CN102115208B - Method for preparing ferrous nitrate and lead sulfate by waste acid generated by preparing titanium white powder with sulfuric acid method - Google Patents
Method for preparing ferrous nitrate and lead sulfate by waste acid generated by preparing titanium white powder with sulfuric acid method Download PDFInfo
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- CN102115208B CN102115208B CN201010615472XA CN201010615472A CN102115208B CN 102115208 B CN102115208 B CN 102115208B CN 201010615472X A CN201010615472X A CN 201010615472XA CN 201010615472 A CN201010615472 A CN 201010615472A CN 102115208 B CN102115208 B CN 102115208B
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Abstract
The invention provides a method for preparing ferrous nitrate and lead sulfate by waste acid generated by preparing titanium white powder with a sulfuric acid method. The method for preparing the ferrous nitrate and the lead sulfate comprises the steps of: mixing and reacting waste acid generated by preparing titanium white powder with the sulfuric acid method with excessive ferrous hydroxide to generate ferrous sulfate; filtering reaction solution to obtain filter liquor which mainly contains ferrous sulfate; adding excessive lead nitrate into the filter liquor which mainly contains the ferrous sulfate to react, generating ferrous nitrate and lead sulfate, filtering the reaction solution, and separating the ferrous nitrate from the lead sulfate solution; washing, drying and smashing the lead sulfate precipitate to obtain a lead sulfate product; and adding a small amount of ferrous sulfate into the ferrous nitrate solution to neutralize the lead nitrate, transmitting a reactant into a pressure-reducing distiller to distill by means of pressure reduction to be ferrous nitrate supersaturated solution, cooling and crystallizing, and drying to obtain a ferrous nitrate product.
Description
Technical field
The present invention relates to the comprehensive utilization of Titanium White Production By Sulfuric Acid Process gained spent acid, particularly, relate to the method
of producing Iron nitrate and lead sulfate with Titanium White Production By Sulfuric Acid Process gained spent acid.
Background technology
The main raw material of sulfuric acid method titanium pigment is titanium ore and sulfuric acid, and its reaction principle is:
Fe2O3+3H2SO4==Fe2(SO4)3+3H2O;
TiO2+2H2SO4==Ti(SO4)2+2H2O;
Fe+Fe2(SO4)3==3FeSO4，
PH value of solution is transferred to 5-6, makes Ti (SO4) 2 hydrolysis:
Ti(SO4)2+3H2O==H2TiO3↓+2H2SO4，
The filtering-depositing heating obtains white titanium pigment:
H2TiO3==TiO2+H2O
Titanium White Production By Sulfuric Acid Process; Mainly contain sulfuric acid and ferrous sulfate in the spent acid in its production process; Also contain a small amount of metatitanic acid and other metals ions, wherein sulfuric acid content is 18-23%, and ferrous sulfate content is 80g/L (ferrous in anhydrous slufuric acid); Only have a spot of spent acid can return recycling, most of waste material can't directly utilize.
At present, more to the method for comprehensive utilization of Titanium White Production By Sulfuric Acid Process gained spent acid, mainly contain and utilize the reaction of spent acid and iron, generate ferrous sulfate and produce iron pigments such as iron oxide black, iron oxide red with ferrous sulfate; Or, produce sulfate of ammoniac and ferrous sulfate ammonia fertilizer material with in the ammonia and spent acid.
Yet because Titanium White Production By Sulfuric Acid Process gained spent acid output is huge, aforesaid method can not completely consumed, therefore, is necessary to explore the novel method of the spent acid comprehensive regulation of Titanium White Production By Sulfuric Acid Process gained and application.
Summary of the invention
Mainly contain sulfuric acid and ferrous sulfate in the Titanium White Production By Sulfuric Acid Process gained spent acid, also contain a small amount of metatitanic acid and other metals ions, wherein sulfuric acid content is 18-23%; Ferrous sulfate content is 80g/L (ferrous in anhydrous slufuric acid), and for it is fully utilized, the applicant provides the method for producing Iron nitrate and lead sulfate with Titanium White Production By Sulfuric Acid Process gained spent acid; This method is simple to operate; Facility investment is few, and sulfuric acid and ferrous sulfate recovery utilization rate are high, are worthy of popularization.
Technical scheme of the present invention is following: with the method that Titanium White Production By Sulfuric Acid Process gained spent acid is produced Iron nitrate and lead sulfate, this method comprises following concrete steps:
Steps A: Titanium White Production By Sulfuric Acid Process gained spent acid is mixed with excessive hydrogen iron protoxide solution, make the reaction of sulfuric acid and ferrous hydroxide, generate ferrous sulfate; Filtering reacting liquid obtains main sulfur acid ferrous filtrating, contains the filter residue of a small amount of unreacted ferrous hydroxide and insoluble impurities, and filter residue is buried or through other art breading;
Step B: in the main sulfur acid ferrous filtrating of steps A gained, add excessive lead nitrate, stir reaction down, generate Iron nitrate and lead sulfate, filtering reacting liquid, separate sulfur lead plumbate deposition and ferrous nitrate solution; In this step, a small amount of unreacted lead nitrate is also in ferrous nitrate solution;
Step C: step B gained lead sulfate deposition through washing, dry and pulverizing, is obtained lead sulfate deposition product;
Step D: with adding in a small amount of ferrous sulfate in the step B gained ferrous nitrate solution and lead nitrate, then send into alkali and press that underpressure distillation is the Iron nitrate supersaturated solution in the distiller, crystallisation by cooling, drying obtains the Iron nitrate product.
Method of producing Iron nitrate and lead sulfate with Titanium White Production By Sulfuric Acid Process gained spent acid according to the invention; The sulfuric acid and the ferrous sulfate that contain in the Titanium White Production By Sulfuric Acid Process gained spent acid have been made full use of; Its step is simple; Facility investment is few, and Iron nitrate and lead sulfate productive rate are higher, are methods that is worthy of popularization.
Embodiment
Embodiment 1: with the method that Titanium White Production By Sulfuric Acid Process gained spent acid is produced Iron nitrate and lead sulfate, this method comprises following concrete steps:
Steps A: Titanium White Production By Sulfuric Acid Process gained spent acid is mixed with excessive hydrogen iron protoxide solution, make the reaction of sulfuric acid and ferrous hydroxide, generate ferrous sulfate; Filtering reacting liquid obtains main sulfur acid ferrous filtrating, contains the filter residue of a small amount of unreacted ferrous hydroxide and insoluble impurities, and filter residue is buried or through other art breading;
Step B: in the main sulfur acid ferrous filtrating of steps A gained, add excessive lead nitrate, stir reaction down, generate Iron nitrate and lead sulfate, filtering reacting liquid, separate sulfur lead plumbate deposition and ferrous nitrate solution; In this step, a small amount of unreacted lead nitrate is also in ferrous nitrate solution;
Step C: step B gained lead sulfate deposition through washing, dry and pulverizing, is obtained lead sulfate deposition product;
Step D: with adding in a small amount of ferrous sulfate in the step B gained ferrous nitrate solution and lead nitrate, then send into alkali and press that underpressure distillation is the Iron nitrate supersaturated solution in the distiller, crystallisation by cooling, drying obtains the Iron nitrate product.
Above content is to combine concrete preferred implementation to the further explain that the present invention did, and can not assert that practical implementation of the present invention is confined to these explanations.For the those of ordinary skill of technical field under the present invention, under the prerequisite that does not break away from the present invention's design, its framework form can be flexible and changeable, can the subseries product.Just make some simple deduction or replace, all should be regarded as belonging to the scope of patent protection
that the present invention is confirmed by claims of being submitted to.
Claims (1)
1. produce the method for Iron nitrate and lead sulfate with Titanium White Production By Sulfuric Acid Process gained spent acid, it is characterized in that this method comprises following concrete steps:
Steps A: Titanium White Production By Sulfuric Acid Process gained spent acid is mixed with excessive hydrogen iron protoxide solution, make the reaction of sulfuric acid and ferrous hydroxide, generate ferrous sulfate; Filtering reacting liquid obtains main sulfur acid ferrous filtrating, contains the filter residue of a small amount of unreacted ferrous hydroxide and insoluble impurities, and filter residue is buried or through other art breading;
Step B: in the main sulfur acid ferrous filtrating of steps A gained, add excessive lead nitrate, stir reaction down, generate Iron nitrate and lead sulfate, filtering reacting liquid, separate sulfur lead plumbate deposition and ferrous nitrate solution; In this step, a small amount of unreacted lead nitrate is also in ferrous nitrate solution;
Step C: step B gained lead sulfate deposition through washing, dry and pulverizing, is obtained lead sulfate deposition product;
Step D: with adding in a small amount of ferrous sulfate in the step B gained ferrous nitrate solution and lead nitrate, send into then that underpressure distillation is the Iron nitrate supersaturated solution in the underpressure distillation device, crystallisation by cooling, drying obtains the Iron nitrate product.
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| CN201010615472XA CN102115208B (en) | 2010-12-31 | 2010-12-31 | Method for preparing ferrous nitrate and lead sulfate by waste acid generated by preparing titanium white powder with sulfuric acid method |
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| CN201010615472XA CN102115208B (en) | 2010-12-31 | 2010-12-31 | Method for preparing ferrous nitrate and lead sulfate by waste acid generated by preparing titanium white powder with sulfuric acid method |
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| CN102115208A CN102115208A (en) | 2011-07-06 |
| CN102115208B true CN102115208B (en) | 2012-11-14 |
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| JP3045751B2 (en) * | 1990-08-06 | 2000-05-29 | 堺化学工業株式会社 | Lumpy tribasic lead sulfate |
| CN1026681C (en) * | 1991-06-03 | 1994-11-23 | 黑龙江省环境保护科学研究所 | Plumbous chromate and lead sulfate produced by waste oxalic acid dregs |
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