CN108793263A - A kind of method and ferric oxide red colorant preparing iron oxide red using iron content waste - Google Patents

A kind of method and ferric oxide red colorant preparing iron oxide red using iron content waste Download PDF

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Publication number
CN108793263A
CN108793263A CN201810770162.1A CN201810770162A CN108793263A CN 108793263 A CN108793263 A CN 108793263A CN 201810770162 A CN201810770162 A CN 201810770162A CN 108793263 A CN108793263 A CN 108793263A
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iron
oxide red
hydroxide
iron oxide
waste
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薛贤
张晗
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Changzhou Runde Graphite Technology Co Ltd
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Changzhou Runde Graphite Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide [Fe2O3]

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Iron (AREA)

Abstract

The present invention relates to technical field of chemical industry, provide a kind of method preparing iron oxide red using iron content waste, include the following steps:3~5h of freeze-day with constant temperature obtains dry powder under the conditions of ferro element in iron-contained waste material being converted to after the mixture of iron hydroxide, ferrous hydroxide or both existing for 120~180 DEG C of oxygen;Dry powder is placed in 400~800 DEG C of 40~180min under confined conditions and obtains γ-Fe2O3.Iron content waste reclamation can have been saved resource by this method, avoid environmental pollution, and the high income of iron oxide red, have higher economic benefit.The present invention also provides a kind of ferric oxide red colorants, through above-mentioned γ-Fe2O3Standardization obtains, which has preferable economic benefit.

Description

A kind of method and ferric oxide red colorant preparing iron oxide red using iron content waste
Technical field
The present invention relates to technical field of chemical industry, and iron oxide red is prepared using iron content waste in particular to a kind of Method and ferric oxide red colorant.
Background technology
Currently, the enterprises such as steel pole and automobile specified thin plate, steel rolling were producing in acid cleaning of steel tube cold-drawn, seamless steel pipe, shop Pickling flush water and sludge solid waste, phosphatization slag solid waste the like waste are generated in journey.And waste total amount is big, it is existing usual Processing method modes, such mode such as is to fill up, burns and handling waste and the utility contained in waste is not made to wave It sends out effect due, results in waste of resources, and also can cause environmental pollution.
In consideration of it, special propose the application.
Invention content
The present invention provides a kind of methods preparing iron oxide red using iron content waste, it is intended to improve existing iron content waste The problem of wasting of resources caused by directly filling or abandon or environmental pollution, while being intended to provide a kind of iron oxide red of high income Preparation method.
The present invention also provides a kind of iron oxide reds, with preferable economic benefit.
The invention is realized in this way:
A method of iron oxide red being prepared using iron content waste, is included the following steps:
Ferro element in iron-contained waste material is converted into iron hydroxide, ferrous hydroxide or iron hydroxide and ferrous hydroxide Mixture after existing for 120~180 DEG C of oxygen under the conditions of freeze-day with constant temperature 3~5h obtain dry powder;
Dry powder is placed in 400~800 DEG C of 40~180min under confined conditions and obtains γ-Fe2O3
Further, further include the γ-Fe to obtaining in preferred embodiments of the present invention2O3It mixes colours.
Further, in preferred embodiments of the present invention, iron-contained waste material is pickling steel pipe, seamless steel pipe, electric power steel The flushing liquor of bar, thin plate and steel rolling steel plate.
Further, in preferred embodiments of the present invention, the ferro element in iron-contained waste material is converted to iron hydroxide, hydrogen The mixture of ferrous oxide or iron hydroxide and ferrous hydroxide is that sodium hydroxide solution is added into flushing liquor.
Further, in preferred embodiments of the present invention, iron-contained waste material is phosphatization slag, by the iron in iron-contained waste material Element is converted to iron hydroxide, ferrous hydroxide or iron hydroxide and the mixture of ferrous hydroxide:By mass percentage Meter, after 25%~35% phosphatization slag is mixed with 65%~75% water, sodium hydroxide solution is added into mixed solution, makes Ferro element is obtained to precipitate completely;Filter cake and filtrate are filtered to obtain, filter cake is then iron hydroxide, ferrous hydroxide or iron hydroxide and hydrogen-oxygen Change ferrous mixture.
Further, further include removal phosphatization slag before mixing phosphatization slag with water in preferred embodiments of the present invention In mechanical admixture.
Further, in preferred embodiments of the present invention, by 25%~35% phosphatization slag and 65%~75% water After mixing, during sodium hydroxide solution is added into mixed solution, is heated to mixed solution and be passed through air and make divalent Iron is oxidized to ferric iron, filters to obtain filter cake and filtrate while hot.
Further, in preferred embodiments of the present invention, filtrate concentration, crystallisation by cooling, filtering means dehydration are obtained into phosphoric acid Trisodium.
Further, in preferred embodiments of the present invention, crystallisation by cooling temperature is 25~70 DEG C.
A kind of iron oxide red, adopts and is made with the aforedescribed process.
The beneficial effects of the invention are as follows:The present invention prepares iron oxide red by what above-mentioned design obtained using iron content waste Method can realize the re-using of waste, avoid waste discharge or landfill pair due to preparing iron oxide red using iron content waste Environment pollutes, simultaneously because drying steps and to turn brilliant step setting reasonable so that the present invention almost can completely will be in waste Iron recycle be made iron oxide red, realize higher economic benefit.
The iron oxide red that the present invention is obtained by above-mentioned design, due to being prepared using iron content waste using provided by the invention The method of iron oxide red is made, and has preferably economic value.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase Product.
Below to the embodiment of the present invention provide it is a kind of using iron content waste prepare iron oxide red method illustrate.
A method of iron oxide red being prepared using iron content waste, is included the following steps:
S1, the mixture that the ferro element in iron-contained waste material is converted to iron hydroxide, ferrous hydroxide or both 3~5h of freeze-day with constant temperature obtains dry powder under the conditions of afterwards existing for 120~180 DEG C of oxygen.
Specifically, it is managed by the flushing liquor of pickling steel pipe, seamless steel pipe, electric power steel pole, thin plate and steel rolling steel plate or just And the phosphatization slag of automobile specified thin plate phosphatization acts on raw material, the main component of flushing liquor is molysite, and the main component of phosphatization slag is Ferric phosphate and micro insignificant trbasic zinc phosphate.
When flushing liquor is as raw material, sodium hydroxide or its solution are added into flushing liquor keeps ferro element therein completely heavy It forming sediment, solution is in neutrality or alkalinity after iron precipitation completely, is added after sodium hydroxide and is measured pH of mixed to judge whether that precipitation is complete, Then filter solid content be at least 30% filter cake, the solid in the filter cake is iron hydroxide, ferrous hydroxide or above-mentioned The mixture of the two.
When phosphatization slag is raw material, first by the stone of the mechanical admixture removal in phosphatization slag, such as bulky grain.By quality Percentage composition meter is added after mixing the phosphatization slag after 25%~35% removal of impurities with 65%~75% water into mixed solution Sodium hydroxide solution so that ferro element precipitates completely, iron completely precipitation after solution be in neutrality or alkalinity, be added sodium hydroxide after survey PH of mixed is determined to judge whether that precipitation is complete;It filters to get filtrate and is at least 30% filter cake with solid content, consolidating in this filter cake Body is iron hydroxide, ferrous hydroxide or both.Preferably, after sodium hydroxide solution precipitation ferro element is added, to mixed Solution heating is closed, heating temperature is passed through air cavitation for a period of time to 80~100 DEG C so that ferrous oxidising is ferric iron, Filter cake and filtrate are obtained by filtration while hot after precipitation is complete, contained solid is iron hydroxide solid in the filter cake at this time.Obtained filter Liquid is concentrated, crystallisation by cooling, filtering means dehydration obtain tertiary sodium phosphate, it is preferable that cooling temperature is 25~70 DEG C.Obtained tricresyl phosphate Sodium can recycle.
Filter cake of the above two raw material through precipitating or aoxidizing is placed in insulating box, is existed in 120~180 DEG C of oxygen Under conditions of 3~5h of freeze-day with constant temperature obtain dry powder.The dry powder is iron hydroxide dry powder.Filter cake heats to incite somebody to action under aerobic conditions What may be contained in filter cake is ferrous oxidising for ferric iron, drying and dehydrating, to carry out follow-up intramolecular dehydration crystallization.
S2,40~180min under confined conditions that dry powder is placed in 400~800 DEG C obtain γ-Fe2O3
The dry powder that S1 steps obtain is placed in and is turned in brilliant stove, in 400~800 DEG C of 40~180min of dehydration under confined conditions So that iron hydroxide intramolecular dehydration obtains γ-Fe2O3That is iron oxide red.This step need to be isolated from the outside world, and prevent oxygen from entering and turn It sets off an explosion in brilliant stove.
Iron oxide red is obtained to be standardized to obtain iron oxide red, standardization refers to mixing colours according to national standards, with The product of not homochromy grade or class is obtained according to the demand of selling.
Below in conjunction with specific embodiment to it is provided by the invention it is a kind of using iron content waste prepare iron oxide red method into Row illustrates.
Embodiment 1
A kind of method preparing iron oxide red using iron content waste is present embodiments provided, is included the following steps:
Using the flushing liquor of the pickling steel pipe of steel maker, seamless steel pipe, electric power steel pole, thin plate and steel rolling steel plate as original Material, into flushing liquor, addition sodium hydroxide keeps precipitation of iron ions in solution complete.Then it is filtered, obtains filter cake, take 500g Filter cake is placed in insulating box, and freeze-day with constant temperature 5h obtains 149g iron hydroxide dry powder under the conditions of existing for 120 DEG C of oxygen;By hydrogen-oxygen Change iron dry powder to be placed in high temperature-resistant vessel, is then transferred to and turns in brilliant stove, in 400 DEG C of intramolecular dehydration under confined conditions 180min is transferred out of brilliant furnace cooling but, and standardization obtains 111g ferric oxide red colorants.149g iron hydroxides should theoretically obtain 111.4g iron oxide reds, therefore yield is 99.64%.
Embodiment 2
A kind of method preparing iron oxide red using iron content waste is present embodiments provided, is included the following steps:
Using the flushing liquor of the pickling steel pipe of steel maker, seamless steel pipe, electric power steel pole, thin plate and steel rolling steel plate as original Material, into flushing liquor, addition sodium hydroxide keeps precipitation of iron ions in solution complete.Then it is filtered, obtains filter cake, take 600g Filter cake is placed in insulating box, and freeze-day with constant temperature 3h obtains 240g iron hydroxide dry powder under the conditions of existing for 180 DEG C of oxygen;By hydrogen-oxygen Change iron dry powder to be placed in high temperature-resistant vessel, is then transferred to and turns in brilliant stove, in 450 DEG C of intramolecular dehydration under confined conditions 120min is transferred out of brilliant furnace cooling but, and standardization obtains 178g ferric oxide red colorants.240g iron hydroxides should theoretically obtain 179.4g iron oxide reds, therefore yield is 99.22%.
Embodiment 3
A kind of method preparing iron oxide red using iron content waste is present embodiments provided, is included the following steps:
Using the flushing liquor of the pickling steel pipe of steel maker, seamless steel pipe, electric power steel pole, thin plate and steel rolling steel plate as original Material, into flushing liquor, addition sodium hydroxide keeps precipitation of iron ions in solution complete.Then it is filtered, obtains filter cake, take 700g Filter cake is placed in insulating box, and freeze-day with constant temperature 3.5h obtains 356g iron hydroxide dry powder under the conditions of existing for 150 DEG C of oxygen;By hydrogen Iron oxide dry powder is placed in high temperature-resistant vessel, is then transferred to and is turned in brilliant stove, in 600 DEG C of intramolecular dehydration under confined conditions 60min is transferred out of brilliant furnace cooling but, and standardization obtains 265.0g ferric oxide red colorants.356g iron hydroxides should theoretically obtain 266.16g iron oxide reds, therefore yield is 99.56%.
Embodiment 4
A kind of method preparing iron oxide red using iron content waste is present embodiments provided, is included the following steps:
By steel pipe and automobile specified thin plate phosphatization using the phosphatization slag of the 700g of solid content 40% as raw material, phosphatization is removed After mechanical admixture in slag, based on mass percentage, phosphatization slag after 25% remove slag is mixed with 75% water, to after mixing Solution in sodium hydroxide is added so that then pH value of solution 10 carries out being heated to 80 DEG C and is passed through air cavitation oxygen to solution Change one hour.It filters to get filtrate while hot and filter cake.Filter cake is placed in constant temperature oven and dehydrates 3h, cooling obtains 221.92g Iron hydroxide dry powder;221.92g dry powder is put into high temperature-resistant vessel and then is transferred among brilliant stove, in 400 DEG C of closed items Intramolecular dehydration 150min under part is transferred out of brilliant furnace cooling but, and standardization obtains 164.43g ferric oxide red colorants.221.92g hydrogen Iron oxide should theoretically obtain 165.92g iron oxide reds, therefore yield is 99.1%.By filtrate concentration, it is cooled to 25 DEG C and crystallized Filter dehydration obtains the Na3PO412H2O crystalline powders of 780g, theoretical deserved 788.14g, therefore yield is 98.97%.
Embodiment 5
A kind of method preparing iron oxide red using iron content waste is present embodiments provided, is included the following steps:
By steel pipe and automobile specified thin plate phosphatization using the phosphatization slag of the 600g of solid content 50% as raw material, phosphatization is removed After mechanical admixture in slag, based on mass percentage, phosphatization slag after 35% remove slag is mixed with 65% water, to after mixing Solution in sodium hydroxide is added so that then pH value of solution 10 carries out being heated to 90 DEG C and is passed through air cavitation oxygen to solution Change one hour.It filters to get filtrate while hot and filter cake.Filter cake is placed in constant temperature oven and dehydrates 4h, cooling obtains 237.7g hydrogen Iron oxide dry powder;237.7g dry powder is put into high temperature-resistant vessel and then is transferred among brilliant stove, under confined conditions at 450 DEG C Intramolecular dehydration 180min is transferred out of brilliant furnace cooling but, and standardization obtains 176.65g ferric oxide red colorants.237.7g hydroxide Iron should theoretically obtain 176.65g iron oxide reds, therefore yield is 99.4%.By filtrate concentration, to be cooled to 25 DEG C of crystallization filterings de- Water obtains the Na3PO412H2O crystalline powders of 836.84g, theoretical deserved 844.44g, therefore yield is 99.1%.
Embodiment 6
A kind of method preparing iron oxide red using iron content waste is present embodiments provided, is included the following steps:
By steel pipe and automobile specified thin plate phosphatization using the phosphatization slag of the 600g of solid content 40% as raw material, phosphatization is removed After mechanical admixture in slag, based on mass percentage, phosphatization slag after 30% remove slag is mixed with 70% water, to after mixing Solution in sodium hydroxide is added so that then pH value of solution 8 carries out being heated to 100 DEG C and is passed through air cavitation oxygen to solution Change one hour.It filters to get filtrate while hot and filter cake.Filter cake is placed in constant temperature oven and dehydrates 5h, cooling obtains 232.32g Iron hydroxide dry powder;232.32g dry powder is put into high temperature-resistant vessel and then is transferred among brilliant stove, in 800 DEG C of closed items Intramolecular dehydration 40min under part is transferred out of brilliant furnace cooling but, and standardization obtains 170.14g ferric oxide red colorants.232.32g hydrogen Iron oxide should theoretically obtain 172.61g iron oxide reds, therefore yield is 98.6%.By filtrate concentration, it is cooled to 50 DEG C and crystallized Filter dehydration obtains the Na3PO412H2O crystalline powders of 822.6g, theoretical deserved 825.1g, therefore yield is 99.7%.
Embodiment 7
A kind of method preparing iron oxide red using iron content waste is present embodiments provided, is included the following steps:
By steel pipe and automobile specified thin plate phosphatization using the phosphatization slag of the 600g of solid content 40% as raw material, phosphatization is removed After mechanical admixture in slag, based on mass percentage, phosphatization slag after 32% remove slag is mixed with 68% water, to after mixing Solution in sodium hydroxide is added so that then pH value of solution 8 be heated to 90 DEG C to solution and is passed through the oxidation of air cavitation One hour.It filters to get filtrate while hot and filter cake.Filter cake is placed in constant temperature oven and dehydrates 4.5h, cooling obtains 231.86g Iron hydroxide dry powder;231.86g dry powder is put into high temperature-resistant vessel and then is transferred among brilliant stove, in 700 DEG C of closed items Intramolecular dehydration 100min under part is transferred out of brilliant furnace cooling but, and standardization obtains 171.01g ferric oxide red colorants.231.86g hydrogen Iron oxide should theoretically obtain 172.27g iron oxide reds, therefore yield is 99.27%.By filtrate concentration, it is cooled to 60 DEG C and crystallized Filter dehydration obtains the Na3PO412H2O crystalline powders of 820.7g, theoretical deserved 823.37g, therefore yield is 99.7%.
It is provided by the invention to prepare oxygen using iron content waste from the point of view of yield by the obtained iron oxide reds of embodiment 1-7 The yield for changing iron oxide red made from the method for iron oxide red is very high, close to 100%, effectively realizes waste resource recycling, avoids Iron content flushing water and iron content phosphatization slag direct emission or landfill pollution on the environment, while preferable warp can also be created Ji benefit.Also, when using phosphatization slag as raw material, moreover it can be used to tertiary sodium phosphate crystal powder is prepared, again by production process Water reuse creates preferable economic benefit.
In conclusion the method provided by the invention for preparing iron oxide red using iron content waste, due to using iron content waste Iron oxide red is prepared, can realize the re-using of waste, waste discharge or landfill is avoided to pollute the environment, simultaneously because Drying steps and turn brilliant step setting are reasonable so that the present invention almost can completely recycle the iron in waste with obtained iron oxide It is red, realize higher economic benefit.
Ferric oxide red colorant provided by the invention, using the side provided by the invention for preparing iron oxide red using iron content waste Method is made, and has preferably economic value.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for this field For technical staff, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of method preparing iron oxide red using iron content waste, which is characterized in that include the following steps:
Ferro element in iron-contained waste material is converted into the mixed of iron hydroxide, ferrous hydroxide or iron hydroxide and ferrous hydroxide 3~5h of freeze-day with constant temperature obtains dry powder under the conditions of after conjunction object existing for 120~180 DEG C of oxygen;
The dry powder is placed in 400~800 DEG C of 40~180min under confined conditions and obtains γ-Fe2O3
2. the method according to claim 1 for preparing iron oxide red using iron content waste, which is characterized in that further include to obtaining γ-the Fe arrived2O3It is mixed colours to obtain ferric oxide red colorant.
3. the method according to claim 1 for preparing iron oxide red using iron content waste, which is characterized in that the iron content is useless Gurry is the flushing liquor of pickling steel pipe, seamless steel pipe, electric power steel pole, thin plate and steel rolling steel plate.
4. the method according to claim 3 for preparing iron oxide red using iron content waste, which is characterized in that iron-contained waste material In ferro element to be converted to iron hydroxide, ferrous hydroxide or iron hydroxide and the mixture of ferrous hydroxide be to the flushing Sodium hydroxide solution is added in liquid.
5. the method according to claim 1 for preparing iron oxide red using iron content waste, which is characterized in that the iron content is useless Gurry be phosphatization slag, by the ferro element in the iron-contained waste material be converted to iron hydroxide, ferrous hydroxide or iron hydroxide and The mixture of ferrous hydroxide is:Based on mass percentage, 25%~35% phosphatization slag is mixed with 65%~75% water After conjunction, sodium hydroxide solution is added into mixed solution so that ferro element precipitates completely;Filter to obtain filter cake and filtrate, the filter Cake is then the mixture of iron hydroxide, ferrous hydroxide or iron hydroxide and ferrous hydroxide.
6. the method according to claim 5 for preparing iron oxide red using iron content waste, which is characterized in that by the phosphorus Slugging further includes the mechanical admixture removed in the phosphatization slag before being mixed with water.
7. the method according to claim 5 for preparing iron oxide red using iron content waste, which is characterized in that
After 25%~35% phosphatization slag is mixed with 65%~75% water, it is molten that sodium hydroxide is added into mixed solution During liquid, heated to mixed solution and be passed through air make it is ferrous oxidising be ferric iron, filter to obtain the filter cake while hot And filtrate.
8. the method according to claim 7 for preparing iron oxide red using iron content waste, which is characterized in that by the filtrate Concentration, crystallisation by cooling, filtering means dehydration obtain tertiary sodium phosphate.
9. the method according to claim 8 for preparing iron oxide red using iron content waste, which is characterized in that crystallisation by cooling temperature Degree is 25~70 DEG C.
10. a kind of ferric oxide red colorant, which is characterized in that be made using method as claimed in claim 2.
CN201810770162.1A 2018-07-13 2018-07-13 A kind of method and ferric oxide red colorant preparing iron oxide red using iron content waste Pending CN108793263A (en)

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CN113603150A (en) * 2021-09-23 2021-11-05 广州大学 Iron oxide red and preparation method thereof
CN115159582A (en) * 2022-06-17 2022-10-11 国环危险废物处置工程技术(天津)有限公司 Method for producing iron oxide red pigment and sodium phosphate by using phosphated slag

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CN113603150A (en) * 2021-09-23 2021-11-05 广州大学 Iron oxide red and preparation method thereof
CN115159582A (en) * 2022-06-17 2022-10-11 国环危险废物处置工程技术(天津)有限公司 Method for producing iron oxide red pigment and sodium phosphate by using phosphated slag

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Application publication date: 20181113