CN101214931A - Concentrating and impurity removing method for dilute sulfuric acid in titanium dioxide powder production process by employing sulfuric acid process - Google Patents
Concentrating and impurity removing method for dilute sulfuric acid in titanium dioxide powder production process by employing sulfuric acid process Download PDFInfo
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Abstract
The invention discloses a concentration and impurity removal method of dilute sulfuric acid in producing titanium dioxide through a sulfuric acid method, which includes the following steps: first the dilute sulfuric acid is fed into a mixing acid tank; after the dilute sulfuric acid is concentrated into concentrated sulfuric acid, part of the concentrated sulfuric acid returns to the mixing acid tank to be mixed into 25 percent to 35 percent of feed acid, and fed into a steam concentration system to receive multi-effect evaporation concentration; part of the concentrated sulfate material returns to the mixing acid tank and the rest enters into a serial back-flow cooling curing crystal growth tank; in the back-flow cooling curing crystal growth tank, the sulfate material after curing crystal growth cooling is fed into a solid-liquid separator to receive solid-liquid separation, and the filtrate is a concentrated sulfuric acid product. Therefore, the invention not only can realize the long-period good operation of devices, but also is characterized by simple process, less investment, low manufacturing expense, obvious economic benefit, etc., and belongs to a novel method of energy saving and emission reduction.
Description
Technical field:
The invention belongs to the method for dilute sulphuric acid concentrating and impurity removing, particularly relate to the concentrating and impurity removing method of dilute sulphuric acid in the sulfuric acid method titanium pigment production process.
Background technology:
No matter Titanium White Production By Sulfuric Acid Process adopts ilmenite concentrate as raw material, and still adopting titanium slag is that raw material all will produce a large amount of dilute sulphuric acids, and one ton of sulfuric acid method titanium pigment will produce the dilute sulphuric acid that the 5.0-7.0 ton contains 17-25% left and right sides concentration.China's sulfate process titanium dioxide powder yield reached nearly 900,000 tons in 2006, about 5,500,000 tons of by-product dilute sulphuric acid.
The contriver is once in " a kind of dilute sulphuric acid concentrating and impurity removing production method " Chinese patent ZL02113704.8, adopt warm air heat exchange evaporation concentration production method, successful solution the production difficult problem that caused because of the concentration heat exchanger fouling of titanium dioxide by-product dilute sulphuric acid, and the tediously long problem such as numerous and diverse of the production technique brought of separating for several times, and economic carrying out suitability for industrialized production.The weak point of this method is that energy consumption is higher relatively, carries out heat exchange evaporation moisture wherein because of using a large amount of warm airs and spray atomization dilute sulphuric acid, causes the eliminating tail large-minded, and a large amount of sensible heats are taken away by tail gas, are unfavorable for energy-saving and emission-reduction.
Chinese patent application " the sulfur waste acid that produces in the production process of titanium pigment, the recovery method of waste gas " (publication number CN1608716A), same the same with Chinese patent " treatment process of rare spent acid of association during Production By Sulfuric Acid Process titanium dioxide " (publication number CN1042527A), production unit is many, investment is big, complex process is tediously long, process cost is high, separating for several times, energy consumption height.
The former (publication number CN1608716A) adopts three sections to concentrate twice solid-liquid separating method and reclaim the titanium dioxide dilute sulphuric acids: one section employing rotary kiln tail gas is concentrated to 30% concentration with dilute sulphuric acid, then the titanium dioxide that brings from furnace gas of solid-liquid separation; Two sections are adopted steam heating to carry out the two-stage three-effect evaporation and condensation with graphite block heat exchanger graphite heat exchanger (the also piece hole graphite heat exchanger of meaning), dilute sulphuric acid concentration is concentrated to 45% reconcentration to 65% by 30%, handles sulfate impurities such as solid-liquid separation ferrous sulfate again through crystallization kettle; Three sections dilute sulphuric acids of 65% after solid-liquid separation are again with its evaporation concentration to 80%.The shortcoming of this method has four: one, uses rotary kiln tail gas only to pay attention to hot utilization and ignored the economic worth of titanium dioxide in the tail gas in one section concentrates; Usually the production of sulfuric acid method titanium pigment is being advanced before rotary kiln burns till, and has passed through a series of tediously long processes and has purified and obtain very pure titanium dioxide (metatitanic acid); Absorb heat exchange with the spent acid that contains all raw ore impurity this moment again, will reduce its economic worth from the powder mixture pollution from the titanium that rotary kiln tail gas is taken out of again; If return that the processing of more preceding operation is reclaimed since a large amount of acid at a middle or low price iron under the effect of tail gas and temperature, be oxidized to high price iron and be adsorbed on and very difficultly on the titanium dioxide remove again, have a strong impact on quality product; The 2nd, the titanium dioxide dust of from rotary kiln tail gas, taking out of, the titanium dioxide that comprises rutile-type, sharp attitude type and three kinds of forms of metatitanic acid (titanium hydroxide), their dissolving poweies in acid are followed successively by metatitanic acid (titanium hydroxide), sharp attitude type, rutile-type, that is to say and remove that not hydrolysis is intact stays in the acid outside the titanyl sulfate, part metatitanic acid from the dust that rotary kiln tail gas is taken out of at peracid than dissolving back in the acid again under the condition, not only cause the viscosity of acid to increase, and bring bigger trouble for the postorder evaporation concentration; The 3rd, this structure formation of the graphite block heat exchanger graphite heat exchangers of employing is unfavorable for containing scale forming matter and the evaporation concentration heat exchange of the sulfuric acid method titanium pigment dilute sulphuric acid of solid phase precipitates in a large number in two sections concentrate; Its main drawback is the higher heat transfer wall thickness that forms between hot acid and the heat exchange steam face structure that adds of cross flow form, causes the heat transfer path of heat long, thermal resistance thermal conversion is big, thermosteresis is big; Also the runner perforate that is heated dilute sulphuric acid is less relatively, resistance is big because of the structural strength of self is limit, and watt consumption was higher when the more and equal sulfuric acid amount of heat waste was passed through when causing sulfuric acid to pass through heat exchanger; Also have the easy fouling of this titanium dioxide dilute sulphuric acid relative with cleaning frequently the time maintenance cost higher, have to adopt the cleaning in a hole, the artificial hole of proprietary instrument during mechanical cleaning, promptly expend consuming time; The 4th, 70% the gelled acid that adopts in three sections concentrate that the silicon carbide vaporizer will be after cooling, crystallization, solid-liquid separation further heats and is concentrated to 80%, not only facility investment cooling intensification energy consumption big, technology is big, and unnecessary increase technical process, make its operation more complicated.
And the latter (publication number CN1042527A) adopts two sections to concentrate three solid-liquid separation except that the impurity in the disacidify.First section same adopt titanium dioxide calcining kiln tail gas with the dilute sulphuric acid pre-concentration of 20-24% to 26-29%, solid-liquid separation is at this residue of separating out for the first time, the filtrate that separation is obtained cools to separate out iron vitriol again, carry out the secondary solid-liquid separation, isolate the solid formation iron vitriol, obtain containing the dilute sulphuric acid of 30-35%; The 30-35% dilute sulphuric acid that contains that will obtain again then, carries out second section sulfuric acid concentration that is concentrated into 60-71% with the vacuum-evaporation concentration method; At last, the postprecipitation thing in the acid is carried out solid-liquid separation for the third time, obtain the sulfuric acid about 70%.This technology is many with the same equipment of aforementioned technology, technical process is long; Crystallisation by cooling is separated out green vitriol, it is energy-conservation that the surface seems, concentrate three isolating tediously long flow processs for two sections through overcooling, separation, heating, it is not to have reduced but significantly increase that facility investment and direct evaporation concentrate energy consumption, and operation is many, process cost is also many.
Summary of the invention:
The objective of the invention is in order to overcome the deficiencies in the prior art, providing does not both have twice solid-liquid separation of three sections evaporation concentration and two sections problems that equipment is many, technical process is long, energy consumption is high that concentrated three solid-liquid separation process cause; Also not for avoiding fouling to adopt the relative problem of higher of energy consumption of the low warm air sensible heat loss that the warm air heat exchange brings; More there are not long flow path, equipment that repeatedly solid-liquid separation increased is many, investment is big problem; Thereby to reach the concentrating and impurity removing method of simplifying technology, shortening flow process, minimizing equipment, reducing dilute sulphuric acid in the Titanium White Production By Sulfuric Acid Process process of investing, save energy and reduce the cost, increase purposes such as economic benefit.
The objective of the invention is to be achieved through the following technical solutions, finished acid after employing concentrates and dilute sulphuric acid are mixed the back as concentrating charging acid, and the steam concentration systems of sending into graphite tubular heat exchange formation carries out multiple-effect evaporation and concentrates; Sulfuric acid material after the multiple-effect evaporation concentration systems concentrates, part return the acid tank that the is mixed acid that is mixed and use, and the remaining in-line adverse current that enters is cooled off slaking growing the grain groove; In adverse current cooling slaking growing the grain groove, the ferrous sulfate monohydrate crystal growth of separating out during concentrated vitriol, the temperature of concentrated vitriol reduces; Through overcuring growing the grain refrigerative sulfuric acid material, send into solid-liquid separating machine and carry out solid-liquid separation; The concentrated vitriol product that filtrate being obtains can return sulfate process titanium dioxide production and be used as the sulfuric acid raw material, also can make other purposes; Filter cake is byproduct and mainly contains ferrous sulfate monohydrate and a spot of sulfuric acid, can be used as production of sulfur from pyrite acid starting material and other purposes.Concrete production technique of the present invention is:
A, return the charging acid that acid is mixed into 25～35% concentration after the sulfuric acid method titanium pigment dilute sulphuric acid sent into be mixed acid tank and diluted acid concentrating unit and concentrate;
B, send into steam concentration systems that the graphite tubular heat exchange constitutes through the charging acid after being mixed and carry out multiple-effect evaporation and concentrate;
C, the sulfuric acid material after concentrating by evaporation concentration system, part is returned the sour operation of being mixed of front as the complex acid charging, and rest part enters in the adverse current cooling slaking growing the grain device and carries out material cooling growing the grain;
D, from the material that cooling slaking growing the grain device comes out, send into and carry out solid-liquid separation in the solid-liquid separating machine;
The liquid of e, solid-liquid separation is concentrated vitriol, send titanium white production acidolysis system to be used as raw material sulphuric acid and uses;
The solid of f, solid-liquid separation is and contains a small amount of vitriolic ferrous sulfate monohydrate, send sulfurous iron ore production sulfuric acid plant to be used as and produces the vitriolic raw material;
The tubulation diameter of above-mentioned graphite tubular heat exchange is Φ 25-Φ 38; Preferred Φ 36-Φ 38;
Above-mentioned cooling slaking growing the grain groove inlet temperature is 105-120 ℃, preferred 115-120 ℃; Temperature out is 30-70 ℃, preferred 45-55 ℃; The residence time is 2-6 hour, is preferably 3-4 hour;
Above-mentioned solid-liquid separating machine is diaphragm filter press or close press or tubular filter press, and filter cake dries up with pressurized air;
The filter cake that above-mentioned solid-liquid separation obtains increases air supply gradually with the pressurized air of 0.1～0.6MPa.
The advantage that the technical scheme that the present invention separates is brought: reclaim the titanium dioxide dilute sulphuric acid owing to adopt one section of steam to concentrate a solid-liquid separation process, shortened technical process widely, reduced facility investment, saved productive expense than two sections concentrated three solid-liquid separation or three sections concentrated secondary solid-liquid separation process; The problem of not using titanium dioxide quality problems that rotary kiln tail gas causes in one section concentration technology and economic worth to reduce, there are not in the air heat-exchanging process a large amount of Cryogenic air take away too much sensible heat problem, the energy expenditure problem that the concentrated material that does not more have the separating for several times solid to bring is repeatedly lowered the temperature and heated up yet; Returning acid owing to employing is concentrated is mixed with the charging diluted acid, improved the concentration of concentrated charging acid, eliminated the degree of supersaturation of the easy scale forming matter calcium sulfate salt of trace residual in the sulfur waste acid, reduced the scaling rate on heat exchanger wall, add and use wide-aperture graphite tubular heat exchange, the enriched material materials flow crosses that resistance is low, heat transfer efficiency is high, thermosteresis is little, to the loose dirt layer easy to clean regeneration that forms on the tube wall.Therefore, but the not only macrocyclic good operation of implement device of the present invention, and have advantages, genus energy-saving and emission-reduction novel procesies such as technical process is simple, reduced investment, productive expense is low, economic benefit is very remarkable.
Description of drawings:
Fig. 1: be process flow diagram of the present invention
1, the acid tank that is mixed; 2, multiple-effect concentration evaporator;
3, multiple-effect graphite tubular heat exchange; 4, vacuum chamber;
5, cooling slaking growing the grain groove; 6, solid-liquid separating machine;
7, gelled acid storage tank.
Specific embodiment:
Below in conjunction with process flow sheet and with specific embodiment the inventive method is described further.
Embodiment 1:
Titanium white dilute sulphuric acid composed as follows: fluid density: 1380 (kg/cm
3)
| Component | Content (%) | Component | Content (%) |
| H 2SO 4 | 23.5 | ||
| Fe 2O 3 | 5.20 | Al 2O 3 | 0.25 |
| MgO | 0.36 | TiO 2 | 0.68 |
| V | 0.02 | Cr | 0.005 |
| Nb | 0.004 | Pb | 0.013 |
| P | 0.004 | CaO | 0.043 |
Per hour 22.2 ton of 23.5% titanium white dilute sulphuric acid and 4.3 ton of 60% sulfuric acid after concentrating per hour enter acid and are mixed in the groove 1, the dilute sulphuric acid of per hour 26.5 ton of 29.4% concentration that is mixed is pumped into multiple-effect graphite tubular heat exchange 3 by sulfuric acid and multiple-effect concentration evaporator 2 carries out evaporation concentration, material per hour obtains the sulphuric acid concentration material of 13.0 ton of 60% concentration after multiple-effect evaporation concentrates, wherein 4.3 tons are returned the front acid groove nitration mixture that is mixed, 8.7 ton enters the slaking growing the grain of lowering the temperature in the cooling slaking growing the grain groove 5, inlet temperature is 110 ℃, temperature out is 50 ℃, 3 hours residence time.Deliver to the diaphragm filter press press filtration then, isolate 6.2 ton of 68% concentration sulfuric acid, enter gelled acid storage tank 7 and send titanium dioxide acid hydrolysis workshop section back to, remaining 2.5 tons of slag separating send vitriol works to produce sulfuric acid.
Embodiment 2:
Titanium white dilute sulphuric acid composed as follows: dilute sulphuric acid density: 1320 (kg/cm
3)
| Component | Content (%) | Component | Content (%) |
| H 2SO 4 | 22.26 | ||
| Fe 2O 3 | 5.03 | Al 2O 3 | 0.2 |
| MgO | 0.40 | TiO 2 | 0.68 |
| V | 0.03 | Cr | 0.006 |
| Nb | 0.004 | Pb | 0.015 |
| P | 0.005 | CaO | 0.033 |
Per hour 20.6 ton of 22.26% titanium dioxide dilute sulphuric acid and 6.0 ton of 70% sulfuric acid after concentrating per hour enter acid and are mixed in the groove 1, the dilute sulphuric acid of per hour 26.6 ton of 33.0% concentration that is mixed is pumped into multiple-effect graphite tubular heat exchange 3 by sulfuric acid and multiple-effect concentration evaporator 2 carries out evaporation concentration, material per hour obtains the sulphuric acid concentration material of 12.6 ton of 70% concentration after concentrating, wherein 6.0 tons are returned the front acid groove nitration mixture that is mixed, 6.6 ton enters the slaking growing the grain of lowering the temperature in the cooling slaking growing the grain groove 5, inlet temperature is 115 ℃, temperature out is 45 ℃, 4 hours residence time.Deliver to the diaphragm filter press press filtration then, isolate 3.9 ton of 80.2% concentration sulfuric acid, enter gelled acid storage tank 7 and send titanium dioxide acid hydrolysis workshop section back to, remaining 2.3 tons of slag separating send vitriol works to produce sulfuric acid.
Embodiment 3:
Titanium white dilute sulphuric acid composed as follows: dilute sulphuric acid density: 1320 (kg/cm
3)
| Component | Content (%) | Component | Content (%) |
| H 2SO 4 | 22.26 | ||
| Fe 2O 3 | 5.03 | Al 2O 3 | 0.2 |
| MgO | 0.40 | TiO 2 | 0.68 |
| V | 0.03 | Cr | 0.006 |
| Nb | 0.004 | Pb | 0.015 |
| P | 0.005 | CaO | 0.033 |
Per hour 15.53 ton of 22.26% titanium dioxide dilute sulphuric acid and 3.0 ton of 70% sulfuric acid after concentrating per hour enter acid and are mixed in the groove 1, the dilute sulphuric acid of per hour 18.53 ton of 30.0% concentration that is mixed is pumped into multiple-effect graphite tubular heat exchange 3 by sulfuric acid and multiple-effect concentration evaporator 2 carries out evaporation concentration, material per hour obtains the sulphuric acid concentration material of 8.96 ton of 62% concentration after concentrating, enter the slaking growing the grain of lowering the temperature in the cooling slaking growing the grain groove 5, inlet temperature is 120 ℃, temperature out is 55 ℃, 3 hours residence time.Deliver to the diaphragm filter press press filtration then and wherein isolate 6.46 ton of 70.2% concentration sulfuric acid, 3.0 tons are returned the front acid groove nitration mixture that is mixed, and send titanium dioxide acid hydrolysis workshop section back to for 3.46 tons, and remaining 2.5 tons of slag separating send vitriol works to produce sulfuric acid.
Claims (8)
1. the concentrating and impurity removing method of dilute sulphuric acid in the Titanium White Production By Sulfuric Acid Process process is characterized in that it comprises:
A, the sulfuric acid method titanium pigment dilute sulphuric acid is sent into the acid tank that is mixed, with concentrate by the dilute sulphuric acid concentrating unit after return the charging acid that acid is mixed into 25～35% concentration;
B, send into steam concentration systems that the graphite tubular heat exchange constitutes through the charging acid after being mixed and carry out multiple-effect evaporation and concentrate;
C, the sulfuric acid material after concentrating by evaporation concentration system, part is returned the sour operation of being mixed of front as the complex acid charging; Rest part enters in the adverse current cooling slaking growing the grain groove and carries out material cooling slaking growing the grain;
D, from the material that cooling slaking growing the grain groove comes out, send into and carry out solid-liquid separation in the solid-liquid separating machine;
The liquid of e, solid-liquid separation is concentrated vitriol; Isolating solid is and contains a small amount of vitriolic ferrous sulfate monohydrate.
2. by the concentrating and impurity removing method of dilute sulphuric acid in the described Titanium White Production By Sulfuric Acid Process process of claim 1, it is characterized in that the acid of returning after described the concentrating can be without concentrated vitriol after the solid-liquid separation or the concentrated vitriol after solid-liquid separation.
3. by the concentrating and impurity removing method of dilute sulphuric acid in the described Titanium White Production By Sulfuric Acid Process process of claim 1, the tubulation diameter that it is characterized in that the graphite tubular heat exchange of described evaporation concentration system is Φ 25-Φ 38.
4. by the concentrating and impurity removing method of dilute sulphuric acid in claim 1 or the 3 described Titanium White Production By Sulfuric Acid Process processes, the tubulation diameter that it is characterized in that the graphite tubular heat exchange of described evaporation concentration system is Φ 36-Φ 38.
5. by the concentrating and impurity removing method of dilute sulphuric acid in the described Titanium White Production By Sulfuric Acid Process process of claim 1, it is characterized in that 105-120 ℃ of described cooling slaking growing the grain groove material inlet temperature, temperature out 30-70 ℃; Residence time 2-6 hour.
6. by the concentrating and impurity removing method of dilute sulphuric acid in claim 1 or the 5 described Titanium White Production By Sulfuric Acid Process processes, it is characterized in that 115-120 ℃ of described cooling slaking growing the grain groove material inlet temperature, temperature out 45-55 ℃; Residence time 3-4 hour.
7. by the concentrating and impurity removing method of dilute sulphuric acid in the described Titanium White Production By Sulfuric Acid Process process of claim 1, it is characterized in that described solid-liquid separating machine is diaphragm filter press, close press, tubular filter press; Filter cake dries up with pressurized air.
8. by the concentrating and impurity removing method of dilute sulphuric acid in claim 1 or the 7 described Titanium White Production By Sulfuric Acid Process processes, it is characterized in that described filter cake blows cake with the pressurized air of 0.1-0.6MPa, progressively increase air supply when blowing cake stage by stage.
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| CN1202989C (en) * | 2002-05-09 | 2005-05-25 | 四川龙蟒集团有限责任公司 | Process for concentrating diluted sulfuric acid and removing impurities |
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Application publication date: 20080709 Assignee: Ningbo Xinfu Titanium Dioxide Co., Ltd. Assignor: Gong Jiazhu Contract record no.: 2010330000432 Denomination of invention: Concentrating and impurity removing method for dilute sulfuric acid in titanium dioxide powder production process by employing sulfuric acid process Granted publication date: 20100120 License type: Exclusive License Record date: 20100407 |