JP2006124547A - Fine particle of iron oxide for coloring material of ink for inkjet, ink for inkjet, and method for producing ink for inkjet - Google Patents

Fine particle of iron oxide for coloring material of ink for inkjet, ink for inkjet, and method for producing ink for inkjet Download PDF

Info

Publication number
JP2006124547A
JP2006124547A JP2004315774A JP2004315774A JP2006124547A JP 2006124547 A JP2006124547 A JP 2006124547A JP 2004315774 A JP2004315774 A JP 2004315774A JP 2004315774 A JP2004315774 A JP 2004315774A JP 2006124547 A JP2006124547 A JP 2006124547A
Authority
JP
Japan
Prior art keywords
iron oxide
ink
fine particles
inkjet
oxide fine
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
JP2004315774A
Other languages
Japanese (ja)
Inventor
Takahiro Kikuchi
孝宏 菊地
Shinichi Kijima
愼一 来島
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.)
JFE Chemical Corp
Original Assignee
JFE Chemical 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 JFE Chemical Corp filed Critical JFE Chemical Corp
Priority to JP2004315774A priority Critical patent/JP2006124547A/en
Publication of JP2006124547A publication Critical patent/JP2006124547A/en
Pending legal-status Critical Current

Links

Landscapes

  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Ink Jet (AREA)
  • Ink Jet Recording Methods And Recording Media Thereof (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide fine particles of iron oxide for coloring material exhibiting a bright red color suitable for magenta by processing an iron oxide pigment used as a coloring agent into fine particles with a size suitable for ink for inkjet, and to provide an ink for inkjet and a method for producing the same. <P>SOLUTION: The fine particles of iron oxide for coloring material of ink for inkjet comprises fine particles of iron oxide having ≤200 nm of average particle size and containing 0.05-3% by mass of Mn and manifesting ≤2 μm of maximum coagulated particle size in dispersing the fine particles of iron oxide in a solvent and has ≤0.7 μm of D50 which means the size of the coagulated particles with 50% of the integrated mass percent. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

本発明は、インクジェット方式による印刷や塗装に用いるインクの着色材に好適な酸化鉄微粒子及びこの酸化鉄微粒子を着色材として用いるインクジェット用インクに関するものである。   The present invention relates to iron oxide fine particles suitable for an ink coloring material used for ink jet printing and painting, and an ink jet ink using the iron oxide fine particles as a coloring material.

近年、パソコンやデジタルカメラのプリンターとして、インクジェット方式のプリンターが多く使われている。これらのインクジェット式プリンターのインクには、着色材として染料や有機顔料が多く使われており、例えば、シアン、マゼンタ、イエロー、ブラックなどの各種インクにより印刷や着色が行われている。   In recent years, inkjet printers are often used as printers for personal computers and digital cameras. In these ink jet printer inks, many dyes and organic pigments are used as coloring materials. For example, printing and coloring are performed with various inks such as cyan, magenta, yellow, and black.

また、最近では、プリンター以外にも、例えば、特開平7−116597号公報(特許文献1)、特開2002−19025号公報(特許文献2)、特開2004−175056号公報(特許文献3)などの記載にあるような建築用化粧板など建材への着色や模様の印刷、或いは、特開2002−293670号公報(特許文献4)の記載にあるような美術タイルやセラミック材など着色後に焼成を伴うような陶材への着色など、様々な分野でインクジェット方式による印刷や着色を行うことが検討されている。   Recently, in addition to printers, for example, JP-A-7-116597 (Patent Document 1), JP-A 2002-19025 (Patent Document 2), JP-A 2004-175056 (Patent Document 3). Coloring and printing of building materials such as decorative decorative boards for buildings as described in the above, or firing after coloring such as art tiles and ceramic materials as described in JP-A-2002-293670 (Patent Document 4) In various fields, such as coloring of porcelain with a color, printing and coloring by an ink jet method are being studied.

さらに、例えば、特開平9−323434号公報(特許文献5)、特開2002−172765号公報(特許文献6)、特開2004−195762号公報(特許文献7)などには建材の着色に適した印刷装置も提案されている。   Furthermore, for example, JP-A-9-323434 (Patent Document 5), JP-A 2002-172765 (Patent Document 6), JP-A 2004-195762 (Patent Document 7), etc. are suitable for coloring building materials. A printing apparatus has also been proposed.

しかし、これらの建材着色用などの分野では、従来のプリンターの印刷物とは異なり、屋外で長期に渡り使用されるものが多い。   However, in fields such as those for coloring building materials, unlike the printed matter of conventional printers, many are used outdoors for a long time.

一方、従来からインクジェット式プリンターには、着色材として発色性や吐出安定性に優れた染料や有機顔料が多く使われてきたが、これら着色材としての染料や有機顔料は、屋外で使用する場合には、紫外線による退色など、耐光性や耐候性に問題があり、建材の着色や印刷用には適していない。また、焼成を伴うような陶材への着色の場合も、前記染料や有機顔料を用いることはできない。   On the other hand, ink-jet printers have traditionally used many dyes and organic pigments with excellent color development and ejection stability as colorants, but these dyes and organic pigments as colorants are used outdoors. Have problems with light resistance and weather resistance, such as fading due to ultraviolet rays, and are not suitable for coloring or printing of building materials. Moreover, the said dye and organic pigment cannot be used also in the case of coloring to porcelain which accompanies baking.

そのため、これらの用途には無機顔料を着色材として用いたインクジェット用のインクが求められるが、従来の無機顔料は粒径が大きく、分散性が悪いため、インクジェット式の記録ヘッドからの吐出安定性が悪いという問題がある。しかし、このような問題はあるものの、屋外での使用を可能とするためには、耐光性や耐候性に優れた無機顔料を着色材として用いたインクジェット用のインクを用いる必要があり、その開発が行われている。このうち、赤系統の色については、酸化鉄顔料(ヘマタイト)をマゼンタインクとして使えないかどうかが検討されている。   For this reason, inkjet inks using inorganic pigments as colorants are required for these applications, but conventional inorganic pigments have a large particle size and poor dispersibility, so that they are stable in ejection from inkjet recording heads. There is a problem that is bad. However, in spite of such problems, in order to be able to use outdoors, it is necessary to use ink-jet inks using inorganic pigments with excellent light resistance and weather resistance as colorants. Has been done. Among these, for red colors, it has been examined whether iron oxide pigments (hematite) can be used as magenta inks.

一般に、顔料用の赤色酸化鉄は、硫酸鉄溶液をアルカリ溶液で中和して空気酸化することでマグネタイトを生成させ、このマグネタイトを熱処理する方法で製造している。これらの赤色酸化鉄の色調の鮮やかさは、酸化鉄中のMn量が影響していることが知られており、鮮やかな赤色を得るため、Mn含有量の少ない原料硫酸鉄溶液を使用したり、マグネタイト中にMnが取り込まれにくい条件で合成するなどの方法が行われている。
特開平7−116597号公報 特開2002−19025号公報 特開2004−175056号公報 特開2002−293670号公報 特開平9−323434号公報 特開2002−172765号公報 特開2004−195762号公報
In general, red iron oxide for pigment is produced by a method in which an iron sulfate solution is neutralized with an alkali solution and air oxidized to generate magnetite, and the magnetite is heat-treated. The vividness of the color tone of these red iron oxides is known to be affected by the amount of Mn in the iron oxide. To obtain a bright red color, the raw iron sulfate solution with a low Mn content can be used. A method of synthesizing under the condition that Mn is hardly taken into magnetite is performed.
Japanese Unexamined Patent Publication No. 7-116597 JP 2002-19025 A JP 2004-175056 A JP 2002-293670 A JP-A-9-323434 JP 2002-172765 A JP 2004-195762 A

しかし、上記方法により製造された赤色の顔料用酸化鉄を、そのまま微粒化してインクジェットのインク用に適した粒子サイズとするだけではオレンジ色がかった黄色味の強い赤色になってしまい、マゼンタには適さなくなるという問題がある。一般的に、酸化鉄は粒径が小さくなるほど黄色味の強い赤色となるからである。   However, the red pigment iron oxide produced by the above method is atomized as it is to obtain a particle size suitable for ink jet ink, resulting in an orange-ish yellowish red. There is a problem that it is not suitable. This is because iron oxide generally becomes red with a strong yellowishness as the particle size decreases.

そこで、本発明は、着色材として用いる酸化鉄顔料をインクジェット用のインクに適した粒子サイズに微粒化した場合においてもマゼンタに適した鮮やかな赤色を呈する着色材用酸化鉄微粒子、インクジェット用インク及びインクジェット用インクの製造方法を提供することを目的とする。   Therefore, the present invention provides an iron oxide fine particle for a colorant that exhibits a bright red color suitable for magenta even when the iron oxide pigment used as a colorant is atomized to a particle size suitable for an ink jet ink, an ink jet ink, and An object of the present invention is to provide a method for producing an inkjet ink.

上記目的を達成するために、本発明は以下のような特徴を有する。
[1]平均粒径が200nm以下、Mn含有量が0.05mass%以上3mass%以下であるインクジェット用インクの着色材用酸化鉄微粒子。
[2]平均粒径が200nm以下、Mn含有量が0.05mass%以上3mass%以下であるインクジェット用インクの着色材用酸化鉄微粒子であって、
前記酸化鉄微粒子を溶媒中に分散させた場合の凝集粒子の最大粒径が2μm以下、前記凝集粒子の積算体積百分率が50%となるD50が0.7μm以下であることを特徴とするインクジェット用インクの着色材用酸化鉄微粒子。
[3]上記[1]または[2]に記載の酸化鉄微粒子を着色材として用いるインクジェット用インク。
[4]平均粒径が200nm以下、Mn含有量が0.05mass%以上3mass%以下である酸化鉄微粒子を、溶媒中に分散させ、前記酸化鉄の凝集粒子の最大粒径を2μm以下、前記凝集粒子の積算体積百分率が50%となるD50を0.7μm以下とするインクジェット用インクの製造方法。
In order to achieve the above object, the present invention has the following features.
[1] Iron oxide fine particles for colorants of ink-jet inks having an average particle size of 200 nm or less and an Mn content of 0.05 mass% to 3 mass%.
[2] Iron oxide fine particles for a coloring material of an inkjet ink having an average particle size of 200 nm or less and a Mn content of 0.05 mass% or more and 3 mass% or less,
When the iron oxide fine particles are dispersed in a solvent, the maximum particle diameter of the aggregated particles is 2 μm or less, and the D50 at which the cumulative volume percentage of the aggregated particles is 50% is 0.7 μm or less. Iron oxide fine particles for ink colorants.
[3] An inkjet ink using the iron oxide fine particles according to [1] or [2] as a coloring material.
[4] Iron oxide fine particles having an average particle diameter of 200 nm or less and an Mn content of 0.05 mass% or more and 3 mass% or less are dispersed in a solvent, and the maximum particle diameter of the aggregated particles of iron oxide is 2 μm or less, A method for producing an ink-jet ink, wherein D50 at which the cumulative volume percentage of aggregated particles is 50% is 0.7 μm or less.

本発明によれば、着色材として用いる酸化鉄顔料をインクジェット用のインクに適した粒子サイズに微粒化した場合においてもマゼンタに適した鮮やかな赤色を呈する着色材用酸化鉄微粒子、インクジェット用インク及びインクジェット用インクの製造方法が提供される。   According to the present invention, even when the iron oxide pigment used as the colorant is atomized to a particle size suitable for an ink jet ink, the iron oxide fine particles for the colorant exhibiting a bright red color suitable for magenta, the ink jet ink, and A method for producing an inkjet ink is provided.

以下、本発明を実施するための最良の形態の一例を説明する。   Hereinafter, an example of the best mode for carrying out the present invention will be described.

本発明のインクジェット用インクの着色材用酸化鉄微粒子は、平均粒径が200nm以下である。平均粒径が200nmよりも大きくなると、インクジェットの記録ヘッドからのインクの安定吐出性が悪くなり、色調も黒ずんだ色となりマゼンタに適さない色となるからである。前記平均粒径は、好ましくは150nm以下、より好ましくは120nm以下、さらに好ましくは100nm以下が色調的には望ましい。   The iron oxide fine particles for coloring material of the inkjet ink of the present invention have an average particle size of 200 nm or less. This is because when the average particle size is larger than 200 nm, the stable ejection property of ink from the ink jet recording head is deteriorated, and the color tone becomes dark and unsuitable for magenta. The average particle diameter is preferably 150 nm or less, more preferably 120 nm or less, and still more preferably 100 nm or less in terms of color tone.

平均粒径の下限は20nm以上であることが好ましい。20nm未満では、黄色味が強くなり、また、均一分散も困難となるからである。   The lower limit of the average particle size is preferably 20 nm or more. This is because if it is less than 20 nm, the yellowish color becomes strong and uniform dispersion becomes difficult.

ここで、前記平均粒径は、透過電子顕微鏡写真を用いて、100個以上の粒子について粒径を測定し、平均した値を用いることが好ましい。なお、酸化鉄微粒子の粒子形状が不定形や針状の場合は、比表面積を測定し、その比表面積値から粒子が球形だと仮定して求めた粒径をその粒子の粒径として用いてもよい。ただし、粒子表面に多数の凹凸があるような場合は、透過電子顕微鏡写真を用いて粒径を測定することが必要である。   Here, it is preferable that the average particle size is a value obtained by measuring the particle size of 100 or more particles using a transmission electron micrograph and averaging the measured particle size. In addition, when the particle shape of the iron oxide fine particles is indefinite or needle-shaped, the specific surface area is measured, and the particle diameter obtained by assuming that the particles are spherical from the specific surface area value is used as the particle diameter of the particles. Also good. However, when there are many irregularities on the particle surface, it is necessary to measure the particle size using a transmission electron micrograph.

本発明にかかる酸化鉄微粒子中にはMnが含まれていることが大きな特徴である。酸化鉄を微粒子化していくと、黄色味が強くなる傾向があるが、Mnがあることにより、黄色味が強くなるのを防ぐことが可能となる。ここで、本発明にかかる酸化鉄微粒子中のMn含有量は、0.05mass%以上3mass%以下である。Mn含有量が0.05mass%未満では黄色味が強くなるのを抑制することができず、3mass%を超えると黒ずんだ色となるので好ましくない。なお、前記酸化鉄微粒子中のMn含有量は、好ましくは0.05mass%以上1mass%以下、より好ましくは0.05mass%以上0.7mass%以下、さらに好ましくは0.05mass%以上0.5mass%以下、一層好ましくは0.05mass%以上0.3mass%以下である。   The iron oxide fine particles according to the present invention are characterized by containing Mn. When iron oxide is finely divided, the yellow color tends to become strong, but the presence of Mn makes it possible to prevent the yellow color from becoming strong. Here, the Mn content in the iron oxide fine particles according to the present invention is 0.05 mass% or more and 3 mass% or less. If the Mn content is less than 0.05 mass%, the yellowishness cannot be suppressed, and if it exceeds 3 mass%, the color becomes dark. The Mn content in the iron oxide fine particles is preferably 0.05 mass% to 1 mass%, more preferably 0.05 mass% to 0.7 mass%, and still more preferably 0.05 mass% to 0.5 mass%. Hereinafter, it is more preferably 0.05 mass% or more and 0.3 mass% or less.

本発明にかかる酸化鉄微粒子は、例えば、噴霧焙焼法、湿式法、水熱法など一般に知られている酸化鉄の製法で得ることができる。なお、直接ヘマタイトを作る方法以外に、マグネタイトやゲータイトなど他の形態の鉄酸化物を熱処理することによりヘマタイトにしたものを用いても構わない。   The iron oxide fine particles according to the present invention can be obtained by generally known iron oxide production methods such as spray roasting, wet method, and hydrothermal method. In addition to the method of directly producing hematite, hematite obtained by heat-treating other forms of iron oxide such as magnetite or goethite may be used.

前記製法により得られた酸化鉄は、粉砕することでその粒径(酸化鉄微粒子)や粒度分布(凝集粒子のD50)の調整が行われる。前記粉砕方法としては、例えば、微粉砕が可能な、ジェットミルや振動ミルなどの乾式粉砕機などを用いる方法により実現することができる。また、ビーズミルなどの湿式粉砕機などを用いても実現することができる。   The particle size (iron oxide fine particles) and particle size distribution (D50 of aggregated particles) are adjusted by pulverizing the iron oxide obtained by the above production method. The pulverization method can be realized by, for example, a method using a dry pulverizer such as a jet mill or a vibration mill capable of fine pulverization. It can also be realized using a wet pulverizer such as a bead mill.

前記方法による粉砕後は、必要に応じて、分級を行い、大きな粒子を除去することにより、酸化鉄の平均粒径を200nm以下とすることができる。前記分級を行うための分級機としては、例えば、一般に知られている気流式分級機などを用いることができる。   After pulverization by the above method, the average particle size of iron oxide can be reduced to 200 nm or less by performing classification as necessary and removing large particles. As a classifier for performing the classification, for example, a generally known airflow classifier can be used.

また、本発明にかかる酸化鉄微粒子の粒子形状は、球形や立方体形状などの粒状であることが好ましい。溶媒中での分散性がより向上し、また、マゼンタにより適した鮮やかな赤色を呈するようになるからである。   Moreover, it is preferable that the particle shape of the iron oxide fine particles according to the present invention is a granular shape such as a spherical shape or a cubic shape. This is because the dispersibility in the solvent is further improved and a bright red color more suitable for magenta is exhibited.

また、前記酸化鉄微粒子を、水または有機溶剤からなる溶媒中に分散させた場合の凝集粒子の最大粒径が2μm以下であることが必要である。2μmを超えるとインクジェットの記録ヘッドからのインクの安定吐出性が悪くなり、色調も黒ずんだ凝集粒子を含むようになり、マゼンタに適さない色となる。前記凝集粒子の最大粒径は、好ましくは1μm以下、さらに好ましくは0.8μm以下が望ましい。   Further, it is necessary that the maximum particle size of the aggregated particles when the iron oxide fine particles are dispersed in a solvent made of water or an organic solvent is 2 μm or less. If it exceeds 2 μm, the stable ejection property of the ink from the ink jet recording head is deteriorated, and the color tone includes agglomerated particles which are darkened, resulting in a color unsuitable for magenta. The maximum particle size of the aggregated particles is preferably 1 μm or less, more preferably 0.8 μm or less.

さらに、前記凝集粒子の積算の体積百分率が50%となるD50が0.7μm以下であることが必要である。前記D50が0.7μmを超えると色調も黒ずんだ色となりマゼンタに適さない色となるからである。好ましくは0.5μm以下、さらに好ましくは0.4μm以下が望ましい。   Further, it is necessary that D50 at which the volume percentage of the aggregated particles is 50% is 0.7 μm or less. This is because when D50 exceeds 0.7 μm, the color tone becomes dark and unsuitable for magenta. Preferably it is 0.5 μm or less, more preferably 0.4 μm or less.

ここで、前記酸化鉄微粒子を、水または有機溶剤からなる溶媒中に分散させる方法としては、例えば、超音波ホモジナイザー、超音波洗浄機等の装置を用いることにより行うことができる。   Here, as a method of dispersing the iron oxide fine particles in a solvent composed of water or an organic solvent, for example, an apparatus such as an ultrasonic homogenizer or an ultrasonic cleaner can be used.

前記超音波ホモジナイザーや超音波洗浄機を用いる場合は、水または有機溶剤からなる溶媒中に前記酸化鉄微粒子を混入し、超音波をかけ続けても凝集粒子の最大粒径やD50が変化しなくなる状態まで充分に分散させることが望ましい。なお、水または有機溶剤からなる溶媒には、分散剤が含まれていても構わない。   When the ultrasonic homogenizer or ultrasonic cleaner is used, the maximum particle diameter and D50 of the aggregated particles are not changed even if the iron oxide fine particles are mixed in a solvent composed of water or an organic solvent and the ultrasonic wave is continuously applied. It is desirable to disperse sufficiently to the state. In addition, the solvent which consists of water or an organic solvent may contain the dispersing agent.

ここで、粒度分布の測定には、レーザー回折式の粒度分布測定装置を用いることができる。   Here, a laser diffraction type particle size distribution measuring device can be used for measuring the particle size distribution.

さらに、本発明はインクジェット方式の印刷や塗装に用いるインクに、本発明にかかる酸化鉄微粒子を着色材として用いることを特徴としている。本発明にかかる酸化鉄微粒子を着色材として用いることにより、マゼンタに適した色調のインクを得ることができる。なお、前記インクには、本発明にかかる酸化鉄微粒子以外には、一般的に知られている組成物を含有させることができる。その製法としては、一般的に用いられているビーズミルなどを用いることができる。また、前記インクの製法も、前記酸化鉄微粒子を溶媒中に分散させた場合の凝集粒子の最大粒径が2μm以下であり、さらに、D50を0.7μm以下とできる方法であれば上記の方法に限られるものではない。   Furthermore, the present invention is characterized in that the iron oxide fine particles according to the present invention are used as a coloring material in an ink used for ink jet printing or painting. By using the iron oxide fine particles according to the present invention as a coloring material, an ink having a color tone suitable for magenta can be obtained. In addition to the iron oxide fine particles according to the present invention, the ink may contain a generally known composition. As its production method, a commonly used bead mill or the like can be used. In addition, the above-described ink can be produced as long as the maximum particle diameter of the aggregated particles when the iron oxide fine particles are dispersed in a solvent is 2 μm or less and the D50 can be 0.7 μm or less. It is not limited to.

以下に本発明を実施例によりさらに詳細に説明する。
(実施例1〜8、比較例1〜2)
塩化第一鉄溶液を噴霧焙焼法により処理することにより作製した、平均粒径250nm、Mnを0.23mass%含有する酸化鉄を原料とし、この酸化鉄をビーズミルにより粉砕し、乾燥させることによりインクジェット用インクの着色材用酸化鉄微粒子を作製した。ビーズミルで粉砕する際に、粉砕時間を変えて粒径、粒度分布の異なる酸化鉄微粒子を作成し、その色調を調べた。
Hereinafter, the present invention will be described in more detail with reference to examples.
(Examples 1-8, Comparative Examples 1-2)
By using iron oxide containing an average particle size of 250 nm and Mn of 0.23 mass%, prepared by treating a ferrous chloride solution by spray roasting, this iron oxide is pulverized by a bead mill and dried. Iron oxide fine particles for a coloring material of an inkjet ink were prepared. When pulverizing with a bead mill, iron oxide fine particles having different particle sizes and particle size distributions were prepared by changing the pulverization time, and the color tone was examined.

以下に示す表1に前記各酸化鉄微粒子の透過電子顕微鏡により、粒子100個以上について粒径を測定して求めた平均粒径、水に加えて超音波ホモジナイザーで、分散させた溶液をマイクロトラック粒度分布測定装置で測定したD50、2μmを超える凝集粒子の体積比率、マゼンタインクの色との色調の比較を行った結果を示す。   Table 1 below shows the average particle size obtained by measuring the particle size of 100 or more particles with a transmission electron microscope of each of the iron oxide fine particles, water, and the solution dispersed with an ultrasonic homogenizer in addition to water. The result of having compared D50 measured with the particle size distribution measuring apparatus, the volume ratio of the aggregated particle exceeding 2 micrometers, and the color tone with the color of a magenta ink is shown.

Figure 2006124547
Figure 2006124547

本発明にかかる実施例1〜8の酸化鉄微粒子は目標の色調に近い色調が得られたが、比較例1〜2の酸化鉄微粒子では目標とは外れた色調となった。また、前記実施例1〜8の酸化鉄微粒子を用いて作製したインクは良好な色調であった。
(実施例9〜19、比較例3〜4)
水にFeCl・4HO試薬を溶解した塩化第一鉄溶液に塩化マンガンを添加し、それを水酸化ナトリウム溶液で中和し、温度85℃、pH10で空気酸化を行い、マグネタイト粒子を作製した。このマグネタイト粒子を600℃で3時間熱処理してMn量の異なるヘマタイトを作製した。このヘマタイトを湿式ボールミルで粉砕し、乾燥させることによりインクジェット用インクの着色材用酸化鉄微粒子を作製した。
(実施例20)
塩化マンガンを含む塩化第一鉄溶液を炭酸ナトリウムで中和し、Fe濃度0.4mol/lの水酸化鉄溶液とし、30℃、pH12.5で空気酸化を行い、ゲータイト粒子を得た。このゲータイトを300℃で2時間熱処理し、ビーズミルで粉砕を行い酸化鉄微粒子を作製した。
(実施例21)
中和後のFe濃度0.1mol/lにした以外は、実施例20と同様な方法で作製した。
In the iron oxide fine particles of Examples 1 to 8 according to the present invention, a color tone close to the target color tone was obtained, but in the iron oxide fine particles of Comparative Examples 1 and 2, the color tone deviated from the target. Moreover, the ink produced using the iron oxide fine particles of Examples 1 to 8 had a good color tone.
(Examples 9 to 19, Comparative Examples 3 to 4)
Manganese chloride is added to ferrous chloride solution in which FeCl 2 · 4H 2 O reagent is dissolved in water, neutralized with sodium hydroxide solution, and air oxidized at a temperature of 85 ° C. and pH 10 to produce magnetite particles. did. The magnetite particles were heat-treated at 600 ° C. for 3 hours to prepare hematite having different amounts of Mn. This hematite was pulverized with a wet ball mill and dried to prepare fine iron oxide particles for ink-jet ink colorants.
(Example 20)
A ferrous chloride solution containing manganese chloride was neutralized with sodium carbonate to obtain an iron hydroxide solution having an Fe concentration of 0.4 mol / l, and air oxidation was performed at 30 ° C. and pH 12.5 to obtain goethite particles. This goethite was heat-treated at 300 ° C. for 2 hours and pulverized with a bead mill to produce iron oxide fine particles.
(Example 21)
It was produced by the same method as in Example 20 except that the Fe concentration after neutralization was 0.1 mol / l.

以下に示す表2及び表3に、前記実施例9〜21、比較例3〜4について、表1の場合と同様に測定した平均粒径、D50、 2μmを超える凝集粒子の体積比率、マゼンタインクの色との色調の比較を行った結果を示す。   In Tables 2 and 3 below, for Examples 9 to 21 and Comparative Examples 3 to 4, the average particle diameter measured in the same manner as in Table 1, D50, the volume ratio of aggregated particles exceeding 2 μm, and magenta ink The result of comparing the color tone with the color of is shown.

Figure 2006124547
Figure 2006124547

Figure 2006124547
Figure 2006124547

本発明にかかる実施例9〜19の酸化鉄微粒子は目標の色調に近い色調が得られるが、比較例3〜4の酸化鉄微粒子では目標とは外れた色調となった。実施例20の酸化鉄微粒子は針状形状を示し、実施例9〜19に比べ色調が劣っていた。また実施例21の酸化鉄微粒子は黄色味が強く、実施例9〜19に比べ色調が劣っていた。
実施例9〜19の酸化鉄微粒子を用いて作製したインクは良好な色調であった。
In the iron oxide fine particles of Examples 9 to 19 according to the present invention, the color tone close to the target color tone was obtained, but in the iron oxide fine particles of Comparative Examples 3 to 4, the color tone deviated from the target. The iron oxide fine particles of Example 20 showed a needle shape, and the color tone was inferior to Examples 9-19. Moreover, the iron oxide fine particles of Example 21 had a strong yellowish taste, and the color tone was inferior to Examples 9-19.
Inks prepared using the iron oxide fine particles of Examples 9 to 19 had good color tone.

Claims (4)

平均粒径が200nm以下、Mn含有量が0.05mass%以上3mass%以下であるインクジェット用インクの着色材用酸化鉄微粒子。   Iron oxide fine particles for colorants of ink-jet inks having an average particle size of 200 nm or less and a Mn content of 0.05 mass% to 3 mass%. 平均粒径が200nm以下、Mn含有量が0.05mass%以上3mass%以下であるインクジェット用インクの着色材用酸化鉄微粒子であって、
前記酸化鉄微粒子を溶媒中に分散させた場合の凝集粒子の最大粒径が2μm以下、前記凝集粒子の積算体積百分率が50%となるD50が0.7μm以下であることを特徴とするインクジェット用インクの着色材用酸化鉄微粒子。
An iron oxide fine particle for a coloring material of an inkjet ink having an average particle diameter of 200 nm or less and a Mn content of 0.05 mass% or more and 3 mass% or less,
When the iron oxide fine particles are dispersed in a solvent, the maximum particle diameter of the aggregated particles is 2 μm or less, and the D50 at which the cumulative volume percentage of the aggregated particles is 50% is 0.7 μm or less. Iron oxide fine particles for ink colorants.
請求項1または請求項2に記載の酸化鉄微粒子を着色材として用いるインクジェット用インク。   An inkjet ink using the iron oxide fine particles according to claim 1 as a coloring material. 平均粒径が200nm以下、Mn含有量が0.05mass%以上3mass%以下である酸化鉄微粒子を、溶媒中に分散させ、前記酸化鉄の凝集粒子の最大粒径を2μm以下、前記凝集粒子の積算体積百分率が50%となるD50を0.7μm以下とするインクジェット用インクの製造方法。   Iron oxide fine particles having an average particle size of 200 nm or less and an Mn content of 0.05 mass% to 3 mass% are dispersed in a solvent, and the maximum particle size of the aggregated particles of iron oxide is 2 μm or less. A method for producing an inkjet ink, wherein the D50 at which the cumulative volume percentage is 50% is 0.7 μm or less.
JP2004315774A 2004-10-29 2004-10-29 Fine particle of iron oxide for coloring material of ink for inkjet, ink for inkjet, and method for producing ink for inkjet Pending JP2006124547A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2004315774A JP2006124547A (en) 2004-10-29 2004-10-29 Fine particle of iron oxide for coloring material of ink for inkjet, ink for inkjet, and method for producing ink for inkjet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2004315774A JP2006124547A (en) 2004-10-29 2004-10-29 Fine particle of iron oxide for coloring material of ink for inkjet, ink for inkjet, and method for producing ink for inkjet

Publications (1)

Publication Number Publication Date
JP2006124547A true JP2006124547A (en) 2006-05-18

Family

ID=36719587

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2004315774A Pending JP2006124547A (en) 2004-10-29 2004-10-29 Fine particle of iron oxide for coloring material of ink for inkjet, ink for inkjet, and method for producing ink for inkjet

Country Status (1)

Country Link
JP (1) JP2006124547A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007321043A (en) * 2006-05-31 2007-12-13 Jfe Chemical Corp Iron oxide fine particles and magenta ink
JP2012121994A (en) * 2010-12-08 2012-06-28 Seiko Epson Corp Inkjet recording ink, deinked pulp, and method for producing thereof
EP2421923A4 (en) * 2009-04-23 2013-05-29 Hewlett Packard Company L P Ink compositions and methods of use

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4932711B1 (en) * 1970-12-25 1974-09-02
JPS5352539A (en) * 1976-10-25 1978-05-13 Toda Kogyo Corp Method of preparing dark red system pigments of iron oxide
JPH08143316A (en) * 1994-11-22 1996-06-04 Titan Kogyo Kk Iron oxide pigment, its production and its use
JPH08239614A (en) * 1995-03-06 1996-09-17 Toto Ltd Ink composition molding resin article, and production of molded resin article
JPH09279075A (en) * 1996-04-11 1997-10-28 Catalysts & Chem Ind Co Ltd Ink for ink jet printer and preparation thereof
JPH11228144A (en) * 1997-10-20 1999-08-24 Bayer Ag Red iron oxide pigment, its production and its use
JP2000038533A (en) * 1998-07-24 2000-02-08 Fuji Shikiso Kk Solvent-based pigment ink for jet printer
JP2000204305A (en) * 1999-01-13 2000-07-25 Fuji Xerox Co Ltd Ink for ink-jet recording
JP2001506049A (en) * 1996-12-03 2001-05-08 コーニンクレッカ フィリップス エレクトロニクス エヌ ヴィ Electric light with coating for displaying information and display ink for this electric light
JP2001200177A (en) * 1999-12-02 2001-07-24 Bayer Ag Method for producing iron oxide pigment

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4932711B1 (en) * 1970-12-25 1974-09-02
JPS5352539A (en) * 1976-10-25 1978-05-13 Toda Kogyo Corp Method of preparing dark red system pigments of iron oxide
JPH08143316A (en) * 1994-11-22 1996-06-04 Titan Kogyo Kk Iron oxide pigment, its production and its use
JPH08239614A (en) * 1995-03-06 1996-09-17 Toto Ltd Ink composition molding resin article, and production of molded resin article
JPH09279075A (en) * 1996-04-11 1997-10-28 Catalysts & Chem Ind Co Ltd Ink for ink jet printer and preparation thereof
JP2001506049A (en) * 1996-12-03 2001-05-08 コーニンクレッカ フィリップス エレクトロニクス エヌ ヴィ Electric light with coating for displaying information and display ink for this electric light
JPH11228144A (en) * 1997-10-20 1999-08-24 Bayer Ag Red iron oxide pigment, its production and its use
JP2000038533A (en) * 1998-07-24 2000-02-08 Fuji Shikiso Kk Solvent-based pigment ink for jet printer
JP2000204305A (en) * 1999-01-13 2000-07-25 Fuji Xerox Co Ltd Ink for ink-jet recording
JP2001200177A (en) * 1999-12-02 2001-07-24 Bayer Ag Method for producing iron oxide pigment

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007321043A (en) * 2006-05-31 2007-12-13 Jfe Chemical Corp Iron oxide fine particles and magenta ink
EP2421923A4 (en) * 2009-04-23 2013-05-29 Hewlett Packard Company L P Ink compositions and methods of use
US8840234B2 (en) 2009-04-23 2014-09-23 Hewlett-Packard Development Company, L.P. Ink compositions and methods of use
JP2012121994A (en) * 2010-12-08 2012-06-28 Seiko Epson Corp Inkjet recording ink, deinked pulp, and method for producing thereof

Similar Documents

Publication Publication Date Title
JP5399633B2 (en) Oxidation-modified pigment and method for preparing jet ink composition containing the pigment
US20060219133A1 (en) Colored resin particles, water-based dispersion containing the colored resin particles, and ink for ink-jet printing or color filter
JP2001164148A (en) Aqueous carbon black dispersion and its production method and use
US6666914B2 (en) Black colorant for ink-jet printing ink, ink-jet printing ink, and aqueous pigment dispersion containing the black colorant
JP2008150507A (en) Colored resin fine particle, aqueous dispersion containing the colored resin fine particle, inkjet recording ink or ink for color filter
US6440561B2 (en) Iron oxide hydroxide composite particles, pigment, paint and resin composition
WO2010001965A1 (en) Coating composition
JP2006307165A (en) Colored resin particles, water-based dispersion containing the colored resin particles, and ink for ink-jet printing or color filter
JP3212065B2 (en) Fine particle composite oxide black pigment and method for producing the same
EP0997500B1 (en) Fine red iron oxide pigment, and paint or resin composition using the same
JP4399886B2 (en) Strontium iron oxide particle powder for non-magnetic black pigment and method for producing the same
JP4856474B2 (en) Iron oxide fine particles and magenta ink
JP2006124547A (en) Fine particle of iron oxide for coloring material of ink for inkjet, ink for inkjet, and method for producing ink for inkjet
CN111748222B (en) High-tinting strength copper-chromium black pigment and preparation method thereof
KR20060129174A (en) Composite black oxide particle, method for producing same, black coating material and black matrix
JP4452958B2 (en) Fine red iron oxide pigment, process for producing the same, paint and resin composition using the pigment
JP4688708B2 (en) Black composite oxide particles, production method thereof, black paste and black matrix
JP2997206B2 (en) Fine particle composite oxide black pigment and method for producing the same
JP4056826B2 (en) Composite oxide black pigment and method for producing the same
JP4336227B2 (en) Composite black oxide particles, method for producing the same, black paint and black matrix
EP2799500A1 (en) Composite oxide black pigment and method for producing same
JP4336224B2 (en) Composite black oxide particles, method for producing the same, black paint and black matrix
JP4444061B2 (en) Composite black oxide particles, method for producing the same, black paint and black matrix
JP2004155979A (en) Composite colored particle for inkjet ink, process for producing it, predispersion for inkjet ink and inkjet ink
JP2007231131A (en) Colored resin fine particle, water-based dispersion containing the colored resin particle, ink for inkjet printing or ink for color filter

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20070312

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20100805

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20100817

A02 Decision of refusal

Free format text: JAPANESE INTERMEDIATE CODE: A02

Effective date: 20101214