CN1807262A - Method for preparing ferriferrous oxide black pigment - Google Patents
Method for preparing ferriferrous oxide black pigment Download PDFInfo
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- CN1807262A CN1807262A CN 200610023844 CN200610023844A CN1807262A CN 1807262 A CN1807262 A CN 1807262A CN 200610023844 CN200610023844 CN 200610023844 CN 200610023844 A CN200610023844 A CN 200610023844A CN 1807262 A CN1807262 A CN 1807262A
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Abstract
The invention discloses a preparation method for Fe3O4 as black paint, which comprises preparing the FeSO4 solution, Fe(OH)2 and Fe3O4 by turns. With USA datacolor color photometer, CIE standard and D65 standard light source, the YP/TD/S-01 testing shows the product comes up to the index completely. Compared with prior art, this invention has short production period and small limit to material; the product has wide product color spectrum range to meet wide market application request with low cost.
Description
Technical field
The present invention relates to prepare the method for black iron oxide pigment.
Background technology
The molecular formula of iron oxide black is Fe
3O
4Be widely used in fields such as concrete, coating, rubber and plastic, printing ink, pottery.Comparatively traditional production technique makes with the ironic hydroxide gel high temperature addition reaction for preparing for the waste water reclamation material of the production of employing iron oxide red, iron oxide yellow.But prepared product tinting strength is lower, and form and aspect are difficult to adjust, and obtained product colour poor stability often needs to carry out a large amount of later stage physics colorant match technology, power consumption, consuming time.Along with the continuous anxiety of resource, the raw material of this method is also fewer and feweri simultaneously, and iron oxide red iron oxide yellow manufacturer constantly makes great efforts to reduce unit consumption.A lot of patents are for the angle of comprehensive utilization, and as described in Chinese patent 93119424.5, but the products obtained therefrom kind is single, and bad dispersibility, tinting strength are also undesirable.Chinese patent 200510075112.4 described methods and for example, though be good method, can only production high strength basket iron black mutually.Chromatogram is narrower, can not satisfy the needs of relevant field development.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of method for preparing ferriferrous oxide black pigment, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
(1) preparation of copperas solution: the concentration at ferrous ion is in the ferrous sulfate aqueous solution of 70～100g/L, the reduced iron powder that adds ferrous sulfate weight 1～5% is or/and the reduction iron sheet, 70～95 ℃ react to the solution the ferric iron reduction fully, mend acid in the process, make PH maintain 3～4, after reaction finishes, adding entry adjustment ferrous ion concentration is 70～100g/L, the flocculation agent that adds solution weight 0.001～0.05%, filter, collect filtrate, be the ferrous sulfate salts solution, residue reclaims and focuses on qualified discharge;
The ferrous sulfate of iron and steel, metallurgy industry exists with the solution form, and titanium powder industry exists with the xln form, copperas solution to iron and steel, metallurgy industry, require in its production process the concentration of ferrous ion is controlled at 70～100g/L, ferrous sulfate can be added the water dissolution of 2～3 times of weight to the useless secondary sulphur Asia of titanium white;
Wherein, the acid that is used for adjusting PH is selected from a kind of of sulfuric acid, hydrochloric acid or industrial waste acid;
Said flocculation agent is selected from modified polyacrylamide or polyaluminium sulfate, and its consumption is done suitable adjustment according to the ferrous situation, is the best with clarifying consumption just, must not be excessive, otherwise will influence the quality of product;
(2) preparation of ferrous hydroxide: will add entry in the copperas solution that prepare, make in the copperas solution, ferrous ion concentration is controlled at 20～100g/L, the high more prepared product tinting strength of concentration is high more, with ammonia or weight concentration is that ferrous sulfate salts solution that 5～30% sodium hydroxide solution adds step (1) is neutralized to and adopts the Tripotassium iron hexacyanide to detect in the solution not have ferrous ion, be that whole ferrous ions exists with the ferrous hydroxide gel form, pH value obtains the hydroxide ferrous solution in 6～10 scopes;
(3) preparation of Z 250: the hydroxide ferrous solution that oxygenant is added step (2), oxidizing reaction, temperature of reaction is 40～90 ℃, PH is 6～8, react that no ferrous hydroxide exists to the solution, the black particle of collecting precipitation is thick product, adopt conventional method washing, oven dry then, pulverize, obtain product;
Said oxygenant is selected from air or ammonium nitrate;
The add-on of ammonium nitrate is 0.1～0.15 kg/kg ferrous hydroxide in the weight of ferrous hydroxide in the hydroxide ferrous solution;
The contriver finds, because the raw material that the present invention adopts is derive from gold smelting, steel industry or titanium powder industry ferrous, wherein contains harmful metal ion, as Ti
+ 4, Cu
+ 2And the heavy metal plasma, solid impurity should be removed, and guaranteeing the quality of product, so the preparation of the solution of ferrous sulfate is crucial.
In addition, by control Fe
+ 3Content can the controlled oxidation iron oxide black pigment tone, as the product of wishing to get basket phase coloured light must thoroughly remove, as wishes to get red phase or Huang will suitably be controlled Fe in the iron oxide black mutually
+ 3Content at total more than 2% of iron ratio.
Under the identical situation of other conditions, the inclined to one side basket phase of product that adopts ammonia to obtain than the liquid caustic soda neutralization, tinctorial strength is low; The inclined to one side basket phase of product that ammonium nitrate makes as oxygenant than air as oxygenant, tinctorial strength is on the low side; Under the situation of air as oxygenant, it is higher that the starting temperature of bubbling air is got over the inclined to one side basket phase of high product intensity, on the contrary inclined to one side reddish yellow tone; Ferric content in ferrous is high more, the suitable reddish yellow tone partially of product.
Product of the present invention adopts YP/TD/S-01 to detect, and its result shows, touches the mark fully.
Compare with the production method of traditional black iron oxide pigment, method of the present invention, with short production cycle, less to the restriction of raw material, can adopt to come from the ferrous of gold smelting, steel industry or titanium powder industry, production cost reduces greatly.After the maximum characteristics of present method can be peeled off the secondary ferrous salt solutions of all kinds of expenses that comprise in the Producing Titanium Dioxide and carry out clarifying treatment steel derusting, gold smelting iron sulphide, main by the variation of oxygenant, concentration and the variation of temperature before the ferrous neutralization, the serial iron oxide black product of chromatogram broad be can obtain, high tinting strength, less colored power, basket form and aspect, red phase, yellow phase or the like comprised.
Embodiment
Embodiment 1
(1) preparation of copperas solution: the water dissolution that 12000 kilograms of ferrous sulfate is added 2 times of weight, add 360 kilograms of iron sheets then, 80 ℃ react to the solution the ferric iron reduction fully, mend sulfuric acid in the process, make PH maintain 3.5, after reaction finished, adding entry adjustment ferrous sulfate ionic concn was 100g/L, adds 6 kilograms of flocculant poly Tai-Ace S 150 of solution, filter, collect filtrate, be the ferrous sulfate salts solution, residue reclaims and focuses on qualified discharge;
(2) preparation of ferrous hydroxide: in the ferrous sulfate salts solution of step (1), add entry, make ferrous ion concentration be controlled at 100g/L, adding weight concentration then and be 30% sodium hydroxide solution is neutralized to and adopts the Tripotassium iron hexacyanide to detect no ferrous sulfate ion in the solution, pH value is 8, obtains the hydroxide ferrous solution;
(3) preparation of Z 250: the hydroxide ferrous solution that air is fed step (2), oxidizing reaction, initial reaction temperature is 40 ℃, and persistently overheatingly keeping this temperature until end to 90 ℃, PH is 8, reacts that no ferrous hydroxide exists to the solution, the black particle of collecting precipitation, be thick product, adopt conventional method washing, oven dry then, pulverize, obtain product.
Adopt the YP/TD/S-01 standard to detect, its result is as follows:
| With 8330 than (the high tinting strength product of popular standard specimen on the market) | ΔL | Δa | Δb | ΔE | Tinting strength | Conclusion |
| -0.2 | 0.1 | -0.25 | 0.34 | 102％ | Qualified |
Embodiment 2
(1) preparation of copperas solution: the water dissolution that 12000 kilograms of ferrous sulfate is added 3 times of weight, add 360 kilograms of reduced iron powders then, 90 ℃ react to the solution the ferric iron reduction fully, mend sulfuric acid in the process, make PH maintain 3.5, after reaction finished, adding entry adjustment ferrous sulfate ionic concn was 70g/L, adds 6 kilograms of flocculation agent modified polyacrylamides, filter, collect filtrate, be the ferrous sulfate salts solution, residue reclaims and focuses on qualified discharge;
(2) preparation of ferrous hydroxide: the ferrous sulfate salts solution that ammonia is added step (1) is neutralized to and adopts the Tripotassium iron hexacyanide to detect no ferrous sulfate ion in the solution, and pH value is 6, obtains the hydroxide ferrous solution, in the ferrous ion concentration with before add water management at 70g/L:
(3) preparation of Z 250: the hydroxide ferrous solution that 1500 kilograms of ammonium nitrate is added step (2), oxidizing reaction, temperature of reaction is 85 ℃, PH is 6, react that no ferrous hydroxide exists to the solution, the black particle of collecting precipitation is thick product, adopt conventional method washing, oven dry then, pulverize, obtain product.
Adopt the YP/TD/S-01 standard to detect, its result is as follows:
。
| With S722 than (on the market popular low strong product standard specimen) | ΔL | Δa | Δb | ΔE | Tinting strength | Conclusion |
| -0.3 | 0.15 | -0.23 | 0.4 | 101.5％ | Qualified |
Claims (7)
1. prepare the method for ferriferrous oxide black pigment, it is characterized in that, comprise the steps:
(1) preparation of copperas solution: the concentration at ferrous ion is in the ferrous sulfate aqueous solution of 70～100g/L, add reduced iron powder or/and the reduction iron sheet, 70～95 ℃ react to the solution the ferric iron reduction fully, mend acid in the process, make PH maintain 3～4, after reaction finishes, adding entry adjustment ferrous sulfate ionic concn is 70～100g/L, adds the flocculation agent of solution weight 0.001～0.05%, filters, collect filtrate, be the ferrous sulfate salts solution;
(2) preparation of ferrous hydroxide: the ferrous sulfate salts solution of ammonia or sodium hydroxide solution adding step (1) is neutralized to no ferrous sulfate ion in the employing Tripotassium iron hexacyanide detection solution, and pH value obtains the hydroxide ferrous solution in 6～10 scopes;
(3) preparation of Z 250: the hydroxide ferrous solution that oxygenant is added step (2), oxidizing reaction, temperature of reaction is 40～90 ℃, PH is 6～8, react that no ferrous hydroxide exists to the solution, the black particle of collecting precipitation adopts conventional method washing, oven dry then, pulverizes, and obtains product.
2. method according to claim 1 is characterized in that, the acid that is used for adjusting PH is selected from a kind of of sulfuric acid hydrochloric acid or industrial waste acid.
3. method according to claim 1 is characterized in that said flocculation agent is selected from modified polyacrylamide or polyaluminium sulfate.
4. method according to claim 1 is characterized in that, is the ferrous sulfate salts solution that 5～30% sodium hydroxide solution adds step (1) with weight concentration.
5. method according to claim 1 is characterized in that said oxygenant is selected from air or ammonium nitrate.
6. method according to claim 5 is characterized in that, the add-on of ammonium nitrate is 0.1～0.15 kg/kg ferrous hydroxide in the weight of ferrous hydroxide in the hydroxide ferrous solution.
7. method according to claim 1 is characterized in that, in step (2), adds entry in the copperas solution for preparing, and makes in the copperas solution, and ferrous ion concentration is controlled at 20～100g/L.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891257A (en) * | 2010-07-30 | 2010-11-24 | 四川长虹电器股份有限公司 | Method for producing ferroferric oxide with chemical activity |
| CN102139927A (en) * | 2011-01-17 | 2011-08-03 | 升华集团德清华源颜料有限公司 | High-purity iron oxide black pigment and production method thereof |
| CN101314678B (en) * | 2008-06-20 | 2011-08-03 | 升华集团德清华源颜料有限公司 | Fire resistant black iron oxide pigment and preparation method thereof |
| CN101445674B (en) * | 2008-12-08 | 2011-12-07 | 温州大学 | Magnetic pearlescent pigment and preparation method thereof |
| CN102515284A (en) * | 2011-12-23 | 2012-06-27 | 东华大学 | Preparation method for Fe3O4/graphene composite powder |
| CN103589196A (en) * | 2013-11-15 | 2014-02-19 | 浙江凯色丽科技发展有限公司 | Preparation method of 3D color changing pearlescent pigment |
| CN103626239A (en) * | 2013-10-11 | 2014-03-12 | 昆明理工大学 | Method for removing manganese out of titanium dioxide byproduct ferrous sulfate |
| CN104261486A (en) * | 2014-09-19 | 2015-01-07 | 上海一品颜料有限公司 | Method for controlling content of iron of black iron oxide |
| CN106673071A (en) * | 2016-12-23 | 2017-05-17 | 天津理工大学 | Method for removing iron from laterite nickel ore pickling liquid and producing iron oxide black pigment at the same time |
| CN107200362A (en) * | 2017-06-26 | 2017-09-26 | 杭州明兴化工有限公司 | A kind of method that pure oxygen oxidizing process produces iron oxide black |
| CN107986337A (en) * | 2017-11-03 | 2018-05-04 | 浙江华源颜料股份有限公司 | A kind of easily scattered high coloring power iron oxide black and preparation method thereof |
| CN108003658A (en) * | 2017-11-03 | 2018-05-08 | 浙江华源颜料股份有限公司 | A kind of easily scattered high coloring power iron oxide black |
| CN110683587A (en) * | 2019-10-21 | 2020-01-14 | 中国科学院山西煤炭化学研究所 | Method for preparing mesoporous nano ferroferric oxide particles from titanium dioxide byproduct ferrous sulfate |
| CN112499690A (en) * | 2020-12-17 | 2021-03-16 | 梅征 | Preparation method of crystal seed for treating brushing water |
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2006
- 2006-02-13 CN CN 200610023844 patent/CN1807262A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314678B (en) * | 2008-06-20 | 2011-08-03 | 升华集团德清华源颜料有限公司 | Fire resistant black iron oxide pigment and preparation method thereof |
| CN101445674B (en) * | 2008-12-08 | 2011-12-07 | 温州大学 | Magnetic pearlescent pigment and preparation method thereof |
| CN101891257A (en) * | 2010-07-30 | 2010-11-24 | 四川长虹电器股份有限公司 | Method for producing ferroferric oxide with chemical activity |
| CN102139927B (en) * | 2011-01-17 | 2012-07-11 | 升华集团德清华源颜料有限公司 | High-purity iron oxide black pigment and production method thereof |
| CN102139927A (en) * | 2011-01-17 | 2011-08-03 | 升华集团德清华源颜料有限公司 | High-purity iron oxide black pigment and production method thereof |
| CN102515284B (en) * | 2011-12-23 | 2014-04-02 | 东华大学 | Preparation method for Fe3O4/graphene composite powder |
| CN102515284A (en) * | 2011-12-23 | 2012-06-27 | 东华大学 | Preparation method for Fe3O4/graphene composite powder |
| CN103626239A (en) * | 2013-10-11 | 2014-03-12 | 昆明理工大学 | Method for removing manganese out of titanium dioxide byproduct ferrous sulfate |
| CN103589196A (en) * | 2013-11-15 | 2014-02-19 | 浙江凯色丽科技发展有限公司 | Preparation method of 3D color changing pearlescent pigment |
| CN103589196B (en) * | 2013-11-15 | 2016-01-20 | 浙江凯色丽科技发展有限公司 | A kind of preparation method of 3D variable color pearly pigment |
| CN104261486A (en) * | 2014-09-19 | 2015-01-07 | 上海一品颜料有限公司 | Method for controlling content of iron of black iron oxide |
| CN106673071B (en) * | 2016-12-23 | 2019-01-11 | 天津理工大学 | A kind of method that lateritic nickel ore pickle liquor produces black iron oxide pigment simultaneously except iron |
| CN106673071A (en) * | 2016-12-23 | 2017-05-17 | 天津理工大学 | Method for removing iron from laterite nickel ore pickling liquid and producing iron oxide black pigment at the same time |
| CN107200362A (en) * | 2017-06-26 | 2017-09-26 | 杭州明兴化工有限公司 | A kind of method that pure oxygen oxidizing process produces iron oxide black |
| CN107986337A (en) * | 2017-11-03 | 2018-05-04 | 浙江华源颜料股份有限公司 | A kind of easily scattered high coloring power iron oxide black and preparation method thereof |
| CN108003658A (en) * | 2017-11-03 | 2018-05-08 | 浙江华源颜料股份有限公司 | A kind of easily scattered high coloring power iron oxide black |
| CN107986337B (en) * | 2017-11-03 | 2020-05-05 | 浙江华源颜料股份有限公司 | Easily-dispersible high-tinting-strength iron oxide black and preparation method thereof |
| CN110683587A (en) * | 2019-10-21 | 2020-01-14 | 中国科学院山西煤炭化学研究所 | Method for preparing mesoporous nano ferroferric oxide particles from titanium dioxide byproduct ferrous sulfate |
| CN112499690A (en) * | 2020-12-17 | 2021-03-16 | 梅征 | Preparation method of crystal seed for treating brushing water |
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