JPH03124772A - Treatment of carbon black - Google Patents
Treatment of carbon blackInfo
- Publication number
- JPH03124772A JPH03124772A JP26300989A JP26300989A JPH03124772A JP H03124772 A JPH03124772 A JP H03124772A JP 26300989 A JP26300989 A JP 26300989A JP 26300989 A JP26300989 A JP 26300989A JP H03124772 A JPH03124772 A JP H03124772A
- Authority
- JP
- Japan
- Prior art keywords
- carbon black
- ozone
- fluidized bed
- gas
- powdered carbon
- 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
Links
- 239000006229 carbon black Substances 0.000 title claims abstract description 83
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 7
- 150000001721 carbon Chemical class 0.000 abstract description 15
- 238000010438 heat treatment Methods 0.000 abstract description 15
- 238000001035 drying Methods 0.000 abstract description 14
- 239000000654 additive Substances 0.000 abstract description 9
- 230000000996 additive effect Effects 0.000 abstract description 9
- 238000004040 coloring Methods 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000011362 coarse particle Substances 0.000 abstract description 5
- 241000872198 Serjania polyphylla Species 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 30
- 238000012986 modification Methods 0.000 description 16
- 230000004048 modification Effects 0.000 description 16
- 239000000976 ink Substances 0.000 description 8
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 239000003973 paint Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000004925 denaturation Methods 0.000 description 3
- 230000036425 denaturation Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 101100145155 Escherichia phage lambda cIII gene Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はオゾン変性カーボンブラックの製造方法に係り
、詳しくはインキ、塗料等の着色用添加剤として好適な
オゾン変性カーボンブラックの製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing ozone-modified carbon black, and more particularly to a method for producing ozone-modified carbon black suitable as a coloring additive for inks, paints, etc.
粉末状カーボンブラックは、ゴム、プラスチック、ペイ
ント、インキ、塗料等の各種製品の着色や補強のための
添加剤又は充填剤として広く用いられている。このとき
、粉末状カーボンブラックの表面性状が、得られる製品
の性質に大きく影響するので、粉末状カーボンブラック
の表面を変性することが行われている。例えば、オゾン
含有気体と接触して表面を酸化すると、製品に添加した
ときの流動性がよくなることが知られており、着色用、
特にインキ用や塗料用として用いる場合に好ましく、種
々の酸化方法が検討されている（特公昭４６−１８３６
８号公報、特公昭４６−４３６０８号公報）。Powdered carbon black is widely used as an additive or filler for coloring or reinforcing various products such as rubber, plastics, paints, inks, and paints. At this time, since the surface properties of the powdered carbon black greatly affect the properties of the obtained product, the surface of the powdered carbon black is modified. For example, it is known that oxidizing the surface by contacting with ozone-containing gas improves fluidity when added to products.
It is particularly suitable for use in inks and paints, and various oxidation methods have been studied (Japanese Patent Publication No. 46-1836).
8, Japanese Patent Publication No. 46-43608).
ところが、オゾンで表面変性するには、オゾン分子とカ
ーボンブラック表面とを十分に接触させることが必要で
あり、そのためには通常の方法で製造したカーボンブラ
ックをそのまま用いたのでは、表面に水や各種の気体等
が付着しており、表面変性を十分に行うことは困難であ
る。However, in order to modify the surface with ozone, it is necessary to bring the ozone molecules into sufficient contact with the carbon black surface. Since various gases and the like are attached, it is difficult to sufficiently modify the surface.
そこで前記特公昭４６−１８３６８号公報記載の方法で
は、オゾンで表面変性する前に乾燥空気で粉末状カーボ
ンブラックを乾燥して表面や空隙から水分や揮発性ガス
をエルトリエイジョンしているが、この乾燥空気はオゾ
ン処理工程で発生する排ガスであり、本発明者の追試に
よると、温度が低いために、表面付着物質の除去が必ず
しも十分ではない。そしてオゾン含有雰囲気にした特殊
なドラム中で粉末状カーボンブラックを繰り返し上昇、
落下させるものであるが、処理中にカーボンブラックが
凝集しやすいという欠点がある。Therefore, in the method described in Japanese Patent Publication No. 46-18368, powdered carbon black is dried with dry air before surface modification with ozone to elutriate moisture and volatile gases from the surface and voids. This dry air is exhaust gas generated in the ozone treatment process, and according to additional tests conducted by the present inventors, the removal of surface-adhering substances is not necessarily sufficient due to the low temperature. Then, powdered carbon black is repeatedly raised in a special drum with an ozone-containing atmosphere.
However, it has the disadvantage that carbon black tends to aggregate during processing.
また前記特公昭４６−４３６０８号公報記載の方法では
粉末状カーボンブラックをジェットミル中でオゾン含有
気体と高圧に接触させているが、装置の運転が煩雑であ
り、コストのかかるものである。Further, in the method described in Japanese Patent Publication No. 46-43608, powdered carbon black is brought into contact with an ozone-containing gas under high pressure in a jet mill, but the operation of the apparatus is complicated and costly.
本発明の目的は、効率よくオゾン変性カーボンブラック
を製造する方法を提供することにある。An object of the present invention is to provide a method for efficiently producing ozone-modified carbon black.
また均一にオゾン変性されたカーボンブラックを製造す
る方法を提供することにある。特にインキ塗料等の着色
用添加剤として良好な性状を有するオゾン変性カーボン
ブラックを製造する方法を提ＩＪ（することにある。Another object of the present invention is to provide a method for producing uniformly ozone-modified carbon black. We propose a method for producing ozone-modified carbon black, which has good properties especially as a coloring additive for ink paints and the like.
本発明者は上記のような課題を解決するために研究を行
い、粉末状カーボンブラックをオゾン含有ガスと接触さ
せる前に、加熱乾燥するとともに凝集塊を除くことによ
りオゾンによる表面変性を均一に行えること及びオゾン
による表面変性を振動流動層にて行うことにより変性の
効率がよくなることを見出し本発明を完成した。The present inventor conducted research to solve the above problems, and found that by heating and drying powdered carbon black and removing aggregates before bringing it into contact with ozone-containing gas, the surface modification by ozone can be uniformly performed. Furthermore, the present invention was completed based on the discovery that the efficiency of the modification can be improved by performing the surface modification using ozone in a vibrating fluidized bed.
すなわち本発明は粉末状カーボンブラックをオゾンガス
を以て処理してカーボンブラック粒子の表面特性を化学
的に変化させる方法において、粉末状カーボンブラック
を温度１００℃以上で加熱乾燥して水分を除去した後に
分級して粒子径ｉ、ｏｏｏμｍ以上のカーボンブラック
凝集塊を除去し、振動流動層にてオゾン含有気体と接触
させて表面変性することを特徴とするカーボンブラック
の処理方法である。That is, the present invention is a method of chemically changing the surface characteristics of carbon black particles by treating powdered carbon black with ozone gas, in which the powdered carbon black is heated and dried at a temperature of 100°C or higher to remove moisture, and then classified. This method of treating carbon black is characterized by removing carbon black agglomerates having a particle diameter of i, ooo μm or more, and surface-modifying the carbon black by bringing it into contact with an ozone-containing gas in a vibrating fluidized bed.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
本発明で用いる粉末状カーボンブラックとしてはファー
ネス式反応炉で製造したものがよく、反応炉で得られる
エアロゾル状カーボンブラックを水で急冷した後にバグ
フィルタ−等の捕集器を用いて捕集した粉末状カーボン
ブラックがよい。この粉末状カーボンブラックには、反
応炉の耐火材の破片等の異物やカーボンブラックの粗大
粒子が含まれていることがあり、そのまま用いると、こ
れらの異物や粗大粒子が、例えば、塗料では塗面の均一
性を損ない品質を低下させるので、風力分級器等の分級
器で分級する等して、それらの異物やカーボンブラック
粗大粒子を除去するのがよい。The powdered carbon black used in the present invention is preferably produced in a furnace type reactor, and the aerosolized carbon black obtained in the reactor is rapidly cooled with water and then collected using a collector such as a bag filter. Powdered carbon black is preferable. This powdered carbon black may contain foreign matter such as fragments of the refractory material of the reactor and coarse particles of carbon black. Since they impair the surface uniformity and lower the quality, it is preferable to remove these foreign substances and coarse particles of carbon black by classifying them using a classifier such as an air classifier.
またインキ用の添加剤として用いるオゾン変性カーボン
ブラックを製造する場合には、粒径１００μｍ以上、好
ましくは１０μｍ以上の粗大粒子を除去するようにする
のがよい。なお、この分級工程は乾燥工程の前後いずれ
でもよいが、前の方が好ましい。Furthermore, when producing ozone-modified carbon black for use as an additive for ink, it is preferable to remove coarse particles with a particle size of 100 μm or more, preferably 10 μm or more. Note that this classification step may be performed either before or after the drying step, but it is preferable to perform the classification step before or after the drying step.
本発明では粉末状カーボンブラックを温度１００℃以上
、好ましくは１０４℃〜１５０℃に加熱して乾燥する。In the present invention, powdered carbon black is dried by heating to a temperature of 100°C or higher, preferably 104°C to 150°C.
加熱温度が１００℃未満では、乾燥効率が悪（、十分に
乾燥するのが難しく、１５０℃を超えると加熱雰囲気が
空気の場合、空気中の酸素分子とカーボンブラックとの
反応が生じるので好ましくない。この加熱乾燥工程での
乾燥の程度が高い程、オゾンによる表面変性を効率よく
できるので、含水率が０％になるまで乾燥するのが好ま
しいが、含水率が１％以下になるまで乾燥すれば十分に
実施可能である。加熱雰囲気は窒素等の不活性ガス雰囲
気が好ましいが、空気でも差し支えない。また、雰囲気
の湿度が低い程、乾燥効率がよい。加熱時間については
、加熱温度や加熱雰囲気、加熱帯域でのカーボンブラッ
クの濃度等にもよるが、通常は１時間以上で、含水率を
１％以下にすることができる。具体的な加熱方法として
は、スチームを流通するジャケットを有する乾燥器を用
いてジャケットに囲まれた乾燥帯域において間接加熱し
て乾燥する方法がある。なおり−ボンブラックの含水率
の測定はＪＩＳ−に５１０１に準じて行うことができる
。If the heating temperature is less than 100°C, the drying efficiency is poor (it is difficult to dry thoroughly), and if the heating temperature exceeds 150°C, if the heating atmosphere is air, a reaction will occur between oxygen molecules in the air and carbon black, which is undesirable. The higher the degree of drying in this heat drying step, the more efficiently the surface modification by ozone can be achieved, so it is preferable to dry until the moisture content is 0%, but it is preferable to dry until the moisture content is 1% or less. The heating atmosphere is preferably an inert gas atmosphere such as nitrogen, but air may also be used.Also, the lower the humidity of the atmosphere, the better the drying efficiency.The heating time depends on the heating temperature and heating time. Although it depends on the atmosphere, the concentration of carbon black in the heating zone, etc., it is usually possible to reduce the moisture content to 1% or less in one hour or more.A specific heating method includes using a jacket through which steam flows. There is a method of drying by indirect heating in a drying zone surrounded by a jacket using a dryer.The moisture content of Naori-bon black can be measured according to JIS-5101.
粉末状カーボンブラックは凝集性を有し、反応炉以降の
各工程で凝集しやすいため、加熱乾燥して得られる粉末
状カーボンブラックにはカーボンブラック凝集塊が含ま
れており、カーボンブラック凝集塊を含む粉末状カーボ
ンブラックをオゾン含有気体と接触すると、凝集塊表面
では表面変性が起こるが、内部では変性が不均一になり
やすく、また振動流動層でオゾン含有気体と接触する際
に凝集塊が流動層の底部に沈澱して操業の障害になるの
で、本発明では加熱乾燥した粉末状カーボンブラックを
分級して粒子径１，０００μｍ以上のカーボンブラック
凝集塊を除去した後に、オゾン含有気体と接触して表面
を変性する。このときの分級方法としては篩による方法
が好ましく、１８メツシユ（口径１，０００μｍ）より
細かい篩、好ましくは１００メツシユ（口径１４７μｍ
）程度の篩を用いて凝集塊を除去するのがよい。Powdered carbon black has cohesive properties and tends to agglomerate in each process after the reactor, so the powdered carbon black obtained by heating and drying contains carbon black agglomerates. When powdered carbon black containing powder comes into contact with an ozone-containing gas, surface modification occurs on the surface of the agglomerates, but the modification tends to be uneven inside, and when the agglomerates come into contact with the ozone-containing gas in a vibrating fluidized bed, the agglomerates flow. Since it settles at the bottom of the layer and becomes a hindrance to operation, in the present invention, heat-dried powdered carbon black is classified to remove carbon black aggregates with a particle size of 1,000 μm or more, and then brought into contact with an ozone-containing gas. to modify the surface. The preferred method for classification at this time is a method using a sieve, which is a sieve finer than 18 meshes (1,000 μm in diameter), preferably 100 meshes (147 μm in diameter).
) It is best to remove aggregates using a sieve.
オゾンによる粉末状カーボンブラックの表面変性は、オ
ゾン含有気体の偏流を防ぐ点から振動流動層で行う。本
発明でいう振動流動層によるオゾン変性方法の一例とし
て、粉末状カーボンブラックが通過しないスクリーンの
下方から気体を流通して、スクリーン上に粉末状カーボ
ンブラックを浮遊させ、下方から流通する気体としてオ
ゾン含有気体を用いてオゾン変性する方法があり、スク
リーンを含む装置全体を振動してオゾン含有気体の（Ｑ
流を防止するようにしたのが、振動流動層である。Surface modification of powdered carbon black with ozone is carried out in a vibrating fluidized bed to prevent uneven flow of ozone-containing gas. As an example of the ozone modification method using a vibrating fluidized bed according to the present invention, gas is passed from below a screen where powdered carbon black does not pass through, the powdered carbon black is suspended on the screen, and ozone is used as the gas flowing from below. There is a method of ozone denaturation using a gas containing ozone, in which the entire device including the screen is vibrated to modify the ozone-containing gas (Q).
A vibrating fluidized bed is used to prevent flow.
本発明で用いる振動流動層式反応機の一例を第２図に示
す。第２図中、１３は孔径３μｍのＳＵＳ製スタスクリ
ーン２は粉末状カーボンブラック投入口、１５はオゾン
含有気体導入管、１６は排気管、１７はオゾン変性カー
ボンブラック排出用コック、２５は振動用スプリング、
２６は振動用モータを示す。なおオゾン変性する際の振
動は振動数５〜６０１１ｚの範囲より適宜選択するのが
よい。An example of a vibrating fluidized bed reactor used in the present invention is shown in FIG. 2. In Figure 2, 13 is an SUS star screen 2 with a pore diameter of 3 μm, which is a powder carbon black inlet, 15 is an ozone-containing gas introduction pipe, 16 is an exhaust pipe, 17 is a cock for discharging ozone-modified carbon black, and 25 is for vibration. spring,
26 indicates a vibration motor. Note that the vibration during ozone modification is preferably selected from a frequency range of 5 to 6011z.
その他、振動流動層式オゾン反応機として、スクリーン
上への粉末状カーボンブラックの導入とオゾン変性カー
ボンブラックの排出とを連続的に行うようにしたものを
用いると、連続的にオゾン変性することができる。In addition, if a vibrating fluidized bed ozone reactor is used that continuously introduces powdered carbon black onto a screen and discharges ozone-modified carbon black, continuous ozone modification is possible. can.
次に、本発明で用いるオゾン含有気体としては、用いる
装置にもより、特に限定はないが、一般的には気体中の
オゾン濃度が０，１〜４０ｇ／Ｎｍ３のものがよく、オ
ゾン以外には活性な分子を含まないものが好ましいが、
オゾンを混合した乾燥空気でも差し支えない。オゾン濃
度が０．１ｇ ／ Ｎ ｍ ３未満の気体では、オゾン
による表面変性の速度が遅くて効率が悪く、４０ｇ／Ｎ
ｍ３を超えると排気ガスに大量のオゾンが残存しやすく
なり、排気ガスの処理が困難になる。Next, the ozone-containing gas used in the present invention is not particularly limited depending on the equipment used, but in general, it is preferable that the ozone concentration in the gas is 0.1 to 40 g/Nm3. preferably does not contain active molecules, but
Dry air mixed with ozone may also be used. In gases with an ozone concentration of less than 0.1 g/N m3, the speed of surface modification by ozone is slow and inefficient;
If it exceeds m3, a large amount of ozone tends to remain in the exhaust gas, making it difficult to treat the exhaust gas.
また接触する際のオゾン含有気体及び粉末状カーボンブ
ラックの温度は常温〜１５０℃程度がよい。この温度が
高い程、オゾンとカーボンブラックの表面との反応の速
度は速くなるが、高すぎるとオゾン分子の熱分解が速く
なるため表面変性の効率が低下する傾向がある。The temperature of the ozone-containing gas and powdered carbon black during contact is preferably from room temperature to about 150°C. The higher the temperature, the faster the rate of reaction between ozone and the surface of carbon black, but if it is too high, the thermal decomposition of ozone molecules becomes faster and the efficiency of surface modification tends to decrease.
オゾンによる表面変性の程度は必要に応じて適宜調節す
ることができるが、通常、インキ着色用添加剤として用
いるカーボンブラックを製造する場合には、酸化度がｐ
Ｈ３以下になるまで表面変性するのがよく、粉末状カー
ボンブラックに対して１〜１５ｆｆｉ量％のオゾンを反
応することにより可能である。The degree of surface modification by ozone can be adjusted as necessary, but usually when producing carbon black used as an ink coloring additive, the degree of oxidation is
It is preferable to modify the surface until the carbon black becomes H3 or less, and this can be done by reacting 1 to 15% of ozone to powdered carbon black.
なお流動状態のカーボンブラックにオゾン含有気体を流
通してオゾンによる表面変性を行う場合には風速１〜５
０（７）／秒程度でオゾン含有気体を流通するのがよい
。１ｃＩＩＩ／秒未満では流動性が悪くなる傾向があり
、５０ｃｍ／秒を超えるとカーボンブラックの飛散が増
え、また排気ガスに未反応オゾンが大量に残存すること
になる。In addition, when performing surface modification with ozone by passing an ozone-containing gas through carbon black in a fluidized state, the wind speed is 1 to 5.
It is preferable to flow the ozone-containing gas at a rate of about 0(7)/second. If it is less than 1 cIII/sec, the fluidity tends to deteriorate, and if it exceeds 50 cm/sec, the scattering of carbon black will increase, and a large amount of unreacted ozone will remain in the exhaust gas.
以下に、実施例によって本発明を更に具体的に説明する
が、本発明はこの実施例によって何等限定されるもので
はない。EXAMPLES The present invention will be explained in more detail below with reference to Examples, but the present invention is not limited to these Examples in any way.
（実施例１）
本発明を実施する装置の一例のフローシートである第１
図によって説明する。(Example 1) The first example is a flow sheet of an example of an apparatus for carrying out the present invention.
This will be explained using figures.
反応炉１で生成したエアロゾル状カーボンブラックを冷
却塔２で水冷し、バッグフィルター３で粉末状カーボン
ブラックを分雛して捕集し、定量供給機４により気送管
５を通じてサイクロン方式の風力分級機６に導入１７て
粉末状カーボンブラック中の異物及び粒径５０μｍ以上
の粗大粒子を除去した。次いで気送管７を通じてバッグ
フィルター８に導入して固気分離し、粉末状カーボンブ
ラックを捕集した。The aerosolized carbon black produced in the reactor 1 is cooled with water in a cooling tower 2, and the powdered carbon black is fractionated and collected in a bag filter 3, and then passed through a pneumatic pipe 5 by a quantitative feeder 4 for air classification using a cyclone method. The powdered carbon black was introduced into a machine 6 to remove foreign matter and coarse particles having a particle size of 50 μm or more. Next, it was introduced into a bag filter 8 through a pneumatic pipe 7 for solid-gas separation, and powdered carbon black was collected.
バッグフィルター８で捕集した粉末状カーボンブラック
をバルブ９を介して、スチームを流通しているジャケッ
トを有する乾燥機１０の乾燥帯域に導入し、温度］−０
５℃で１時間加熱乾燥した後、１８メツシユの篩を供え
た振動篩１１を通過してカーボンブラック凝集塊を除去
した。The powdered carbon black collected by the bag filter 8 is introduced through a valve 9 into a drying zone of a dryer 10 having a jacket through which steam is passed, and the temperature is set to −0.
After drying by heating at 5° C. for 1 hour, it was passed through a vibrating sieve 11 equipped with an 18-mesh sieve to remove carbon black aggregates.
さらに振動９１１を通過した粉末状カーボンブラックを
投入口１２から振動流動層式オゾン反応機１４内に設置
しであるスクリーン１３玉に導入し、一方で、オゾン含
有量１０ｇ／Ｎｍ”の乾燥空気をオゾン反応機１４内部
において１０艶／秒の線速となるような流速で配管１５
を通して振動数５０１１ｚで振動している振動流動層式
オゾン反応機１４内に導入し、スクリーン１３を通して
、スクリーン１３上で粉末状カーボンブラックと接触さ
せた。このとき排気ガスのオゾン含有量は１ｇ／Ｎｍ３
以下であった。なお、反応は常温で行った。Further, the powdered carbon black that has passed through the vibration 911 is introduced from the inlet 12 into the screen 13 installed in the vibrating fluidized bed ozone reactor 14, while dry air with an ozone content of 10 g/Nm'' is introduced. The pipe 15 is heated at a flow rate of 10 g/sec inside the ozone reactor 14.
The mixture was introduced into a vibrating fluidized bed ozone reactor 14 vibrating at a frequency of 5011z through a screen 13, and was brought into contact with powdered carbon black on the screen 13. At this time, the ozone content of the exhaust gas is 1g/Nm3
It was below. Note that the reaction was performed at room temperature.
粉末状カーボンブラックの量に対し、消費されたオゾン
の量が５重量％となる量のオゾン含有乾燥空気と接触さ
せ、ついで乾燥空気でオゾンを除去し、バルブ１７から
系外に排出させる。It is brought into contact with ozone-containing dry air in an amount such that the amount of ozone consumed is 5% by weight based on the amount of powdered carbon black, and then ozone is removed with the dry air and discharged from the system through a valve 17.
回収したオゾン変性カーボンブラックの平均粒子径は１
５．０％ｍ、ジブチルフタレート吸／ｒｈｆｆｉは６０
ｍｌ／ １００ ｇ−酸化度はｐＨ３、表面揮発分は１
０％、黒色度は７９であり、インキむ色用添加剤として
優れた性状を有するものであった。The average particle size of the recovered ozone-modified carbon black is 1
5.0%m, dibutyl phthalate absorption/rhffi is 60
ml/100 g - Oxidation degree is pH 3, surface volatile content is 1
0%, blackness was 79, and had excellent properties as an ink color additive.
酸化度及び表面揮発分の測定はＪ Ｉｓ−に６６２１に
準じて行った。The degree of oxidation and surface volatile matter were measured according to JIS-6621.
尚第１図中の２１は製品回収タンク、２３はオゾン分解
装置を示す。In FIG. 1, 21 is a product recovery tank, and 23 is an ozone decomposition device.
（比較例１）
振動篩１１によるカーボンブラック凝集塊の除去を行わ
なかった他は実施例１と同様にしたところ、流動層式オ
ゾン反応機Ｊ４によるオゾン変性の際に、スクリーン１
３上にカーボンブラック凝集塊の沈澱が発生してオゾン
含有気体の流通が偏流し、オゾンの転化率が悪く、排気
ガスのオゾン含有量はＩｇ／ｍ３を超えていた。(Comparative Example 1) The same procedure as Example 1 was carried out except that carbon black aggregates were not removed using the vibrating sieve 11. During ozone modification using the fluidized bed ozone reactor J4, the screen 1
Precipitation of carbon black agglomerates occurred on No. 3, and the flow of the ozone-containing gas became uneven, the conversion rate of ozone was poor, and the ozone content of the exhaust gas exceeded Ig/m3.
また、回収したオゾン変性カーボンブラックの酸化度は
ｐＨ５，２、表面揮発分は４％であった。Further, the oxidation degree of the recovered ozone-modified carbon black was pH 5.2, and the surface volatile content was 4%.
（比較例２）
振動篩１１の篩を１０メツシユの篩（口径２．０００μ
ｍ）に換えた他は実施例１と同様にしたところ、流動層
式オゾン反応機１４によるオゾン変性の際に、スクリー
ン１３上にカーボンブラック凝集塊の沈澱が発生した。(Comparative Example 2) The sieve of the vibrating sieve 11 was a 10-mesh sieve (diameter 2.000μ).
When the same procedure as in Example 1 was carried out except that m) was used, carbon black aggregates were precipitated on the screen 13 during ozone modification using the fluidized bed ozone reactor 14.
回収したオゾン変性カーボンブラック中の凝集塊の酸化
度はｐＨ３，５、表面揮発分は９％であった。The degree of oxidation of the aggregates in the recovered ozone-modified carbon black was pH 3.5, and the surface volatile content was 9%.
（比較例３）
乾燥機１０による加熱乾燥を行わなかった曲は実施例１
と同様にした。(Comparative Example 3) The songs that were not heated and dried using the dryer 10 were those of Example 1.
I did the same thing.
回収したオゾン変性カーボンブラックの酸化度はｐＨ４
、表面揮発分は８％であった。The degree of oxidation of the recovered ozone-modified carbon black is pH 4.
The surface volatile content was 8%.
（比較例４）
オゾン反応機１４の振動を停止してオゾン変性を行った
他は実施例１と同様にしたところ、オゾン含有乾燥空気
が１闇流し、反応機の周壁付近の粉末状カーボンブラッ
クの変性を十分に行うのが困難であった。(Comparative Example 4) The same procedure as Example 1 was carried out except that the vibration of the ozone reactor 14 was stopped and ozone denaturation was carried out. Ozone-containing dry air was flowed darkly, and the powdered carbon black near the peripheral wall of the reactor was It was difficult to carry out sufficient denaturation.
本発明によれば、粉末状カーボンブラックの表面変性を
効率よく行うことができ、インキ着色用添加剤として優
れた性状を有するオゾン変性カーボンブラックを効率よ
く製造できる。According to the present invention, the surface of powdered carbon black can be efficiently modified, and ozone-modified carbon black having excellent properties as an ink coloring additive can be efficiently produced.
第１図は本発明を実施する装置の一例のフローシートを
示す図面である。
第２図は本発明で用い
る振動流動層式オゾン反応機の一例を示す断面立面図で
ある。FIG. 1 is a drawing showing a flow sheet of an example of an apparatus for carrying out the present invention. FIG. 2 is a cross-sectional elevational view showing an example of a vibrating fluidized bed type ozone reactor used in the present invention.
Claims (1)
して水分を除去した後に分級して粒子径１，０００μｍ
以上のカーボンブラック凝集塊を除去し、振動流動層に
てオゾン含有気体と接触させて表面変性することを特徴
とするカーボンブラックの処理方法。Powdered carbon black is heat-dried at a temperature of 100°C or higher to remove moisture, and then classified to a particle size of 1,000 μm.
A method for treating carbon black, which comprises removing the above carbon black agglomerates and surface-modifying the carbon black by bringing it into contact with an ozone-containing gas in a vibrating fluidized bed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26300989A JPH03124772A (en) | 1989-10-11 | 1989-10-11 | Treatment of carbon black |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26300989A JPH03124772A (en) | 1989-10-11 | 1989-10-11 | Treatment of carbon black |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03124772A true JPH03124772A (en) | 1991-05-28 |
Family
ID=17383625
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26300989A Pending JPH03124772A (en) | 1989-10-11 | 1989-10-11 | Treatment of carbon black |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03124772A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19511240A1 (en) * | 1994-03-28 | 1995-10-05 | Mitsubishi Chem Corp | Carbon black, esp. furnace black useful for pigmenting paint, ink or resin |
| US6471933B1 (en) | 1995-02-21 | 2002-10-29 | Anderson Oliver Dotson | Ozone-oxidized carbon black composition with low conductivity and improved color |
| DE102007060307A1 (en) | 2007-12-12 | 2009-06-18 | Evonik Degussa Gmbh | Process for the aftertreatment of carbon black |
| CN102585565A (en) * | 2012-03-19 | 2012-07-18 | 苏州宝化炭黑有限公司 | Method and device for manufacturing carbon black pigment |
| JP2014172963A (en) * | 2013-03-07 | 2014-09-22 | Ricoh Co Ltd | Ink for inkjet recording, ink cartridge, inkjet recording method, inkjet recording device and ink printed matter |
| US8852739B2 (en) | 2010-02-23 | 2014-10-07 | Evonik Carbon Black Gmbh | Carbon black, method for the production thereof, and use thereof |
| US8915998B2 (en) | 2008-11-27 | 2014-12-23 | Evonik Carbon Black Gmbh | Pigment granulate, method for producing the same and use thereof |
| CN116441171A (en) * | 2023-06-19 | 2023-07-18 | 烁元新材料(东营)股份有限公司 | Carbon black environment-friendly hierarchical refining device |
-
1989
- 1989-10-11 JP JP26300989A patent/JPH03124772A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19511240A1 (en) * | 1994-03-28 | 1995-10-05 | Mitsubishi Chem Corp | Carbon black, esp. furnace black useful for pigmenting paint, ink or resin |
| DE19511240B4 (en) * | 1994-03-28 | 2005-07-21 | Mitsubishi Chemical Corp. | Soot and method of production |
| US6471933B1 (en) | 1995-02-21 | 2002-10-29 | Anderson Oliver Dotson | Ozone-oxidized carbon black composition with low conductivity and improved color |
| DE102007060307A1 (en) | 2007-12-12 | 2009-06-18 | Evonik Degussa Gmbh | Process for the aftertreatment of carbon black |
| US8915998B2 (en) | 2008-11-27 | 2014-12-23 | Evonik Carbon Black Gmbh | Pigment granulate, method for producing the same and use thereof |
| US8852739B2 (en) | 2010-02-23 | 2014-10-07 | Evonik Carbon Black Gmbh | Carbon black, method for the production thereof, and use thereof |
| CN102585565A (en) * | 2012-03-19 | 2012-07-18 | 苏州宝化炭黑有限公司 | Method and device for manufacturing carbon black pigment |
| JP2014172963A (en) * | 2013-03-07 | 2014-09-22 | Ricoh Co Ltd | Ink for inkjet recording, ink cartridge, inkjet recording method, inkjet recording device and ink printed matter |
| CN116441171A (en) * | 2023-06-19 | 2023-07-18 | 烁元新材料(东营)股份有限公司 | Carbon black environment-friendly hierarchical refining device |
| CN116441171B (en) * | 2023-06-19 | 2023-08-11 | 烁元新材料(东营)股份有限公司 | Carbon black environment-friendly hierarchical refining device |
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