JPS5818328B2 - Method for stabilizing silica sol - Google Patents
Method for stabilizing silica solInfo
- Publication number
- JPS5818328B2 JPS5818328B2 JP3387975A JP3387975A JPS5818328B2 JP S5818328 B2 JPS5818328 B2 JP S5818328B2 JP 3387975 A JP3387975 A JP 3387975A JP 3387975 A JP3387975 A JP 3387975A JP S5818328 B2 JPS5818328 B2 JP S5818328B2
- Authority
- JP
- Japan
- Prior art keywords
- silica sol
- weight
- sol
- water
- 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.)
- Expired
Links
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 title claims description 22
- 238000000034 method Methods 0.000 title claims description 13
- 230000000087 stabilizing effect Effects 0.000 title claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- 239000004640 Melamine resin Substances 0.000 claims description 5
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 4
- 239000003973 paint Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- -1 silica anhydride Chemical class 0.000 description 1
- 239000010454 slate Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
- Silicon Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Description
【発明の詳細な説明】 本発明はシリカゾルの安定化方法に関するものである。[Detailed description of the invention] The present invention relates to a method for stabilizing silica sol.
本発明者らは５ｉ−０結合で形成されているケイ酸塩骨
格が、熱的にも化学的にも高い安定性を有し、特に無機
異核高分子の特徴は部分的なイオン性を示し、同核の一
重結合よりイオン共鳴分だけ結合エネルギーが高いため
、耐熱性の比較に結合エネルギーを用いると、有機高分
子のＣ−Ｃ共有結合の結合エネルギー８２．６ｋｃａｌ
／ｍｏｌに対し、無機異核高分子のＳ ｉ −０結合エ
ネルギー１０６ｋｃａｌ ／ｍｏｌで高く、これは酸化
に対し高温で安定であるが、低温ではイオン的不純物や
水の存在によって結合が切れる点に注目した。The present inventors found that the silicate skeleton formed by 5i-0 bonds has high thermal and chemical stability, and that inorganic heteronuclear polymers in particular have partial ionicity. Since the bond energy is higher by the amount of ion resonance than the single bond of the same nucleus, when bond energy is used to compare heat resistance, the bond energy of the C-C covalent bond of an organic polymer is 82.6 kcal.
/mol, the Si-0 bond energy of inorganic heteronuclear polymers is high at 106 kcal/mol, which is stable against oxidation at high temperatures, but at low temperatures the bonds break due to the presence of ionic impurities and water. noticed.
ケイ酸塩骨格を持つシリカゾルは無水ケイ酸含有量２０
〜３１％程度のものが現在市販されているが、これ等の
市販品は０°Ｃ以下で凍結し、融解後も、ゾルにもどら
ず使用不能となり、その安定性特に低温における安定化
に上記した問題があるため、応用面が制約され、この点
の解決が装架されていた。Silica sol with silicate skeleton has silicic anhydride content of 20
About 31% of these products are currently on the market, but these commercially available products freeze at temperatures below 0°C, and even after thawing, they do not return to sol and are unusable. This problem has limited its application, and a solution to this point has not yet been developed.
シリガゾルの安定化については従来種々の方法が提案さ
れているが、試薬添加による方法としては有機アミン、
または第４級アンモニウム水酸化物等の低分子量の蒸発
性窒素塩基を使用することが知られていた。Various methods have been proposed for stabilizing siligasol, but methods using reagents include organic amines,
Alternatively, it has been known to use a low molecular weight vaporizable nitrogen base such as quaternary ammonium hydroxide.
しかしこれ等の試薬はより高い塩基性のためシリカゾル
のｐＨを上昇させ、またその蒸発性のため貯蔵中の温度
上昇、水分蒸発にともない添加した蒸発性窒素塩基が除
去されると同時にシリカゾルが濃縮され、そのためゾル
がゲル化してシリカ結晶が析出するという重大な欠点が
ある。However, these reagents increase the pH of the silica sol due to their higher basicity, and due to their evaporative nature, the added evaporable nitrogen base is removed as the temperature rises during storage and water evaporates, causing the silica sol to become concentrated. This has the serious drawback that the sol gels and silica crystals precipitate.
なお、エチレングリコールなどの水溶性有機液体の添加
による安定化についても知られているが、冷却条件によ
るゲル化するなどの問題があった。Note that stabilization by adding a water-soluble organic liquid such as ethylene glycol is also known, but there are problems such as gelation due to cooling conditions.
またシリカゾルの池の利用面である表面処理剤としての
使用については、特許出願公告昭４５−１４８９７１一
表面処理方法」が提案されているが、これはシリカゾル
で無機または有機物の表面を被覆処理する際、その塗面
の補強と改質を目的として、シリカゾル中の一定粒子表
面積のシリカ粒子と分散液にメタノールを加えそのメタ
ノールと水のモル比を一定範囲内に限定し、シリカゾル
を処理面に塗布して被膜を形成し強化する方法と、塗布
直後処理面に残留しているメタノールを燃焼させ、それ
によって被膜形成を早める吉同時に改質する方法である
。Regarding the use of silica sol ponds as a surface treatment agent, Patent Application Publication No. 148971/1971, ``Surface Treatment Method'' has been proposed, which involves coating the surface of inorganic or organic materials with silica sol. For the purpose of reinforcing and modifying the coated surface, methanol is added to the silica particles with a constant particle surface area in the silica sol and the dispersion liquid, and the molar ratio of methanol and water is limited within a certain range, and the silica sol is applied to the treated surface. There are two methods: one is to apply it to form a film and strengthen it, and the other is to burn the methanol remaining on the treated surface immediately after application, thereby speeding up the film formation and simultaneously reforming it.
しかし前者による被膜の強度は弱く、後者の方法は作業
管理上実施に間頂がある。However, the strength of the coating produced by the former method is weak, and the latter method is difficult to implement in terms of work management.
本発明者らはシリカゾルの低温または貯蔵安定性を改善
すると共に、シリカゾルに充填剤を加えて成膜する際に
十分な強度と接着力を有する被膜を形成させることにつ
いて種々検討し、トリエチレングリコールさ少量の水溶
性メラミン樹脂とを添加した場合にシリカゾルの低温安
定性がいちじるしく改善されることを見出し、本発明を
完成した。The present inventors have conducted various studies to improve the low-temperature or storage stability of silica sol, as well as to form a film with sufficient strength and adhesive strength when forming a film by adding a filler to silica sol. The present invention was completed based on the discovery that the low temperature stability of silica sol was significantly improved when a small amount of water-soluble melamine resin was added to the silica sol.
一本発明はシリカゾルに炭素数３個以上のより長い鎖
の２価のアルコール類の１種以上と水溶性メラミン樹脂
を添加することを特徴とするシリカゾルの安定化方法で
ある。One aspect of the present invention is a method for stabilizing silica sol, which is characterized by adding one or more types of longer chain dihydric alcohols having 3 or more carbon atoms and a water-soluble melamine resin to silica sol.
本発明において使用する炭素数３個以上の２価のアルコ
ールとは、たとえばプロピレングリコール、トリメチレ
ングリコール、トリエチレングリコールなどの長い炭素
鎖を有し、シリカゾル（無水ケイ酸として３０％含有の
ものを基準として）１００重量部に対し５重量部以上添
加される。The dihydric alcohol having 3 or more carbon atoms used in the present invention has a long carbon chain, such as propylene glycol, trimethylene glycol, triethylene glycol, etc. It is added in an amount of 5 parts by weight or more per 100 parts by weight (as a standard).
水溶性メラミン樹脂としては、市販のものでよく、同様
にシリカゾル１００重量部に対し２重量部以上添加され
る。The water-soluble melamine resin may be a commercially available one, and is added in an amount of 2 parts by weight or more per 100 parts by weight of silica sol.
本発明では従来のように安定化に有機アミン。In the present invention, an organic amine is used for stabilization as in the conventional method.
蒸発性窒素塩基を使用しないため、シリカゾルのｐＨに
影響をおよぼすことなく、かつ貯蔵中に添加物の蒸発に
よる性能低下を生ぜず、貯蔵中のゲル化を生じないばか
りでなく、凍結の場合も融解によりゾルになりゲル化す
ることはない。Since no evaporable nitrogen base is used, it does not affect the pH of the silica sol, does not cause performance deterioration due to additive evaporation during storage, does not cause gelation during storage, and is also resistant to freezing. It becomes a sol by melting and does not gel.
本発明の安定化されたシルカゾルを塗料のバインダーと
して使用し、塗料を製造する場合は、一般にこのシルカ
ゾルを１０〜３０重量％（無水ケイ酸として３０％含有
量のものを基準）骨材または充填剤５０〜７０重量％と
、適当量の顔料を配合したものにさらにスプレー、ロー
ラ、刷毛塗り等の種々の塗布方法に応じ、水分、増粘剤
、消泡剤等を適当に添加調整して製することができる。When the stabilized silca sol of the present invention is used as a paint binder to produce a paint, generally 10 to 30% by weight of this silka sol (based on 30% silica anhydride content) is used as an aggregate or filler. A mixture of 50 to 70% by weight of agent and an appropriate amount of pigment is further added with water, thickener, antifoaming agent, etc. according to various application methods such as spray, roller, and brush coating. can be manufactured.
したがってこの塗料は有機溶剤を必要とせず、処理工程
も塗布工程のみで加熱乾燥工程を必要とすることなく、
構成成分も主として無機質で不燃性で建造物の特にスレ
ート、コンクリート、モルタル等の内外壁面用塗料とし
てすぐれた性質を有するものである。Therefore, this paint does not require organic solvents, and the treatment process is only the coating process, without the need for heating and drying.
The constituent components are mainly inorganic and nonflammable, and have excellent properties as a paint for the interior and exterior walls of buildings, particularly slate, concrete, mortar, and the like.
以下実施例により本発明の詳細な説明する。The present invention will be explained in detail below with reference to Examples.
実施例 １
ポリビニル製ビーカー中に１００ｇｒのシリカゾル（無
水ケイ酸含有量３０重量％、ｐＨ２５℃で８〜１０）を
加え、第１表の配合割合により、添加剤としてプロピレ
ングリコール、トリエチレングリコール、水溶性メラミ
ン樹脂を加えてかくはん棒で均一になる才でかくはんし
た。Example 1 100g of silica sol (silicic anhydride content: 30% by weight, pH 8 to 10 at 25°C) was added to a polyvinyl beaker, and propylene glycol, triethylene glycol, and water-soluble additives were added according to the blending ratios shown in Table 1. The melamine resin was added and stirred until homogeneous using a stirring stick.
その混合液を恒温恒湿器中の異なった条件下で凍結状態
や融解後の分散状態を観察した結果、本発明による。The present invention is based on the results of observing the frozen state and the dispersion state after thawing of the mixed liquid under different conditions in a constant temperature and humidity chamber.
４６１および／１６２はいずれも良好な安定性を示した
。Both 461 and /162 showed good stability.
註１）良好：室温１５℃で放置融解後ゾルにもどる。Note 1) Good: Returns to sol after being left to melt at room temperature of 15°C.
２）ゲル化：室温１５°Ｃで放置融解後ゾルにもどらず
。2) Gelation: After being left to melt at room temperature of 15°C, it did not return to a sol.
Claims (1)
）１００重量部に、炭素数３個以上の２価の長鎖アルコ
ールの一種以上を少なくとも５重量部と水溶性メラミン
樹脂を少なくとも２重量部添加することを特徴とするシ
リカゾルの安定化方法。1 100 parts by weight of silica sol (based on 30% silicic acid anhydride content), at least 5 parts by weight of one or more divalent long chain alcohols having 3 or more carbon atoms, and at least 2 parts by weight of water-soluble melamine resin. A method for stabilizing silica sol, the method comprising adding silica sol.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3387975A JPS5818328B2 (en) | 1975-03-20 | 1975-03-20 | Method for stabilizing silica sol |
| US05/667,141 US4057525A (en) | 1975-03-20 | 1976-03-15 | Methods for preparing stable silica sols and inorganic coating compositions |
| GB1087576A GB1502722A (en) | 1975-03-20 | 1976-03-18 | Silica sols |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3387975A JPS5818328B2 (en) | 1975-03-20 | 1975-03-20 | Method for stabilizing silica sol |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16253481A Division JPS59536B2 (en) | 1981-10-12 | 1981-10-12 | Improved silica sol paint |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS51108696A JPS51108696A (en) | 1976-09-27 |
| JPS5818328B2 true JPS5818328B2 (en) | 1983-04-12 |
Family
ID=12398793
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3387975A Expired JPS5818328B2 (en) | 1975-03-20 | 1975-03-20 | Method for stabilizing silica sol |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5818328B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS64314U (en) * | 1987-06-19 | 1989-01-05 |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5258732A (en) * | 1975-11-11 | 1977-05-14 | Kowa Kagaku Kougiyou Kk | Inorganic paint composite |
| JPH0786177B2 (en) * | 1986-08-12 | 1995-09-20 | 触媒化成工業株式会社 | Non-sedimentable silica composition for coating and method for producing the same |
-
1975
- 1975-03-20 JP JP3387975A patent/JPS5818328B2/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS64314U (en) * | 1987-06-19 | 1989-01-05 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS51108696A (en) | 1976-09-27 |
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