyst Kasei Kogyo Co., Ltd. Cataloid S-20L / S-20H (20%, alkaline), Cataloid S-30L / S-30H (30%, alkaline), Cataloid SI-30 / SI-350 (30%,
Alkaline), Cataloid SI-40 / SI-45P /
SI-80 (40%, alkaline), Cataloid SI-
50 (50%, alkaline), Cataloid SI-SN
(20%, acidic), Cataloid SI-SA (30%, alkaline), Cataloid SN-350 (15%, acidic), Nihon Kagaku Kogyo Co., Ltd. Silica Doll-20 (2
0%, alkaline), Silicadol-20A (20%,
Acidic), silicadol-20G (20%, alkaline), silicadol-20GA (20%, acidic), silicadol-30 (30%, alkaline), silicadol-40 (40%, alkaline), etc. Alternatively, it can be used by diluting with water, but when an acidic type colloidal silica is used, the transparency of the resulting aqueous inorganic composition is high, which is particularly preferable.

【0007】シラン化合物としては、数多くのものが市
販されているが、基材への密着性,風乾性(自然乾燥
性)を付与するためにγ−グリシドキシプロピルトリメ
トキシシラン、耐水性を付与するためにジメチルジメト
キシシランを特定の混合比で混合することが好ましいも
のである。
Although many silane compounds are commercially available, γ-glycidoxypropyltrimethoxysilane, a water-resistant compound, is used to impart adhesion to a substrate and air-drying property (natural drying property). It is preferable to mix dimethyldimethoxysilane in a specific mixing ratio for imparting.

【0008】つまり、γ−グリシドキシプロピルトリメ
トキシシランのみを用いると基材への密着性,風乾性
(自然乾燥性)に優れた水性無機系組成物が得られる
が、その乾燥被膜は沸騰水に十分の抵抗性を持たない。
これにジメチルジメトキシシランを配合すると耐水性が
向上し沸騰水に十分の抵抗性をもつようになる。しか
し、これの割合があまり多くなると、得られた水性無機
系組成物の安定性が悪くなり短時間でゲル化してしま
う。したがって、γ−グリシドキシプロピルトリメトキ
シシランとジメチルジメトキシシランの比率が重量比で
85:15ないし60:40、さらに好ましくは、7
5:25である。
That is, when only γ-glycidoxypropyltrimethoxysilane is used, an aqueous inorganic composition having excellent adhesion to a substrate and excellent air-drying property (natural drying property) can be obtained, but the dry film is boiled. Not sufficiently resistant to water.
When dimethyldimethoxysilane is added to this, the water resistance is improved and it becomes sufficiently resistant to boiling water. However, if the ratio is too large, the stability of the obtained aqueous inorganic composition deteriorates and gelation occurs in a short time. Therefore, the weight ratio of γ-glycidoxypropyltrimethoxysilane to dimethyldimethoxysilane is 85:15 to 60:40, and more preferably 7:15.
It is 5:25.

【0009】また、コロイダルシリカとシラン化合物の
混合液に、加水分解・重縮合触媒として、りん酸を加え
ることによって、反応が室温で進行し、得られた反応生
成物の透明度が高く、しかも、それの乾燥被膜の硬度と
耐沸騰水性が向上する。ここでりん酸としては、化学用
純85%りん酸が好ましいが、75%,89%,100
%のりん酸や、105%,115ないし116%のポリ
りん酸も使用できる。りん酸のシラン化合物に対する比
率は、シラン化合物100部に対し1ないし20部、好
ましくは5ないし15部である。
Further, by adding phosphoric acid as a hydrolysis / polycondensation catalyst to a mixed solution of colloidal silica and a silane compound, the reaction proceeds at room temperature, the obtained reaction product has high transparency, and The hardness and boiling water resistance of its dry coating are improved. As the phosphoric acid, pure 85% chemical phosphoric acid is preferable, but 75%, 89%, 100%
% Phosphoric acid and 105%, 115 to 116% polyphosphoric acid can also be used. The ratio of phosphoric acid to the silane compound is 1 to 20 parts, preferably 5 to 15 parts, relative to 100 parts of the silane compound.

【0010】シラン化合物に対するコロイダルシリカの
比率は10:90ないし90:10、最も好ましくは4
0:60(20%コロイダルシリカ)である。
The ratio of colloidal silica to silane compound is from 10:90 to 90:10, most preferably 4
It is 0:60 (20% colloidal silica).

【0011】本発明において、必要に応じて顔料などの
着色剤,無機フィラー,あるいは消泡剤,チクソ性付与
剤などを組成物に配合することもできる。
In the present invention, a colorant such as a pigment, an inorganic filler, an antifoaming agent, a thixotropy-imparting agent or the like may be added to the composition, if necessary.

【0012】本発明の水性無機系組成物は、例えば水系
コロイダルシリカ中にシラン化合物の混合物を撹拌しな
がら添加し、その混合物に酸触媒を撹拌しながら添加
し、次に必要に応じて他の添加物(着色剤,無機フィラ
ー等)を加えた後、得られた混合物を室温で約24ない
し48時間反応させて加水分解・重縮合することにより
製造できる。上記のようにして製造された本発明の組成
物を基板上に塗布し、室温またはそれ以上の温度で約2
4時間乾燥させることにより、所望の被膜を得ることが
できた。
In the aqueous inorganic composition of the present invention, for example, a mixture of silane compounds is added to aqueous colloidal silica while stirring, and an acid catalyst is added to the mixture while stirring. It can be produced by adding additives (coloring agent, inorganic filler, etc.), and then allowing the resulting mixture to react at room temperature for about 24 to 48 hours for hydrolysis / polycondensation. The composition of the present invention prepared as described above is coated on a substrate, and the temperature of room temperature or higher is about 2
The desired coating could be obtained by drying for 4 hours.

【0013】[0013]

【作用】本発明によって、水で希釈が可能な水性の無機
系組成物が提供される。その水性無機系組成物は、これ
を塗布し、室温またはそれ以上の温度で乾燥した場合、
沸騰水に十分の抵抗性をもち、硬く、撥水性の被膜を形
成する。したがって、建材,電気機器などの各種コーテ
ィング剤やそれのバインダーとしてきわめて有用であ
る。
The present invention provides an aqueous inorganic composition which can be diluted with water. The aqueous inorganic composition, when applied and dried at room temperature or higher,
It has a sufficient resistance to boiling water and forms a hard, water-repellent film. Therefore, it is extremely useful as a coating material for building materials, electrical equipment, etc. and a binder therefor.

【0014】[0014]

【実施例】実施例1 コロイダルシリカ(カタロイドSI−SN,触媒化成工
業株式会社製)60gの中に撹拌しつつ、KBM−40
3(γ−グリシドキシプロピルトリメトキシシラン,信
越化学工業株式会社製)30gとKBM−22(ジメチ
ルジメトキシシラン,信越化学工業株式会社製)10g
の混合液を添加した後、さらに撹拌しつつ化学用純85
%りん酸(試薬)5gを加えて、室温で24時間反応さ
せて、乳白色半透明の水性無機系組成物溶液を得た。こ
れの不揮発分は50%で、粘度は5.8cps(B型粘
度計,25℃)であった。
Example 1 KBM-40 while stirring in 60 g of colloidal silica (Cataloid SI-SN, manufactured by Catalysts & Chemicals Industry Co., Ltd.).
3 (γ-glycidoxypropyltrimethoxysilane, manufactured by Shin-Etsu Chemical Co., Ltd.) 30 g and KBM-22 (dimethyldimethoxysilane, manufactured by Shin-Etsu Chemical Co., Ltd.) 10 g
After adding the mixed solution of, 85
% Phosphoric acid (reagent) was added and reacted at room temperature for 24 hours to obtain a milky white translucent aqueous inorganic composition solution. It had a nonvolatile content of 50% and a viscosity of 5.8 cps (B-type viscometer, 25 ° C.).

【0015】また、ガラス基板にこれを5ないし15ミ
クロンの厚さに塗布し、室温で24時間放置後の鉛筆硬
さは9Hであり、80℃で1時間処理したもの、150
℃で1時間処理したものも鉛筆硬さは9Hであった。表
1に塗膜特性の結果を示す。
Further, a glass substrate was coated with this to a thickness of 5 to 15 μm, and the pencil hardness after standing at room temperature for 24 hours was 9H, and the pencil hardness was treated at 80 ° C. for 1 hour.
The pencil hardness of the sample treated at 1 ° C for 1 hour was 9H. Table 1 shows the results of coating film characteristics.

【0016】[0016]

【表1】 [Table 1]

【0017】なお、上記の反応物100gにシリカ粉末
(クリスタライトAA,龍森製)100gを加えた組成
物を調製し、これを上記と同様に塗布し評価した結果、
絶縁破壊電圧は9KV/0.1mmであった。
A composition was prepared by adding 100 g of silica powder (Crystallite AA, manufactured by Tatsumori) to 100 g of the above reaction product, and the composition was applied and evaluated in the same manner as above.
The dielectric breakdown voltage was 9 KV / 0.1 mm.

【0018】実施例2〜4および比較例1〜3 実施例1と同様な手順で表2に示す組成物を配合して水
性無機系組成物溶液を製造した。得られた組成物の塗膜
を実施例1と同様に評価した(ただし、基板としてステ
ンレスのプレートを使用)。
Examples 2 to 4 and Comparative Examples 1 to 3 The compositions shown in Table 2 were blended in the same procedure as in Example 1 to prepare aqueous inorganic composition solutions. The coating film of the obtained composition was evaluated in the same manner as in Example 1 (however, a stainless plate was used as the substrate).

【0019】[0019]

【表2】 [Table 2]

【0020】比較例1のものは、80℃/30分+15
0℃/60分で硬化させても、沸騰水1時間の処理で被
膜が溶解してしまった。また、比較例2の反応生成物は
室温で1日で、比較例3の反応生成物は反応中にゲル化
してしまいコーティング剤やバインダーとして使用する
ことは不可能であった。これに対し、実施例2〜4の反
応生成物は、実施例1のそれとほぼ同等の特性を示し
た。
In Comparative Example 1, 80 ° C./30 minutes + 15
Even when cured at 0 ° C./60 minutes, the coating was dissolved by the treatment with boiling water for 1 hour. Further, the reaction product of Comparative Example 2 was at room temperature for 1 day, and the reaction product of Comparative Example 3 gelled during the reaction, and it was impossible to use it as a coating agent or a binder. On the other hand, the reaction products of Examples 2 to 4 exhibited almost the same characteristics as those of Example 1.

【0021】[0021]

【発明の効果】本発明によって、水の希釈が可能な、水
性の無機系組成物が提供され、その水性無機系組成物
は、これを所要の厚さで塗布し、室温またはそれ以上の
温度で乾燥した場合、沸騰水に十分の抵抗性をもち、硬
く、撥水性で帯電防止効果のある被膜を形成するので、
建材,電気機器などの各種コーティング剤として、ある
いはこれらのコーティング剤のバインダーとしてきわめ
て有用である。
INDUSTRIAL APPLICABILITY The present invention provides an aqueous inorganic composition capable of diluting water, which is applied at a required thickness at room temperature or higher. When dried with water, it has sufficient resistance to boiling water and forms a hard, water-repellent and antistatic film.
It is extremely useful as various coating agents for building materials and electrical equipment, or as a binder for these coating agents.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】水系コロイダルシリカの存在下で、酸を加
水分解・重縮合触媒として、重量比で85:15ないし
60:40の比率のγ−グリシドキシプロピルトリメト
キシシランとジメチルジメトキシシランのシラン化合物
の混合物を加水分解・重縮合せしめて得られることを特
徴とする水性無機系組成物。
1. An acid is added in the presence of aqueous colloidal silica.
As a water splitting / polycondensation catalyst, the weight ratio is 85:15 or
60:40 ratio of γ-glycidoxypropyltrimetho
Silane compounds of xysilane and dimethyldimethoxysilane
It can be obtained by hydrolyzing and polycondensing a mixture of
Aqueous inorganic composition for collection.
【請求項2】請求項1記載の水性無機系組成物におい
て、加水分解・重縮合触媒としての酸が、りん酸である
ことを特徴とする水性無機系組成物。
2. The odor of the aqueous inorganic composition according to claim 1.
The acid as the hydrolysis / polycondensation catalyst is phosphoric acid.
An aqueous inorganic composition characterized by the above.
JP3069384A 1991-03-11 1991-03-11 Aqueous inorganic composition Expired - Fee Related JPH0791387B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3069384A JPH0791387B2 (en) 1991-03-11 1991-03-11 Aqueous inorganic composition

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3069384A JPH0791387B2 (en) 1991-03-11 1991-03-11 Aqueous inorganic composition

Publications (2)

Publication Number Publication Date
JPH05306339A JPH05306339A (en) 1993-11-19
JPH0791387B2 true JPH0791387B2 (en) 1995-10-04

Family

ID=13401038

Family Applications (1)

Application Number Title Priority Date Filing Date
JP3069384A Expired - Fee Related JPH0791387B2 (en) 1991-03-11 1991-03-11 Aqueous inorganic composition

Country Status (1)

Country Link
JP (1) JPH0791387B2 (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2787100B1 (en) 1998-12-15 2001-03-09 Essilor Int PROCESS FOR THE PREPARATION OF ORGANOSILICY SOIL AND MATERIALS OBTAINED FROM SUCH SOIL
JP2007138144A (en) * 2005-10-18 2007-06-07 Hitachi Chem Co Ltd Silica-based coated film-forming composition
CN102056669B (en) * 2008-06-06 2014-11-05 道达尔研究技术弗吕公司 Process for making crystalline metallosilicates
JP5408606B2 (en) * 2008-12-09 2014-02-05 Hoya株式会社 Hard coating agent and plastic lens using the same
DE102011050872A1 (en) 2011-06-06 2012-12-06 Inomat Gmbh Semitransparent coating material
CN114426704B (en) * 2020-10-29 2023-11-07 广东生益科技股份有限公司 Silica slurry composition, resin composition containing silica slurry composition, prepreg and laminated board

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3986997A (en) * 1974-06-25 1976-10-19 Dow Corning Corporation Pigment-free coating compositions
US4173553A (en) * 1977-12-23 1979-11-06 Dow Corning Corporation Non-coloring, abrasion resistant, adherent coating for gold and silver surfaces
EP0048114A1 (en) * 1980-09-12 1982-03-24 Dow Corning Limited Siloxane resin compositions and preparation and use

Also Published As

Publication number Publication date
JPH05306339A (en) 1993-11-19

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