CN104176776A - Hydrolysis method of titanyl sulfate solution with high concentration and low ferrous and titanium ratio - Google Patents

Hydrolysis method of titanyl sulfate solution with high concentration and low ferrous and titanium ratio Download PDF

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Publication number
CN104176776A
CN104176776A CN201310207589.8A CN201310207589A CN104176776A CN 104176776 A CN104176776 A CN 104176776A CN 201310207589 A CN201310207589 A CN 201310207589A CN 104176776 A CN104176776 A CN 104176776A
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hydrolysis
steam
titanium
minutes
valve
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曹波
殷红忠
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SHANDONG DAWN TITANIUM INDUSTRY Co Ltd
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SHANDONG DAWN TITANIUM INDUSTRY Co Ltd
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Abstract

The invention belongs to the technical field of titanium dioxide production, and particularly relates to a hydrolysis method of a titanyl sulfate solution with high concentration and low ferrous and titanium ratio. The method is characterized by comprises the following steps: first rapidly mixing a concentrated titanium solution with NaOH solution at a temperature of 80-85 DEG C to complete preparation of hydrolysis crystal seed; then adding the crystal seed in the volume 2-3% of the hydrolysis titanium liquid into the concentrated titanium liquid preheated to 90-96 DEG C, stirring evenly, and heating with steam of 0.4 MPa to a boiling state; stopping stirring after appearance of grayed points, and closing a steam valve; mixing again 30 min later, and opening the steam valve to heat the material to a boiling state again; maintaining a micro boiling state for 180 min under micro pressure of 200-500 pa, so as to finish hydrolysis. The process has the advantages of simpleness, stable product quality and high hydrolysis rate.

Description

High density, low iron titanium ratio titanyl sulfate solution method for hydrolysis
Technical field: the invention belongs to titanium white production technical field, be specifically related to a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis.
Background technology: at present, the production technique of domestic titanium dioxide adopts sulfuric acid process more, wherein, hydrolysis process mainly comprises two kinds, one is automatic growing crystal species hydrolysis process, another kind is plus seed hydrolysis process, and most of Producing Titanium Dioxide enterprise adopts plus seed hydrolysis process, forms crystal seed with sodium hydroxide solution and titanium liquid.And large multiple enterprises adopts ilmenite acidolysis technique to prepare titanium liquid, the titanium concentration of preparation is on the low side, iron titanium ratio is higher, must be again through Crystallization Procedure, ferrously separate, enrichment process process after titanium concentration and iron titanium ratio just can reach processing requirement.Its shortcoming one is complex process, the 2nd, and between product batches, quality fluctuation is larger, and quality is unstable, and the 3rd, after hydrolysis, in metatitanic acid, contain a large amount of ferrous ions, after hydrolysis, percent hydrolysis is on the low side.
Summary of the invention: the object of this invention is to provide a kind of technique simple, constant product quality, the high density that percent hydrolysis is high, low iron titanium ratio titanyl sulfate solution method for hydrolysis.
Technical scheme of the present invention is: a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis, is characterized in that: comprise following processing step:
(1) the NaOH solution that is, 8~10% by dense titanium liquid and the percentage concentration of total titanium content 220-240g/l, iron titanium ratio 0.15-0.16 mixes rapidly at temperature 80-85 DEG C, and being warming up to 90-96 DEG C, the stability of system reaches 100-140ml and has completed the preparation of hydrolysis crystal seed;
(2), being the long-pending 2-3% of Hydrolysis of Titanium liquid by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 90-96 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 200-500pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
The reasonable technical scheme of the present invention is: a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis, is characterized in that: comprise following processing step:
(1) the NaOH solution that is, 8~10% by dense titanium liquid and the percentage concentration of total titanium content 225-235g/l, iron titanium ratio 0.15-0.16 mixes rapidly at temperature 80-85 DEG C, and being warming up to 90-96 DEG C, the stability of system reaches the preparation that has completed hydrolysis crystal seed after 110-130ml;
(2), being the long-pending 2-3% of Hydrolysis of Titanium liquid by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 90-96 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 300-400pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
Best-of-breed technology scheme of the present invention is: a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis, is characterized in that: comprise following processing step:
(1) the NaOH solution that is, 9% by dense titanium liquid and the percentage concentration of total titanium content 230g/l, iron titanium ratio 0.155 mixes rapidly in 4 minutes at 82.5 DEG C of temperature, and being warming up to 93 DEG C, the stability of system reaches the preparation that has completed hydrolysis crystal seed after 120ml;
(2), being Hydrolysis of Titanium liquid long-pending 2.5% by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 93 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 350pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
Owing to adopting technique scheme, reasonably crystal seed preparation method and adding proportion, make to be hydrolyzed rear metatitanic acid size distribution even; Because the maintenance slight boiling condition time that hydrolysis is last is long, percent hydrolysis is up to 96%, and total titanium content of solution is higher, equipment capacity has been improved greatly, thereby it is simple to have technique, constant product quality, the advantage that percent hydrolysis is high.
Embodiment: further illustrate technical scheme of the present invention below in conjunction with specific embodiment.
Embodiment 1: a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis, is characterized in that: comprise following processing step:
(1), the NaOH solution that is 10% by dense titanium liquid and the percentage concentration of total titanium content 240g/l, iron titanium ratio 0.15 mixes rapidly at 80 DEG C of temperature, and is warming up to 96 DEG C, the stability of system reaches 100ml and has completed the preparation of hydrolysis crystal seed;
(2), being Hydrolysis of Titanium liquid long-pending 3% by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 90 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 500pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
Embodiment 2: a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis, is characterized in that: comprise following processing step:
(1), the NaOH solution that is 8% by dense titanium liquid and the percentage concentration of total titanium content 220g/l, iron titanium ratio 0.16 mixes rapidly at 85 DEG C of temperature, and is warming up to 90 DEG C, the stability of system reaches 140ml and has completed the preparation of hydrolysis crystal seed;
(2), being Hydrolysis of Titanium liquid long-pending 2% by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 96 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 200pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
Embodiment 3: a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis, is characterized in that: comprise following processing step:
(1), the NaOH solution that is 10% by dense titanium liquid and the percentage concentration of total titanium content 235g/l, iron titanium ratio 0.15 mixes rapidly at 80 DEG C of temperature, and is warming up to 96 DEG C, the stability of system reaches the preparation that has completed hydrolysis crystal seed after 110ml;
(2), being Hydrolysis of Titanium liquid long-pending 3% by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 90 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 400pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
Embodiment 4: a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis, is characterized in that: comprise following processing step:
(1), the NaOH solution that is 8% by dense titanium liquid and the percentage concentration of total titanium content 225g/l, iron titanium ratio 0.16 mixes rapidly at 85 DEG C of temperature, and is warming up to 90 DEG C, the stability of system reaches the preparation that has completed hydrolysis crystal seed after 130ml;
(2), being Hydrolysis of Titanium liquid long-pending 2% by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 96 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 300pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
Embodiment 5: a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis, is characterized in that: comprise following processing step:
(1) the NaOH solution that is, 9% by dense titanium liquid and the percentage concentration of total titanium content 230g/l, iron titanium ratio 0.155 mixes rapidly in 4 minutes at 82.5 DEG C of temperature, and being warming up to 93 DEG C, the stability of system reaches the preparation that has completed hydrolysis crystal seed after 120ml;
(2), being Hydrolysis of Titanium liquid long-pending 2.5% by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 93 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 350pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
After hydrolysis, metatitanic acid size distribution is as following table:
? D10um D50um D90um Span um
Embodiment 1 0.255 0.347 0.672 1.200
Embodiment 2 0.254 0.346 0.733 1.385
Embodiment 3 0.252 0.336 0.637 1.146
Embodiment 4 0.238 0.319 0.611 1.170
Embodiment 5 0.252 0.333 0.621 1.108
Experimental data proves, owing to adopting above-mentioned technique, is hydrolyzed rear size distribution even; Thereby improved the quality of metatitanic acid after water, and total titanium concentration is high, and percent hydrolysis is high, in improving equipment capacity 20%-25%, reduces energy consumption 8-10%.

Claims (3)

1. high density, a low iron titanium ratio titanyl sulfate solution method for hydrolysis, is characterized in that: comprise following processing step:
(1) the NaOH solution that is, 8~10% by dense titanium liquid and the percentage concentration of total titanium content 220-240g/l, iron titanium ratio 0.15-0.16 mixes rapidly at temperature 80-85 DEG C, and being warming up to 90-96 DEG C, the stability of system reaches 100-140ml and has completed the preparation of hydrolysis crystal seed;
(2), being the long-pending 2-3% of Hydrolysis of Titanium liquid by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 90-96 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 200-500pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
2. by a kind of high density claimed in claim 1, low iron titanium ratio titanyl sulfate solution method for hydrolysis, it is characterized in that: comprise following processing step:
(1) the NaOH solution that is, 8~10% by dense titanium liquid and the percentage concentration of total titanium content 225-235g/l, iron titanium ratio 0.15-0.16 mixes rapidly at temperature 80-85 DEG C, and being warming up to 90-96 DEG C, the stability of system reaches the preparation that has completed hydrolysis crystal seed after 110-130ml;
(2), being the long-pending 2-3% of Hydrolysis of Titanium liquid by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 90-96 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, be under 300-400pa in minute-pressure, keep slight boiling condition after 180 minutes, can complete hydrolysis.
3. by a kind of high density, low iron titanium ratio titanyl sulfate solution method for hydrolysis described in claim 1 or 2, it is characterized in that: comprise following processing step:
(1) the NaOH solution that is, 9% by dense titanium liquid and the percentage concentration of total titanium content 230g/l, iron titanium ratio 0.155 mixes rapidly in 4 minutes at 82.5 DEG C of temperature, and being warming up to 93 DEG C, the stability of system reaches the preparation that has completed hydrolysis crystal seed after 120ml;
(2), being Hydrolysis of Titanium liquid long-pending 2.5% by volume, above-mentioned crystal seed is put into the dense titanium liquid that is preheated in advance 93 DEG C of temperature, after stirring, is discharged in hydrolyzer, the steam direct heating that is 0.4MPa with pressure is to seething with excitement;
(3), there is stopping stirring after change ash point steam off valve;
(4), after 30 minutes, stir again, open steam valve simultaneously the heating material in hydrolyzer is made it to boiling again after 20 minutes;
(5), steam off valve, regulate little steam valve and automatic pressure maintaining device, under minute-pressure 350pa, keep slight boiling condition after 180 minutes, can complete hydrolysis.
CN201310207589.8A 2013-05-20 2013-05-20 Hydrolysis method of titanyl sulfate solution with high concentration and low ferrous and titanium ratio Pending CN104176776A (en)

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Cited By (7)

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CN105883913A (en) * 2014-09-18 2016-08-24 攀枝花新中钛钒钛技术研发有限公司 Method for external seed normal pressure introduced hydrolysis of high-concentration titaniferous solution
CN106241866A (en) * 2016-08-30 2016-12-21 襄阳龙蟒钛业有限公司 A kind of method using high concentration plus seed to prepare titanium dioxide
CN106430300A (en) * 2016-08-30 2017-02-22 襄阳龙蟒钛业有限公司 Alkali-neutralization seed crystal external addition method for producing titanium dioxide
CN107640785A (en) * 2017-11-10 2018-01-30 广西顺风钛业有限公司 A kind of preparation method of plastic color master grain titanium dioxide
CN108545772A (en) * 2018-05-04 2018-09-18 广西金茂钛业有限公司 A kind of preparation method of colorant titanium dioxide additional hydrolyzing seed crystal
CN110028100A (en) * 2019-05-21 2019-07-19 四川大学 The preparation method of the method for Production By Sulfuric Acid Process rutile titanium white and double-effect seed crystal used
CN110554715A (en) * 2019-10-25 2019-12-10 攀钢集团攀枝花钢铁研究院有限公司 RBF neural network-based PID control method for hydrolysis process temperature of titanyl sulfate plus seed crystal

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105883913A (en) * 2014-09-18 2016-08-24 攀枝花新中钛钒钛技术研发有限公司 Method for external seed normal pressure introduced hydrolysis of high-concentration titaniferous solution
CN106241866A (en) * 2016-08-30 2016-12-21 襄阳龙蟒钛业有限公司 A kind of method using high concentration plus seed to prepare titanium dioxide
CN106430300A (en) * 2016-08-30 2017-02-22 襄阳龙蟒钛业有限公司 Alkali-neutralization seed crystal external addition method for producing titanium dioxide
CN106430300B (en) * 2016-08-30 2018-04-17 襄阳龙蟒钛业有限公司 A kind of method that alkali neutralization plus seed prepares titanium dioxide
CN106241866B (en) * 2016-08-30 2018-08-07 襄阳龙蟒钛业有限公司 A method of preparing titanium dioxide using plus seed
CN107640785A (en) * 2017-11-10 2018-01-30 广西顺风钛业有限公司 A kind of preparation method of plastic color master grain titanium dioxide
CN108545772A (en) * 2018-05-04 2018-09-18 广西金茂钛业有限公司 A kind of preparation method of colorant titanium dioxide additional hydrolyzing seed crystal
CN110028100A (en) * 2019-05-21 2019-07-19 四川大学 The preparation method of the method for Production By Sulfuric Acid Process rutile titanium white and double-effect seed crystal used
CN110028100B (en) * 2019-05-21 2021-11-12 四川大学 Method for producing rutile titanium white by sulfuric acid process and preparation method of used double-effect seed crystal
CN110554715A (en) * 2019-10-25 2019-12-10 攀钢集团攀枝花钢铁研究院有限公司 RBF neural network-based PID control method for hydrolysis process temperature of titanyl sulfate plus seed crystal

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Application publication date: 20141203