CN102502861A - Process for synthesizing iron oxide brown - Google Patents
Process for synthesizing iron oxide brown Download PDFInfo
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- CN102502861A CN102502861A CN2011103052216A CN201110305221A CN102502861A CN 102502861 A CN102502861 A CN 102502861A CN 2011103052216 A CN2011103052216 A CN 2011103052216A CN 201110305221 A CN201110305221 A CN 201110305221A CN 102502861 A CN102502861 A CN 102502861A
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- iron oxide
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- reaction kettle
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Abstract
The invention discloses a process for synthesizing iron oxide brown, comprising the following steps of: feeding a ferrous sulfate solution into a reaction kettle; slowly adding caustic soda liquid in three times; then heating to a temperature in the reaction kettle of 75-78 DEG C and incubating for 50-70 min; adding water to dilute mixed slurry until solid content of the mixed slurry is 8-10%; slowly adding sodium nitrite into the reaction kettle and introducing oxygen simultaneously; then turning on spraying equipment to sufficiently mix the slurry, oxygen gas and NO which is generated in a reaction process; continuously sampling and comparing a sample with a standard sample in the reaction process; stopping the reaction when the colored light of a product is similar to the yellowish-brown or reddish brown colored light of standard sample; and carrying out plate pressure filtration, washing, drying and crashing the taken-out slurry so as to obtain the product. The iron oxide brown produced by the invention includes brownish red iron oxide brown and brownish yellow iron oxide brown. Compared with the traditional method for preparing the iron oxide brown by physically mixing iron oxide red, iron oxide black and iron oxide yellow, the iron oxide brown produced by the invention is stable in quality and pure in colored light, the synthesis method is simple and the operation is convenient.
Description
Technical field
The present invention relates to the working method of a kind of cologne earth, exactly is the synthesis technique of a kind of cologne earth.
Background technology
The molecular formula of cologne earth is (Fe
2O
3+ FeO) nH
2O, it is a kind of brown ceramic powder, and water insoluble, pure, ether are dissolved in hot strong acid, and simultaneously tinting strength and opacifying power are very high, and photostabilization, alkali resistance are good, anhydrous oozing property and oozing property of oil.Its form and aspect are divided into yellowish-brown, reddish brown, black palm fibre etc. with the difference of technology.Painted and the coating of goods such as it is widely used in painting, printing ink, plastics, shoe powder, building, rubber, plastics etc. painted.
Traditional cologne earth is to form through piecing together to mix with iron oxide black, iron oxide yellow and three kinds of pigment physics of iron oxide red, and quality product is unstable, has the uneven deficiency of form and aspect, so directly synthesize the cologne earth product is superior to physical mixed on performance product
Summary of the invention
The objective of the invention is for a kind of color is provided is yellowish-brown and reddish-brown, has good tinting strength, form and aspect and stability, prepares the synthesis technique of easy cologne earth simultaneously.
Technical scheme of the present invention is following:
The synthesis technique of a kind of cologne earth is characterized in that: may further comprise the steps:
(1), in reaction kettle, adds copperas solution, again according to mass ratio NaOH: FeSO
4Slowly add liquid caustic soda at=3: 1～0.8, and liquid caustic soda divides three addings, each 28-32 minute at interval; Again reactor temperature is warmed up to 75-78 ℃; Temperature-rise period needs controlled temperature to be undertaken by per hour heating up 5 ℃, reaches to temperature to stop more than 75 ℃ heating up, and is incubated after 50-70 minute; Thin up mixed slurry to solid content is 8-10%;
(2), the ratio in product input 45-50KG per ton slowly adds Sodium Nitrite in reaction kettle; Sodium Nitrite divides three addings; Each 30-32 minute at interval; The while aerating oxygen, the feeding pressure of oxygen is the 10-13cm water column, opens the NO thorough mixing of sprinkling equipment with the generation in slip, oxygen and the reaction process again;
(3), in the reaction process, constantly the sample circuit standard model relatively, the approximate back of the standard model coloured light of product coloured light and yellowish-brown or reddish-brown coloured light stopped reaction promptly gets product with the slip of taking-up after filter press, washing, oven dry, fragmentation.
The preparation method of described iron oxide brown is characterized in that: described copperas solution is to contain assorted copperas solution to use that method for hydrolysis is removed titanium impurity, water adjusting concentration gets after as 33-37% again; Described liquid caustic soda concentration is 30-45%.
Principle equation of the present invention:
FeSO
4+2NaOH＝Fe(OH)
2↓+Na
2SO
4；
NaNO
2+Fe(OH)
2+H
2O＝Fe(OH)
3+NaOH+NO；
2NO+O
2＝2NO
2；
3NO
2+H
2O＝2HNO
3+NO；
HNO
3+3Fe(OH)
2+H
2O＝3Fe(OH)
3+NO；
2Fe(OH)
3＝Fe
2O
3+3H
2O。
Beneficial effect of the present invention is:
The cologne earth that the present invention produces is reddish brown and pale brown two kinds, compares with the cologne earth that iron oxide red, iron oxide black, the assembly of iron oxide yellow physics blend together with tradition, and the cologne earth steady quality of the inventive method production, coloured light is pure and compound method is simple, easy to operate.
Embodiment
The synthesis technique of a kind of cologne earth is characterized in that: may further comprise the steps:
(1), in reaction kettle, adds copperas solution, again according to mass ratio NaOH: FeSO
4Slowly add liquid caustic soda at=3: 1～0.8, and liquid caustic soda divides three addings, each 28-32 minute at interval; Again reactor temperature is warmed up to 75-78 ℃; Temperature-rise period needs controlled temperature to be undertaken by per hour heating up 5 ℃, reaches to temperature to stop more than 75 ℃ heating up, and is incubated after 50-70 minute; Thin up mixed slurry to solid content is 8-10%;
(2), the ratio in product input 45-50KG per ton slowly adds Sodium Nitrite in reaction kettle; Sodium Nitrite divides three addings; Each 30-32 minute at interval; The while aerating oxygen, the feeding pressure of oxygen is the 10-13em water column, opens the NO thorough mixing of sprinkling equipment with the generation in slip, oxygen and the reaction process again;
(3), in the reaction process, constantly the sample circuit standard model relatively, the approximate back of the standard model coloured light of product coloured light and yellowish-brown or reddish-brown coloured light stopped reaction promptly gets product with the slip of taking-up after filter press, washing, oven dry, fragmentation.
The preparation method of described iron oxide brown is characterized in that: described copperas solution is to contain assorted copperas solution to use that method for hydrolysis is removed titanium impurity, water adjusting concentration gets after as 33-37% again; Described liquid caustic soda concentration is 30-45%.
The detected result table of product of the present invention
The cologne earth that the present invention produces is reddish brown and pale brown two kinds, compares with the cologne earth that iron oxide red, iron oxide black, the assembly of iron oxide yellow physics blend together with tradition, and the cologne earth steady quality of the inventive method production, coloured light is pure and compound method is simple, easy to operate.
Claims (2)
1. the synthesis technique of a cologne earth is characterized in that: may further comprise the steps:
(1), in reaction kettle, adds copperas solution, again according to mass ratio NaOH:FeSO
4=3:1～0.8 slowly adds liquid caustic soda, and liquid caustic soda divides three addings, each 28-32 minute at interval; Again reactor temperature is warmed up to 75-78 ℃; Temperature-rise period needs controlled temperature to be undertaken by per hour heating up 5 ℃, reaches to temperature to stop more than 75 ℃ heating up, and is incubated after 50-70 minute; Thin up mixed slurry to solid content is 8-10%;
(2), the ratio in product input 45-50KG per ton slowly adds Sodium Nitrite in reaction kettle; Sodium Nitrite divides three addings; Each 30-32 minute at interval; The while aerating oxygen, the feeding pressure of oxygen is the 10-13cm water column, opens the NO thorough mixing of sprinkling equipment with the generation in slip, oxygen and the reaction process again;
(3), in the reaction process, constantly the sample circuit standard model relatively, the approximate back of the standard model coloured light of product coloured light and yellowish-brown or reddish-brown coloured light stopped reaction promptly gets product with the slip of taking-up after filter press, washing, oven dry, fragmentation.
2. the preparation method of iron oxide brown according to claim 1 is characterized in that: described copperas solution is to contain assorted copperas solution to use that method for hydrolysis is removed titanium impurity, water adjusting concentration gets after as 33-37% again; Described liquid caustic soda concentration is 30-45%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110305221.6A CN102502861B (en) | 2011-10-11 | 2011-10-11 | Process for synthesizing iron oxide brown |
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|---|---|---|---|
| CN201110305221.6A CN102502861B (en) | 2011-10-11 | 2011-10-11 | Process for synthesizing iron oxide brown |
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|---|---|
| CN102502861A true CN102502861A (en) | 2012-06-20 |
| CN102502861B CN102502861B (en) | 2014-01-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318967A (en) * | 2013-06-25 | 2013-09-25 | 升华集团德清华源颜料有限公司 | Method for preparing liquid-phase low-heavy-metal iron oxide brown |
| CN103318971A (en) * | 2013-06-25 | 2013-09-25 | 升华集团德清华源颜料有限公司 | Liquid-phase low-heavy-metal iron oxide brown |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109027A (en) * | 1994-11-30 | 1995-09-27 | 华南理工大学 | Production of iron polysulfate |
| CN101381109A (en) * | 2008-10-24 | 2009-03-11 | 天津大学 | Method for preparing spherical Fe3O4 nano powder |
| CN101786670A (en) * | 2010-01-20 | 2010-07-28 | 安徽明珠颜料科技有限公司 | Method for synthesizing iron oxide black through liquid phase oxidation with oxygen |
-
2011
- 2011-10-11 CN CN201110305221.6A patent/CN102502861B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1109027A (en) * | 1994-11-30 | 1995-09-27 | 华南理工大学 | Production of iron polysulfate |
| CN101381109A (en) * | 2008-10-24 | 2009-03-11 | 天津大学 | Method for preparing spherical Fe3O4 nano powder |
| CN101786670A (en) * | 2010-01-20 | 2010-07-28 | 安徽明珠颜料科技有限公司 | Method for synthesizing iron oxide black through liquid phase oxidation with oxygen |
Non-Patent Citations (4)
| Title |
|---|
| 《山西化工》 19931231 李省云等 "氧化铁黄生产的最佳条件" 33-36 1-2 , 第1期 * |
| 《河南化工》 19921231 任知忠等 "氨水中和-NO催化法制取铁黄" 24-26 1-2 , 第7期 * |
| 任知忠等: ""氨水中和-NO催化法制取铁黄"", 《河南化工》, no. 7, 31 December 1992 (1992-12-31), pages 24 - 26 * |
| 李省云等: ""氧化铁黄生产的最佳条件"", 《山西化工》, no. 1, 31 December 1993 (1993-12-31), pages 33 - 36 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318967A (en) * | 2013-06-25 | 2013-09-25 | 升华集团德清华源颜料有限公司 | Method for preparing liquid-phase low-heavy-metal iron oxide brown |
| CN103318971A (en) * | 2013-06-25 | 2013-09-25 | 升华集团德清华源颜料有限公司 | Liquid-phase low-heavy-metal iron oxide brown |
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|---|---|
| CN102502861B (en) | 2014-01-29 |
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