JP2000262883A - In-oil dispersant for inorganic powder - Google Patents

In-oil dispersant for inorganic powder

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Publication number
JP2000262883A
JP2000262883A JP11075434A JP7543499A JP2000262883A JP 2000262883 A JP2000262883 A JP 2000262883A JP 11075434 A JP11075434 A JP 11075434A JP 7543499 A JP7543499 A JP 7543499A JP 2000262883 A JP2000262883 A JP 2000262883A
Authority
JP
Japan
Prior art keywords
inorganic powder
powder
oil
inorg
dispersant
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.)
Pending
Application number
JP11075434A
Other languages
Japanese (ja)
Inventor
Akira Takenaka
晃 武中
Masaaki Dobashi
正明 土橋
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.)
Kao Corp
Original Assignee
Kao Corp
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 Kao Corp filed Critical Kao Corp
Priority to JP11075434A priority Critical patent/JP2000262883A/en
Publication of JP2000262883A publication Critical patent/JP2000262883A/en
Pending legal-status Critical Current

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  • Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
  • Detergent Compositions (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide an in-oil dispersant for an inorg. powder easily dispersing the inorg. powder in oil within a short time to hold the stable dispersion state thereof over a long time and capable of easily re-dispersing the same even if the sedimentation of the inorg. powder is generated and showing good particle flocculation preventing capacity and dispersibility even if used as a surface modifier of the inorg. powder. SOLUTION: An in-oil dispersant for an inorg. powder comprises a compd. represented by the formula: R1O(AO)nCH2COOM (wherein R1 is a 6-24C alkyl or alkenyl, AO is a 2-3C oxyalkylene, n is a number of 1-20 and M is hydrogen or an alkali metal). An inorg. powder dispersion compsn. containing the in-oil dispersant and the inorg. powder of which the surface is treated with the in-oil dispersant are obtained.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、無機粉末用油中分
散剤及びそれを含有する無機粉末分散体組成物及びそれ
を表面に処理してなる無機粉末に関する。
TECHNICAL FIELD The present invention relates to an inorganic powder dispersant for inorganic powder, an inorganic powder dispersion composition containing the same, and an inorganic powder obtained by treating the surface of the composition.

【0002】[0002]

【従来の技術及び発明が解決しようとする課題】無機粉
末用油中分散剤は種々の産業分野に応用されており、顔
料や充填剤を樹脂溶液に分散させた塗料やインク、炭酸
カルシウム、酸化チタン等充填剤をポリ塩化ビニル樹脂
等とともに可塑剤に分散させた床材・壁紙・シーリング
材用樹脂組成物、フィラードPPで代表される無機充填
剤を分散させた樹脂組成物、あるいは無機系研磨剤を配
合したスプレー洗浄剤等に使用される。このように無機
粉末を有機溶剤、可塑剤、樹脂等の油中に分散させる場
合、一般的に油中分散剤が使用される。
2. Description of the Related Art Dispersants in oils for inorganic powders have been applied to various industrial fields, such as paints and inks in which pigments and fillers are dispersed in a resin solution, calcium carbonate, oxides, and the like. A resin composition for flooring, wallpaper, and sealing materials in which a filler such as titanium is dispersed in a plasticizer together with a polyvinyl chloride resin, a resin composition in which an inorganic filler represented by filler PP is dispersed, or inorganic polishing. It is used as a spray cleaner containing an agent. When the inorganic powder is dispersed in an oil such as an organic solvent, a plasticizer, and a resin, a dispersant in oil is generally used.

【0003】このような分散剤の要求性能は、容易に短
時間で無機粉末を油中に分散させるとともに、長時間に
わたって無機粉末を沈降させることなく安定に分散さ
せ、あるいは無機粉末が沈降を起こしても容易に再分散
できる性能が挙げられる。また油中分散体の粘度が無機
粉末の配合によって高くなり目的用途で使用困難になる
場合、良好な分散特性を発揮し粘度を低減させる効果も
期待される。
[0003] The required performance of such a dispersant is to easily disperse the inorganic powder in the oil in a short time, stably disperse the inorganic powder without sedimentation for a long time, or cause the inorganic powder to sediment. Performance that can be easily redispersed. In addition, when the viscosity of the dispersion in oil becomes high due to the blending of the inorganic powder and it becomes difficult to use it in the intended application, the effect of exhibiting good dispersion characteristics and reducing the viscosity is expected.

【0004】また、無機粉末を、溶剤、可塑剤等の油
中、あるいはポリオレフィン樹脂等に添加する前の段階
で、酸性ガス、有機酸又はその塩等で表面処理する方法
(ここで無機粉末表面に吸着させる化合物を表面改質剤
と呼ぶ)がある。この場合、無機粉末粒子同士の凝集防
止性、かつ添加後に良好な油中分散性が望まれる。
In addition, a method in which the inorganic powder is subjected to a surface treatment with an acidic gas, an organic acid or a salt thereof in an oil such as a solvent or a plasticizer or before addition to a polyolefin resin or the like (here, the surface of the inorganic powder is used) The compound adsorbed on the surface is called a surface modifier). In this case, it is desired that the inorganic powder particles have a property of preventing aggregation and good dispersibility in oil after addition.

【0005】上記要求性能に対し、ポリオキシエチレン
アルキルフェニルエーテル等のエーテル類、アルキルス
ルホサクシネート塩、脂肪酸石鹸等の有機酸塩類、ある
いは官能基としてカルボキシル基、スルホン酸基、リン
酸基を持ったマレイン酸共重合体等のポリマー型分散剤
等が提案されている。また、無機粉末の表面改質剤とし
て、ステアリン酸又はそのナトリウム塩、ロジン酸ナト
リウム等の有機酸及び有機酸塩類等が用いられている。
[0005] With respect to the above required performance, ethers such as polyoxyethylene alkyl phenyl ether, organic acid salts such as alkylsulfosuccinate salts and fatty acid soaps, or carboxyl, sulfonic acid and phosphoric acid groups as functional groups. Polymer-type dispersants such as maleic acid copolymers have been proposed. Organic acids and organic acid salts such as stearic acid or its sodium salt, sodium rosinate, and the like are used as a surface modifier for the inorganic powder.

【0006】しかし、上記従来技術では、ある程度の分
散性能及び分散安定性を示すが、要求性能を十分に満足
させるものは見出されていない。
[0006] However, the above-mentioned prior art shows a certain level of dispersion performance and dispersion stability, but has not been found to satisfy the required performance sufficiently.

【0007】本発明の課題は、容易に短時間で無機粉末
を油中に分散させるとともに、長時間にわたって無機粉
末を沈降させることなく安定に分散させ、あるいは無機
粉末が沈降を起こしても容易に再分散でき、また無機粉
末を要因とする油中分散体組成物の粘度上昇を低減さ
せ、あるいは無機粉末の表面改質剤として使用した場合
でも良好な粒子凝集防止性能及び分散性を示す無機粉末
用油中分散剤を提供することである。
An object of the present invention is to easily disperse inorganic powder in oil in a short time and stably disperse the inorganic powder for a long time without causing sedimentation. Inorganic powder that can be redispersed and also exhibits good particle agglomeration prevention performance and dispersibility even when used as a surface modifier of the inorganic powder to reduce the increase in viscosity of the in-oil dispersion composition due to the inorganic powder. It is to provide a dispersant in oil for use.

【0008】[0008]

【課題を解決するための手段】本発明は、一般式(I)
で表される化合物(以下化合物(I)という)からなる
無機粉末用油中分散剤、それを含有する無機粉末分散体
組成物、及びそれを表面に処理してなる無機粉末であ
る。
The present invention provides a compound represented by the general formula (I):
(Hereinafter referred to as compound (I)), a dispersant for an inorganic powder in oil, an inorganic powder dispersion composition containing the same, and an inorganic powder obtained by treating the surface of the composition.

【0009】R1O(AO)nCH2COOM (I) (式中、R1は炭素数6〜24の直鎖あるいは分岐鎖のアル
キル基又はアルケニル基、もしくはそのようなアルキル
基で置換されたフェニル基を示し、AOは炭素数2〜3の
オキシアルキレン基、nはアルキレンオキサイドの平均
付加モル数を示す1〜20の数で、n個のAOは同一でも異
なっていても良い。M は水素原子、アルカリ金属、アル
カリ土類金属、アンモニウム又はアルカノールアンモニ
ウムを示す。)
R 1 O (AO) n CH 2 COOM (I) wherein R 1 is a straight-chain or branched-chain alkyl or alkenyl group having 6 to 24 carbon atoms, or is substituted by such an alkyl group. AO is an oxyalkylene group having 2 to 3 carbon atoms, n is a number of 1 to 20 indicating an average addition mole number of alkylene oxide, and n AOs may be the same or different. Represents a hydrogen atom, an alkali metal, an alkaline earth metal, ammonium or alkanol ammonium.)

【0010】[0010]

【発明の実施の形態】化合物(I)において、R1とし
て、ラウリル基、ミリスチル基、パルミチル基、ステア
リル基、オレイル基、ノニルフェニル基等が挙げられ、
炭素数12〜18、特に炭素数12〜14のものが好ましい。ま
た、AOとして、オキシエチレン基、オキシプロピレン基
が挙げられ、オキシエチレン基が好ましい。n個のAOは
オキシエチレン基とオキシプロピレン基のランダム付加
又はブロック付加のいずれでもよい。nは3〜12が好ま
しい。M は水素原子又はアルカリ金属が好ましく、特に
水素原子又はナトリウムが好ましい。
BEST MODE FOR CARRYING OUT THE INVENTION In the compound (I), R 1 includes a lauryl group, a myristyl group, a palmityl group, a stearyl group, an oleyl group, a nonylphenyl group, and the like.
Those having 12 to 18 carbon atoms, particularly those having 12 to 14 carbon atoms are preferred. AO includes an oxyethylene group and an oxypropylene group, and an oxyethylene group is preferable. The n AOs may be either random additions or block additions of oxyethylene and oxypropylene groups. n is preferably 3 to 12. M is preferably a hydrogen atom or an alkali metal, particularly preferably a hydrogen atom or sodium.

【0011】化合物(I)の具体例として、ポリオキシ
エチレン(エチレンオキサイド付加モル数10、以下POE
(10)のように略して表す)ラウリルエーテル酢酸及び
そのナトリウム塩、POE(4.5)ラウリルエーテル酢酸及び
そのナトリウム塩、POE(8)ミリスチルエーテル酢酸及び
そのナトリウム塩、POE(4)ステアリルエーテル酢酸及び
そのナトリウム塩等が挙げられる。
As a specific example of the compound (I), polyoxyethylene (ethylene oxide addition mole number: 10, hereinafter referred to as POE)
(Abbreviated as (10)) lauryl ether acetic acid and its sodium salt, POE (4.5) lauryl ether acetic acid and its sodium salt, POE (8) myristyl ether acetic acid and its sodium salt, POE (4) stearyl ether acetic acid and And its sodium salt.

【0012】化合物(I)を得るには、まず一般式(II) R1−OH (II) (式中、R1は前記の意味を示す。)で表されるアルコー
ルにエチレンオキサイド又はプロピレンオキサイドを付
加するか、あるいはそれらをランダム又はブロックで付
加して、一般式(III) R1O(AO)nH (III) (式中、R1, A 及びnは前記の意味を示す。)で表され
る化合物を合成する。一般式(II)で表されるアルコール
として、デシルアルコール、ラウリルアルコール、ミリ
スチルアルコール、セチルアルコール、ステアリルアル
コール等の炭素数6〜24の直鎖脂肪族アルコール、オキ
ソ法やチーグラー法を用いて合成された分岐鎖を有する
炭素数6〜24の分岐鎖アルコール等が挙げられ、これら
は単独でも混合して用いても良い。
In order to obtain the compound (I), first, ethylene alcohol or propylene oxide is added to an alcohol represented by the general formula (II) R 1 -OH (II) (wherein R 1 has the above-mentioned meaning). Or by adding them randomly or in blocks, to obtain a compound represented by the general formula (III) R 1 O (AO) n H (III) (wherein R 1 , A and n have the same meanings as described above) Is synthesized. As the alcohol represented by the general formula (II), straight-chain aliphatic alcohols having 6 to 24 carbon atoms such as decyl alcohol, lauryl alcohol, myristyl alcohol, cetyl alcohol, and stearyl alcohol, and synthesized using the oxo method or the Ziegler method. And a branched alcohol having 6 to 24 carbon atoms having a branched chain. These may be used alone or as a mixture.

【0013】次に一般式(III) で表される化合物に水酸
化ナトリウム等のアルカリを当量添加し、これとクロロ
酢酸とを脱塩反応させ、場合によってはこれをアルカリ
で中和し、塩を生成させて、化合物(I)を得る。
Next, an equivalent amount of an alkali such as sodium hydroxide is added to the compound represented by the general formula (III), and this is subjected to a desalting reaction with chloroacetic acid. To give compound (I).

【0014】本発明の無機粉末分散体組成物は、必須成
分として化合物(I)と無機粉末を含有する。無機粉末
として、充填剤、顔料、研磨剤等が挙げられ、具体的に
は、炭酸カルシウム、炭酸マグネシウム、炭酸バリウム
等の炭酸塩、カオリン、ケイ酸アルミニウム、ケイ酸カ
ルシウム、クレー、タルク、マイカ、セリサイト、ベン
トナイト等のケイ酸塩、硫酸カルシウム、硫酸バリウム
等の硫酸塩、シリカ、アルミナ、マグネシア、三酸化ア
ンチモン、酸化チタン、ホワイトカーボン、ケイソウ
土、酸化鉄等の金属酸化物、水酸化アルミニウム、水酸
化鉄等の金属水酸化物、その他、ベンガラ、炭化ケイ
素、窒化ケイ素、窒化ホウ素、ジルコニア、チタン酸バ
リウム、カーボンブラック、グラファイト等が挙げられ
る。なお、これらの無機粉末の平均粒径は 100μm以下
が好ましく、50μm以下がさらに好ましい。
The inorganic powder dispersion composition of the present invention contains the compound (I) and inorganic powder as essential components. Examples of the inorganic powder include fillers, pigments, abrasives, and the like.Specifically, calcium carbonate, magnesium carbonate, carbonates such as barium carbonate, kaolin, aluminum silicate, calcium silicate, clay, talc, mica, Silicates such as sericite and bentonite, sulfates such as calcium sulfate and barium sulfate, silica, alumina, magnesia, antimony trioxide, metal oxides such as titanium oxide, white carbon, diatomaceous earth, iron oxide, and aluminum hydroxide And metal hydroxides such as iron hydroxide and the like, and bengara, silicon carbide, silicon nitride, boron nitride, zirconia, barium titanate, carbon black, graphite and the like. The average particle size of these inorganic powders is preferably 100 μm or less, more preferably 50 μm or less.

【0015】本発明において無機粉末を分散させる分散
媒として、ジ−2−エチルヘキシルフタレート、ジオク
チルフタレート、酢酸エチル、大豆油、アマニ油等のエ
ステル類、灯油、軽油、重油等の燃料油、ヘキサン、シ
クロヘキサン、イソオクタン等の脂肪族炭化水素類、ベ
ンゼン、トルエン、キシレン等の芳香族炭化水素類、
1,1,1−トリクロロエタン、トリクロロエチレン、
クロロジフルオロメタン等のハロゲン化炭化水素、流動
パラフィン、塗料用液状樹脂、及びポリプロピレンに代
表される樹脂等が挙げられる。
In the present invention, as a dispersion medium for dispersing the inorganic powder, esters such as di-2-ethylhexyl phthalate, dioctyl phthalate, ethyl acetate, soybean oil and linseed oil, fuel oils such as kerosene, light oil and heavy oil, hexane, Aliphatic hydrocarbons such as cyclohexane and isooctane, aromatic hydrocarbons such as benzene, toluene and xylene,
1,1,1-trichloroethane, trichloroethylene,
Examples include halogenated hydrocarbons such as chlorodifluoromethane, liquid paraffin, liquid resins for paints, and resins represented by polypropylene.

【0016】本発明の無機粉末分散体組成物中の化合物
(I)の配合量は、無機粉末 100重量部に対して、分散
効果と経済性の観点から0.05〜10重量部、更に 0.1〜5
重量部、特に 0.5〜5重量部が好ましい。
The compounding amount of the compound (I) in the inorganic powder dispersion composition of the present invention is 0.05 to 10 parts by weight, more preferably 0.1 to 5 parts by weight, based on 100 parts by weight of the inorganic powder, from the viewpoint of dispersing effect and economy.
Part by weight, especially 0.5 to 5 parts by weight is preferred.

【0017】本発明の無機粉末分散体組成物には、本発
明の効果を損なわない範囲で、他の分散剤、例えばアル
キルスルホサクシネート塩、脂肪酸塩、ソルビタンモノ
オレート等の多価アルコール脂肪酸エステル類、ロジン
酸ナトリウム等の樹脂酸塩、また無機粉末と共に樹脂を
分散させる場合には、その樹脂分散剤であるポリオキシ
エチレンノニルフェニルエーテル等のアルキルエーテル
類、ポリエチレングリコール、ポリプロピレングリコー
ル等のエーテル類及びそれの脂肪酸エステル類、ポリオ
キシエチレン多価アルコール脂肪酸エステル等を併用し
てもよい。
The inorganic powder dispersion composition of the present invention may contain other dispersants such as alkylsulfosuccinate salts, fatty acid salts, polyhydric alcohol fatty acid esters such as sorbitan monooleate, as long as the effects of the present invention are not impaired. , A resin salt such as sodium rosin acid, or when dispersing a resin together with an inorganic powder, an alkyl ether such as polyoxyethylene nonyl phenyl ether as a resin dispersant, and an ether such as polyethylene glycol and polypropylene glycol. And fatty acid esters thereof, polyoxyethylene polyhydric alcohol fatty acid esters, and the like.

【0018】本発明の油中分散剤を用いて無機粉末の油
中分散体を得るには、通常の分散体の製法に従えばよ
く、例えば化合物(I)を溶解した油中に無機粉末を配
合して、撹拌機により撹拌混合する等の方法を用いれば
よい。
In order to obtain a dispersion of inorganic powder in oil using the dispersant in oil of the present invention, a conventional method of preparing a dispersion may be used. For example, the inorganic powder is dissolved in oil in which the compound (I) is dissolved. A method such as mixing and stirring with a stirrer may be used.

【0019】本発明の化合物(I)からなる油中分散剤
は、無機粉末表面に吸着するように処理して無機粉末の
分散性を向上させる表面処理剤としても用いることがで
きる。油中分散剤を表面に処理してなる無機粉末を用い
て無機粉末の油中分散体を製造すると、油中分散剤が効
率良く無機粉末表面上に吸着しているので、分散剤の性
能をより発揮させることができる。
The dispersant in oil comprising the compound (I) of the present invention can also be used as a surface treatment agent for improving the dispersibility of the inorganic powder by treating it so as to be adsorbed on the surface of the inorganic powder. When an inorganic powder dispersion of an inorganic powder is produced using an inorganic powder obtained by treating a surface of the dispersant in an oil, the dispersant in the oil is efficiently adsorbed on the surface of the inorganic powder. It can be demonstrated more.

【0020】かかる表面処理された無機粉末を得るに
は、例えば無機粉末の水懸濁液中に化合物(I)を添加
して撹拌混合することにより、無機粉末の表面に化合物
(I)を吸着させた後、脱水、乾燥、解砕、分級する
か、又は無機粉末に化合物(I)を噴霧する等の方法が
用いられる。化合物(I)の使用量は、分散効果と経済
性の観点から、無機粉末100 重量部に対して、0.05〜10
重量部、更に0.1 〜5重量部、特に0.5 〜5重量部が好
ましい。
In order to obtain such a surface-treated inorganic powder, the compound (I) is adsorbed on the surface of the inorganic powder by, for example, adding the compound (I) to an aqueous suspension of the inorganic powder and mixing with stirring. After that, a method of dehydrating, drying, crushing, classifying, or spraying the compound (I) on the inorganic powder is used. The amount of the compound (I) used is 0.05 to 10 parts by weight based on 100 parts by weight of the inorganic powder from the viewpoint of the dispersing effect and economic efficiency.
Parts by weight, more preferably 0.1 to 5 parts by weight, particularly preferably 0.5 to 5 parts by weight.

【0021】ここで使用される無機粉末は、無機充填剤
が好ましく、具体的には炭酸カルシウム、水酸化アルミ
ニウム、水酸化マグネシウム、タルク、クレー、シリ
カ、ベンガラ、酸化チタン、カーボンブラック、特に炭
酸カルシウム、水酸化マグネシウム、タルク、クレー、
カオリンが好ましい。
The inorganic powder used here is preferably an inorganic filler, specifically, calcium carbonate, aluminum hydroxide, magnesium hydroxide, talc, clay, silica, red iron oxide, titanium oxide, carbon black, and particularly calcium carbonate. , Magnesium hydroxide, talc, clay,
Kaolin is preferred.

【0022】[0022]

【発明の効果】本発明の油中分散剤を、有機溶剤、可塑
剤、樹脂組成物等に無機粉末を分散させる際に用いる
と、良好な分散性、分散安定性を付与でき、粘度上昇を
抑えることができる。また本発明の油中分散剤を無機粉
末の表面に処理すると、良好な粒子凝集防止性、分散性
を付与することができる。
When the dispersant in oil of the present invention is used for dispersing an inorganic powder in an organic solvent, a plasticizer, a resin composition, or the like, good dispersibility and dispersion stability can be imparted, and the viscosity increases. Can be suppressed. When the surface of an inorganic powder is treated with the dispersant in oil of the present invention, good particle aggregation prevention and dispersibility can be imparted.

【0023】[0023]

【実施例】実施例1〜18及び比較例1〜12 無機粉末として重質炭酸カルシウム(白石工業(株)ホ
ワイトンH)、分散媒としてジ−2−エチルヘキシルフ
タレート(DOP)(花王(株)ビニサイザー80)又は
流動パラフィン、分散剤として下記の本発明品及び比較
品を用い、表1〜4に示す割合で配合し、らいかい機で
均一に撹拌分散した後、真空下で脱泡して無機粉末分散
体組成物を調製した。
Examples 1 to 18 and Comparative Examples 1 to 12 Heavy calcium carbonate (Whiteton H, Shiroishi Kogyo Co., Ltd.) as an inorganic powder and di-2-ethylhexyl phthalate (DOP) as a dispersion medium (Kao Corporation) Vinicizer 80) or liquid paraffin, using the following product of the present invention and a comparative product as a dispersing agent, blended in the ratio shown in Tables 1 to 4, uniformly stirred and dispersed by a grinder, and then defoamed under vacuum. An inorganic powder dispersion composition was prepared.

【0024】<分散剤> 本発明品1:POE(4.5)ラウリルエーテル酢酸 本発明品2:POE(4)ステアリルエーテル酢酸 本発明品3:POE(10)ラウリルエーテル酢酸 本発明品4:POE(12)ステアリルエーテル酢酸 本発明品5:POE(10)ラウリルエーテル酢酸ナトリウム 比較品1:POE(10)ノニルフェニルエーテル 比較品2:ステアリン酸 比較品3:ビス−2−エチルヘキシルスルホサクシネー
トナトリウム塩 比較品4:ポリカルボン酸系高分子活性剤:ホモゲノー
ルL-95, 花王(株)製 得られた無機粉末分散体組成物について、下記方法で粘
度を測定し、分散性及び分散安定性を評価した。結果を
表1〜4に示す。
<Dispersant> Invention product 1: POE (4.5) lauryl ether acetic acid Invention product 2: POE (4) stearyl ether acetic acid Invention product 3: POE (10) lauryl ether acetic acid Invention product 4: POE ( 12) Stearyl ether acetic acid Invention product 5: POE (10) sodium lauryl ether acetate Comparative product 1: POE (10) nonylphenyl ether Comparative product 2: Stearic acid Comparative product 3: Bis-2-ethylhexyl sulfosuccinate sodium salt Comparison Article 4: Polycarboxylic acid polymer activator: Homogenol L-95, manufactured by Kao Corporation The viscosity of the obtained inorganic powder dispersion composition was measured by the following method, and the dispersibility and dispersion stability were evaluated. . The results are shown in Tables 1 to 4.

【0025】(1) 分散性及び粘度 分散性は無機粉末分散体組成物を100 mLのふた付きガラ
ス製サンプル管(直径3.5cm)に入れて25℃の恒温水槽に
2時間放置した後、以下の基準で評価した。 ○:すべての無機粉末が均一に分散し、全く分散媒と無
機粉末の分離が起こらない △:ほとんどの無機粉末は分散しているが、わずかに分
離している ×:分散不良で、分散体の流動性が全くない 粘度は、上記分散性が△以上のものについて、25℃、相
対湿度60%の恒温恒湿室内でブルックフィールドBL型
粘度計を用い、回転数6r/min の条件で測定した。粘度
が低いほど分散性が良好である。
(1) Dispersibility and Viscosity Dispersibility was measured by placing an inorganic powder dispersion composition in a 100 mL glass sample tube (3.5 cm in diameter) with a lid and leaving it in a constant temperature water bath at 25 ° C. for 2 hours. The evaluation was based on the following criteria. :: All inorganic powders are uniformly dispersed, and no separation of the dispersion medium and the inorganic powders occurs. Δ: Most of the inorganic powders are dispersed but slightly separated. X: Poorly dispersed, dispersion No fluidity is measured. The viscosity is measured with a Brookfield BL viscometer at 25 ° C and a relative humidity of 60% using a Brookfield BL viscometer at a rotational speed of 6 r / min. did. The lower the viscosity, the better the dispersibility.

【0026】(2) 分散安定性 (1) の分散性の試験で△以上の評価であったものを、上
記サンプル管中にて25℃の恒温室で24時間静置し、分散
状態、無機粉末の沈降状態を観察して、下記基準で評価
した。 ○:分散媒と分散体の分離がなく、無機粉末の沈降も見
られない △:分散媒が少し分離し、無機粉末の沈降も若干見られ
る ×:分散媒がかなり分離し、無機粉末の沈降もかなりあ
(2) Dispersion Stability The dispersibility test of (1), which was evaluated as △ or more, was allowed to stand in a constant temperature room at 25 ° C. for 24 hours in the sample tube, and the dispersion state, inorganic The sedimentation state of the powder was observed and evaluated according to the following criteria. :: Dispersion medium and dispersion were not separated, and no sedimentation of inorganic powder was observed. Δ: Dispersion medium was slightly separated, and sedimentation of inorganic powder was slightly observed. X: Dispersion medium was considerably separated, and sedimentation of inorganic powder was observed. Is also quite

【0027】[0027]

【表1】 [Table 1]

【0028】[0028]

【表2】 [Table 2]

【0029】[0029]

【表3】 [Table 3]

【0030】[0030]

【表4】 [Table 4]

【0031】実施例19〜27及び比較例13〜15 実施例1〜9及び比較例1〜6と同じ炭酸カルシウムを
用い、この水懸濁液に、分散剤として上記本発明品1〜
5、比較品2、及びロジン酸ナトリウム(以下比較品5
という)を表5及び6に示した所定量添加し、ホモミキ
サーで十分に撹拌混合した。それを脱水、乾燥、解砕処
理を行い、表面処理した無機粉末を得た。この無機粉末
と実施例1〜9及び比較例1〜6と同じDOPを表5及
び6に示した所定量配合し、らいかい機で均一に撹拌分
散した後、真空下で脱泡して無機粉末分散体組成物を調
製した。得られた無機粉末分散体組成物について、実施
例1〜9及び比較例1〜6と同じ方法で粘度を測定し、
分散性及び分散安定性を評価した。結果を表5及び6に
示す。
Examples 19 to 27 and Comparative Examples 13 to 15 The same calcium carbonate as used in Examples 1 to 9 and Comparative Examples 1 to 6 was used.
5, comparative product 2, and sodium rosinate (hereinafter referred to as comparative product 5
) Was added in a predetermined amount shown in Tables 5 and 6, and thoroughly mixed with a homomixer. It was dehydrated, dried and crushed to obtain a surface-treated inorganic powder. The inorganic powder and the same DOP as in Examples 1 to 9 and Comparative Examples 1 to 6 were blended in predetermined amounts shown in Tables 5 and 6, and uniformly stirred and dispersed by a grinder, and then defoamed under vacuum to remove inorganic particles. A powder dispersion composition was prepared. About the obtained inorganic powder dispersion composition, the viscosity was measured by the same method as in Examples 1 to 9 and Comparative Examples 1 to 6,
Dispersibility and dispersion stability were evaluated. The results are shown in Tables 5 and 6.

【0032】[0032]

【表5】 [Table 5]

【0033】[0033]

【表6】 [Table 6]

───────────────────────────────────────────────────── フロントページの続き Fターム(参考) 4D077 AA03 AA10 AB04 AC05 BA03 DD03X DD08X DD29X DE07X DE10X 4H003 AB05 BA12 BA20 EA24 EA26 EB09 ED02 FA05 FA16 FA30 FA32 FA37 4J002 AE052 BB122 CH051 DA026 DA036 DE076 DE096 DE116 DE126 DE136 DE146 DE236 DG056 DJ006 DJ026 DJ036 DJ046 DK006 EA017 EA027 EA057 EB027 EB067 EH037 EH047 FD016 FD096 GD00 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4D077 AA03 AA10 AB04 AC05 BA03 DD03X DD08X DD29X DE07X DE10X 4H003 AB05 BA12 BA20 EA24 EA26 EB09 ED02 FA05 FA16 FA30 FA32 FA37 4J002 AE052 BB122 CH051 DA026 DE036 DE126 DE076 DE036 DJ006 DJ026 DJ036 DJ046 DK006 EA017 EA027 EA057 EB027 EB067 EH037 EH047 FD016 FD096 GD00

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 一般式(I)で表される化合物からなる
無機粉末用油中分散剤。 R1O(AO)nCH2COOM (I) (式中、R1は炭素数6〜24の直鎖あるいは分岐鎖のアル
キル基又はアルケニル基、もしくはそのようなアルキル
基で置換されたフェニル基を示し、AOは炭素数2〜3の
オキシアルキレン基、nはアルキレンオキサイドの平均
付加モル数を示す1〜20の数で、n個のAOは同一でも異
なっていても良い。M は水素原子、アルカリ金属、アル
カリ土類金属、アンモニウム又はアルカノールアンモニ
ウムを示す。)
1. A dispersant for an inorganic powder in oil comprising a compound represented by the general formula (I). R 1 O (AO) n CH 2 COOM (I) (wherein, R 1 is a linear or branched alkyl or alkenyl group having 6 to 24 carbon atoms, or a phenyl group substituted with such an alkyl group) Wherein AO is an oxyalkylene group having 2 to 3 carbon atoms, n is a number of 1 to 20 indicating an average addition mole number of the alkylene oxide, and n AOs may be the same or different, and M is a hydrogen atom. , Alkali metal, alkaline earth metal, ammonium or alkanol ammonium.)
【請求項2】 請求項1記載の油中分散剤を含有する無
機粉末分散体組成物。
2. An inorganic powder dispersion composition containing the dispersant in oil according to claim 1.
【請求項3】 請求項1記載の油中分散剤を表面に処理
してなる無機粉末。
3. An inorganic powder obtained by treating the surface with the dispersant in oil according to claim 1.
JP11075434A 1999-03-19 1999-03-19 In-oil dispersant for inorganic powder Pending JP2000262883A (en)

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