CN102320667A - Color-modulation and color-stabilization control method of orange-red-toned iron-oxide pigment - Google Patents
Color-modulation and color-stabilization control method of orange-red-toned iron-oxide pigment Download PDFInfo
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- CN102320667A CN102320667A CN201110233338A CN201110233338A CN102320667A CN 102320667 A CN102320667 A CN 102320667A CN 201110233338 A CN201110233338 A CN 201110233338A CN 201110233338 A CN201110233338 A CN 201110233338A CN 102320667 A CN102320667 A CN 102320667A
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- color
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- crystal seed
- oxide pigment
- sulfate
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Abstract
The invention discloses a color-modulation and color-stabilization control method of an orange-red-toned iron-oxide pigment, which is characterized by comprising the following steps of: step 1: when crystal seeds are prepared by a method of wet-method sulfate oxidation, controlling oxidation reaction at the temperature of 35 to 55 DEG C according to the requirements of tones, and adding a phosphate as a crystal-seed structure-adjusting aid to prepare the crystal seeds; and step 2: when iron sulfate is oxidized in the existence of the crystal seeds, continuously dropwise adding the iron sulfate and ammonia water, and simultaneously adjusting the iron-sulfate concentration of a reaction system to be 30 to 70g/L and the pH value of the reaction system to be 2.5 to 5.5. The color-modulation and color-stabilization control method has the advantages that: on a traditional basis, the temperature conditions of crystal-seed preparation are changed in emphasis, the phosphate is added as a crystal-seed crystal-type structure regulator to obtain a series of orange-red-toned iron-oxide pigments from light colors to deep colors, the uniformity of a paint color paste can be kept, and the iron-oxide pigment is stable and is not layered or deposited within storage time.
Description
Technical field
The present invention relates to a kind of toning of orange red tone iron oxide pigment, steady color control method, is to realize on the basis that the wet method oxide sulfate prepares iron red crystal seed formation.
Background technology
That mars pigment mainly contains is red, yellow, black three big chromatic serieses, has nontoxic, fast light, weather-proof, strong covering power, tinctorial property is good, can be widely used in fields such as building materials, plastics, papermaking, coating and pottery.
The currently available products close: though the report of present type of having chalybeate orange serial pigment with the present invention; But this pigment is to utilize iron oxide red, two kinds of pigment of iron oxide yellow to mix to piece together and pulverize through machinery to form; Because iron oxide red, two kinds of pigment of iron oxide yellow are prepared from different process respectively; Thereby crystalline structure of its pigment particles, globule size, specific surface area, dispersiveness etc. there are differences, thereby finally influence the service performance of this type of pigment.For example in preparation dispersible pigment color paste process, occur phenomenons such as layering, loose colour, bad dispersibility sometimes, steady look property is poor.In addition, because the defective of the manufacture craft of this series products itself makes its color series dull relatively.
Summary of the invention
The purpose of this invention is to provide a kind of toning of orange red tone iron oxide pigment, steady color control method; Specifically be a kind ofly will realize both having overcome present type chalybeate orange serial pigment (machinery mixes and pieces together gained) and phenomenons such as layering, loose colour, bad dispersibility generally in mill base and application of paints, occur, can also access the toning of the orange red tone iron oxide pigment of serial colour system, steady color control method.
In order to solve above technical problem; The control method of the toning of a kind of orange red tone iron oxide pigment of the present invention, steady look; The formation of its orange red tone iron oxide pigment is mainly adopts wet method oxide sulfate method to obtain crystal seed, in the presence of crystal seed, continues the iron oxide pigment that the oxidation ferrous sulfate gets orange red tone; It is characterized in that: the toning of orange red tone iron oxide pigment, steady color control method are controlled in forming process, in two steps; The first step: when the method for wet method oxide sulfate makes crystal seed, according to tone require controlled temperature 35-55 ℃ of following oxidizing reactions, and add phosphoric acid salt and make crystal seed structural adjustment auxiliary agent, the preparation crystal seed; Second step: under crystal seed, during the oxidation ferrous sulfate, drip ferrous sulfate and ammoniacal liquor continuously, the while is according to the requirement of tone, adjusts reaction system ferrous sulfate concentration 30-70g/L, reacting system PH value is 2.5-5.5.
The adjustment relation in above-mentioned two steps is: improve with the crystal seed temperature, the red color tone of pigment can progressively reduce, and yellow hue and brightness value can progressively raise; When reaction system ferrous sulfate concentration increased in above-mentioned interval, the red color tone of pigment can slightly reduce, and yellow hue can slightly raise; And when reacting system PH value increased in above-mentioned interval, the red color tone of pigment had small size reduction equally, and yellow hue can small size rising phenomenon.
Its process step is following:
One, crystal seed preparation
Configuration 40 ~ 80 g/L copperas solutions, the sodium phosphate that adds 0.2 ~ 0.6% weight ratio (serves as to calculate benchmark with 100% ferrous sulfate amount) are simultaneously made crystal seed structural adjustment auxiliary agent; Use then in about 8 ~ 10% concentration ammoniacal liquor with above-mentioned solution to PH=9.0 ~ 10.0, the bubbling air oxidation makes this pigment crystal seed under 35 ~ 55 ℃ of temperature.
Reaction equation is following:
FeSO
4+2NaOH=Fe(OH)
2↓+Na
2SO
4
2Fe(OH)
2+1/2O
2=2γ-FeOOH+H
2O
Crystal seed transforms: 2 γ-FeOOH → α-Fe
2O
3. xH
2O (crystal seed)+H
2O.
Two, second oxidation
Above-mentioned crystal seed is added water latting drown to 1 ~ 1.5 times; Adding ferrous sulfate solution to ferrous content is 30 ~ 70g/L, and bubbling air carried out oxidation after intensification reached 80 ~ 85 ℃, and the red oxide of iron of generation is deposited on the nucleus; The sulfuric acid that generates simultaneously is with 8% left and right sides weak ammonia neutralization; Hierarchy of control PH=3.0 ~ 5.0 drip ferrous sulfate and weak ammonia continuously, and nucleus is grown up gradually and formed orange red iron oxide pigment.The second oxidation reaction formula is following:
2FeSO
4+1/2O
2+2H
2O=Fe
2O
3↓+2H
2SO
4
H
2SO
4+2NH
3?.H
2O?=(NH
4)
2SO
4?+2H
2O。
In the second oxidation stage, when reacting when the ferrous sulfate total amount consumed is 6 times of the ferrous amount of crystal seed, stopped reaction immediately, prepared orange red tone iron oxide pigment, through filter, washing, dry, pulverize and get product.
Advantage of the present invention: the present invention relates to a kind of tone control method of orange red tone iron oxide pigment, is to prepare on the basis of iron red crystal seed formation at the traditional wet oxide sulfate, and emphasis changes crystal seed preparation temperature condition; Add a kind of phosphoric acid salt simultaneously as crystal seed crystalline structure regulator, can play toning and steady look effect, passing through series reaction; Provide a kind of orange red tone iron oxide pigment kind to replace common red stone orange, finally can obtain the iron oxide pigment of a series of orange red tones from light color to the dark color, be used in pigment printing paste after; The homogeneity that can keep mill base; Stable, not stratified in the storage time, do not precipitate.When increasing new color, can also accomplish stable performance for the iron oxide pigment chromatogram.
Embodiment
Embodiment 1:
Measuring concentration is 2 liters of the ferrous iron solutions (rolling over the 100% ferrous 120g of being) of 60g/L; Be positioned over volume and be in 8 liters the stainless steel beaker; Add 0.36 gram sodium phosphate auxiliary agent simultaneously, with in the 8% concentration ammoniacal liquor with above-mentioned ferrous iron solution to PH=9.0 ~ 10.0, intensification reaches 40 ℃; The bubbling air oxidation prepares the crystal seed of reddish yellow phase, and oxidising process approximately needs 1 hour.
After above-mentioned crystal seed added water latting drown to 3 liter; Adding ferrous sulfate solution to ferrous content is 30 ~ 40g/L, and bubbling air carried out oxidation after intensification reached 80 ~ 85 ℃, dripped ferrous sulfate and weak ammonia continuously; Guarantee that the reaction system ferrous iron concentration is at 30 ~ 40g/L; Control pH value simultaneously between 3 ~ 4, when reacting when the ferrous sulfate total amount consumed is 6 times of the ferrous amount of crystal seed (roll over 100% ferrous be 720g) stopped reaction; With prepared orange red tone iron oxide pigment, get product through filtration, washing, drying, pulverizing.The pairing color data measured value of this pigment is following:
L=46.73, a=20.58, b=25.11; This shows that this pigment has good color tone and form and aspect.
The comparative example
Sequence number 1 is embodiment 1, and the preparation method of sequence number 2-7 is with embodiment 1, and the result lists in table simultaneously, and these pigment have good color tone and form and aspect equally.
Claims (1)
1. the control method of the toning of an orange red tone iron oxide pigment, steady look; The formation of its orange red tone iron oxide pigment is mainly adopts wet method oxide sulfate method to obtain crystal seed, in the presence of crystal seed, continues the iron oxide pigment that the oxidation ferrous sulfate gets orange red tone; It is characterized in that: the toning of orange red tone iron oxide pigment, steady color control method are mainly controlled in forming process, in two steps; The first step: when the method for wet method oxide sulfate made crystal seed, according to the requirement of tone, controlled temperature was 35-55 ℃ of following oxidizing reactions, and adding phosphoric acid salt is made crystal seed structural adjustment auxiliary agent, the preparation crystal seed; Second step: under crystal seed, during the oxidation ferrous sulfate, drip ferrous sulfate and ammoniacal liquor continuously, the while is according to the requirement of tone, adjusts reaction system ferrous sulfate concentration 30-70g/L, reacting system PH value is 2.5-5.5.
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|---|---|---|---|
| CN201110233338A CN102320667A (en) | 2011-08-16 | 2011-08-16 | Color-modulation and color-stabilization control method of orange-red-toned iron-oxide pigment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110233338A CN102320667A (en) | 2011-08-16 | 2011-08-16 | Color-modulation and color-stabilization control method of orange-red-toned iron-oxide pigment |
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|---|---|
| CN102320667A true CN102320667A (en) | 2012-01-18 |
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|---|---|---|---|
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4942597A (en) * | 1972-08-30 | 1974-04-22 | ||
| JPH0942597A (en) * | 1995-07-28 | 1997-02-14 | Sanyo Electric Co Ltd | Natural gas charging device |
| CN1162477C (en) * | 2001-11-15 | 2004-08-18 | 上海氧化铁颜料厂 | Prepn of medicinal iron oxide pigment |
| CN1613917A (en) * | 2003-09-03 | 2005-05-11 | 拜尔化学公司 | Process for preparing yellow iron oxide pigments with CaCO3 precipitant |
| CN1699477A (en) * | 2005-05-27 | 2005-11-23 | 华南理工大学 | Process for preparing iron oxide red by using sulfuric acid crystal seed mixed acid method and products thereby |
| CN101423257A (en) * | 2008-11-07 | 2009-05-06 | 浙江正奇化工有限公司 | Method for preparing nano grade iron oxide red |
-
2011
- 2011-08-16 CN CN201110233338A patent/CN102320667A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4942597A (en) * | 1972-08-30 | 1974-04-22 | ||
| JPH0942597A (en) * | 1995-07-28 | 1997-02-14 | Sanyo Electric Co Ltd | Natural gas charging device |
| CN1162477C (en) * | 2001-11-15 | 2004-08-18 | 上海氧化铁颜料厂 | Prepn of medicinal iron oxide pigment |
| CN1613917A (en) * | 2003-09-03 | 2005-05-11 | 拜尔化学公司 | Process for preparing yellow iron oxide pigments with CaCO3 precipitant |
| CN1699477A (en) * | 2005-05-27 | 2005-11-23 | 华南理工大学 | Process for preparing iron oxide red by using sulfuric acid crystal seed mixed acid method and products thereby |
| CN101423257A (en) * | 2008-11-07 | 2009-05-06 | 浙江正奇化工有限公司 | Method for preparing nano grade iron oxide red |
Non-Patent Citations (1)
| Title |
|---|
| 朱骥良、吴申年: "《颜料工艺学》", 30 June 1993, article "硫酸盐湿法铁红", pages: 184-194 * |
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Application publication date: 20120118 |
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