JPH07300568A - Production of fine inorganic powder - Google Patents

Production of fine inorganic powder

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Publication number
JPH07300568A
JPH07300568A JP9320094A JP9320094A JPH07300568A JP H07300568 A JPH07300568 A JP H07300568A JP 9320094 A JP9320094 A JP 9320094A JP 9320094 A JP9320094 A JP 9320094A JP H07300568 A JPH07300568 A JP H07300568A
Authority
JP
Japan
Prior art keywords
wet
drying
pass
inorganic powder
inorganic
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
JP9320094A
Other languages
Japanese (ja)
Inventor
Manabu Abe
Yumiko Takase
Saburo Yashima
三郎 八嶋
学 阿部
祐美子 高瀬
Original Assignee
Fuaimatetsuku:Kk
株式会社ファイマテック
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 Fuaimatetsuku:Kk, 株式会社ファイマテック filed Critical Fuaimatetsuku:Kk
Priority to JP9320094A priority Critical patent/JPH07300568A/en
Publication of JPH07300568A publication Critical patent/JPH07300568A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To produce a fine inorganic powder which does not undergo secondary agglomeration and can give an easily disintegrable dry cake by wet-grinding an inorganic powder and drying the product of grinding. CONSTITUTION:An inorganic powder is wet-ground in an aqueous medium in the presence of a water-soluble cationic copolymer dispersant comprising 10-99mol% structural units derived from a diallylamine salt and/or alkyldiallylamine salt and 1-90mol% structural units derived from a nonionic vinyl monomer.

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、プラスチック用フィラ
ーなどとして幅広く利用することができる重質炭酸カル
シウム、軽質炭酸カルシウム、タルク、セリサイト、硫
酸カルシウム、モンモリロナイトなどの無機微粉体の製
造方法に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing inorganic fine powders such as heavy calcium carbonate, light calcium carbonate, talc, sericite, calcium sulfate and montmorillonite which can be widely used as fillers for plastics. Is.
【0002】[0002]
【従来の技術】無機微粉体の製造方法には、軽質炭酸カ
ルシウムのような合成法と、重質炭酸カルシウムのよう
に天然の石灰石を粉砕する方法がある。重質炭酸カルシ
ウムなどの無機粉体の微細化は、主に乾式粉砕で行われ
ており、この場合、粉砕後の平均粒径は2μ程度であ
る。そして、2μ以下の粒径の細かいものが必要な場合
には、湿式粉砕が行なわれている。具体的には、石灰石
のような無機物を乾式粉砕により粗粉砕した後、アニオ
ン系の分散剤の存在下で湿式粉砕している。このように
して得られた湿式粉砕品はスラリー状のため製紙用のフ
ィラーやコーティング剤などに使用が限られるという問
題がある。従って、より広範な用途を目指して、前記湿
式粉砕後、次いで分級した後、必要に応じて沈殿、濃縮
又は脱水を行い、乾燥後、粉砕して製品とすることがし
ばしば行われている。しかしながら、このように湿式粉
砕した後、乾燥して得られた無機粉体は、プラスチック
などのフィラーとして使用が可能となるものの、無機微
粉体自体が強い2次凝集を起こし、乾燥後に多量の粗粒
子が発生し、その処理が問題となるとともに、得られる
無機微粉体の収量が低下し、コスト高になってしまう。
又、粗粒子の混在した無機微粉体を使用すると所望の性
能が得られないとの問題がある。一方、特開平5−26
3010号公報には、杪紙用填料として使用する炭酸カ
ルシウムなどの顔料を水中に分散するのに適した水溶性
カチオン性コポリマー分散剤が記載されている。
2. Description of the Related Art As a method for producing an inorganic fine powder, there are a synthetic method such as light calcium carbonate and a method in which natural limestone such as heavy calcium carbonate is crushed. Refining of inorganic powder such as ground calcium carbonate is mainly carried out by dry crushing, and in this case, the average particle size after crushing is about 2μ. When a fine particle having a particle size of 2 μ or less is required, wet pulverization is performed. Specifically, an inorganic substance such as limestone is roughly pulverized by dry pulverization and then wet pulverized in the presence of an anionic dispersant. The wet pulverized product obtained in this manner has a problem that its use is limited to fillers and coating agents for papermaking because it is a slurry. Therefore, for a wider range of applications, it is often the case that after the wet pulverization, then classification, then, if necessary, precipitation, concentration or dehydration, drying and pulverization to obtain a product. However, although the inorganic powder obtained by wet-milling and drying in this way can be used as a filler for plastics and the like, the inorganic fine powder itself causes strong secondary agglomeration, and a large amount of coarse powder is formed after drying. Particles are generated and the treatment thereof becomes a problem, and the yield of the obtained inorganic fine powder is reduced, resulting in high cost.
Further, there is a problem that the desired performance cannot be obtained when the inorganic fine powder in which coarse particles are mixed is used. On the other hand, JP-A-5-26
Japanese Patent No. 3010 describes a water-soluble cationic copolymer dispersant suitable for dispersing a pigment such as calcium carbonate used as a paper filler in water.
【0003】[0003]
【発明が解決しようとする課題】本発明は、湿式粉砕し
た後、乾燥した時に無機微粉体の2次凝集が少なく、乾
燥ケーキが潰れ易い無機微粉体を製造できる方法を提供
することを目的とする。
SUMMARY OF THE INVENTION It is an object of the present invention to provide a method for producing an inorganic fine powder which is less likely to have secondary agglomeration of the inorganic fine powder when dried after being wet-milled and whose dry cake is easily crushed. To do.
【0004】[0004]
【課題を解決するための手段】本発明は、特開平5−2
63010号公報に記載の水溶性カチオン性コポリマー
分散剤の存在下で湿式粉砕し、次いで乾燥すると上記課
題を効率よく達成できるとの知見に基づいてなされたの
である。すなわち、本発明は、無機粉体を、ジアリルア
ミン塩及び/又はアルキルジアリルアミン塩10〜99
モル%と非イオン性ビニルモノマー1〜90モル%とを
構成単位とする水溶性カチオン性コポリマー分散剤の存
在下、水性媒体中で湿式粉砕し、次いで乾燥することを
特徴とする無機微粉体の製造方法を提供する。本発明で
使用する水溶性カチオン性コポリマー分散剤としては、
特開平5−263010号公報などに記載のカチオン性
コポリマー分散剤の一種又は二種以上の混合物を使用す
ることができる。特開平5−263010号公報の記載
内容は本明細書に含まれるものとする。本発明で使用す
る水溶性カチオン性コポリマー分散剤を構成するアルキ
ルジアリルアミン塩としては、炭素数1〜8のアルキル
基、好ましくは炭素数1〜4のアルキル基を有するもの
があげられる。又、ジアリルアミン及びアルキルジアリ
ルアミンの塩としては、塩酸、硫酸、硝酸、酢酸などの
無機酸や有機酸との塩があげられる。
The present invention is disclosed in Japanese Laid-Open Patent Publication No. 5-2.
This was made based on the finding that the above-mentioned problems can be efficiently achieved by wet-milling in the presence of a water-soluble cationic copolymer dispersant described in JP-A-63010 and then drying. That is, in the present invention, the inorganic powder is used as the diallylamine salt and / or the alkyldiallylamine salt 10 to 99.
Inorganic fine powder characterized by being wet-ground in an aqueous medium in the presence of a water-soluble cationic copolymer dispersant having mol% and 1 to 90 mol% of a nonionic vinyl monomer as a constituent unit, and then dried. A manufacturing method is provided. As the water-soluble cationic copolymer dispersant used in the present invention,
One or a mixture of two or more of the cationic copolymer dispersants described in JP-A-5-263010 and the like can be used. The contents described in JP-A-5-263010 are included in the present specification. Examples of the alkyldiallylamine salt constituting the water-soluble cationic copolymer dispersant used in the present invention include those having an alkyl group having 1 to 8 carbon atoms, preferably an alkyl group having 1 to 4 carbon atoms. Examples of salts of diallylamine and alkyldiallylamine include salts with inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid and acetic acid, and organic acids.
【0005】本発明で使用する水溶性カチオン性コポリ
マー分散剤を構成する非イオン性ビニルモノマーとして
は、アクリルアミド、メタクリルアミド、N−ビニルピ
ロリドン、(メタ)アクリル酸2−ヒドロキシエチルエ
ステル、(メタ)アクリル酸メチルエステル、(メタ)
アクリル酸エチルエステル、(メタ)アクリル酸ブチル
エステルなどが挙げられる。これらのうちアクリルアミ
ド及び/又はメタクリルアミドが好ましい。本発明で使
用する水溶性カチオン性コポリマー分散剤の構成単位で
あるジアリルアミン塩及び/又はアルキルジアリルアミ
ン塩と非イオン性ビニルモノマーとのモル比は、任意と
することができるが、10/90〜99/1(モル比:
以下同じ)とするのがよく、好ましくは50/50〜9
9/1、更に好ましくは80/20〜98/2である。
該カチオン性コポリマー分散剤の極限粘度は通常0.05
〜3.00、好ましくは0.10〜1.80、特に好ましくは
0.15〜0.70である。該カチオン性コポリマー分散剤
は、特開平5−263010号公報に記載の方法により
容易に製造することができる。
As the nonionic vinyl monomer constituting the water-soluble cationic copolymer dispersant used in the present invention, acrylamide, methacrylamide, N-vinylpyrrolidone, (meth) acrylic acid 2-hydroxyethyl ester, (meth) Acrylic acid methyl ester, (meth)
Examples include acrylic acid ethyl ester and (meth) acrylic acid butyl ester. Of these, acrylamide and / or methacrylamide are preferred. The molar ratio of the diallylamine salt and / or the alkyldiallylamine salt, which is a constituent unit of the water-soluble cationic copolymer dispersant used in the present invention, and the nonionic vinyl monomer may be any, but it is 10/90 to 99. / 1 (molar ratio:
The same applies hereinafter), and preferably 50/50 to 9
9/1, more preferably 80/20 to 98/2.
The intrinsic viscosity of the cationic copolymer dispersant is usually 0.05.
~ 3.00, preferably 0.10 to 1.80, particularly preferably
It is 0.15 to 0.70. The cationic copolymer dispersant can be easily produced by the method described in JP-A-5-263010.
【0006】本発明で対象とする無機物としては、重質
炭酸カルシウム、軽質炭酸カルシウム、タルク、セリサ
イト、硫酸カルシウム、モンモリロナイト、ゼオライ
ト、亜硫酸カルシウム、水酸化アルミニウム、酸化アル
ミニウム、酸化亜鉛、硫酸バリウム、カオリンなどの各
種無機物の一種又は二種以上の混合物があげられる。本
発明では、このような無機物を、直ちに湿式粉砕するこ
とができるが、湿式粉砕に先立って、予め乾式粉砕して
おくのがよい。この際、無機物の粒径を40mm以下、好
ましくは平均粒径を2mm〜2μ程度に粉砕しておくのが
よい。本発明では、次いで上記カチオン性コポリマー分
散剤の存在下で無機物を湿式粉砕する。具体的には、無
機物/水性媒体(好ましくは水)との重量比が70/3
0〜30/70、好ましくは60/40〜40/60の
範囲となるように無機物に水性媒体を加え、ここにカチ
オン性コポリマー分散剤を固形分として、無機物100
重量部当り0.01〜1重量部、好ましくは0.01〜0.7
重量部添加し、常法により湿式粉砕する。又は、上記範
囲の量となるカチオン性コポリマー分散剤を予め溶解し
てなる水性媒体を無機物と混合し、常法により湿式粉砕
する。湿式粉砕は、バッチ式でも連続式でもよく、サン
ドミル、アトライター、ボールミルなどの粉砕媒体を使
用したミルなどが使用するのが好ましい。このように湿
式粉砕することにより、平均粒径が2μm 以下、好まし
くは平均粒径1〜0.3μmのものが得られる。
Inorganic substances of the present invention include heavy calcium carbonate, light calcium carbonate, talc, sericite, calcium sulfate, montmorillonite, zeolite, calcium sulfite, aluminum hydroxide, aluminum oxide, zinc oxide, barium sulfate, Examples thereof include one kind or a mixture of two or more kinds of various inorganic substances such as kaolin. In the present invention, such an inorganic substance can be immediately wet-milled, but it is preferable to dry-mill it in advance prior to wet-milling. At this time, it is preferable to grind the inorganic particles to a particle size of 40 mm or less, preferably about 2 mm to 2 μ. In the present invention, the inorganic material is then wet-milled in the presence of the above cationic copolymer dispersant. Specifically, the weight ratio of inorganic material / aqueous medium (preferably water) is 70/3.
An aqueous medium is added to the inorganic substance so that the amount of the inorganic copolymer is 0 to 30/70, preferably 60/40 to 40/60, and the cationic copolymer dispersant is added as a solid content to the inorganic substance 100.
0.01 to 1 part by weight, preferably 0.01 to 0.7, per part by weight
Add by weight, and wet pulverize by a conventional method. Alternatively, an aqueous medium prepared by previously dissolving a cationic copolymer dispersant in an amount within the above range is mixed with an inorganic substance, and wet pulverized by a conventional method. The wet pulverization may be a batch type or a continuous type, and it is preferable to use a mill using a grinding medium such as a sand mill, an attritor, or a ball mill. By such wet pulverization, an average particle size of 2 μm or less, preferably an average particle size of 1 to 0.3 μm can be obtained.
【0007】本発明では、次いで、湿式粉砕品を乾燥す
るが、乾燥前に、分級工程を設けて、350メッシュオ
ンといった祖粉を除くことができる。本発明における乾
燥は、熱風乾燥、粉噴乾燥など公知の方法により行うこ
とができるが、媒体流動乾燥により行なうのが好まし
い。媒体流動乾燥は、乾燥塔内で熱風により流動化状態
にある媒体粒子群(流動層)にスラリー状物質を供給
し、供給されたスラリー状物質は、活発に流動化してい
る媒体粒子の表面に膜状に付着しながら流動層内に分散
され、熱風による乾燥作用を受けることにより各種物質
を乾燥する方法である。このような媒体流動乾燥は、例
えば、株式会社 奈良機械製作所製の媒体流動乾燥装
置、メディア スラリー ドライヤーなどを用いて容易
に行うことができる。この媒体流動乾燥を用いると乾燥
と凝集粒子の一次粒子化が同時に行われるので好まし
い。また、乾燥と同時にステアリン酸などの脂肪酸によ
る表面処理を同時に行なうことができる。本発明の方法
により得られた湿式粉砕スラリーを媒体流動乾燥する
と、祖粉量が極めて少ない無機微粉体が得られる。しか
しながら、媒体流動乾燥後、所望の方法で粒子の粉砕と
分級とを行うことができる。一方、媒体流動乾燥の代わ
りに、通常の熱風乾燥により湿式粉砕品を乾燥した場合
には、得られたケーキをさらに所望の方法で粒子の粉砕
と分級とを行うのがよい。本発明の方法により得られた
湿式粉砕品の乾燥ケーキは、潰れ易く、容易に無機微粉
体を得ることができる。従って、乾燥ケーキを粉砕する
ことなく、製品とすることができる。
In the present invention, the wet pulverized product is then dried. Before the drying, a classification step may be provided to remove the coarse powder such as 350 mesh on. The drying in the present invention can be carried out by a known method such as hot air drying or powder spray drying, but it is preferably carried out by medium fluidized drying. In fluidized medium drying, a slurry-like substance is supplied to a group of medium particles (fluidized bed) in a fluidized state by hot air in a drying tower, and the supplied slurry-like substance is applied to the surface of the actively fluidized medium particles. It is a method in which various substances are dried while being dispersed in a fluidized bed while adhering in a film form and subjected to a drying action by hot air. Such medium fluidized drying can be easily performed using, for example, a medium fluidized drying device and a media slurry dryer manufactured by Nara Machinery Co., Ltd. It is preferable to use this medium fluidized drying because drying and primary particle formation of agglomerated particles are performed at the same time. Further, the surface treatment with a fatty acid such as stearic acid can be carried out simultaneously with the drying. When the wet pulverized slurry obtained by the method of the present invention is fluidized and dried in a medium, an inorganic fine powder having an extremely small amount of base powder is obtained. However, after fluidized drying of the medium, the particles can be pulverized and classified by a desired method. On the other hand, when the wet pulverized product is dried by ordinary hot air drying instead of the medium fluidized drying, it is preferable to further pulverize and classify the obtained cake by a desired method. The dry cake of the wet pulverized product obtained by the method of the present invention is easily crushed, and the inorganic fine powder can be easily obtained. Therefore, the dried cake can be made into a product without crushing.
【0008】[0008]
【発明の効果】本発明の方法によれば、湿式粉砕した
後、乾燥した時に無機微粉体の2次凝集が少なく、乾燥
ケーキが潰れ易く、無機微粉体がポリマーマトリックス
中などに対して分散性がよい無機微粉体を製造できる。
従って、本発明の方法により得られた乾燥ケーキや無機
微粉体は、そのままポリマー添加用フィラーや製紙用フ
ィラーや体質顔料として幅広く利用することができる。
次に実施例により本発明を説明する。
EFFECTS OF THE INVENTION According to the method of the present invention, the secondary agglomeration of the inorganic fine powder is small when dried after wet pulverization, the dried cake is easily crushed, and the inorganic fine powder is dispersible in the polymer matrix. It is possible to produce a fine inorganic powder having good quality.
Therefore, the dried cake and the inorganic fine powder obtained by the method of the present invention can be widely used as they are as a filler for polymer addition, a filler for papermaking and an extender pigment.
Next, the present invention will be described with reference to examples.
【0009】[0009]
【実施例】参考例1 還流冷却器、温度計、滴下ロート、攪拌装置およびガス
導入管を備えた反応器(容量1L)にジアリルアミン塩
酸塩(60%)500部とアクリルアミド(40%)2
00部を入れ、窒素ガスを流入させながら系内温度を5
0℃に昇温した。攪拌下で重合開始剤、2,2−アゾビ
ス(2−アミジノプロパン)ジヒドロクロライド(10
%)40部を2時間おきに4回に分けて加えた。10時
間反応し粘稠な淡黄色液状物を得た。これを50g採
り、500mlのアセトン中に注ぐと白色の沈澱を生じ
た。沈澱を濾別しさらに2回 100mlのアセトンでよ
く洗浄した後真空乾燥して白色固体状の水溶性カチオン
性コポリマー分散剤23.5gを得た。得られたコポリマ
ーの1N−NaCl水溶液中、25℃での極限粘度は2.
30(dl/g)、GPCより求めた重量平均分子量は
65.0万であった。
EXAMPLES Reference Example 1 500 parts of diallylamine hydrochloride (60%) and acrylamide (40%) were placed in a reactor (capacity: 1 L) equipped with a reflux condenser, a thermometer, a dropping funnel, a stirrer and a gas introduction tube.
Introduce 00 parts and keep the system temperature at 5 while introducing nitrogen gas.
The temperature was raised to 0 ° C. The polymerization initiator, 2,2-azobis (2-amidinopropane) dihydrochloride (10
%) 40 parts were added every 2 hours in 4 portions. After reacting for 10 hours, a viscous pale yellow liquid was obtained. When 50 g of this was taken and poured into 500 ml of acetone, a white precipitate was formed. The precipitate was separated by filtration, washed twice more with 100 ml of acetone, and then vacuum dried to obtain 23.5 g of a white solid water-soluble cationic copolymer dispersant. The intrinsic viscosity of the obtained copolymer in an aqueous 1N-NaCl solution at 25 ° C is 2.
30 (dl / g), the weight average molecular weight determined by GPC was 650000.
【0010】実施例1 平均粒径30μm の粗粒重質炭酸カルシウム(日本セメ
ント石灰石原料の乾式粉砕品)と水との重量比が40/
60となるように水を加え、ここに参考例1で製造した
水溶性カチオン性コポリマー分散剤を、石灰石粉100
重量部当り0.06重量部加え、テーブル式アトライター
型媒体攪はんミルを用いてφ1.2mmガラスビーズ充填率
170%周速10m/sec で湿式粉砕した。次に350メ
ッシュのスクリーンを通して分級し、350メッシュの
スクリーンを通ったスラリーを(株)奈良機械製作所M
SD−200媒体流動乾燥機で乾燥した。媒体流動乾燥
機の条件を変化と得られた無機微粉体の粒度分布をまと
めて表−1に示す。尚、表中の粒度分布はアンドレアゼ
ンピペット法(A.P)で測定した。
Example 1 The weight ratio of coarse-grained heavy calcium carbonate having an average particle size of 30 μm (dry crushed product of Nippon Cement Limestone raw material) and water was 40 /.
Water was added so as to be 60, and the water-soluble cationic copolymer dispersant produced in Reference Example 1 was added to the limestone powder 100.
0.06 part by weight was added per part by weight, and wet milling was carried out using a table type attritor type medium agitator mill at a φ1.2 mm glass bead filling rate of 170% and a peripheral speed of 10 m / sec. Next, classify through a 350-mesh screen, and the slurry that passed through the 350-mesh screen is Nara Machinery M Co., Ltd.
It was dried on a SD-200 medium fluid dryer. Table 1 shows a summary of the particle size distribution of the resulting inorganic fine powder, with changes in the conditions of the medium fluidized dryer. The particle size distribution in the table was measured by the Andreazen pipette method (AP).
【0011】[0011]
【表1】 表−1 No 1 2 3 テスト条件 熱風温度℃ 150 150 150 排気温度℃ 90 100 120 スラリー供給量kg/h 14.4 10.56 5.28 粒度分布(A.P)% 325メッシュオン 0.0076 0.0058 0.0280 325メッシュパス 99.99 99.99 99.97 10μパス 99.99 99.99 99.94 5μパス 99.54 99.85 99.14 2μパス 96.97 97.24 96.67 水分 % 0.12 0.12 0.16 [Table 1] Table-1 No 1 2 3 Test conditions Hot air temperature ℃ 150 150 150 Exhaust temperature ℃ 90 100 120 Slurry supply amount kg / h 14.4 10.56 5.28 Particle size distribution (AP)% 325 mesh on 0.0076 0.0058 0.0280 325 mesh pass 99.99 99.99 99.97 10μ pass 99.99 99.99 99.94 5μ pass 99.54 99.85 99.14 2μ pass 96.97 97.24 96.67 Moisture% 0.12 0.12 0.16
【0012】比較例1 平均粒径30μm の粗粒重質炭酸カルシウム(日本セメ
ント石灰石原料の乾式粉砕品)と水との重量比が75/
25となるように水を加え、ここに水溶性アニオン分散
剤(ポリカルボン酸ナトリウム:サンノブコ社製 SN
ディスパーザント5040)を、石灰石粉100重量
部当り0.5重量部加え、テーブル式アトライター型媒体
攪はんミルを用いてφ1.2mmガラスビーズ充填率170
%周速10m/sec で湿式粉砕した。次に350メッシュ
のスクリーンを通して分級し、350メッシュのスクリ
ーンを通ったスラリーを(株)奈良機械製作所MSD−
200媒体流動乾燥機で乾燥した。媒体流動乾燥機の条
件を変化と得られた無機微粉体の粒度分布をまとめて表
−2に示す。尚、表中の粒度分布はアンドレアゼンピペ
ット法(A.P)で測定した。
Comparative Example 1 The weight ratio of coarse-grained heavy calcium carbonate having an average particle diameter of 30 μm (dry crushed product of Nippon Cement Limestone raw material) to water is 75 /
Water was added so as to be 25, and a water-soluble anion dispersant (sodium polycarboxylate: SN manufactured by San Nobuco Co., Ltd.) was added thereto.
Dispersant 5040) is added to 0.5 parts by weight per 100 parts by weight of limestone powder, and a table type attritor type medium agitator mill is used to obtain a glass bead packing ratio of φ1.2 mm of 170.
Wet milling was performed at a peripheral speed of 10 m / sec. Next, it classifies through a 350-mesh screen, and the slurry that passes through the 350-mesh screen is MSD-Nara Machinery Co., Ltd.
It was dried in a 200 medium fluid dryer. Table 2 shows a summary of the particle size distribution of the resulting inorganic fine powder, with changes in the conditions of the medium fluidized dryer. The particle size distribution in the table was measured by the Andreazen pipette method (AP).
【0013】[0013]
【表2】 表−2 No 1 2 テスト条件 熱風温度℃ 110 110 排気温度℃ 73 80 スラリー供給量kg/h 20.8 16.4 粒度分布(A.P)% 325メッシュオン 10.51 7.34 325メッシュパス 89.49 92.66 10μパス 86.14 89.07 5μパス 84.98 85.50 2μパス 72.95 70.37 水分 % 0.03 0.03 [Table 2] Table-2 No 1 2 Test condition Hot air temperature ℃ 110 110 Exhaust temperature ℃ 73 80 Slurry supply amount kg / h 20.8 16.4 Particle size distribution (AP)% 325 mesh on 100.51 7.34 325 mesh pass 89.49 92. 66 10μ pass 86.14 89.07 5μ pass 84.98 85.50 2μ pass 72.95 70.37 Moisture% 0.03 0.03
【0014】実施例2 平均粒径30μm の粗粒重質炭酸カルシウム(日本セメ
ント石灰石原料の乾式粉砕品)と水との重量比が40/
60となるように水を加え、ここに参考例1で製造した
水溶性カチオン性コポリマー分散剤を、石灰石粉100
重量部当り0.06重量部加え、テーブル式アトライター
型媒体攪はんミルを用いてφ1.2mmガラスビーズ充填率
170%周速10m/sec で湿式粉砕した。次に湿式粉砕
により得られたスラリーを120℃の恒温乾燥機内で乾
燥後、高速回転式粉砕機((株)奈良機械制作所の自由
粉砕機 M−2型)で粉砕して無機微粉体を得た。
EXAMPLE 2 Coarse-grained heavy calcium carbonate having an average particle size of 30 μm (dry-ground product of Nippon Cement Limestone raw material) and water in a weight ratio of 40 /
Water was added so as to be 60, and the water-soluble cationic copolymer dispersant produced in Reference Example 1 was added to the limestone powder 100.
0.06 part by weight was added per part by weight, and wet milling was carried out using a table type attritor type medium agitator mill at a φ1.2 mm glass bead filling rate of 170% and a peripheral speed of 10 m / sec. Next, the slurry obtained by wet pulverization is dried in a constant temperature dryer at 120 ° C., and then pulverized by a high-speed rotary pulverizer (free pulverizer M-2 type manufactured by Nara Kikai Seisakusho Co., Ltd.) to obtain an inorganic fine powder. Obtained.
【0015】比較例2 石灰石粉と水との重量比が75/25となるように水を
加え、ここに水溶性アニオン分散剤(ポリカルボン酸ナ
トリウム:サンノブコ社製 SN ディスパーザント5
040)を、石灰石粉100重量部当り0.5重量部加え
た以外は実施例2の方法と同様にして無機微粉体を得
た。実施例2及び比較例2の乾燥前の湿式粉砕スラリー
中の無機微粉体の粒度分布をまとめて表−3に示す。
尚、表中の粒度分布はセイシン企業のMICRON PHOTO SIZ
ER SKC-2000 により測定した値である。
Comparative Example 2 Water was added so that the weight ratio of limestone powder to water was 75/25, and a water-soluble anionic dispersant (sodium polycarboxylate: SN Dispersant 5 manufactured by San Nobuco Co., Ltd.) was added thereto.
040) was added in an amount of 0.5 parts by weight per 100 parts by weight of limestone powder to obtain an inorganic fine powder in the same manner as in Example 2. Table 3 collectively shows the particle size distribution of the inorganic fine powder in the wet pulverized slurries before drying in Example 2 and Comparative Example 2.
In addition, the particle size distribution in the table is MICRON PHOTO SIZ
It is the value measured by ER SKC-2000.
【0016】[0016]
【表3】 表−3 比較例2 実施例2 粒度分布(セイシン)% 15μパス 100.00 100.00 10μパス 100.00 100.00 8μパス 100.00 100.00 6μパス 100.00 100.00 4μパス 99.52 100.00 2μパス 95.19 95.57 1μパス 82.78 86.13 0.8μパス 77.07 80.04 0.6μパス 65.78 68.51 0.4μパス 43.70 48.77 0.2μパス 5.82 8.17 50% (平均粒径) 0.46 0.41 [Table 3] Table-3 Comparative Example 2 Example 2 Particle size distribution (seishin)% 15μ pass 100.00 100.00 10μ pass 100.00 100.00 8μ pass 100.00 100.00 6μ pass 100.00 100.00 4μ pass 99.52 100.00 2μ pass 95.19 95.57 1μ pass 82.78 86.13 0.8μ pass 77.07 80.04 0.6μ pass 65.78 68.51 0.4 μ pass 43.70 48.77 0.2 μ pass 5.82 8.17 50% (average particle size) 0.46 0.41
【0017】比較例2及び実施例2において、湿式粉砕
後のスラリーを乾燥し、次いで粉砕して得た無機微粉体
の粒度分布を表−4に示す。
In Comparative Example 2 and Example 2, the particle size distribution of the inorganic fine powder obtained by drying and then pulverizing the slurry after wet pulverization is shown in Table-4.
【表4】 表−4 比較例2 実施例2 325メッシュオン重量% 20.92 1.62 粒度分布(セイシン)% 325メッシュパス 79.08 98.38 15μパス 75.13 96.95 10μパス 71.60 96.13 8μパス 69.51 94.05 6μパス 68.31 92.55 4μパス 67.45 91.47 2μパス 62.32 87.17 1μパス 53.58 72.56 0.8μパス 48.64 67.42 0.6μパス 40.72 52.80 0.4μパス 26.74 31.50 0.2μパス 2.73 8.07 [Table 4] Table-4 Comparative Example 2 Example 2 325 mesh on weight% 20.92 1.62 Particle size distribution (Seishin)% 325 mesh Pass 79.08 98.38 15μ pass 75.13 96.95 10μ pass 71.60 96.13 8μ pass 69.51 94.05 6μ pass 68.31 92.55 4μ pass 67.45 91.47 2μ pass 62.32 87.17 53.58 72.56 0.8 μ pass 48.64 67.42 0.6 μ pass 40.72 52.80 0.4 μ pass 26.74 31.50 0.2 μ pass 2.73 8.07
【0018】表−3と表−4との比較から明らかなよう
に、比較例2及び実施例2とも、湿式粉砕後のスラリー
中に含まれる無機微粉体の粒度分布はほぼ同じである
(表−3)が、一旦スラリーを乾燥すると、粉砕しても
比較例2では 325メッシュオンの祖粒子の量が約21重
量%と多くなってしまうのに対して、本発明の方法によ
れば、約2重量%と極めて少なく、本発明の方法が、湿
式粉砕した後、乾燥した時に無機微粉体の2次凝集が少
なく、乾燥ケーキが潰れ易い無機微粉体を製造する優れ
た方法であることがわかる。
As is clear from the comparison between Table 3 and Table 4, the particle size distribution of the inorganic fine powder contained in the slurry after wet grinding is almost the same in both Comparative Example 2 and Example 2 (Table -3), once the slurry is dried, the amount of 325 mesh-on progenitor particles in Comparative Example 2 increases to about 21% by weight even when pulverized, whereas according to the method of the present invention, It is an extremely small amount of about 2% by weight, and the method of the present invention is an excellent method for producing an inorganic fine powder in which secondary aggregation of the inorganic fine powder is small when dried after wet pulverization and the dry cake is easily crushed. Recognize.
【0019】実施例3 石灰石の代わりに、亜硫酸カルシウム、水酸化アルミニ
ウム、酸化亜鉛、硫酸バリウム、炭酸マグネシウム又は
カオリンを用いた以外は、実施例2の方法を繰りかえ
し、得られた無機微粉体の325メッシュオンを測定し
た。結果をまとめて表−5に示す。
Example 3 The procedure of Example 2 was repeated except that calcium sulfite, aluminum hydroxide, zinc oxide, barium sulfate, magnesium carbonate or kaolin was used instead of limestone, and 325 of the inorganic fine powder obtained was obtained. The mesh on was measured. The results are summarized in Table-5.
【表5】 表−5 無機材料 325メッシュオン(重量%) 亜硫酸カルシウム 1.4 水酸化アルミニウム 0.2 酸化亜鉛 0.1 硫酸バリウム 3.0 炭酸マグネシウム、 2.5 カオリン 0.01 [Table 5] Table-5 Inorganic material 325 mesh on (wt%) Calcium sulfite 1.4 Aluminum hydroxide 0.2 Zinc oxide 0.1 Barium sulfate 3.0 Magnesium carbonate, 2.5 Kaolin 0.01
───────────────────────────────────────────────────── フロントページの続き (72)発明者 高瀬 祐美子 東京都港区新橋3丁目4番5号 新橋フロ ンティアビル5階 株式会社社ファイマテ ック内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Yumiko Takase 3-4-5 Shimbashi, Minato-ku, Tokyo Shimbashi Frontier Building, 5th floor, within the company Fimatec Co., Ltd.

Claims (5)

    【特許請求の範囲】[Claims]
  1. 【請求項1】 無機粉体を、ジアリルアミン塩及び/又
    はアルキルジアリルアミン塩10〜99モル%と非イオ
    ン性ビニルモノマー1〜90モル%とを構成単位とする
    水溶性カチオン性コポリマー分散剤の存在下、水性媒体
    中で湿式粉砕し、次いで乾燥することを特徴とする無機
    微粉体の製造方法。
    1. An inorganic powder in the presence of a water-soluble cationic copolymer dispersant comprising 10 to 99 mol% of a diallylamine salt and / or an alkyldiallylamine salt and 1 to 90 mol% of a nonionic vinyl monomer. A method for producing an inorganic fine powder, which comprises wet-milling in an aqueous medium and then drying.
  2. 【請求項2】 無機粉体が予め乾式粉砕されたものであ
    る請求項1記載の製造方法。
    2. The manufacturing method according to claim 1, wherein the inorganic powder is previously dry-milled.
  3. 【請求項3】 非イオン性ビニルモノマーがアクリルア
    ミド及び/又はメタクリルアミドである請求項1記載の
    製造方法。
    3. The production method according to claim 1, wherein the nonionic vinyl monomer is acrylamide and / or methacrylamide.
  4. 【請求項4】 乾燥が媒体流動乾燥により行われる請求
    項1記載の製造方法。
    4. The production method according to claim 1, wherein the drying is performed by fluidized medium drying.
  5. 【請求項5】 無機粉体が炭酸カルシウムである請求項
    1記載の製造方法。
    5. The production method according to claim 1, wherein the inorganic powder is calcium carbonate.
JP9320094A 1994-05-02 1994-05-02 Production of fine inorganic powder Pending JPH07300568A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
JP9320094A JPH07300568A (en) 1994-05-02 1994-05-02 Production of fine inorganic powder

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Publication Number Publication Date
JPH07300568A true JPH07300568A (en) 1995-11-14

Family

ID=14075941

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