CN102351231A - Resource utilization method for titanium white by-product ferrous sulphate - Google Patents
Resource utilization method for titanium white by-product ferrous sulphate Download PDFInfo
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- CN102351231A CN102351231A CN2011101770787A CN201110177078A CN102351231A CN 102351231 A CN102351231 A CN 102351231A CN 2011101770787 A CN2011101770787 A CN 2011101770787A CN 201110177078 A CN201110177078 A CN 201110177078A CN 102351231 A CN102351231 A CN 102351231A
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Abstract
The invention discloses a resource utilization method for titanium white by-product ferrous sulphate, which solves the technical problem of incomplete utilization of titanium white by-product ferrous sulphate with low cost in the prior art. The method of the invention comprises the following steps: a, purifying and processing titanium white by-product ferrous sulphate; b, introducing ammonia gas in a ferrous sulphate solution obtained by purifying and processing, fully reacting and filtering to obtain ferrous hydroxide deposition and an ammonium sulfate solution; c, adding calcium hydrate in the ammonium sulfate solution and fully reacting to obtain dihydrate calcium sulphate deposition and ammonia gas, recovering ammonia gas as a raw material of a step b, drying the dihydrate calcium sulfate deposition and processing to obtain the product gypsum. According to the invention, sulfur and iron resources in titanium white by-product ferrous sulphate are fully used for producing industrial grade gypsum and iron ore concentrate, the problem of titanium white by-product on environmental pollution is solved; The ammonia gas can be circularly used without consumption based on theory, the loss amount needs to be added in practical production, and the production cost is low.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of titanium white by product thing ferrous sulfate resource utilization method.
Background technology
At present; Because China mainly adopts Titanium White Production By Sulfuric Acid Process; And one ton of white titanium pigment of every production will produce the by-product ferrous sulfate during about 3.5 tons, and in titanium white by product thing ferrous sulfate, the quality percentage composition of its staple iron vitriol is about 90%.Along with the development of white titanium pigment industry, the output of titanium white by product thing ferrous sulfate is cumulative year after year also, and through statistics, just Panzhihua Region last year is with regard to about 50～1,000,000 tons of titanium white by product thing ferrous sulfate of output.If so a large amount of titanium white by product thing ferrous sulfate still adopts the primary accumulation mode to handle; Will take a large amount of soils; And contain a small amount of dilute sulphuric acid in the titanium white waste and all can produce serious pollution, thereby cause titanium white by product thing ferrous sulfate to become a kind of breakneck chemical industry waste water body and soil.
Now, the method for consumption titanium white waste mainly contains following several kinds: 1, treated as fodder additives; 2, treated as industrial water purification agent; 3, make high-end products such as iron oxide black, iron oxide red or nanometer iron powder.Above method complex process, processing costs is high, and its consumption is very little for the quantum of output of titanium white waste.As utilize titanium white by product thing ferrous sulfate to prepare the method for red iron oxide: purifying treatment titanium white by product thing ferrous sulfate at first; Temperature (50～70 ℃) iron sheet reduction control hydrolysis is 6～10 hours in promptly adopting; Flocculation, settlement separate, the refining iron vitriol solution, the recovery 95～98% of obtaining; Adopt steps such as the neutralization of lower concentration iron vitriol solution and ammonia, oxidation to make red iron oxide then.This method processing costs is high, can not make full use of titanium white by product thing ferrous sulfate, should not big area promote the use of.
By on can know; The titanium white by product thing ferrous sulfate that produces in the production process of titanium pigment not only is not utilized effectively; Waste sulphur, fe source; Environment is caused severe contamination, and produce the processing costs that white titanium pigment per ton is also wanted expensive, the sulfate process titanium dioxide industry will be difficult to develop in a healthy way if things go on like this.Nowadays, how low-cost a large amount of processing titanium white by product thing ferrous sulfate has become a technical barrier of sulfuric acid method titanium pigment industry.
Therefore, be badly in need of the resource utilization method that a kind of processing costs is low, can handle titanium white by product thing ferrous sulfate in a large number at present.
Summary of the invention
To be solved by this invention is the technical problem that can not low-cost make full use of titanium white by product thing ferrous sulfate in the prior art.
The present invention solve the technical problem the technical scheme that is adopted and provides a kind of titanium white by product thing ferrous sulfate resource utilization method, and this method may further comprise the steps:
A, purifying treatment titanium white by product thing ferrous sulfate; Feed ammonia in b, the copperas solution that after purifying treatment, obtains, fully react after-filtration and get ferrous hydroxide deposition and ammoniumsulphate soln; C, in ammoniumsulphate soln, add calcium hydroxide and fully react and obtain sulfate dihydrate calcium deposit and ammonia, reclaim ammonia and use as the raw material of step b, the sulfate dihydrate calcium deposit is handled through oven dry and is obtained the product gypsum.
Wherein, aforesaid method also comprises steps d: step b gained ferrous hydroxide deposition is made the product iron concentrate through washing, press filtration, roasting.
Said iron ore concentrate is meant the powdered iron ore that can directly be used for pig iron smelting that iron-holder is higher.
Wherein, the feeding amount of ammonia described in the step b is in the aforesaid method: the ammonia amount of substance: ferrous sulfate amount of substance=2～3.
Further, the feeding amount of ammonia described in the step b is: the ammonia amount of substance: ferrous sulfate amount of substance=2.1～2.2.
Wherein, calcium hydroxide described in the step c is to add the water reaction by unslaked lime to make in the aforesaid method.
Wherein, the add-on of calcium hydroxide described in the step c is in the aforesaid method: the calcium hydroxide amount of substance: ammonium sulfate amount of substance=1～1.1.
Further, the add-on of calcium hydroxide is described in the step c: the calcium hydroxide amount of substance: ammonium sulfate amount of substance=1.05.
The inventive method specifically can be implemented in such a way:
A, purifying treatment titanium white by product thing ferrous sulfate.
Feed ammonia in b, the copperas solution that after purifying treatment, obtains, fully react after-filtration and get ferrous hydroxide deposition and ammoniumsulphate soln; Wherein, the feeding amount of said ammonia is: the ammonia amount of substance: ferrous sulfate amount of substance=2～3, the feeding amount is preferably: the ammonia amount of substance: ferrous sulfate amount of substance=2.1～2.2.
C, in ammoniumsulphate soln, add calcium hydroxide and fully react and obtain sulfate dihydrate calcium deposit and ammonia, reclaim ammonia and use as the raw material of step b, the sulfate dihydrate calcium deposit is handled through oven dry and is obtained the product gypsum; Wherein, said calcium hydroxide is to add the water reaction by unslaked lime to make; The add-on of calcium hydroxide is: the calcium hydroxide amount of substance: ammonium sulfate amount of substance=1～1.1, preferred add-on is: calcium hydroxide amount of substance: ammonium sulfate amount of substance=1.05.
D, step b gained ferrous hydroxide deposition is made the product iron concentrate through washing, press filtration, roasting.
The beneficial effect of the inventive method is: the inventive method makes full use of sulphur and the fe source in the titanium white by product thing ferrous sulfate, manufacture level gypsum and iron ore concentrate, the problem of solution titanium white by product thing environmental pollution; This method recycles ammonia, does not consume in theory, in actual production, only needs to mend loss amount and gets final product, and is with low cost; This method can be handled titanium white by product thing ferrous sulfate in a large number; Do not produce secondary pollution; Direct discharging of waste water; Solve the technical barrier of processing titanium white by product thing ferrous sulfate that can not be low-cost a large amount of in the sulfuric acid method titanium pigment industry, economic benefit and social benefit very significantly have the excellent popularization prospect.
Embodiment
A kind of titanium white by product thing ferrous sulfate resource utilization method, this method specifically comprises the steps:
A, with art methods purifying treatment titanium white by product thing ferrous sulfate.
Feed ammonia in b, the copperas solution that after purifying treatment, obtains, fully react after-filtration and get ferrous hydroxide deposition and ammoniumsulphate soln; Wherein, in order to practice thrift cost, do not waste resource, the feeding amount of the said ammonia of this step is: the ammonia amount of substance: ferrous sulfate amount of substance=2～3, preferred feeding amount is: ammonia amount of substance: ferrous sulfate amount of substance=2.1～2.2.The principal reaction equation is following:
FeSO
4·7H
2O+2NH
3＝Fe(OH)
2+(NH
4)
2SO
4+5H
2O
C, in ammoniumsulphate soln, add calcium hydroxide and fully react and obtain sulfate dihydrate calcium deposit and ammonia, reclaim ammonia and use as the raw material of step b, the sulfate dihydrate calcium deposit is handled through oven dry and is obtained the product gypsum; In order to practice thrift cost, the said calcium hydroxide of this step is to add the water reaction by unslaked lime to make; Wherein, In order to improve transformation efficiency; And can produce qualified gypsum, the add-on of this step calcium hydroxide is: the calcium hydroxide amount of substance: ammonium sulfate amount of substance=1～1.1, preferred add-on is: calcium hydroxide amount of substance: ammonium sulfate amount of substance=1.05.The principal reaction equation is following:
CaO+H
2O＝Ca(OH)
2
Ca(OH)
2+(NH
4)
2SO
4＝CaSO
4·2H
2O↓+2NH
3↑
D, step b gained ferrous hydroxide deposition is made the product iron concentrate through washing, press filtration, roasting.
Below in conjunction with embodiment the present invention is done further description, but therefore do not limit the present invention among the described scope of embodiments.
The embodiment of the invention is as follows raw materials used: titanium white by product thing ferrous sulfate: iron vitriol quality percentage composition is 90.5%; Other composition is free state sulfuric acid, free state water, metatitanic acid, sal epsom, Tai-Ace S 150 and small amount of calcium, manganese etc., derives from Flos Bombacis Malabarici family happiness chemical industry ltd.Commercially available calcium lime powder: quicklime quality percentage composition 84%.
Embodiment one usefulness the inventive method is handled titanium white by product thing ferrous sulfate
Purifying treatment titanium white by product thing ferrous sulfate: prepare titanium white by product thing ferrous sulfate 100g; Temperature (50～70 ℃) iron sheet reduction control hydrolysis is 6～10 hours in the employing; Flocculation, settlement separate is made with extra care and is obtained iron vitriol solution 510g, contains iron vitriol 17%.
Feed ammonia 27.5L in the copperas solution that after purifying treatment, obtains, fully react after-filtration and get ferrous hydroxide deposition 98g and ammoniumsulphate soln 405g.The ferrous hydroxide deposition makes product iron concentrate 45.3g through washing, press filtration, roasting.Iron ore concentrate iron content 68%.
Prepare unslaked lime 38g, after adding 100g water fully stirs, mix stirring, it is fully reacted, reclaim and obtain ammonia 23.5L, filter and obtain sulfate dihydrate calcium deposit 175g, obtaining product gypsum 91g through the oven dry processing with above-mentioned ammoniumsulphate soln 405g.The folding strength 2.8Mp of gypsum, presetting period 7min, final setting time 18min satisfies the requirement of technical grade gypsum, and waste water can directly discharge or reclaim use.
Embodiment dual-purpose the inventive method is handled titanium white by product thing ferrous sulfate
Purifying treatment titanium white by product thing ferrous sulfate: prepare titanium white by product thing ferrous sulfate 200g; Temperature (50～70 ℃) iron sheet reduction control hydrolysis is 6～10 hours in the employing; Flocculation, settlement separate is made with extra care and is obtained iron vitriol 980g, contains iron vitriol 17.7%.
Feed ammonia 56L in the copperas solution that after purifying treatment, obtains, fully react after-filtration and get ferrous hydroxide deposition 185g and ammoniumsulphate soln 790g.The ferrous hydroxide deposition makes product iron concentrate 90.5g through washing, press filtration, roasting.Iron ore concentrate iron content 69%.
Prepare unslaked lime 75g, after adding 200g water fully stirs, mix stirring, it is fully reacted, reclaim and obtain ammonia 49L, filter and obtain sulfate dihydrate calcium deposit 355g, obtaining product gypsum 186g through the oven dry processing with above-mentioned ammoniumsulphate soln 790g.The folding strength 2.7Mp of gypsum, presetting period 7min, final setting time 17min satisfies the requirement of technical grade gypsum, and waste water can directly discharge or reclaim use.
Embodiment three usefulness the inventive method are handled titanium white by product thing ferrous sulfate
Purifying treatment titanium white by product thing ferrous sulfate: prepare titanium white by product thing ferrous sulfate 300g; Temperature (50～70 ℃) iron sheet reduction control hydrolysis is 6～10 hours in the employing; Flocculation, settlement separate is made with extra care and is obtained iron vitriol solution 1455g, contains iron vitriol 17.8%.
Feed ammonia 82L in the copperas solution that after purifying treatment, obtains, fully react after-filtration and get ferrous hydroxide deposition 258g and ammoniumsulphate soln 1188g.The ferrous hydroxide deposition makes product iron concentrate 136g through washing, press filtration, roasting.Iron ore concentrate iron content 68%.
Prepare unslaked lime 115g, after adding 300g water fully stirs, mix stirring, it is fully reacted, reclaim and obtain ammonia 71.3L, filter and obtain sulfate dihydrate calcium deposit 535g, obtaining product gypsum 280g through the oven dry processing with above-mentioned ammoniumsulphate soln 1188g.The folding strength 2.7Mp of gypsum, presetting period 6min, final setting time 18min satisfies the requirement of technical grade gypsum, and waste water can directly discharge or reclaim use.
Can find out from embodiment, can make full use of sulphur resource and fe source in the titanium white by product thing ferrous sulfate, produce qualified technical grade gypsum and iron ore concentrate, solve the problem of titanium white by product thing environmental pollution with the inventive method; This method recycles ammonia, in actual production, only needs to mend 12～15% of each usage quantity and gets final product, and is with low cost; This method does not produce secondary pollution; Waste water can directly discharge or matter uses; Therefore this method is fit to a large amount of titanium white by product thing ferrous sulfate of handling; Solve the technical barrier of processing titanium white by product thing ferrous sulfate that can not be low-cost a large amount of in the sulfuric acid method titanium pigment industry, economic benefit and social benefit very significantly have the excellent popularization using value.
Claims (7)
1. titanium white by product thing ferrous sulfate resource utilization method is characterized in that comprising the steps: a, purifying treatment titanium white by product thing ferrous sulfate; Feed ammonia in b, the copperas solution that after purifying treatment, obtains, fully react after-filtration and get ferrous hydroxide deposition and ammoniumsulphate soln; C, in ammoniumsulphate soln, add calcium hydroxide and fully react and obtain sulfate dihydrate calcium deposit and ammonia, reclaim ammonia and use as the raw material of step b, said sulfate dihydrate calcium deposit is handled through oven dry and is obtained the product gypsum.
2. titanium white by product thing ferrous sulfate resource utilization method according to claim 1 is characterized in that also comprising steps d: step b gained ferrous hydroxide deposition is made the product iron concentrate through washing, press filtration, roasting.
3. titanium white by product thing ferrous sulfate resource utilization method according to claim 1, it is characterized in that: the feeding amount of ammonia described in the step b is: the ammonia amount of substance: ferrous sulfate amount of substance=2～3.
4. titanium white by product thing ferrous sulfate resource utilization method according to claim 3, it is characterized in that: the feeding amount of ammonia described in the step b is: the ammonia amount of substance: ferrous sulfate amount of substance=2.1～2.2.
5. titanium white by product thing ferrous sulfate resource utilization method according to claim 1 is characterized in that: calcium hydroxide described in the step c is to add the water reaction by unslaked lime to make.
6. titanium white by product thing ferrous sulfate resource utilization method according to claim 1, it is characterized in that: the add-on of calcium hydroxide described in the step c is: the calcium hydroxide amount of substance: ammonium sulfate amount of substance=1～1.1.
7. titanium white by product thing ferrous sulfate resource utilization method according to claim 6, it is characterized in that: the add-on of calcium hydroxide described in the step c is: the calcium hydroxide amount of substance: ammonium sulfate amount of substance=1.05.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103922926A (en) * | 2014-04-17 | 2014-07-16 | 绍兴县远程树脂科技有限公司 | Process for purifying residual solid waste generated after alkali peeling wastewater treatment |
| CN105174287A (en) * | 2015-09-09 | 2015-12-23 | 江西玛德精细化学工业有限公司 | Method for recovering ammonia and coproducing calcium sulfate through lime neutralization of T acid mother liquid |
| CN108658131A (en) * | 2018-08-14 | 2018-10-16 | 西南科技大学 | A kind of iron oxide red and gypsum plaster and preparation method thereof based on titanium gypsum |
| CN109354072A (en) * | 2018-09-25 | 2019-02-19 | 河南省睿博环境工程技术有限公司 | A kind of alkali round-robin method hamlessizing technology ferric oxide red colorant technique |
| CN110129061A (en) * | 2019-05-31 | 2019-08-16 | 北京建工环境修复股份有限公司 | A kind of stabilizer of repairing heavy metal pollution and its preparation method and application |
| CN110436483A (en) * | 2019-08-21 | 2019-11-12 | 贵州新东浩化工材料科技有限公司 | A kind of titanium white waste acid resource recycle method |
| CN112390295A (en) * | 2020-10-30 | 2021-02-23 | 龙蟒佰利联集团股份有限公司 | Method for utilizing artificial rutile mother liquor |
| CN113173592A (en) * | 2021-04-28 | 2021-07-27 | 郑州大学 | Method for purifying sulfuric acid process titanium dioxide waste acid and coproducing titanium gypsum step by step |
| CN113968578A (en) * | 2021-12-06 | 2022-01-25 | 紫金矿业集团股份有限公司 | Method for synthesizing iron phosphate by using ferrous sulfate as titanium dioxide byproduct |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103922926A (en) * | 2014-04-17 | 2014-07-16 | 绍兴县远程树脂科技有限公司 | Process for purifying residual solid waste generated after alkali peeling wastewater treatment |
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| CN108658131A (en) * | 2018-08-14 | 2018-10-16 | 西南科技大学 | A kind of iron oxide red and gypsum plaster and preparation method thereof based on titanium gypsum |
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| CN110129061A (en) * | 2019-05-31 | 2019-08-16 | 北京建工环境修复股份有限公司 | A kind of stabilizer of repairing heavy metal pollution and its preparation method and application |
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| CN112390295A (en) * | 2020-10-30 | 2021-02-23 | 龙蟒佰利联集团股份有限公司 | Method for utilizing artificial rutile mother liquor |
| CN113173592A (en) * | 2021-04-28 | 2021-07-27 | 郑州大学 | Method for purifying sulfuric acid process titanium dioxide waste acid and coproducing titanium gypsum step by step |
| CN113968578A (en) * | 2021-12-06 | 2022-01-25 | 紫金矿业集团股份有限公司 | Method for synthesizing iron phosphate by using ferrous sulfate as titanium dioxide byproduct |
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