JPH06210631A - Silica composite granule - Google Patents

Silica composite granule

Info

Publication number
JPH06210631A
JPH06210631A JP2498593A JP2498593A JPH06210631A JP H06210631 A JPH06210631 A JP H06210631A JP 2498593 A JP2498593 A JP 2498593A JP 2498593 A JP2498593 A JP 2498593A JP H06210631 A JPH06210631 A JP H06210631A
Authority
JP
Japan
Prior art keywords
fine powder
carbon black
silica
granule
kneading
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
Application number
JP2498593A
Other languages
Japanese (ja)
Other versions
JP3289360B2 (en
Inventor
Taisuke Yamada
泰輔 山田
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.)
Nok Corp
Original Assignee
Nok 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 Nok Corp filed Critical Nok Corp
Priority to JP2498593A priority Critical patent/JP3289360B2/en
Publication of JPH06210631A publication Critical patent/JPH06210631A/en
Application granted granted Critical
Publication of JP3289360B2 publication Critical patent/JP3289360B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Abstract

PURPOSE:To shorten the kneading process time of synthetic rubber and to enhance dispersibility by using an integrated granule of a silica fine powder and a carbon black fine powder. CONSTITUTION:The integral granulation of a silica fine powder and a carbon black fine powder is performed by using about 50-80 pts.wt. of the carbon black fine powder with respect to 100 pts.wt. of the silica fine powder and granulating both fine powders using water as a wetting agent by a stirring and tumbling type granulator to dry the obtained granules. Therefore, by using the silica fine powder as the silica composite granule integrally granulated along with the carbon black fine powder, kneading can be performed at once when this silica composite granule is compounded and kneaded with various synthetic rubbers. By this constitution, a kneading process time can be shortened and the dispersibility in the case of kneading can be enhanced. Further, when the granule obtained by coating the surface of the integrated granule with the carbon black fine powder is used, the viscosity of synthetic rubber can be preliminarily increased because of the surface wettability of the granule and dispersibility can be further enhanced.

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、シリカ複合造粒物に関
する。更に詳しくは、合成ゴムの混練工程時間を短縮
し、かつ分散性を向上せしめたシリカ複合造粒物に関す
る。
FIELD OF THE INVENTION The present invention relates to a silica composite granulated product. More specifically, the present invention relates to a silica composite granulated product in which the synthetic rubber kneading step time is shortened and the dispersibility is improved.

【0002】[0002]

【従来の技術】シリカ微粉末は、各種ゴム生地の補強性
充填配合剤として、それの混練工程において用いられて
いる。しかしながら、シリカ微粉末は、そのままでは取
り扱い難く、また呼吸器に対しても有害であるため、一
般に数100μm〜数mm程度の直径の造粒物として用いられ
ている。しかるに、シリカ粒子は合成ゴムと濡れ性が悪
いばかりではなく、その造粒物はカーボンブラックなど
の造粒物に比べてかなり硬くなり、特に低粘度の合成ゴ
ムに配合した場合分散不良を生ずるという問題がみられ
る。
BACKGROUND OF THE INVENTION Silica fine powder is used in a kneading process as a reinforcing filler compounding agent for various rubber materials. However, since silica fine powder is difficult to handle as it is and is harmful to the respiratory organs, it is generally used as a granulated product having a diameter of about several 100 μm to several mm. However, silica particles not only have poor wettability with synthetic rubber, but their granules become considerably harder than granules such as carbon black, and in particular when mixed with low-viscosity synthetic rubber, poor dispersion occurs. There are problems.

【0003】このため、一般には濡れ性の高いカーボン
ブラックを先に合成ゴムと混練し、ゴム生地の粘度を上
げた後にシリカ造粒物を加え、再度混練するという工程
がとられている。この場合には、混練を2回に分けて行
うため混練時間が長くなり、またシリカ造粒物が硬いた
め、分散不良が生じ易いという問題がある。
For this reason, in general, a step of kneading carbon black having high wettability with synthetic rubber first, increasing the viscosity of the rubber material, adding a silica granule, and kneading again is taken. In this case, since the kneading is performed twice, the kneading time becomes long, and since the silica granules are hard, there is a problem in that poor dispersion easily occurs.

【0004】[0004]

【発明が解決しようとする課題】本発明の目的は、合成
ゴムの混練工程時間を短縮し、かつ分散性を向上せしめ
たシリカ複合造粒物を提供することにある。
SUMMARY OF THE INVENTION It is an object of the present invention to provide a silica composite granulated product in which the time for the kneading step of synthetic rubber is shortened and the dispersibility is improved.

【0005】[0005]

【課題を解決するための手段】かかる本発明の目的は、
シリカ微粉末およびカーボンブラック微粉末の一体造粒
物あるいはそれを更にカーボンブラック微粉末で被覆し
たシリカ複合造粒物によって達成される。
The object of the present invention is as follows.
This is achieved by an integrated granulation product of silica fine powder and carbon black fine powder or a silica composite granulation product obtained by further coating it with carbon black fine powder.

【0006】シリカ微粉末としては、結晶性シリカ、溶
融シリカなどであって、その粒径が約200nm以下、好ま
しくは約100nm以下のものが用いられる。また、カーボ
ンブラック微粉末としては、粒径が約100nm以下、好ま
しくは約80nm以下のものであれば任意のものを用いるこ
とができ、特に構造をもたないものが好んで用いられ
る。
As the fine silica powder, crystalline silica, fused silica or the like having a particle size of about 200 nm or less, preferably about 100 nm or less is used. As the carbon black fine powder, any powder having a particle size of about 100 nm or less, preferably about 80 nm or less can be used, and one having no structure is preferably used.

【0007】このような粒径を有し、造粒時の硬度が低
いものであれば、カーボンブラック以外の他のゴム用充
填剤微粉末、例えば活性化炭酸カルシウム、塩基性炭酸
マグネシウム等の微粉末も、カーボンブラック微粉末の
代わりに用い得るが、カーボンブラック微粉末が最も好
ましい。また、これらの他のゴム用充填剤微粉末は、カ
ーボンブラック微粉末と併用することもできる。
Fine powders of rubber fillers other than carbon black, such as activated calcium carbonate and basic magnesium carbonate, as long as they have such a particle size and a low hardness during granulation. Powders may also be used instead of carbon black fine powder, but carbon black fine powder is most preferable. Further, these other fine filler powders for rubber can be used together with the fine carbon black powder.

【0008】シリカ微粉末とカーボンブラック微粉末と
の一体造粒は、シリカ微粉末100重量部に対して約50〜8
0重量部のカーボンブラック微粉末を用い、水を湿潤剤
として、撹拌転動式造粒機などを用いて行われ、その後
乾燥される。各種粒径を有する一体造粒物が得られる
が、一般には約0.5〜1.5mm程度の粒径のものが選別して
用いられる。この一体造粒物はまた、更にカーボンブラ
ック微粉末で被覆して用いることもできる。この被覆
は、一体造粒物に更にカーボンブラック微粉末を加え、
造粒、乾燥することによって行われる。カーボンブラッ
ク微粉末以外のゴム用充填剤微粉末も用いられるが、こ
の場合にもカーボンブラック微粉末が最も好ましい。ま
た、カーボンブラック微粉末と他のゴム用充填剤微粉末
の併用も、一体造粒物の場合と同様に行われる。
The integral granulation of fine silica powder and fine carbon black powder is about 50 to 8 per 100 parts by weight of fine silica powder.
It is carried out using 0 part by weight of carbon black fine powder, water as a wetting agent, and a stirring tumbling granulator, and then dried. Although monolithic granules having various particle diameters can be obtained, those having a particle diameter of about 0.5 to 1.5 mm are generally selected and used. The integrally granulated product can also be used by being further coated with carbon black fine powder. This coating is made by adding carbon black fine powder to the integrally granulated product,
It is performed by granulating and drying. Fine powders of rubber fillers other than the fine powders of carbon black are also used, but fine powders of carbon blacks are most preferable in this case as well. Further, the combined use of the carbon black fine powder and the other fine filler powder for rubber is performed in the same manner as in the case of the integrally granulated product.

【0009】このようにして得られたシリカ複合造粒物
は、アクリルゴム、ニトリルゴム、フッ素ゴムなどの各
種合成ゴムに配合されて用いられる。
The silica composite granules thus obtained are used by being mixed with various synthetic rubbers such as acrylic rubber, nitrile rubber and fluororubber.

【0010】[0010]

【発明の効果】シリカ微粉末をカーボンブラック微粉末
と一体造粒したシリカ複合造粒物として用いることによ
り、これを各種合成ゴムに配合し、混練したとき、混練
を一度で済ませることができるので、混練工程時間を短
縮することができ、しかもその場合の分散性を向上させ
ることもできる。更に、一体造粒物の表面をカーボンブ
ラック微粉末で被覆したものを用いると、それの表面濡
れ性によって合成ゴムの粘度を予め上げることができ、
シリカ微粉末の分散性は更に向上する。
EFFECTS OF THE INVENTION By using silica fine powder as a silica composite granule integrally granulated with carbon black fine powder, when this is compounded into various synthetic rubbers and kneaded, the kneading can be completed only once. In addition, the kneading step time can be shortened, and the dispersibility in that case can be improved. Furthermore, if the surface of the integrally granulated product is coated with carbon black fine powder, the viscosity of the synthetic rubber can be increased in advance due to the surface wettability thereof.
The dispersibility of fine silica powder is further improved.

【0011】[0011]

【実施例】次に、実施例について本発明を説明する。EXAMPLES The present invention will now be described with reference to examples.

【0012】実施例1 溶融シリカ(キャボット社製品CABOSIL M-70,粒径7〜50
nm)100gおよびカーボンブラック(三菱化成製品ダイアブ
ラックH,一次粒径30nm)100gの混合物を、水の存在下に
おいて、撹拌転動式造粒機を用いて造粒し、乾燥させ
た。
Example 1 Fused silica (CABOSIL M-70, a product of Cabot Corporation, particle size 7 to 50)
100g) and 100g of carbon black (Mitsubishi Kasei product Diablack H, primary particle size 30nm) were granulated in the presence of water using a stirring tumbling granulator and dried.

【0013】造粒物の内、粒径約0.5〜1.5mmのものを選
び、その30〜60重量部をアクリルゴム(日本メクトロン
製品ノックスタイトA-1095)100重量部に加え、ニーダ型
混練機を用いて、スクリュー回転数14/18rpmで15分間混
練した。
Among the granulated products, one having a particle size of about 0.5 to 1.5 mm is selected, and 30 to 60 parts by weight thereof are added to 100 parts by weight of acrylic rubber (Nippon Mektron product Knoxtite A-1095) and a kneader type kneader Was kneaded for 15 minutes at a screw rotation speed of 14/18 rpm.

【0014】実施例2 実施例1において、100gのシリカと100gのカーボンブラ
ックとを造粒した時点で、更にカーボンブラック100gを
加え、造粒、乾燥したものが、アクリルゴムとの混練に
用いられた。
Example 2 In Example 1, when 100 g of silica and 100 g of carbon black were granulated, 100 g of carbon black was further added, and the granulated and dried product was used for kneading with acrylic rubber. It was

【0015】比較例1 実施例1で用いられたシリカおよびカーボンブラックを
別々に造粒し、それの1:2混合物30〜60重量部をアク
リルゴム100重量部に加え、混練した。
Comparative Example 1 The silica and carbon black used in Example 1 were granulated separately, and 30 to 60 parts by weight of a 1: 2 mixture thereof was added to 100 parts by weight of acrylic rubber and kneaded.

【0016】比較例2 アクリルゴム100重量部に、カーボンブラックのみを投
入して5分間混練した後、その半分量のシリカを加えて1
0分間混練し、これら両者を合計30〜60重量部混練し
た。
Comparative Example 2 To 100 parts by weight of acrylic rubber, only carbon black was charged and kneaded for 5 minutes, and then half the amount of silica was added to obtain 1
The mixture was kneaded for 0 minutes, and a total of 30 to 60 parts by weight of both were kneaded.

【0017】比較例3 比較例2において、カーボンブラックおよびシリカの混
練時間をそれぞれ2倍に延長した。
Comparative Example 3 In Comparative Example 2, the kneading times of carbon black and silica were each doubled.

【0018】以上の各実施例および比較例における混練
物の分散状態を観察した。その結果は、次の表に示され
る。 カーボンブラック・シリカ合計量(重量部) 30 40 50 60 実施例1 ○ ○ ○ ○ 〃 2 ○ ○ ○ ○ 比較例1 × × × △ 〃 2 × × △ ○ 〃 3 △ ○ ○ ○ [評価] ○:分散良好 △:一部にシリカ塊あり ×:全般的に分散不良
The dispersed state of the kneaded material in each of the above Examples and Comparative Examples was observed. The results are shown in the table below. Carbon black / silica total amount (parts by weight) Example 30 40 50 60 Example 1 ○ ○ ○ ○ 〃 2 ○ ○ ○ ○ Comparative Example 1 × × × △ 〃 2 × × △ ○ 〃 3 △ ○ ○ ○ [Evaluation] ◯: Dispersion is good Δ: Silica lumps are partly present ×: Dispersion is poor in general

─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───

【手続補正書】[Procedure amendment]

【提出日】平成5年4月22日[Submission date] April 22, 1993

【手続補正1】[Procedure Amendment 1]

【補正対象書類名】明細書[Document name to be amended] Statement

【補正対象項目名】0008[Correction target item name] 0008

【補正方法】変更[Correction method] Change

【補正内容】[Correction content]

【0008】 シリカ微粉末とカーボンブラック微粉末
との一体造粒は、シリカ微粉末100重量部に対して約
50〜80重量部のカーボンブラック微粉末を用い、水
を湿潤剤として、撹拌転動式造粒機などを用いて行わ
れ、その後乾燥される。各種粒径を有する一体造粒物が
得られるが、一般には約0.5〜1.5mm程度の粒径
のものが選別して用いられる。この一体造粒物はまた、
更にカーボンブラック微粉末で被覆して用いることもで
きる。この被覆は、一体造粒物に更にカーボンブラック
微粉末を加え、造粒、乾燥することによって行われる。
被覆には、カーボンブラック微粉末以外のゴム用充填剤
微粉末も用いられるが、この場合にもカーボンブラック
微粉末が最も好ましい。また、カーボンブラック微粉末
と他のゴム用充填剤微粉末の併用も、一体造粒物の場合
と同様に行われる。
The integral granulation of the silica fine powder and the carbon black fine powder uses about 50 to 80 parts by weight of the carbon black fine powder to 100 parts by weight of the silica fine powder, and water is used as a wetting agent while stirring and rolling. It is carried out using a granulator or the like, and then dried. Although monolithic granules having various particle sizes are obtained, those having a particle size of about 0.5 to 1.5 mm are generally selected and used. This monolithic granule also
Further, it can be used by coating with carbon black fine powder. This coating is performed by further adding carbon black fine powder to the integrally granulated product, granulating and drying.
For the coating, fine powder of filler for rubber other than fine powder of carbon black can be used, and fine powder of carbon black is most preferable also in this case. Further, the combined use of the carbon black fine powder and the other fine filler powder for rubber is performed in the same manner as in the case of the integrally granulated product.

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 FI 技術表示箇所 B29K 105:16 ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Office reference number FI technical display location B29K 105: 16

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 シリカ微粉末およびカーボンブラック微
粉末の一体造粒物よりなるシリカ複合造粒物。
1. A silica composite granulated product comprising an integrated granulated product of silica fine powder and carbon black fine powder.
【請求項2】 請求項1記載の一体造粒物を更にカーボ
ンブラック微粉末で被覆したシリカ複合造粒物。
2. A silica composite granulated product obtained by further coating the monolithic granulated product according to claim 1 with carbon black fine powder.
【請求項3】 請求項1または2記載のシリカ複合造粒
物を合成ゴムに配合したゴム組成物。
3. A rubber composition in which the silica composite granulated product according to claim 1 or 2 is mixed with a synthetic rubber.
JP2498593A 1993-01-21 1993-01-21 Silica composite granules Expired - Fee Related JP3289360B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2498593A JP3289360B2 (en) 1993-01-21 1993-01-21 Silica composite granules

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2498593A JP3289360B2 (en) 1993-01-21 1993-01-21 Silica composite granules

Publications (2)

Publication Number Publication Date
JPH06210631A true JPH06210631A (en) 1994-08-02
JP3289360B2 JP3289360B2 (en) 2002-06-04

Family

ID=12153278

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2498593A Expired - Fee Related JP3289360B2 (en) 1993-01-21 1993-01-21 Silica composite granules

Country Status (1)

Country Link
JP (1) JP3289360B2 (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997015620A1 (en) * 1995-10-25 1997-05-01 The Yokohama Rubber Co., Ltd. Rubber composition comprising carbon black having surface treated with silica
WO1998049241A1 (en) * 1997-04-30 1998-11-05 The Yokohama Rubber Co., Ltd. Process for producing modified carbon black for reinforcing rubber and process for producing rubber composition containing modified carbon black
US6479582B1 (en) 1997-05-21 2002-11-12 Otsuka Chemical Co., Ltd. Rubber composition
EP1352930A3 (en) * 2002-02-07 2004-05-19 Toda Kogyo Corporation Black composite particles for semiconductor sealing material, and semiconductor sealing material using the same
WO2017061098A1 (en) * 2015-10-09 2017-04-13 日本板硝子株式会社 Carbon black-containing composite particles and method for producing carbon black-containing composite particles

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997015620A1 (en) * 1995-10-25 1997-05-01 The Yokohama Rubber Co., Ltd. Rubber composition comprising carbon black having surface treated with silica
US5883179A (en) * 1995-10-25 1999-03-16 The Yokohama Rubber Co., Ltd. Rubber composition comprising carbon black surface treated with silica
WO1998049241A1 (en) * 1997-04-30 1998-11-05 The Yokohama Rubber Co., Ltd. Process for producing modified carbon black for reinforcing rubber and process for producing rubber composition containing modified carbon black
KR100321269B1 (en) * 1997-04-30 2002-09-09 요코하마 고무 가부시키가이샤 Manufacture method of modified carbon black for rubber reinforcement, Rubber composition containing modified carbon black for rubber reinforcement and manufacturing method thereof
US6962952B2 (en) 1997-04-30 2005-11-08 The Yokohama Rubber Co., Ltd. Process for production of modified carbon black for rubber reinforcement and process of production of rubber composition containing modified carbon black
US7144943B2 (en) 1997-04-30 2006-12-05 The Yokohama Rubber Co., Ltd. Process for production of modified carbon black for rubber reinforcement and process of production of rubber composition containing modified carbon black
US6479582B1 (en) 1997-05-21 2002-11-12 Otsuka Chemical Co., Ltd. Rubber composition
EP1352930A3 (en) * 2002-02-07 2004-05-19 Toda Kogyo Corporation Black composite particles for semiconductor sealing material, and semiconductor sealing material using the same
US7025905B2 (en) 2002-02-07 2006-04-11 Toda Kogyo Corporation Black composite particles for semiconductor sealing material, and semiconductor sealing material using the same
WO2017061098A1 (en) * 2015-10-09 2017-04-13 日本板硝子株式会社 Carbon black-containing composite particles and method for producing carbon black-containing composite particles

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