CN107200362A - A kind of method that pure oxygen oxidizing process produces iron oxide black - Google Patents
A kind of method that pure oxygen oxidizing process produces iron oxide black Download PDFInfo
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- CN107200362A CN107200362A CN201710492766.XA CN201710492766A CN107200362A CN 107200362 A CN107200362 A CN 107200362A CN 201710492766 A CN201710492766 A CN 201710492766A CN 107200362 A CN107200362 A CN 107200362A
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- pure oxygen
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- iron oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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Abstract
The invention discloses a kind of method that pure oxygen oxidizing process produces iron oxide black, comprise the following steps:S1:Ferrous salt solution is added in reaction vessel, aqueous slkali is added afterwards and adjusts pH to 89,80 90 DEG C are warming up to, pure oxygen reaction is passed through, the reaction time is 60 120min;S2:The mixed solution in container is circulated with circulating pump, circulating pump extracts mixed solution from the bottom of container out, and is poured at the top of container in jet pump, and mixed solution is spurted into container again after being mixed with pure oxygen in jet pump;Control pH between 79 in course of reaction, control temperature is at 80 95 DEG C, until being reacted to required color, recording reacting time is incubated 30 60min, discharging;S3:Through rinsing, press filtration, drying, crush, be packaged into finished product.With the effective discharge for improving gas, the effect of oxidation efficiency is improved.
Description
Technical field
The present invention relates to iron oxide black production technical field, more particularly to a kind of pure oxygen oxidizing process produces the side of iron oxide black
Method.
Background technology
Iron oxide pigment is a kind of quite varied inorganic pigment of purposes, and the main component of wherein iron oxide black is four oxidations
Three-iron, its tone is attractive in appearance durable, and covering power and tinting strength, tinting power are very high, while having good alkali resistance, light fastness, extensively
Apply in fields such as building materials, coating, ink, rubber, plastics, glassware, drawing.
The most frequently used production method of existing iron oxide black is that ferrous iron solution adds alkali oxidizing process, i.e., added in ferrous iron solution
Aqueous slkali, then be passed through air or oxygen and reacted, existing air is passed directly into oxidation barrel, is roused in the form of air bubble
Enter in reaction mixture, the contact surface of air and mixed solution is only limitted to the outer rim of bubble, be wrapped in oxygen in bubble without
Method participates in oxidation reaction, causes the effective discharge of gas low, influences oxidation efficiency.
The content of the invention
It is an object of the invention to provide a kind of method that pure oxygen oxidizing process produces iron oxide black, existing oxidation is which solved
The problem of mixed effect of air and reaction mixture is bad in iron black production method, with the effective discharge for improving gas,
Improve the effect of oxidation efficiency.
The present invention above-mentioned technical purpose technical scheme is that:
A kind of method that pure oxygen oxidizing process produces iron oxide black, it is characterized in that, comprise the following steps:S1:Add in reaction vessel
Enter copperas solution, aqueous slkali is added afterwards and adjusts pH to 8-9,80-90 DEG C is warming up to, pure oxygen reaction, reaction time is passed through
For 60-120min;S2:The mixed solution in container is circulated with circulating pump, circulating pump is by mixed solution from the bottom of container
Portion is extracted out, and is poured at the top of container in jet pump, and mixed solution is sprayed again after being mixed with pure oxygen in jet pump
Inject in container;Control pH between 7-9 in course of reaction, control temperature is at 80-95 DEG C, until being reacted to required color, remember
The reaction time is recorded, 30-60min, discharging is incubated;S3:Through rinsing, press filtration, drying, crush, be packaged into finished product.
More preferably:Step S2 includes first stage and second stage, and the first stage is:Opened from step S1 temperature
Beginning is gradually heating to 90-95 DEG C, is incubated 20-40h, during control pH for 8-9;Second stage is, from the temperature of first stage
Gradually be cooled to 85-90 DEG C, until be reacted to required color, during control pH for 7-9;React and lead to from step S1 total time
Enter pure oxygen and start into step S2 recording reacting time to terminate, required reaction total time is 40-52h.
More preferably:Temperature fall time in second stage is 40-60min.
More preferably:Heating-up time in first stage is 15-30min.
More preferably:The flow of jet pump is controlled in 400-800m3/h。
More preferably:In step S2, the Stress control of system is in 1-1.2 atmospheric pressure.
More preferably:Aqueous slkali includes one kind in sodium hydroxide solution, potassium hydroxide solution and ammoniacal liquor.
More preferably:Aqueous slkali is 1.2-1.5mol/L sodium hydroxide solution.
More preferably:Ferrous salt solution includes one kind in copperas solution, solution of ferrous chloride.
In summary, the invention has the advantages that:1st, replace air with pure oxygen, use jet pump during the course of the reaction
Two measures of circulation are carried out after pure oxygen and mixed solution are mixed and advantageously reduce reaction total time, energy consumption is reduced;2nd, exist
In the case that the basic holding reaction time is constant, reaction is divided into three phases, initial reaction stage and the temperature in later stage can be reduced,
So as to reduce energy consumption;3rd, in the case where other conditions are constant, with the extension of the soaking time of first stage in step S2, instead
The trend for first reducing and increasing afterwards should be presented total time, when soaking time is 35h, with minimum reaction total time, contributes to
Oxidation efficiency is improved, energy consumption is reduced;4th, the temperature of step S1, first stage and second stage is different, has total time to reaction
Obvious influence, when the temperature of three stages of reaction increases, reaction total time is reduced;5th, with second stage temperature fall time
Increase, tinting strength, tinting power be in obvious ascendant trend, temperature fall time during 50-60min, tinting strength, tinting power improve degree declined,
It is preferred that 50min.
Embodiment
The present invention is described in further detail below.
This specific embodiment is only explanation of the invention, and it is not limitation of the present invention, people in the art
Member can make the modification without creative contribution to the present embodiment as needed after this specification is read, but as long as at this
All protected in the protection domain of invention by Patent Law.
Embodiment 1:A kind of method that pure oxygen oxidizing process produces iron oxide black, comprises the following steps:
S1:In 50m3Copperas solution is added in reactor, sodium hydroxide solution is added afterwards and adjusts pH to 8-9, is warming up to
90 DEG C, it is passed through pure oxygen reaction;
S2:The mixed solution in reactor is circulated with circulating pump, circulating pump takes out mixed solution from the bottom of reactor
Go out, and poured at the top of reactor in jet pump, mixed solution is sprayed again after being mixed with pure oxygen in jet pump
Enter in reactor;Control pH between 7-9 in course of reaction, control temperature is at 90 DEG C, until being reacted to required color, record is anti-
Between seasonable, 30-60min, discharging are incubated;Reaction total time is 48.0h;
S3:Through rinsing, press filtration, drying, crush, be packaged into finished product;
Wherein, the flow of jet pump is 600m3/h;System pressure is controlled in 1.2 atmospheric pressure;The concentration of sodium hydroxide solution is
1.2mol/L。
Embodiment 2:A kind of method that pure oxygen oxidizing process produces iron oxide black, comprises the following steps:
S1:In 50m3Copperas solution is added in reactor, sodium hydroxide solution is added afterwards and adjusts pH to 8-9, is warming up to
90 DEG C, pure oxygen reaction is passed through, the reaction time is 120min;
S2:The mixed solution in reactor is circulated with circulating pump, circulating pump takes out mixed solution from the bottom of reactor
Go out, and poured at the top of reactor in jet pump, mixed solution is sprayed again after being mixed with pure oxygen in jet pump
Enter in reactor;95 DEG C are warming up to, the heating-up time is 20min;PH is controlled in course of reaction between 7-9, until being reacted to institute
Color is needed, recording reacting time is incubated 30-60min, discharging;Reaction total time is 43.3h;
S3:Through rinsing, press filtration, drying, crush, be packaged into finished product;
Wherein, the flow of jet pump is 600m3/h;System pressure is controlled in 1.2 atmospheric pressure;The concentration of sodium hydroxide solution is
1.2mol/L。
Embodiment 3:A kind of method that pure oxygen oxidizing process produces iron oxide black, comprises the following steps:
S1:In 50m3Copperas solution is added in reactor, sodium hydroxide solution is added afterwards and adjusts pH to 8-9, is warming up to
85 DEG C, pure oxygen reaction is passed through, the reaction time is 120min;
S2:The mixed solution in reactor is circulated with circulating pump, circulating pump takes out mixed solution from the bottom of reactor
Go out, and poured at the top of reactor in jet pump, mixed solution is sprayed again after being mixed with pure oxygen in jet pump
Enter in reactor;Course of reaction includes first stage and second stage, and the first stage is:Gradually risen since step S1 temperature
Temperature is to 95 DEG C, and the heating-up time is 20min, is incubated 20h, during control pH for 8-9;Second stage is:From the temperature of first stage
Degree is gradually cooled to 90 DEG C, and temperature fall time is 50min, continues to react to required color after cooling, during control pH for 7-9;
Reaction total time be passed through pure oxygen since step S1 into step S2 recording reacting time terminate, it is required reaction total time be
49.7h。
Control pH between 7-9 in course of reaction, control temperature is at 90 DEG C, until required color is reacted to, record reaction
Time, it is incubated 30-60min, discharging;Reaction total time is 48.0h;
S3:Through rinsing, press filtration, drying, crush, be packaged into finished product;
Wherein, the flow of jet pump is 600m3/h;System pressure is controlled in 1.2 atmospheric pressure;The concentration of sodium hydroxide solution is
1.2mol/L。
Embodiment 4-21:A kind of method that pure oxygen oxidizing process produces iron oxide black, is with the difference of embodiment 3,
Step S1 soaking times, step S1 temperature, heating-up time first stage, first stage temperature, first stage soaking time,
Two-stage temperature fall time, second stage temperature are different with reaction total time, and specific reaction condition is referring to table 1.
The reaction condition that table 1 implements 1-21 collects
Embodiment 22:A kind of method that pure oxygen oxidizing process produces iron oxide black, the difference with embodiment 6 is jet pump
Flow is 200m3/h。
Embodiment 23:A kind of method that pure oxygen oxidizing process produces iron oxide black, the difference with embodiment 6 is jet pump
Flow is 400m3/h。
Embodiment 24:A kind of method that pure oxygen oxidizing process produces iron oxide black, the difference with embodiment 6 is jet pump
Flow is 800m3/h。
Embodiment 25:A kind of method that pure oxygen oxidizing process produces iron oxide black, the difference with embodiment 6 is jet pump
Flow is 900m3/h。
In order to probe into every reaction condition of the present invention and the relation of reaction result, following comparative example is prepared as control.
Comparative example 1:A kind of method that pure oxygen oxidizing process produces iron oxide black, comprises the following steps:
S1:In 50m3Copperas solution is added in reactor, sodium hydroxide solution is added afterwards and adjusts pH to 8-9, is warming up to
90 DEG C, it is passed through pure oxygen reaction;
S2:Pure oxygen directly from the bottom of reactor be passed through reactor in reacted;PH is controlled in course of reaction between 7-9,
Temperature is controlled at 90 DEG C, until being reacted to required color, recording reacting time is incubated 30-60min, discharging;Reaction total time be
58.0h;
S3:Through rinsing, press filtration, drying, crush, be packaged into finished product;
Wherein, the flow that pure oxygen is passed through reactor is 600m3/h;System pressure is controlled in 1.2 atmospheric pressure;Sodium hydroxide solution
Concentration be 1.2mol/L.
Comparative example 2:A kind of method that pure oxygen oxidizing process produces iron oxide black, comprises the following steps:
S1:In 50m3Copperas solution is added in reactor, sodium hydroxide solution is added afterwards and adjusts pH to 8-9, is warming up to
90 DEG C, it is passed through air reaction;
S2:The mixed solution in reactor is circulated with circulating pump, circulating pump takes out mixed solution from the bottom of reactor
Go out, and poured at the top of reactor in jet pump, mixed solution is sprayed again after being mixed with air in jet pump
Enter in reactor;Control pH between 7-9 in course of reaction, control temperature is at 90 DEG C, until being reacted to required color, record is anti-
Between seasonable, 30-60min, discharging are incubated;Reaction total time is 64.0h;
S3:Through rinsing, press filtration, drying, crush, be packaged into finished product;
Wherein, the flow that air is passed through reactor is 600m3/h;System pressure is controlled in 1.2 atmospheric pressure;Sodium hydroxide solution
Concentration be 1.2mol/L.
Comparative example 3:A kind of method that pure oxygen oxidizing process produces iron oxide black, comprises the following steps:
S1:In 50m3Copperas solution is added in reactor, sodium hydroxide solution is added afterwards and adjusts pH to 8-9, is warming up to
90 DEG C, it is passed through pure oxygen reaction;
S2:The mixed solution in reactor is circulated with circulating pump, circulating pump takes out mixed solution from the bottom of reactor
Go out, and poured at the top of reactor in jet pump, mixed solution is sprayed again after being mixed with pure oxygen in jet pump
Enter in reactor;PH is controlled in course of reaction between 6.5-7 (not including 7), control temperature is at 90 DEG C, until reaction 60h, is protected
Warm 30-60min, discharging;
S3:Through rinsing, press filtration, drying, crush, be packaged into finished product;
Wherein, the flow of jet pump is 600m3/h;System pressure is controlled in 1.2 atmospheric pressure;The concentration of sodium hydroxide solution is
1.2mol/L。
Use the iron oxide black yield that the method for comparative example 3 is prepared for 2/3 or so of embodiment 1, show to react
PH in journey is less than 7 generations for being unfavorable for product.
Interpretation of result:
Comparative example 1-2, comparative example 1-2 result are understood, are replaced air with pure oxygen, reaction total time can be reduced, anti-
Circulation is carried out after being mixed pure oxygen and mixed solution with jet pump during answering and advantageously reduces reaction total time.
Comparative example 3-8 result is understood, in the case where other conditions are constant, with the first stage in step S2
The trend for first reducing and increasing afterwards is presented in the extension of soaking time, reaction total time, when soaking time is 35h, with minimum
Total time is reacted, oxidation efficiency is favorably improved, energy is saved.
Comparative example 6, embodiment 9-17 result understand, the heating-up time of first stage and second stage in reaction
Influence of the temperature fall time to reacting total time is little.
Comparative example 6, embodiment 18-21 result understand that step S1, first stage and second stage temperature are not
Together, there is obvious influence on reaction total time, when the temperature of three stages of reaction increases, reaction total time is reduced.
The result of comparative example 2 and embodiment 6 is understood, in the case where keeping the reaction time constant substantially, can be dropped
Low reaction initial stage and the temperature in later stage, so as to reduce energy consumption.
Tinting strength, tinting power is tested
Tinting strength, tinting power test is done to embodiment 1-21 respectively, test result is referring to table 2
Embodiment | Tinting strength, tinting power/% | Embodiment | Tinting strength, tinting power/% | Embodiment | Tinting strength, tinting power/% |
Embodiment 1 | 99.2 | Embodiment 8 | 98.7 | Embodiment 15 | 99.6 |
Embodiment 2 | 99.0 | Embodiment 9 | 98.2 | Embodiment 16 | 99.8 |
Embodiment 3 | 98.5 | Embodiment 10 | 99.0 | Embodiment 17 | 97.7 |
Embodiment 4 | 98.9 | Embodiment 11 | 98.6 | Embodiment 18 | 98.7 |
Embodiment 5 | 99.0 | Embodiment 12 | 96.1 | Embodiment 19 | 99.3 |
Embodiment 6 | 99.7 | Embodiment 13 | 98.6 | Embodiment 20 | 99.5 |
Embodiment 7 | 99.3 | Embodiment 14 | 99.2 | Embodiment 21 | 99.4 |
The embodiment 1-21 of table 2 tinting strength, tinting power test result.
Comparative example 3-8 results showed that is presented slightly with the increase of first stage soaking time, tinting strength, tinting power
First increases and then decreases trend, but change amplitude it is little;Comparative example 6,9-11 result are understood, with the first stage
The trend of first increases and then decreases is presented in the increase of heating-up time, tinting strength, tinting power, and amplitude of variation is also little;Comparative example 6, embodiment
12-16 result is understood, with the increase of second stage temperature fall time, and tinting strength, tinting power is in obvious ascendant trend, and temperature fall time exists
During 50-60min, tinting strength, tinting power improves unobvious;The result of comparative example 6 and embodiment 17 is understood, when being reacted in step S1
Between 120min when, obtained iron oxide black tinting strength, tinting power is more preferable;Knowable to comparative example 18-21 experimental result, step S1, first
Stage is different with the temperature of second stage, iron oxide black tinting strength, tinting power tool is had a certain impact, when the temperature of three stages of reaction
When increasing, tinting strength, tinting power increases, and increasing degree is gradually reduced.
Claims (9)
1. a kind of method that pure oxygen oxidizing process produces iron oxide black, it is characterized in that, comprise the following steps: S1:In reaction vessel
Ferrous salt solution is added, aqueous slkali is added afterwards and adjusts pH to 8-9,80-90 DEG C is warming up to, pure oxygen reaction, reaction time is passed through
For 60-120min; S2:The mixed solution in container is circulated with circulating pump, circulating pump is by mixed solution from the bottom of container
Portion is extracted out, and is poured at the top of container in jet pump, and mixed solution is sprayed again after being mixed with pure oxygen in jet pump
Inject in container;Control pH between 7-9 in course of reaction, control temperature is at 80-95 DEG C, until being reacted to required color, remember
The reaction time is recorded, 30-60min, discharging is incubated; S3:Through rinsing, press filtration, drying, crush, be packaged into finished product.
2. the method that a kind of pure oxygen oxidizing process according to claim 1 produces iron oxide black, it is characterized in that:The step S2
Including first stage and second stage, the first stage is:Started to warm up from step S1 temperature to 90-95 DEG C, be incubated 20-40h,
During control pH be 8-9;Second stage is that the greenhouse cooling from the first stage is to 85-90 DEG C, until being reacted to required face
Color, during control pH be 7-9;Reaction total time be passed through pure oxygen since step S1 into step S2 recording reacting time knot
Beam, required reaction total time is 40-52h.
3. the method that a kind of pure oxygen oxidizing process according to claim 2 produces iron oxide black, it is characterized in that:The second-order
Temperature fall time in section is 40-60min.
4. the method that a kind of pure oxygen oxidizing process according to claim 3 produces iron oxide black, it is characterized in that:First rank
Heating-up time in section is 15-30min.
5. the method that a kind of pure oxygen oxidizing process according to claim 1 produces iron oxide black, it is characterized in that:The jet pump
Flow control in 400-800m3/h。
6. the method that a kind of pure oxygen oxidizing process according to claim 1 produces iron oxide black, it is characterized in that:The step S2
In, the Stress control of system is in 1-1.2 atmospheric pressure.
7. the method that a kind of pure oxygen oxidizing process according to claim 1 produces iron oxide black, it is characterized in that:The aqueous slkali
Including one kind in sodium hydroxide solution, potassium hydroxide solution and ammoniacal liquor.
8. the method that a kind of pure oxygen oxidizing process according to claim 1 produces iron oxide black, it is characterized in that:The aqueous slkali
For 1.2-1.5mol/L sodium hydroxide solution.
9. the method that a kind of pure oxygen oxidizing process according to claim 1 produces iron oxide black, it is characterized in that:The ferrous salt
Solution includes one kind in copperas solution, solution of ferrous chloride.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111573740A (en) * | 2020-07-02 | 2020-08-25 | 正太新材料科技有限责任公司 | Preparation method of iron oxide black |
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CN86107137A (en) * | 1986-10-24 | 1987-11-04 | 蒋则伟 | Iron oxide pigment and preparation method thereof |
CN2158872Y (en) * | 1993-06-24 | 1994-03-16 | 上海冶金设计研究院 | Gas-liquid quick-reacting apparatus for production of polyiron |
CN1611449A (en) * | 2003-10-30 | 2005-05-04 | 中国科学院兰州化学物理研究所 | Method for preparing Fe3 O4 superfine powder |
CN1807262A (en) * | 2006-02-13 | 2006-07-26 | 上海一品颜料有限公司 | Method for preparing ferriferrous oxide black pigment |
CN1861527A (en) * | 2006-04-29 | 2006-11-15 | 北矿磁材科技股份有限公司 | Preparation process of Fe3O4 magnetic powder |
CN104402061A (en) * | 2014-11-21 | 2015-03-11 | 周淑华 | Production process for preparing iron oxide black by ferrous sulfate solution |
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CN86107137A (en) * | 1986-10-24 | 1987-11-04 | 蒋则伟 | Iron oxide pigment and preparation method thereof |
CN2158872Y (en) * | 1993-06-24 | 1994-03-16 | 上海冶金设计研究院 | Gas-liquid quick-reacting apparatus for production of polyiron |
CN1611449A (en) * | 2003-10-30 | 2005-05-04 | 中国科学院兰州化学物理研究所 | Method for preparing Fe3 O4 superfine powder |
CN1807262A (en) * | 2006-02-13 | 2006-07-26 | 上海一品颜料有限公司 | Method for preparing ferriferrous oxide black pigment |
CN1861527A (en) * | 2006-04-29 | 2006-11-15 | 北矿磁材科技股份有限公司 | Preparation process of Fe3O4 magnetic powder |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN111573740A (en) * | 2020-07-02 | 2020-08-25 | 正太新材料科技有限责任公司 | Preparation method of iron oxide black |
CN111573740B (en) * | 2020-07-02 | 2022-08-23 | 正太新材料科技有限责任公司 | Preparation method of iron oxide black |
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