CN101559986A - Method for producing iron oxide black - Google Patents
Method for producing iron oxide black Download PDFInfo
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- CN101559986A CN101559986A CNA2009100512545A CN200910051254A CN101559986A CN 101559986 A CN101559986 A CN 101559986A CN A2009100512545 A CNA2009100512545 A CN A2009100512545A CN 200910051254 A CN200910051254 A CN 200910051254A CN 101559986 A CN101559986 A CN 101559986A
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- feed liquid
- iron oxide
- oxide black
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- ferrous sulfate
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Abstract
The invention discloses a method for producing iron oxide black, comprising the steps of (1) adjusting pH value of ferrous sulphate liquid to be alkaline by an alkaline matter, infusing air and water vapour, performing reaction to generate short grained iron oxide black; and (2) continuously adding the ferrous sulphate and the alkaline matter, adjusting the pH value of the liquid to be alkaline, infusing air and water vapour, performing reaction, repeating the process, and collecting pure black iron oxide black with high purity from the reaction products. The method of the invention can greatly improve the yield of iron oxide black liquid and reduce production cost. The granular size of the iron oxide black can be controlled according to the times of the repeated operations so as to generate iron oxide black particles with different granular sizes and satisfy the requirements of users for different purposes. The invention is simply operated, has a high yield, can save production cost, and is convenient for industrialisation.
Description
Technical field
The present invention relates to the production method of black iron oxide pigment.
Background technology
Black iron oxide pigment is very important in a iron oxide pigment serial color, in fields such as chemical industry, building, daily-use chemical industries, has very and uses widely.
At present, the production of black iron oxide pigment is that raw material is prepared with titanium white ferrous sulfate as side product (solid) generally, and preparation process comprises the steps:
Dissolving titanium white ferrous sulfate as side product, ferrous sulfate and alkali substance reaction generate ferrous hydroxide, and ferrous hydroxide and oxidant reaction generate the hydroxide high ferro, are hydrolyzed into Z 250.
Aforesaid method, not only the main content of Z 250 is not high, and the recovery rate of Z 250 is not high, has increased production cost, and the blackness of its color is impure, presents grey black.
Summary of the invention
The production process that the purpose of this invention is to provide a kind of iron oxide black is to overcome the above-mentioned defective that prior art exists.
The production method of iron oxide black of the present invention comprises the steps:
(1) the ferrous sulfate feed liquid is regulated the pH value to alkalescence with alkaline matter, bubbling air and water vapor reacted 10～6 hours, preferred 8～5 hours, generated short grained iron oxide black;
(2) continue to add ferrous sulfate and alkaline matter, the pH value of regulating feed liquid is to alkalescence, bubbling air and water vapor, reacted 8～4 hours, and preferred 5～3 hours, made initiate ferrous sulfate continue to generate the iron oxide black particle, be deposited on the ferriferrous oxide particles that has formed, particle is grown up, repeat said process, collection has the highly purified iron oxide black of ater from reaction product then;
Described alkaline matter is selected from sodium hydroxide or ammonium hydroxide;
The said said process that repeatedly repeats is 3～8 times;
Said ferrous sulfate can pass through purification and impurity removal, and the content of iron oxide black that makes generation is up to 97%.
The pH value of said feed liquid is preferably 7～12;
Said air size is so that feed liquid is slightly seethed to good;
The consumption of said water vapor, so that feed temperature remains on 85～105 ℃, preferred 90～100 ℃.
Said ferrous sulfate feed liquid, its ferrous sulfate content is 30～70g/100ml.
Method of the present invention can improve yield of iron oxide black liquid, greatly to reduce production costs; And can be according to what of repetitive operation number of times, the granular size of control iron oxide black to generate the iron oxide black particle of variable grain size, satisfies different purposes clients' demand;
Method of the present invention, simple to operate, the recovery rate height, and can save production cost, be convenient to industrializing implementation.
Embodiment
Embodiment 1
3600 kilograms of sulfuric acid are added in the water of 2000 kilograms of iron sheets and 16000 kilograms, the preparation copperas solution, with the copperas solution purification and impurity removal, 6000 kilograms copperas solution is delivered in the reactor, added 1870 kilogram weights of concentration and be 30% sodium hydroxide solution, regulate the pH value to 8 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed temperature at more than 90 ℃ 8 hours;
The repetitive operation said process, deliver to 4400 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 1450 kilogram weights of concentration 30%, regulate the pH value to 8 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 90 ℃ 5 hours; Repetitive operation said process once more, deliver to 3300 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 900 kilogram weights of concentration 30%, regulate the pH value to 8 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 90 ℃ 3 hours; In the reaction process, the ferrous sulfate amount of adding can gradually reduce, and then, with the feed liquid press filtration that reaction obtains, collects filter cake, washes with water, and 95 ℃ of oven dry can obtain ater iron oxide black pigment;
Detected result is as follows: in the iron oxide black pigment, and Z 250 weight content 97.2%, water solubles weight content 0.3%, form and aspect L=55.05, A=-1.27, B=-6.01, common iron black L=49.76, A=-1.20, B=-5.79, wherein the L value is represented shading value; The red blue phase of A value representative; The yellowish green phase of B value representative; The L value of product Z 250 of the present invention is 110.63% of common iron oxide black.
| Add number of times | Iron-holder % | L | A | B |
| Once add | 95.4 | 51.34 | -1.23 | -5.85 |
| Secondary is added | 96.5 | 53.45 | -1.25 | -5.93 |
| Add for three times | 97.2 | 55.05 | -1.27 | -6.01 |
Embodiment 2
3600 kilograms of sulfuric acid are added in the water of 2000 kilograms of iron sheets and 16000 kilograms, the preparation copperas solution, with the copperas solution purification and impurity removal, 7100 kilograms copperas solution is delivered in the reactor, add 2050 kilogram weights of concentration and be 30% sodium hydroxide solution, regulate the pH value to 9 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed temperature at more than 95 ℃ 5 hours; The repetitive operation said process, deliver to 4400 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 1200 kilogram weights of concentration 30%, regulate the pH value to 9 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 95 ℃ 4 hours; Repetitive operation said process once more, deliver to 4400 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 1200 kilogram weights of concentration 30%, regulate the pH value to 9 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 95 ℃ 3 hours; The repetitive operation said process, deliver to 3300 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 900 kilogram weights of concentration 30%, regulate the pH value to 9 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 95 ℃ 3 hours; Repetitive operation said process once more, deliver to 2200 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 620 kilogram weights of concentration 30%, regulate the pH value to 9 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 95 ℃ 3 hours; In the reaction process, the ferrous sulfate amount of adding can gradually reduce, and then, with the feed liquid press filtration that reaction obtains, collects filter cake, washes with water, and 90 ℃ of oven dry can obtain ater iron oxide black pigment;
Detected result is as follows: in the iron oxide black pigment, and Z 250 weight content 98.3%, water solubles weight content 0.2%, form and aspect L=58.71, A=-1.33, B=-6.16, common iron black L=49.76, A=-1.20, B=-5.79, wherein the L value is represented shading value; The red blue phase of A value representative; The yellowish green phase of B value representative; The L value of product Z 250 of the present invention is 117.99% of common iron oxide black.
| Add number of times | Iron-holder % | L | A | B |
| Once add | 95.3 | 51.21 | -1.22 | -5.82 |
| Secondary is added | 96.2 | 53.05 | -1.24 | -5.88 |
| Add for three times | 97.1 | 54.83 | -1.27 | -5.96 |
| Add for four times | 97.8 | 56.58 | -1.30 | -6.11 |
| Add for five times | 98.3 | 58.71 | -1.33 | -6.16 |
Embodiment 3
3600 kilograms of sulfuric acid are added in the water of 2000 kilograms of iron sheets and 16000 kilograms, the preparation copperas solution, with the copperas solution purification and impurity removal, 7000 kilograms copperas solution is delivered in the reactor, added 1950 kilogram weights of concentration and be 30% sodium hydroxide solution, regulate the pH value to 10 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed temperature at more than 100 ℃ 4 hours; The repetitive operation said process, deliver to 4400 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 1300 kilogram weights of concentration 30%, regulate the pH value to 10 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 100 ℃ 3 hours; Repetitive operation said process once more, deliver to 2200 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 600 kilogram weights of concentration 30%, regulate the pH value to 10 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 100 ℃ 2 hours; The repetitive operation said process, deliver to 2200 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 600 kilogram weights of concentration 30%, regulate the pH value to 10 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 100 ℃ 2 hours; Repetitive operation said process once more, deliver to 2200 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 600 kilogram weights of concentration 30%, regulate the pH value to 10 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 100 ℃ 2 hours; Repetitive operation said process once more, deliver to 2200 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 600 kilogram weights of concentration 30%, regulate the pH value to 10 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 100 ℃ 2 hours; The repetitive operation said process, deliver to 2200 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 600 kilogram weights of concentration 30%, regulate the pH value to 10 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 100 ℃ 2 hours; Repetitive operation said process once more, deliver to 1700 kilograms copperas solutions in the reactor once more, the sodium hydroxide solution that adds 520 kilogram weights of concentration 30%, regulate the pH value to 10 of feed liquid, to the feed liquid bubbling air, feed liquid is slightly seethed, feed liquid is fed steam, keep feed liquid more than 100 ℃ 2 hours; In the reaction process, the ferrous sulfate amount of adding can gradually reduce, and then, with the feed liquid press filtration that reaction obtains, collects filter cake, washes with water, and 98 ℃ of oven dry can obtain ater iron oxide black pigment;
Detected result is as follows: in the iron oxide black pigment, and Z 250 weight content 98.5%, water solubles weight content 0.2%, form and aspect L=64.29, A=-1.42, B=-6.30, common iron black L=49.76, A=-1.20, B=-5.79, wherein the L value is represented shading value; The red blue phase of A value representative; The yellowish green phase of B value representative; The L value of product Z 250 of the present invention is 129.20% of common iron oxide black.
| Add number of times | Iron-holder % | L | A | B |
| Once add | 95.3 | 51.21 | -1.22 | -5.82 |
| Secondary is added | 96.2 | 53.05 | -1.24 | -5.88 |
| Add for three times | 96.7 | 54.13 | -1.26 | -5.95 |
| Add for four times | 97.2 | 56.08 | -1.29 | -6.10 |
| Add for five times | 97.6 | 58.21 | -1.32 | -6.15 |
| Add for six times | 98.1 | 60.38 | -1.36 | -6.21 |
| Add for seven times | 98.3 | 62.07 | -1.39 | -6.26 |
| Add for eight times | 98.5 | 64.29 | -1.42 | -6.30 |
Claims (8)
1. the production method of iron oxide black is characterized in that, comprises the steps:
(1) the ferrous sulfate feed liquid is regulated the pH value to alkalescence with alkaline matter, bubbling air and water vapor, reaction generates short grained iron oxide black;
(2) continue to add ferrous sulfate and alkaline matter, the pH value of regulating feed liquid is extremely alkaline, bubbling air and water vapor, and reaction repeats said process, collects then to have the highly purified iron oxide black of ater from reaction product.
2. method according to claim 1 is characterized in that described alkaline matter is selected from sodium hydroxide or ammonium hydroxide.
3. method according to claim 1 is characterized in that, the said number of times that repeatedly repeats said process is 3～8 times.
4. method according to claim 1 is characterized in that, the pH value of said feed liquid is 7～12.
5. method according to claim 1 is characterized in that, said air consumption is so that feed liquid is seethed.
6. method according to claim 1 is characterized in that, the consumption of said water vapor is so that feed temperature remains on 85～105 ℃.
7. method according to claim 1, it is characterized in that, (1) the ferrous sulfate feed liquid is regulated the pH value to alkalescence with alkaline matter, bubbling air and water vapor, reacted 10～6 hours, (2) continue to add ferrous sulfate and alkaline matter, and the pH value of regulating feed liquid is to alkalescence, bubbling air and water vapor reacted 8～4 hours.
8. according to each described method of claim 1～7, it is characterized in that, said ferrous sulfate feed liquid, its ferrous sulfate content is 30～70g/100ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009100512545A CN101559986A (en) | 2009-05-14 | 2009-05-14 | Method for producing iron oxide black |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2009100512545A CN101559986A (en) | 2009-05-14 | 2009-05-14 | Method for producing iron oxide black |
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| CN101559986A true CN101559986A (en) | 2009-10-21 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824236A (en) * | 2010-04-29 | 2010-09-08 | 南通宝聚颜料有限公司 | Preparation process of medium temperature resistant iron oxide black |
| CN101746836B (en) * | 2009-12-25 | 2012-05-23 | 浙江工业大学 | Method for preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater |
| CN103370428A (en) * | 2010-12-15 | 2013-10-23 | 浦项产业科学研究院 | Method for enrichment-recovering ferronickel from raw material containing nickel, method for recovering nickel from enriched ferronickel, and method for recycling solution containing iron produced from same |
| CN104071850A (en) * | 2013-03-25 | 2014-10-01 | 北京三聚环保新材料股份有限公司 | Preparation method for iron oxide black |
| 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 |
| CN105712408A (en) * | 2014-12-03 | 2016-06-29 | 镇江金盛源信息科技有限公司 | Iron oxide black preparation reactor |
-
2009
- 2009-05-14 CN CNA2009100512545A patent/CN101559986A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101746836B (en) * | 2009-12-25 | 2012-05-23 | 浙江工业大学 | Method for preparing iron oxide black pigment by carrying out resourceful treatment on pyrite wastewater |
| CN101824236A (en) * | 2010-04-29 | 2010-09-08 | 南通宝聚颜料有限公司 | Preparation process of medium temperature resistant iron oxide black |
| CN101824236B (en) * | 2010-04-29 | 2012-10-31 | 南通宝聚颜料有限公司 | Preparation process of medium temperature resistant iron oxide black |
| CN103370428A (en) * | 2010-12-15 | 2013-10-23 | 浦项产业科学研究院 | Method for enrichment-recovering ferronickel from raw material containing nickel, method for recovering nickel from enriched ferronickel, and method for recycling solution containing iron produced from same |
| CN104071850A (en) * | 2013-03-25 | 2014-10-01 | 北京三聚环保新材料股份有限公司 | Preparation method for iron oxide black |
| CN104071850B (en) * | 2013-03-25 | 2016-03-30 | 北京三聚环保新材料股份有限公司 | A kind of preparation method of iron oxide black |
| 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 |
| CN105712408A (en) * | 2014-12-03 | 2016-06-29 | 镇江金盛源信息科技有限公司 | Iron oxide black preparation reactor |
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Open date: 20091021 |