JPH058127B2 - - Google Patents
Info
- Publication number
- JPH058127B2 JPH058127B2 JP62201837A JP20183787A JPH058127B2 JP H058127 B2 JPH058127 B2 JP H058127B2 JP 62201837 A JP62201837 A JP 62201837A JP 20183787 A JP20183787 A JP 20183787A JP H058127 B2 JPH058127 B2 JP H058127B2
- Authority
- JP
- Japan
- Prior art keywords
- silicon dioxide
- binder
- water
- organic solvent
- specific gravity
- 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 - Lifetime
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 64
- 235000012239 silicon dioxide Nutrition 0.000 claims description 39
- 239000000377 silicon dioxide Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000011230 binding agent Substances 0.000 claims description 14
- 239000003960 organic solvent Substances 0.000 claims description 12
- 238000005469 granulation Methods 0.000 claims description 10
- 230000003179 granulation Effects 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 3
- 239000003209 petroleum derivative Substances 0.000 claims 1
- 230000005484 gravity Effects 0.000 description 15
- 239000002245 particle Substances 0.000 description 15
- 239000008187 granular material Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 239000008188 pellet Substances 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 239000013065 commercial product Substances 0.000 description 4
- 239000003350 kerosene Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001694 spray drying Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 229910052910 alkali metal silicate Inorganic materials 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 229940075614 colloidal silicon dioxide Drugs 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000010446 mirabilite Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- RSIJVJUOQBWMIM-UHFFFAOYSA-L sodium sulfate decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-]S([O-])(=O)=O RSIJVJUOQBWMIM-UHFFFAOYSA-L 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
Description
産業上の利用分野
本発明は、湿式法あるいは乾式法によつて製造
された微粒状二酸化珪素を粒状化する方法に関す
るものである。
従来技術
微細な非晶質二酸化珪素は別名ホワイトカーボ
ンと呼ばれ、湿式法または乾式法のいずれかによ
つて製造され公知の方法になつている。
湿式法による非晶質二酸化珪素の製造の場合に
は、例えば特公昭38−17651号および特公昭51−
25235号公報に記載されているように、例えば、
珪酸ソーダ水溶液と鉱酸、一般には硫酸との中和
反応により二酸化珪素を析出させ、析出物を水で
洗條した後、脱水、乾燥、粉砕を経て微細な二酸
化珪素を製造する方法が記載されている。
しかし、微粉状の二酸化珪素は上記製法におい
て述べたように中和反応による析出物であり、一
次粒子はコロイド状の超微細粒子であるので、極
めて軽く、飛散しやすく、かさ高であり、流動性
に問題があり、貯蔵、運搬その他取扱いが困難で
ある。
一方、この二酸化珪素は天然または合成ゴムの
充填剤、農薬の担体、印刷用紙、塗料、インク、
接着剤等の多方面に使用されており、運搬や取扱
い上の難点に対する問題解決の要請は大きい。
これらの難点を解決するものとして現在粒状の
ものが知られている。これは生成する水和珪酸を
水で洗條した後、水和珪酸スラリーをつくりこれ
を噴霧乾燥することによつて得られる。
しかし、この場合、スラリーの固形分濃度が20
％以上ではスラリー化が困難であり、一般には固
形分濃度15％程度のスラリーを噴霧している。
従つて、この場合には噴霧乾燥するのに莫大な
水の蒸発エネルギーコストを要することになる。
また、特開昭57−56314号公報には中和法によ
つて生成した微細な非晶質水和けい酸の沈澱物を
濾過、洗浄後要すればこれを再びスラリーとな
し、これを圧搾して固形分濃度20％以上に脱水す
る。この際強固なケーキが得られるのでこれを所
望の粒度に粉砕する方法が記載されている。
以上にのべたように、二酸化珪素の顆粒状化は
困難な問題である。
発明が解決しようとする問題点
前記のように、二酸化珪素の一次粒子はコロイ
ド状の超微粒子であるのできわめて軽く、かさ高
であるので飛散し易く貯蔵、運搬その他の取扱い
が困難である。
従つて顆粒状でしかも流動性もよく、使用に際
して主原料その他の原料との混練作業中に容易に
微細化、分散する二酸化珪素の製法が要請されて
いる。
問題点を解決するための手段
本発明は、従来の噴霧乾燥法による顆粒状二酸
化珪素の製造上の欠点を解決するため種々試験研
究の結果、従来法で製造された微粉状二酸化珪素
を有機溶媒中に懸濁させて水をバインダーとして
液中造粒し、有機溶媒を分離した後造粒物を乾燥
させることにより顆粒状二酸化珪素を製造する方
法を提供することにある。
本発明方法によつて粒径のそろつたしかも粒度
分布範囲の狭い顆粒を得るには、使用する有機溶
媒の種類、有機溶媒懸濁液中の二酸化珪素の濃
度、添加する水量、添加方法、攪拌方法、時間、
温度等の顆粒条件によつて左右される。
粒径0.05mm〜５mm範囲の所望の顆粒を得るため
には、以下の顆粒条件によるのが適当である。
使用する有機溶媒は、パラフイン基、ナフテン
基、芳香族基の炭化水素、あるいはこれらの混合
物のいずれであつてもよい。
上記有機溶媒中に懸濁させる二酸化珪素の量
（濃度）には特に制限がないが、好ましく、二酸
化珪素１ｇｒに対して有機溶媒の量は、20ml〜90
ml範囲である。
また添加する水の量は二酸化珪素とバインダー
との合計に対して55％重量〜80％重量、好ましく
は60％重量〜78％重量の範囲である。
懸濁液中の二酸化珪素は、一種のコロイド状を
呈しており、攪拌の初期には各々のコロイド粒子
が水をバインダーとして点で接合し、次の段階で
これらのコロイド粒子が凝集し、フロツクを形成
する。バインダー（水）の量が少なすぎる（55％
重量以下）と攪拌を続けてもフロツクはそのまま
の状態で変化しない。バインダーが適正量の場合
（55％重量ないし80％重量）は、攪拌によりフロ
ツクはさらに凝集し、圧密化されてフロツク中に
存在する有機溶媒が押出されてペレツト化する。
しかし、ペレツト化した後も攪拌をつづけると
生成したペレツト同志が相重なり、さらに大きな
ペレツトとなり、これら大きなペレツト同志が接
合し、ペレツトが崩壊し、団塊となり、遂には水
分の少ないペースト状になる。
一方、バインダー量が多すぎると（80％重量以
上）フロツク状態から水分量の多いペースト状に
なり、ペレツトを形成することは不可能となる。
寸法の揃つた顆粒を得るためには、バインダー
が均一に分散され、コロイド状の二酸化珪素粒子
に万遍なく衝突するように攪拌条件を整えること
が必要である。このためにはバインダーとしての
水の中に極く少量の界面活性剤を添加し、これを
二酸化珪素懸濁液を構成する有機溶媒中に混合、
分散して使用することが好ましい。
使用する界面活性剤は、カチオン系、アニオン
系および非イオン系界面活性剤のいずれでもよ
く、通常使用される界面活性剤である。
珪酸アルカリと硫酸とを反応させて微細な水和
珪酸スラリーを生成させる反応工程は、既に公知
の方法として知られている。この方法により得ら
れる水和珪酸スラリーを洗條、乾燥、粉砕によつ
て製造された二酸化珪素はシラノール基を有して
おり、親水性に富む。
従つて、二酸化珪素の有機溶媒懸濁液中にバイ
ンダーとして水を添加する場合、攪拌槽内の混合
系中でバインダー濃度の局部的不均一性を避ける
ようにすることが肝要である。
また、所望の寸法の顆粒を得るためには、適正
な顆粒条件の設定が大切である。
本発明方法で製造された顆粒状の非晶質二酸化
珪酸は使用に際して他の原料と混合あるいは混練
するとき何等問題なく微細化して通常の微細な二
酸化珪酸と同様に使用することができる。
得られる顆粒状の二酸化珪酸の顆粒の大きさや
粒度分布については造粒条件により異なるが、そ
の一例を示せば次のようである。
例 １
粒径1.9μｍ〜188μｍの範囲で分布しており、そ
のうち50.7％（重量）が4.7μｍ〜20.5μｍの範囲に
あつた。
例 ２
粒径898.3μｍ〜1880μｍの範囲で分布している。
INDUSTRIAL APPLICATION FIELD The present invention relates to a method for granulating finely divided silicon dioxide produced by a wet method or a dry method. PRIOR ART Fine amorphous silicon dioxide is also called white carbon, and is produced by either a wet method or a dry method, which is a known method. In the case of manufacturing amorphous silicon dioxide by a wet method, for example, Japanese Patent Publication Nos. 17651-1982 and 1973-
For example, as described in Publication No. 25235,
A method is described in which silicon dioxide is precipitated by a neutralization reaction between an aqueous sodium silicate solution and a mineral acid, generally sulfuric acid, and the precipitate is washed with water, followed by dehydration, drying, and pulverization to produce fine silicon dioxide. ing. However, as described in the above manufacturing method, fine powder silicon dioxide is a precipitate resulting from a neutralization reaction, and the primary particles are colloidal ultrafine particles, so they are extremely light, easily scattered, bulky, and flowable. It is difficult to store, transport, and otherwise handle. On the other hand, silicon dioxide can be used as a filler in natural or synthetic rubber, as a carrier for agricultural chemicals, in printing papers, paints, inks, etc.
It is used in a variety of applications such as adhesives, and there is a great demand for solutions to problems in transportation and handling. Granular materials are currently known to solve these difficulties. This can be obtained by washing the resulting hydrated silicic acid with water, creating a hydrated silicic acid slurry, and spray-drying the slurry. However, in this case, the solid content concentration of the slurry is 20
% or more, it is difficult to form a slurry, and generally a slurry with a solid content concentration of about 15% is sprayed. Therefore, in this case, spray drying requires a huge amount of water evaporation energy cost. In addition, Japanese Patent Application Laid-Open No. 57-56314 discloses that after filtering and washing fine precipitates of amorphous hydrated silicic acid produced by the neutralization method, if necessary, this is made into a slurry again, and this is compressed. and dehydrate to a solid content of 20% or more. Since a strong cake is obtained in this case, a method is described in which this is pulverized to a desired particle size. As stated above, granulation of silicon dioxide is a difficult problem. Problems to be Solved by the Invention As mentioned above, the primary particles of silicon dioxide are colloidal ultrafine particles, so they are extremely light, and because they are bulky, they easily scatter, making storage, transportation, and other handling difficult. Therefore, there is a need for a method for producing silicon dioxide which is granular and has good fluidity, and which can be easily refined and dispersed during kneading with the main raw material and other raw materials during use. Means for Solving the Problems In order to solve the drawbacks in the production of granular silicon dioxide by the conventional spray drying method, the present invention was developed as a result of various tests and studies, and as a result of the present invention, fine powder silicon dioxide produced by the conventional method was dried in an organic solvent. An object of the present invention is to provide a method for producing granular silicon dioxide by suspending the silicon dioxide in a liquid and granulating it in a liquid using water as a binder, separating the organic solvent, and then drying the granulated product. In order to obtain granules with a uniform particle size and a narrow particle size distribution range by the method of the present invention, the types of organic solvent to be used, the concentration of silicon dioxide in the organic solvent suspension, the amount of water to be added, the addition method, stirring, etc. method, time,
It depends on granule conditions such as temperature. In order to obtain desired granules having a particle size in the range of 0.05 mm to 5 mm, the following granulation conditions are suitable. The organic solvent used may be a hydrocarbon having a paraffinic group, a naphthenic group, an aromatic group, or a mixture thereof. There is no particular limit to the amount (concentration) of silicon dioxide suspended in the organic solvent, but it is preferable that the amount of organic solvent be 20 ml to 90 ml per 1 gr of silicon dioxide.
ml range. The amount of water added is in the range of 55% to 80%, preferably 60% to 78%, based on the total weight of silicon dioxide and binder. The silicon dioxide in the suspension has a kind of colloidal shape, and at the beginning of stirring, each colloidal particle joins at a point using water as a binder, and in the next stage, these colloidal particles aggregate and form a flocculate. form. The amount of binder (water) is too low (55%
weight or less) and the flocs remain unchanged even if stirring is continued. When the binder is in the correct amount (55% to 80% by weight), stirring causes the flocs to further agglomerate and become compacted, forcing out the organic solvent present in the flocs and forming pellets. However, if stirring is continued even after pelletization, the resulting pellets will overlap and form even larger pellets, and these larger pellets will join together, causing the pellets to collapse and form a lump, eventually becoming a paste with little moisture. On the other hand, if the amount of binder is too large (more than 80% by weight), the floc-like state becomes a pasty state with a high water content, and it becomes impossible to form pellets. In order to obtain granules with uniform dimensions, it is necessary to adjust the stirring conditions so that the binder is uniformly dispersed and evenly collides with the colloidal silicon dioxide particles. For this purpose, a very small amount of surfactant is added to water as a binder, and this is mixed into the organic solvent that makes up the silicon dioxide suspension.
It is preferable to use it in a dispersed manner. The surfactant used may be a cationic, anionic or nonionic surfactant, and is a commonly used surfactant. The reaction step of reacting an alkali silicate with sulfuric acid to produce a fine hydrated silicate slurry is already known as a publicly known method. Silicon dioxide produced by washing, drying, and pulverizing the hydrated silicic acid slurry obtained by this method has silanol groups and is highly hydrophilic. Therefore, when water is added as a binder to a suspension of silicon dioxide in an organic solvent, it is important to avoid local non-uniformity in the binder concentration in the mixing system in the stirred tank. Furthermore, in order to obtain granules of desired dimensions, it is important to set appropriate granulation conditions. The granular amorphous silicic acid produced by the method of the present invention can be pulverized without any problems when mixed or kneaded with other raw materials and used in the same manner as ordinary fine silicic acid. The size and particle size distribution of the resulting granular silicic acid dioxide particles vary depending on the granulation conditions, and an example thereof is as follows. Example 1 The particle size was distributed in the range of 1.9 μm to 188 μm, of which 50.7% (weight) was in the range of 4.7 μm to 20.5 μm. Example 2 Particle size is distributed in the range of 898.3 μm to 1880 μm.
【表】
本発明方法において、造粒に使用する攪拌装置
は、特公昭39−21502号公報、実公昭44−19507号
公報、実公昭48−41284号公報および実公昭53−
39737号公報に記載されている造粒分離装置の試
験室規模の小型のもので、攪拌槽の内容積は3000
mlである。
実施例
次に実施例を掲げて本発明を説明するが、これ
に限定されるものではない。
実施例 １
内容積80の加温管付攪拌槽に、SiO228.40％
（重量）、Na2O9.13％（重量）、SiO2／Na2Oモル
比3.11の市販の珪酸ナトリウム水溶液12.14Kgを
とり、純水を加えて51.6とし、攪拌しながら、
90±１℃に保ち、70％硫酸1.15Kgを加えた後、１
時間熟成し、その後さらに70％硫酸を添加し、PH
を4.8に調整して二酸化珪酸を生成させ、得られ
た乳白色の懸濁液を濾過し、残液中の芒硝を水洗
により除去、乾燥して微粉末状の二酸化珪素を得
た。
この二酸化珪素を対象試料として使用した。
二酸化珪素48.6ｇ、市販家庭用灯油2800ml、お
よび水70mlを上記造粒機（インペラー回転数
1180r.p.m）に入れ、室温で44分間攪拌して造粒
試験を行なつた。
界面活性剤として、ソルビタンモノオレートを
バインダー（水）に対して75ppmを使用した。
固液分離後、造粒物を70℃の乾燥室内にて乾燥
して目的の二酸化珪素造粒物を得た。
上記の市販の家庭用灯油の性状は次のとおりで
ある。
比重：0.8038、
反応：中性、
色調（セイボルト）：30以上、
銅板腐蝕（50℃×3hrs）：１、
引火点（ダグ）：49℃、
全硫黄分：0.002％（重量）以下、
煙点：23.0℃
蒸留性状：１
初留点 163℃
10％ 181℃
50％ 209℃
90％ 245℃
95％ 252.5℃
97％ 257.5℃
終 点 264℃
得られた顆粒物の粒度分布、見掛比重、カサ容
量は、次のとおりである。[Table] In the method of the present invention, the stirring device used for granulation is disclosed in Japanese Patent Publication No. 39-21502, Japanese Utility Model Publication No. 19507-1982, Japanese Utility Model Publication No. 48-41284, and Japanese Utility Model Publication No. 48-41284.
This is a small laboratory-scale granulation and separation device described in Publication No. 39737, and the internal volume of the stirring tank is 3000.
ml. Examples Next, the present invention will be explained with reference to examples, but the present invention is not limited thereto. Example 1 28.40% SiO 2 was placed in a stirring tank with an internal volume of 80 mm and a heating tube.
(by weight), Na 2 O 9.13% (weight), SiO 2 /Na 2 O molar ratio 3.11, 12.14 kg of a commercially available sodium silicate aqueous solution was added, pure water was added to make a total concentration of 51.6, and while stirring,
After keeping at 90±1℃ and adding 1.15kg of 70% sulfuric acid,
Aged for an hour, then further added 70% sulfuric acid, pH
was adjusted to 4.8 to produce silicic acid dioxide, and the resulting milky white suspension was filtered, and the remaining liquid was washed with water to remove Glauber's salt and dried to obtain finely powdered silicon dioxide. This silicon dioxide was used as a target sample. 48.6 g of silicon dioxide, 2800 ml of commercially available household kerosene, and 70 ml of water were added to the above granulator (impeller rotation speed
1180 rpm) and stirred at room temperature for 44 minutes to conduct a granulation test. As a surfactant, sorbitan monooleate was used at 75 ppm based on the binder (water). After solid-liquid separation, the granules were dried in a drying chamber at 70°C to obtain the desired silicon dioxide granules. The properties of the above commercially available household kerosene are as follows. Specific gravity: 0.8038, Reaction: Neutral, Color tone (Saybolt): 30 or more, Copper plate corrosion (50℃ x 3hrs): 1, Flash point (Dag): 49℃, Total sulfur content: 0.002% (weight) or less, Smoke point :23.0℃ Distillation properties: 1 Initial boiling point 163℃ 10% 181℃ 50% 209℃ 90% 245℃ 95% 252.5℃ 97% 257.5℃ End point 264℃ Particle size distribution, apparent specific gravity, bulk capacity of the obtained granules is as follows.
【表】
見掛比重ｇ／ml、 カサ比重ml／100ｇｒ、
実施例１ 0.316 319
市販品Ａ 0.285 349
市販品Ｂ 0.180 870
見掛比重：試料50ｇ／cm2の荷重をかけた場合の比
重である。
カサ比重：試料50ｇを内容500mlのビーカーに入
れ、数回タツピングしたときのカ
サ容積。
市販品Ａ：二酸化珪素の噴霧乾燥品。
市販品Ｂ：微粉末状（粒度範囲1.9μｍ〜23.8μｍ）
の二酸化珪素。
実施例 ２
上記実施例１で使用した二酸化珪素48.6ｇ、市
販家庭用灯油2800mlおよび水83mlを造粒機（イン
ペラー回転数450r.p.m）に入れ、室温にて65分間
造粒試験した。
界面活性剤は実施例１と同様であつた。
得られた顆粒物の粒度分布、見掛比重、カサ比
重は次のとうりである。[Table] Apparent specific gravity g/ml, bulk specific gravity ml/100gr, Example 1 0.316 319 Commercial product A 0.285 349 Commercial product B 0.180 870 Apparent specific gravity: Specific gravity when a load of 50 g/cm 2 is applied to the sample . Bulk specific gravity: Bulk volume when 50g of sample is placed in a 500ml beaker and tapped several times. Commercial product A: Spray-dried product of silicon dioxide. Commercial product B: Fine powder (particle size range 1.9 μm to 23.8 μm)
silicon dioxide. Example 2 48.6 g of silicon dioxide used in Example 1 above, 2800 ml of commercial household kerosene, and 83 ml of water were placed in a granulator (impeller rotation speed: 450 rpm), and a granulation test was conducted at room temperature for 65 minutes. The surfactant was the same as in Example 1. The particle size distribution, apparent specific gravity, and bulk specific gravity of the obtained granules are as follows.
【表】
見掛比重、カサ比重は実施例１と同様であつ
た。
実施例 ３
上記実施例１で使用した二酸化珪素48.6ｇ、市
販家庭用灯油2800ml、および水80mlを造粒機（イ
ンペラー回転数460rpm）に入れ、室温にて80分
間造粒試験した。
界面活性剤は実施例１と同様であつた。
得られた顆粒物の粒度分布、見掛比重、カサ比
重は次のとうりである。[Table] The apparent specific gravity and bulk specific gravity were the same as in Example 1. Example 3 48.6 g of silicon dioxide used in Example 1 above, 2800 ml of commercially available household kerosene, and 80 ml of water were placed in a granulator (impeller rotation speed: 460 rpm), and a granulation test was conducted at room temperature for 80 minutes. The surfactant was the same as in Example 1. The particle size distribution, apparent specific gravity, and bulk specific gravity of the obtained granules are as follows.
【表】
見掛比重、カサ比重は実施例１と同様であつ
た。
発明の効果
本発明方法によつて得られた顆粒の流動性はよ
く、粉塵の発生は殆どなく、カサ高の欠点も除去
され、貯蔵、運搬及び取扱いの面でも好適であ
る。[Table] The apparent specific gravity and bulk specific gravity were the same as in Example 1. Effects of the Invention The granules obtained by the method of the present invention have good fluidity, hardly generate dust, eliminate the drawback of bulkiness, and are suitable in terms of storage, transportation, and handling.
Claims (1)
水をバインダーとして液中造粒し、造粒物を分
離、乾燥させることを特徴とする顆粒状二酸化珪
素の製造方法。 ２ バインダーを微粉状二酸化珪素とバインダー
との合計重量当たり55％重量乃至80％重量を使用
する特許請求の範囲第１項記載の方法。 ３ 界面活性剤を併用する特許請求の範囲第１項
記載の方法。 ４ 有機溶媒が石油系炭化水素である特許請求の
範囲第１項記載の方法。[Claims] 1. Suspending particulate silicon dioxide in an organic solvent,
A method for producing granular silicon dioxide, comprising submerged granulation using water as a binder, separation and drying of the granulated product. 2. The method according to claim 1, wherein the binder is used in an amount of 55% to 80% by weight based on the total weight of the finely divided silicon dioxide and the binder. 3. The method according to claim 1, which uses a surfactant in combination. 4. The method according to claim 1, wherein the organic solvent is a petroleum hydrocarbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20183787A JPS6445711A (en) | 1987-08-14 | 1987-08-14 | Production of granular silicon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20183787A JPS6445711A (en) | 1987-08-14 | 1987-08-14 | Production of granular silicon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6445711A JPS6445711A (en) | 1989-02-20 |
| JPH058127B2 true JPH058127B2 (en) | 1993-02-01 |
Family
ID=16447714
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20183787A Granted JPS6445711A (en) | 1987-08-14 | 1987-08-14 | Production of granular silicon dioxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6445711A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5255507B2 (en) * | 2009-04-22 | 2013-08-07 | 電気化学工業株式会社 | Granule and method for producing the same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6340715A (en) * | 1986-06-06 | 1988-02-22 | ロ−ヌ−プ−ラン・シミ | Silica base granule, manufacture and use as reinforcing filler for elastomer |
-
1987
- 1987-08-14 JP JP20183787A patent/JPS6445711A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6340715A (en) * | 1986-06-06 | 1988-02-22 | ロ−ヌ−プ−ラン・シミ | Silica base granule, manufacture and use as reinforcing filler for elastomer |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6445711A (en) | 1989-02-20 |
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