JPS5938259A - Preparation of heat-resistant yellow iron oxide pigment - Google Patents
Preparation of heat-resistant yellow iron oxide pigmentInfo
- Publication number
- JPS5938259A JPS5938259A JP14682182A JP14682182A JPS5938259A JP S5938259 A JPS5938259 A JP S5938259A JP 14682182 A JP14682182 A JP 14682182A JP 14682182 A JP14682182 A JP 14682182A JP S5938259 A JPS5938259 A JP S5938259A
- Authority
- JP
- Japan
- Prior art keywords
- iron oxide
- yellow iron
- antimony
- aluminum
- heat
- 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
Landscapes
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は耐熱性の優れた特性を有する黄色酸化鉄顔料の
製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a yellow iron oxide pigment having excellent heat resistance.
現在黄色酸化鉄顔料は黄鉛、カドミウム黄及びベンジジ
ンエロー等の有毒黄色顔料の代替品としての用途を拡大
しつつある。しかし黄色酸化鉄は上記有毒顔料に比べ耐
熱性が劣るだめに代替品としての使用範囲は狭く、更に
耐熱性の良好な黄色酸化鉄顔料の開発が待たれていた。Currently, yellow iron oxide pigments are finding increasing use as replacements for toxic yellow pigments such as yellow lead, cadmium yellow, and benzidine yellow. However, yellow iron oxide has inferior heat resistance compared to the above-mentioned toxic pigments, so its range of use as a substitute is narrow, and the development of a yellow iron oxide pigment with even better heat resistance has been awaited.
そこで本発明者らは黄色酸化鉄の大きな欠点である耐熱
性を向上させるために鋭意研究を重ね、市販黄色酸化鉄
より１００℃程度耐熱性の向上した新しい耐熱性黄色酸
化鉄顔料及びその製造方法を開発し、これにより無毒性
の黄色酸化鉄顔料のポリエチレン、ポリプロピレン及び
ＡＢＳ等の高温度で成形加工することが必要な分野への
使用を可能にした。（特開昭５５−１５８１３０号及び
特開昭５５−１５８１３１号各公報参照）
この方法は市販黄色酸化鉄を第二鉄塩水溶液に加え、ア
ルカリを添加し更にアルミニウム化合物と１種又は２種
以上の金属化合物、特に一般式２．５ （ＸｉＶｉ （
３，５（ここにおいてＸｌは第３成分として添加した各
金属のモル分率Ｖ＋ １は第３成分として添加した各金
属の原子価である。）で示される金属化合物を添加した
後、１００〜２５０℃の範囲で加圧加熱処理を行なって
市販黄色酸化鉄粒子表面にＡ１００Ｈと第３成分の金属
化合物が固溶した黄色酸化鉄を被覆する工程、該黄色酸
化鉄と母液とを分離しアルカリを除く工程及び該黄色酸
化鉄を水に分散し再度加圧加熱処理を施す工程を経て著
しく耐熱性の向上した黄色酸化鉄顔料を製造するもので
ある。Therefore, the present inventors have conducted extensive research to improve heat resistance, which is a major drawback of yellow iron oxide, and have developed a new heat-resistant yellow iron oxide pigment that has improved heat resistance by approximately 100°C compared to commercially available yellow iron oxide pigments, and a method for producing the same. This made it possible to use a non-toxic yellow iron oxide pigment in fields that require high-temperature molding of polyethylene, polypropylene, ABS, etc. (Refer to JP-A-55-158130 and JP-A-55-158131.) In this method, commercially available yellow iron oxide is added to an aqueous ferric salt solution, an alkali is added, and one or more aluminum compounds are added. Metal compounds of the general formula 2.5 (XiVi (
3,5 (here, Xl is the molar fraction V+ of each metal added as the third component; 1 is the valence of each metal added as the third component). A step of coating the surface of commercially available yellow iron oxide particles with yellow iron oxide in which A100H and a third component metal compound are solidly dissolved by applying pressure and heat treatment in the range of 250°C, separating the yellow iron oxide and the mother liquor, and treating the surface with an alkali. A yellow iron oxide pigment with significantly improved heat resistance is produced through the steps of removing the yellow iron oxide and dispersing the yellow iron oxide in water and subjecting it to pressure and heat treatment again.
しかしながら、この方法の工業的な実施を考慮する場合
、２回の加圧加熱処理操作（基体黄色酸化鉄に特公昭５
３−２８１５８号公報に記載されているアルカリ水溶液
において２５０℃以下の温度で加圧加熱処理を施した黄
色酸化鉄を用いると３回の加圧加熱処理操作）を要する
ため製造原価が高くなり前記酬熱黄色酸化鉄が優れた耐
熱特性を有するにもかかわらずその広範囲な使用を制限
されているのが実情である。However, when considering the industrial implementation of this method, two pressurized and heat treatment operations (the yellow iron oxide substrate was treated with
If yellow iron oxide, which has been subjected to pressure and heat treatment in an aqueous alkaline solution at a temperature of 250° C. or lower, as described in Japanese Patent No. 3-28158, requires three times of pressure and heat treatment, the production cost will be high. Despite the fact that hot yellow iron oxide has excellent heat resistance properties, its widespread use is currently restricted.
そこで市販黄色酸化鉄よりも１００℃程度耐熱性の向上
した黄色酸化鉄を大量安価に製造する方法について種々
検討した結果、黄色酸化鉄粒子表面をアンチモン及びア
ルミニウムの含水酸化物あるいはアンチモン、アルミニ
ウム及びケイ素の含水酸化物で被覆処理した後、熱水中
において加圧加熱処理を施すという操作法により基体黄
色酸化鉄の耐熱性を一挙に１００℃近く向上させること
ができることを発見し、本発明を完成するに至った。即
ち従来の処理方法により基体黄色酸化鉄にこの程度の耐
熱性を付与しようとすると２回の加圧加熱処理を必要と
したが、本発明による処理方法によれば１回の加圧加熱
処理しか必要としないことから処理費が大巾に低下し、
著しく耐熱性の向上した黄色酸化鉄を大量安価に供給す
ることが可能になった。Therefore, as a result of various studies on methods for producing yellow iron oxide in large quantities and at low cost, which has improved heat resistance by about 100 degrees Celsius compared to commercially available yellow iron oxide, we found that the surface of yellow iron oxide particles could be made of hydrous oxides of antimony and aluminum, or hydrated oxides of antimony, aluminum, and silicon. discovered that the heat resistance of the yellow iron oxide substrate could be improved by nearly 100°C at once by coating it with a hydrous oxide and then applying pressure and heat treatment in hot water, and completed the present invention. I ended up doing it. In other words, in order to impart this level of heat resistance to the yellow iron oxide substrate using the conventional treatment method, two pressure and heat treatments were required, but with the treatment method of the present invention, only one pressure and heat treatment is required. Since it is not necessary, processing costs are greatly reduced,
It has become possible to supply large amounts of yellow iron oxide with significantly improved heat resistance at low cost.
次に本発明の構成について説明する。Next, the configuration of the present invention will be explained.
本発明は、市販黄色酸化鉄の水性スラリーにアンチモン
塩水溶液及びアルミニウム塩水溶液かあるいはアンチモ
ン塩水溶液、アルミニウム塩水溶液及びケイ酸塩水溶液
を添加して加水分解させ、該黄色酸化鉄粒子表面にアン
チモン及びアルミニウムの含水酸化物あるいはアンチモ
ン、アルミニウム及びケイ素の含水酸化物を沈積被覆せ
しめた後、オートクレーブに仕込み、１５０℃〜３００
℃の温度で加圧加熱処理することを特徴とする耐熱性黄
色酸化鉄顔料の製造方法である。In the present invention, an aqueous antimony salt solution and an aqueous aluminum salt solution, or an aqueous antimony salt solution, an aqueous aluminum salt solution, and an aqueous silicate solution are added to a commercially available aqueous slurry of yellow iron oxide to cause hydrolysis, and the surface of the yellow iron oxide particles is coated with antimony and After depositing and coating the hydrous oxide of aluminum or the hydrous oxides of antimony, aluminum and silicon, the mixture is charged into an autoclave and heated at 150°C to 300°C.
This is a method for producing a heat-resistant yellow iron oxide pigment, which is characterized by carrying out pressure and heat treatment at a temperature of °C.
本発明はまた市販黄色酸化鉄をアルカリ性水溶液中で２
５０℃以下の温度で加圧水熱処理を施して得だ黄色酸化
鉄のアルカリ水性スラリーに、アンチモン塩水溶液及び
アルミニウム塩水溶液かあるいはアンチモン塩水溶液、
アルミニウム塩水溶液及びケイ酸塩溶液を添加して加水
分解させ、該黄色酸化鉄粒子表面にアンチモン及びアル
ミニウムの含水酸化物あるいはアンチモノ、アルミニウ
ム及びケイ素の含水酸化物を沈積被覆せしめた後、オー
トクレーブに仕込み、１５０℃〜３００℃の温度で加圧
加熱処理することを特徴とする耐熱性黄色酸化鉄顔料の
製造方法でもある。The present invention also uses commercially available yellow iron oxide in an alkaline aqueous solution.
An aqueous antimony salt solution and an aqueous aluminum salt solution, or an aqueous antimony salt solution, are added to an alkaline aqueous slurry of yellow iron oxide obtained by applying pressure hydrothermal treatment at a temperature of 50°C or less.
An aqueous aluminum salt solution and a silicate solution are added and hydrolyzed to deposit and coat the surface of the yellow iron oxide particles with hydrated oxides of antimony and aluminum or hydrated oxides of antimono, aluminum and silicon, and then charged into an autoclave. It is also a method for producing a heat-resistant yellow iron oxide pigment, characterized by carrying out pressure and heat treatment at a temperature of 150°C to 300°C.
本発明の方法によって、黄色酸化鉄粒子表面の酸化アン
チモン・アルミナ水系被膜あるいは酸化アンチモン・ア
ルミナ・シリカ・水系被膜の強化及び基体黄色酸化鉄と
これら被膜との結合の強化が行なわれるのである。The method of the present invention strengthens the antimony oxide/alumina aqueous coating or antimony oxide/alumina/silica/aqueous coating on the surface of the yellow iron oxide particles and strengthens the bond between the yellow iron oxide substrate and these coatings.
上記本発明においてアンチモン塩とは、三塩化アンチモ
ン、三フッ化アンチモン、亜アンチモン酸塩等の如きア
ンチモン化合物類、アルミニウム塩とはアルミン酸塩、
塩化アルミニウム、臭化アルミニウム、硫酸アルミニウ
ム、及び硝酸アルミニウム等の如きアルミニウム化合物
類、ケイ酸塩とはケイ酸エステル、ケイ酸のアルカリ金
属塩等の如きケイ素化合物類等をあげることができる。In the present invention, antimony salts refer to antimony compounds such as antimony trichloride, antimony trifluoride, and antimonites, and aluminum salts refer to aluminates,
Aluminum compounds such as aluminum chloride, aluminum bromide, aluminum sulfate, and aluminum nitrate, and silicates include silicon compounds such as silicate esters and alkali metal salts of silicic acid.
被覆処理量としては総量が酸化物として０．５〜１５％
、好ましくは１〜１０％が適当である。被覆処理剤がア
ンチモン及びアルミニウムの含水酸化物の場合のアンチ
モン対アルミニウムの比率、及び被覆処理剤がアンチモ
ン、アルミニウム及びケイ素の含水酸化物の場合のアン
チモン対アルミニウム対ケイ素の比率等に関しては特に
制ましい。処理剤から金属水酸化物を顔料の粒子表面に
沈着させるだめにはその金属水酸化物が沈殿するに十分
なｐＨまで中和することが必要であるが、ｐＨ６〜７が
適当である。又被覆処理時の温度の影響は余りないので
常圧であれば常温又は加熱のいずれでもよく通常は常温
で充分である。The total amount of coating treatment is 0.5 to 15% as oxide.
, preferably 1 to 10%. There are no particular restrictions regarding the ratio of antimony to aluminum when the coating agent is a hydrous oxide of antimony and aluminum, and the ratio of antimony to aluminum to silicon when the coating agent is a hydrous oxide of antimony, aluminum, and silicon. stomach. In order to deposit the metal hydroxide from the treatment agent onto the pigment particle surface, it is necessary to neutralize the treatment agent to a pH sufficient to precipitate the metal hydroxide, and a pH of 6 to 7 is suitable. Furthermore, since the temperature during the coating treatment is not significantly affected, either room temperature or heating may be used as long as it is under normal pressure, and normal temperature is usually sufficient.
被覆処理時のスラリー濃度は約１５０ｇ／ｌ以下特に好
ましくは５０〜１００ｇ／ｌの範囲にあり、加圧加熱処
理時のスラリー濃度は４００ｇ／ｌ以下、好ましくは１
００〜３００ｇ／ｌの範囲にある。又加圧加熱処理時の
温度については１５０〜３００℃の範囲が適当である。The slurry concentration during the coating treatment is about 150 g/l or less, particularly preferably in the range of 50 to 100 g/l, and the slurry concentration during the pressure and heat treatment is about 400 g/l or less, preferably 1
It is in the range of 00 to 300 g/l. Further, the temperature during the pressure and heat treatment is suitably in the range of 150 to 300°C.
即ち１５０℃よりも低い温度では処理効果が表われるま
で非常に長時間を要するので実用的でなく、３００℃を
越えると黄色酸化鉄が分解してα−酸化鉄が生成する。That is, if the temperature is lower than 150°C, it will take a very long time for the treatment effect to appear, which is impractical, and if it exceeds 300°C, the yellow iron oxide will decompose and α-iron oxide will be produced.
処理温度は所定範囲において高い方が処理時間が短かく
てすむ。圧力については処理温度における水あるいは水
溶液の飽和蒸気圧でよくこれ以上に加圧する必要はない
。The higher the processing temperature within a predetermined range, the shorter the processing time. Regarding the pressure, the saturated vapor pressure of water or aqueous solution at the processing temperature is sufficient, and there is no need to increase the pressure higher than this.
本発明を更に充分に示すために以下に実施例を記載する
。Examples are included below to more fully illustrate the invention.
実施例１゜
市販黄色酸化鉄１００ｇを水１０００ｍｌ中に分散した
後、Ａｌ２Ｏ３として５０ｇ／ｌの三塩化アルミニウム
水溶液４０ｍ１を徐々に滴下し１５分間攪拌を続ける。Example 1 After dispersing 100 g of commercially available yellow iron oxide in 1000 ml of water, 40 ml of an aluminum trichloride aqueous solution containing 50 g/l as Al2O3 was gradually added dropwise and stirring was continued for 15 minutes.
次に５ｂ２０３として５０ｇ／ｌの三塩化アンチモン水
溶液４０ｍｌを徐々に滴下し１５分間攪拌を続けた後、
１００ｇ／ｌの水酸化す） ＩＪウム水溶液を用いてｐ
Ｈ＝７まで徐々に中和する。このスラリーをステンレス
製オートクレーブに仕込み２６０℃で４時間加圧加熱処
理を施す。Next, 40 ml of a 50 g/l antimony trichloride aqueous solution was gradually added dropwise as 5b203, and stirring was continued for 15 minutes.
100 g/l of hydroxide) using an IJium aqueous solution
Gradually neutralize until H=7. This slurry was placed in a stainless steel autoclave and subjected to pressure heat treatment at 260° C. for 4 hours.
処理後、水洗、乾燥、粉砕を行なって製品とする。得ら
れた酸化アンチモン−アルミナ被覆黄色酸化鉄をトーレ
シリコーン製シリコーン５Ｈ−８０６Ａレジンを用いて
下記配合割合でレッドデビル社製ペイントコンディショ
ナーにて２０分間振盪して塗料化し厚さ０．１ｍｍのア
ルミ箔にバーコーターを用いて塗付し３０分間セツティ
ングの後、焼付温度を変えて焼付した。各焼付温度にお
ける塗膜の色調を日本電位（株）製測色色差コンピュー
ター（ＮＤ−１０１ＤＣ）で測定し、各焼付温度に於け
る塗膜の色調とハンターの色差式による１５０℃焼伺時
の色に対する色差△Ｅ（ＮＢＳ）を求めた。After treatment, the product is washed, dried, and crushed. The obtained antimony oxide-alumina-coated yellow iron oxide was shaken for 20 minutes in Red Devil's paint conditioner using Toray Silicone's silicone 5H-806A resin at the following mixing ratio to form a paint, which was then coated with 0.1 mm thick aluminum foil. It was coated using a bar coater, and after setting for 30 minutes, it was baked at different baking temperatures. The color tone of the paint film at each baking temperature was measured using a colorimetric color difference computer (ND-101DC) manufactured by Nihon Denki Co., Ltd., and the color tone of the paint film at each baking temperature was compared with that at 150℃ baking using Hunter's color difference formula. The color difference ΔE (NBS) for each color was determined.
塗料配合割合
黄色酸化鉄 層舎 ８ｇシリコーン樹脂
（東し／リコ〜ン製５Ｈ−８０６Ａ） ２４ｇビー
ズ ＧＢ−５０３４０ｇ
マヨネーズ瓶 １５０ｍ１第１表はハ
ンター＝−Ｌ、 ａ、 ｂと△Ｅを示したものであるが
（１）は基体顔料として使用した市販黄色酸化鉄（２）
は実施例１によシ得られた耐熱性黄色酸化鉄である。Paint composition ratio Yellow iron oxide Layer 8g Silicone resin (Toshi/Licon 5H-806A) 24g beads GB-50 340g Mayonnaise bottle 150m1 Table 1 shows Hunter = -L, a, b and △E However, (1) is the commercially available yellow iron oxide (2) used as the base pigment.
is the heat-resistant yellow iron oxide obtained in Example 1.
第１表
１５０℃焼付時の色に対する色差△Ｅが１．５になる温
度をその顔料の耐熱温度と判定すると（１）の市販黄色
酸化鉄の耐熱温度は２００℃（２）の本発明の処理施し
た耐熱性黄色酸化鉄の耐熱温度は２９０℃となり、本発
明の処理を施した耐熱性黄色酸化鉄の耐熱温度は市販黄
色酸化鉄より ９０１：向上した。Table 1 If the temperature at which the color difference ΔE for the color when baked at 150°C is 1.5 is determined as the heat-resistant temperature of the pigment, the heat-resistant temperature of the commercially available yellow iron oxide (1) is 200°C (2) of the present invention. The heat-resistant yellow iron oxide treated had a heat-resistant temperature of 290° C., which was 901 times higher than that of the commercially available yellow iron oxide.
実施例２゜
市販黄色酸化鉄１００ｇを水１５０ ｏｍｘ中に分散し
た後、ＡｌＯとして５０ｇ／、６の三塩化アルミニウム
水３
溶液５０ｍｌ！を徐々に滴下した後更に１５分間攪拌を
続ける。次に５ｂ２０３として５０ｇ／ｌの三塩化アン
チモン水溶液８０ｍ１を徐々に滴下し１５分間攪拌を続
けた後、５ｉ０２として２０ｇ／ｌのケイ酸ナトリウム
水溶液２５ｍ１を添加する。３０分間攪拌を続けた後、
１００ｇ／ｌの水酸化ナトリウム水溶液を用いてｐＨ＝
７まで徐々に中和してアンモチンアルミニウム及びケイ
素の含水酸化物で被覆した黄色酸化鉄を得た。Example 2 After dispersing 100 g of commercially available yellow iron oxide in 150 omx of water, 50 g of AlO/50 ml of 6 aluminum trichloride aqueous solution! After gradually dropping the mixture, stirring was continued for an additional 15 minutes. Next, 80 ml of a 50 g/l aqueous solution of antimony trichloride as 5b203 was gradually added dropwise and stirring was continued for 15 minutes, and then 25 ml of a 20 g/l aqueous sodium silicate solution was added as 5i02. After continuing stirring for 30 minutes,
pH= using 100g/l aqueous sodium hydroxide solution
It was gradually neutralized to 7 to obtain yellow iron oxide coated with hydrous oxides of ammothine aluminum and silicon.
固液分離を行なった後、アンチモンアルミニウム及びケ
イ素の含水酸化物被覆黄色酸化鉄をｐＨ＝１２の水酸化
ナトリウム水溶液中に分散させ、スラリー濃度を３００
ｇ／ｌに調整する。該スラリーをオートクレーブに仕込
み、２７０℃で５時間加圧加熱処理を施す。After solid-liquid separation, yellow iron oxide coated with hydrous oxides of antimony aluminum and silicon was dispersed in an aqueous sodium hydroxide solution with a pH of 12, and the slurry concentration was adjusted to 300.
Adjust to g/l. The slurry was charged into an autoclave and subjected to pressure and heat treatment at 270°C for 5 hours.
処理後、濾過、水洗、乾燥、粉砕を行なって得られた酸
化アンチモン−アルミナ−シリカ被覆耐熱性黄色酸化鉄
の耐熱性を実施例１と同様にして調べた。その結果は第
２表のようであり、ΔＥが１．５に々る耐熱温度は２９
６℃であり、基体顔料として用いた市販黄色酸化鉄より
９６℃向上している。After the treatment, the heat resistance of the antimony oxide-alumina-silica coated heat-resistant yellow iron oxide obtained by filtration, water washing, drying and pulverization was examined in the same manner as in Example 1. The results are shown in Table 2, and the heat-resistant temperature at which ΔE is 1.5 is 29
6°C, which is 96°C higher than the commercially available yellow iron oxide used as the base pigment.
実施例３゜
市販黄色酸化鉄１５０ｇを１６ｇ／ｌの水酸化ナト１ノ
ウム水溶液１０００ｍｌ中にかきまぜつつ投入した後、
ステンレス製オートクレーブ中に仕込み、１９０℃で３
時間加圧加熱処理を施す。処理終了後、オートクレーブ
より内容物をと９だした後、水を加えてスラリー濃度を
６０ｇ／ｌに調整し、Ａｌ２Ｏ３として１００ｇ／ｌの
アルミン酸ナトリウム水溶液３７．５ｍｌ及びＳｂＯと
して５０ｇ／ｌの三塩化アンチモン水溶３
液６０ｍ６を添加する。３０分間攪拌を続けた後、１０
０ｇＡの硫酸を用いてｐＨ＝６４で徐々に中和して、ア
ンチモン及びアルミニウムの含水酸化物で被覆した黄色
酸化鉄を得た。Example 3 After stirring 150 g of commercially available yellow iron oxide into 1000 ml of a 16 g/l sodium hydroxide aqueous solution,
Place in a stainless steel autoclave and heat at 190℃ for 3 hours.
Apply pressure and heat treatment for a period of time. After the treatment was completed, the contents were removed from the autoclave, water was added to adjust the slurry concentration to 60 g/l, and 37.5 ml of a sodium aluminate aqueous solution containing 100 g/l as Al2O3 and 50 g/l as SbO were added. Add 60 m6 of antimony chloride aqueous solution. After continuing stirring for 30 minutes, 10
Gradual neutralization using 0 gA sulfuric acid at pH=64 yielded yellow iron oxide coated with hydrous oxides of antimony and aluminum.
固液分離を行なった後、アンチモン及びアルミニウムの
含水酸化物被覆黄色酸化鉄を水中に分散させ、スラリー
濃度を２００ｇ／ｌに調整する。After solid-liquid separation, yellow iron oxide coated with hydrous oxides of antimony and aluminum is dispersed in water, and the slurry concentration is adjusted to 200 g/l.
該スラリーをオートクレーブに仕込み、２８０℃で４時
間加圧加熱処理を施す。The slurry was charged into an autoclave and subjected to pressure and heat treatment at 280° C. for 4 hours.
処理後、濾過、水洗、乾燥、粉砕を行なって得られた酸
化アンチモン−アルミナ被覆耐熱性黄色酸化鉄の耐熱性
を実施例１と同様にして調べた。その結果は第３表のよ
うであり、△Ｅが１５になる耐熱温度は３０６℃であり
、市販黄色酸化鉄より１０６℃向上している。After the treatment, the heat resistance of the antimony oxide-alumina coated heat-resistant yellow iron oxide obtained by filtration, water washing, drying and pulverization was examined in the same manner as in Example 1. The results are shown in Table 3, and the heat resistance temperature at which ΔE is 15 is 306°C, which is 106°C higher than the commercially available yellow iron oxide.
実施例４゜
市販黄色酸化鉄１５０ｇを１．２ｇ／ｌ！の水酸化ナト
リウム水溶液１０００ｒｎｌＪにかきまぜつつ投入した
後、ステンレス製オートクレーブに仕込み、１７０℃で
２時間加圧加熱処理を施す。処理終了後オートクレーブ
より内容物をとりだし、水を加えてスラリー濃度を６０
ｇ、／ｌに調整する。次いでＡｌ２Ｏ３として１００ｇ
／ｌのアルミン酸ナトリウム水溶液２２．５ｎＪＳｂ２
０３として５０ｇ／ｌの三塩化アンチモン水溶液６０ｍ
ｌ及び５ＩＯ２として２０ｇ／Ａのケイ酸ナトリウム水
溶液７５ｍ１を添加する。３０分間攪拌を続けた後、硫
酸を用いてｐＨ＝６４で徐々に中和して、アンチモン、
アルミニウム及びケイ素の含水酸化物で被覆した黄色酸
化鉄を得た。Example 4゜150g of commercially available yellow iron oxide at 1.2g/l! The mixture was poured into an aqueous sodium hydroxide solution of 1,000 rnlJ with stirring, then placed in a stainless steel autoclave and subjected to pressure and heat treatment at 170°C for 2 hours. After the treatment is completed, take out the contents from the autoclave and add water to make the slurry concentration 60.
g,/l. Then 100g as Al2O3
/l sodium aluminate aqueous solution 22.5nJSb2
60ml of 50g/l antimony trichloride aqueous solution as 03
75 ml of a 20 g/A aqueous sodium silicate solution are added as l and 5IO2. After stirring for 30 minutes, it was gradually neutralized using sulfuric acid to pH=64, and antimony,
A yellow iron oxide coated with hydrous oxides of aluminum and silicon was obtained.
固液分離を行なった後アンチモン、アルミニウム及びケ
イ素の含水酸化物で被覆した黄色酸化鉄を水中に分散さ
せ、スラリー濃度を２ｏｏｇ／Ａに調整する。該スラリ
ーをオートクレーブに仕込み、２９０℃で８時間加圧加
熱処理を施す。After solid-liquid separation, yellow iron oxide coated with hydrous oxides of antimony, aluminum and silicon is dispersed in water, and the slurry concentration is adjusted to 20og/A. The slurry was placed in an autoclave and subjected to pressure and heat treatment at 290°C for 8 hours.
処理後、濾過、水洗、乾燥、粉砕を行なって耐熱性黄色
酸化鉄の耐熱性を実施例１と同様にして調べた。その結
果は第４表のようであり、△Ｅが１５になる耐熱温度は
３１１℃であり、市販黄色酸化鉄より１１１℃向上して
いる。After the treatment, the heat resistance of the heat-resistant yellow iron oxide was examined in the same manner as in Example 1 by filtration, washing with water, drying, and pulverization. The results are shown in Table 4, and the heat resistance temperature at which ΔE is 15 is 311°C, which is 111°C higher than the commercially available yellow iron oxide.
Claims (4)
及びアルミニウム塩水溶液を添加して加水分解させ、該
黄色酸化鉄粒子表面にアンチモン及びアルミニウムの含
水酸化物を被覆せしめた後、１５０℃〜３００℃の温度
で加圧加熱処理することを特徴とする耐熱性黄色酸化鉄
顔料の製造方法。(1) An antimony salt aqueous solution and an aluminum salt aqueous solution are added to an aqueous slurry of yellow iron oxide and hydrolyzed to coat the surface of the yellow iron oxide particles with hydrous oxides of antimony and aluminum, and the temperature is then heated to 150°C to 300°C. 1. A method for producing a heat-resistant yellow iron oxide pigment, which comprises performing pressure and heat treatment at a temperature of .
、アルミニウム塩水溶液及びケイ酸塩水溶液を添加して
加水分解させ、該黄色酸化鉄粒子表面にアンチモン、ア
ルミニウム及びケイ素の含水酸化物を被覆せしめた後、
１５０〜３００℃の温度で加圧加熱処理することを特徴
とする耐熱性黄色酸化鉄顔料の製造方法。(2) An antimony salt aqueous solution, an aluminum salt aqueous solution, and a silicate aqueous solution were added to an aqueous slurry of yellow iron oxide to cause hydrolysis, and the surfaces of the yellow iron oxide particles were coated with hydrous oxides of antimony, aluminum, and silicon. rear,
A method for producing a heat-resistant yellow iron oxide pigment, which comprises performing pressure and heat treatment at a temperature of 150 to 300°C.
の温度で加圧加熱処理を施して得たアルカリ水性スラリ
ーにアンチモン塩水溶液及びアルミニウム塩水溶液を添
加して加水分解させ、該黄色酸化鉄粒子表面にアンチモ
ン及びアルミニウムの含水酸化物を被覆せしめた後、１
５０℃〜３００℃の温度で再度加圧加熱処理することを
特徴とする耐熱性黄色酸化鉄顔料の製造方法。(3) An aqueous antimony salt solution and an aqueous aluminum salt solution are added to an alkaline aqueous slurry obtained by subjecting yellow iron oxide to a pressure and heat treatment in an alkaline aqueous solution at a temperature of 250°C or lower to hydrolyze the yellow iron oxide particles. After coating the surface with hydrous oxides of antimony and aluminum, 1
A method for producing a heat-resistant yellow iron oxide pigment, which comprises performing pressure and heat treatment again at a temperature of 50°C to 300°C.
の温度で加圧加熱処理を施して得た←←童格撫→アルカ
リ水性スラリーにアンチモン塩水溶液、アルミニウム塩
水溶液及びケイ酸塩水溶液を添加して加水分解させて、
該黄色酸化鉄粒子表面にアンチモン、アルミニウム及び
ケイ素の含水酸化物を沈着被覆せしめた後、ｂ ことを特徴とする耐熱性黄色酸化鉄顔料の製造方法。(4) Antimony salt aqueous solution, aluminum salt aqueous solution and silicate aqueous solution are added to the alkaline aqueous slurry obtained by subjecting yellow iron oxide to pressure and heat treatment in an alkaline aqueous solution at a temperature below 250°C. and hydrolyze it,
A method for producing a heat-resistant yellow iron oxide pigment, which comprises depositing and coating the surfaces of the yellow iron oxide particles with hydrous oxides of antimony, aluminum, and silicon, and then b.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14682182A JPS5938259A (en) | 1982-08-26 | 1982-08-26 | Preparation of heat-resistant yellow iron oxide pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14682182A JPS5938259A (en) | 1982-08-26 | 1982-08-26 | Preparation of heat-resistant yellow iron oxide pigment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS5938259A true JPS5938259A (en) | 1984-03-02 |
Family
ID=15416286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14682182A Pending JPS5938259A (en) | 1982-08-26 | 1982-08-26 | Preparation of heat-resistant yellow iron oxide pigment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5938259A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111269588A (en) * | 2020-03-26 | 2020-06-12 | 正太新材料科技有限责任公司 | Heat-resistant iron oxide yellow with high tinting strength and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5334827A (en) * | 1976-09-13 | 1978-03-31 | Nippon Chem Ind Co Ltd:The | Production of stabilized iron oxide pigment |
| JPS5340022A (en) * | 1976-09-27 | 1978-04-12 | Nippon Chem Ind Co Ltd:The | Production of stabilized iron oxide pigment |
| JPS5343729A (en) * | 1976-10-04 | 1978-04-20 | Nippon Chem Ind Co Ltd:The | Stable iron oxide pigments and their preparation |
| JPS55158131A (en) * | 1979-05-30 | 1980-12-09 | Titan Kogyo Kk | Heat-resistant yellow iron oxide pigment and its manufacture |
| JPS55158132A (en) * | 1979-05-30 | 1980-12-09 | Titan Kogyo Kk | Antimony-containing heat-resistant yellow iron oxide pigment and its manufacture |
-
1982
- 1982-08-26 JP JP14682182A patent/JPS5938259A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5334827A (en) * | 1976-09-13 | 1978-03-31 | Nippon Chem Ind Co Ltd:The | Production of stabilized iron oxide pigment |
| JPS5340022A (en) * | 1976-09-27 | 1978-04-12 | Nippon Chem Ind Co Ltd:The | Production of stabilized iron oxide pigment |
| JPS5343729A (en) * | 1976-10-04 | 1978-04-20 | Nippon Chem Ind Co Ltd:The | Stable iron oxide pigments and their preparation |
| JPS55158131A (en) * | 1979-05-30 | 1980-12-09 | Titan Kogyo Kk | Heat-resistant yellow iron oxide pigment and its manufacture |
| JPS55158132A (en) * | 1979-05-30 | 1980-12-09 | Titan Kogyo Kk | Antimony-containing heat-resistant yellow iron oxide pigment and its manufacture |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111269588A (en) * | 2020-03-26 | 2020-06-12 | 正太新材料科技有限责任公司 | Heat-resistant iron oxide yellow with high tinting strength and preparation method and application thereof |
| CN111269588B (en) * | 2020-03-26 | 2021-09-03 | 正太新材料科技有限责任公司 | Heat-resistant iron oxide yellow with high tinting strength and preparation method and application thereof |
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