CN105152207A - High-efficiency sulfuric acid method titanium dioxide washing system and washing process thereof - Google Patents
High-efficiency sulfuric acid method titanium dioxide washing system and washing process thereof Download PDFInfo
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- CN105152207A CN105152207A CN201510465539.9A CN201510465539A CN105152207A CN 105152207 A CN105152207 A CN 105152207A CN 201510465539 A CN201510465539 A CN 201510465539A CN 105152207 A CN105152207 A CN 105152207A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/0475—Purification
Abstract
The invention discloses a high-efficiency sulfuric acid method titanium dioxide washing system and a washing process thereof. The washing system comprises a purifier, a waste acid recovery device, a beater, a washing circulating pot, a first filtration system and a second filtration system; the washing technology comprises the following steps: (1) placing a hydrolysis material into the filter for filtering; (2) extruding the hydrolysis material into a filter cake by the filter, and conveying the filter cake to the beater by the filter; (3) beating the filter cake by the filter and conveying the beat slurry to the washing circulating pot; (4) conveying the washed slurry and washing water to the first filtration system by the washing circulating pot; (5) reconveying intercepted metatitanic acid particle-containing dense liquid to the washing circulating pot by the first filtering system, and conveying filtered clear liquid to the second filtration system; (6) conveying the clear liquid to the washing circulating pot by the second filtration system to continue usage of the clear liquid, and conveying the filtered dense liquid to the waste acid recovery device for recovery. A bleaching kettle operation step in a present washing system is canceled, first washing and second washing in a traditional washing system are not distinguished, compared with the traditional washing system, the washing system has a concise flow.
Description
Technical field
The present invention relates to a kind of water wash system of sulfuric acid method titanium pigment, be specifically related to a kind of sulfuric acid method titanium pigment water wash system and washing process thereof efficiently.
Background technology
In traditional sulfuric acid method titanium pigment water washing process, along with the carrying out of washing, acidity in filter filter cake, metal ion and reducing substances all progressively reduce, owing to containing dissolved oxygen in washing water, so the Fe2+ in metatitanic acid has the chance being oxidized to Fe3+ to exist, and more there is this tendency latter stage in washing.Simultaneously due to the reduction of acidity, Fe3+ will generate Fe (OH) 3 and precipitate, and other metal ion also can generate precipitation when acidity is reduced to a certain degree.These precipitations are mixed in metatitanic acid, can have a huge impact the quality of the finished product.In order to eliminate above-mentioned impact, current production line all adds the vitriol oil and reductive agent by after washing after the making beating of metatitanic acid filter cake, after the precipitation formed or high oxide are dissolved as ionic condition, then carry out second time and washes and removed in water washing process.Whole technical process is long, complex operation.
Current washing process is quite large to the demand of water, conventional is, and two wash waters directly apply mechanically washes to one, one wash water (i.e. plain boiled water) after filtration or precipitation after be disposed between water treatment vehicle, the plain boiled water water yield is 20-30 ton/ton titanium dioxide, and also containing the metatitanic acid particle much wearing filter in plain boiled water, cause the loss of titanium dioxide.
Summary of the invention
The present invention in order to solve the problem, thus provides a kind of sulfuric acid method titanium pigment water wash system and washing process thereof efficiently.
For achieving the above object, technical scheme of the present invention is as follows:
A kind of sulfuric acid method titanium pigment water wash system efficiently, described sulfuric acid method titanium pigment water wash system comprises:
Filter;
Acid-restoring plant, described acid-restoring plant is connected with the spent acid discharge port of filter;
Hollander, described hollander is connected with the filter cake discharge port of filter;
Water washing cycles tank, described water washing cycles tank is communicated with hollander;
First filtering system, described first filtering system is communicated with water washing cycles tank;
Second filtering system, described second filtering system is communicated with acid-restoring plant with water washing cycles tank, the first filtering system respectively;
In a preferred embodiment of the invention, described first filtering system is cross-current type microfiltration membrane, and the precision of described cross-current type microfiltration membrane is 50-1000 nanometer, and transmembrane pressure is 0.05-0.8MPa.
In a preferred embodiment of the invention, described second filtering system is made up of nanofiltration membrane and reverse osmosis membrane, described nanofiltration membrane is 85-99.8% to the rejection of ferrous ion, be 80-99.8% to the rejection of titanyl sulfate, resistance to sulfuric acid concentration is 0-30%, working pressure is 1.0-6.5MPa, described reverse osmosis membrane is 85-99.8% to the rejection of ferrous ion, be 80-99.8% to the rejection of titanyl sulfate, be 85-99.8% to the rejection of sulfuric acid, resistance to sulfuric acid concentration is 0-15%, and working pressure is 1.5-6.5MPa.
In a preferred embodiment of the invention, described water washing cycles tank is encloses container, and described water washing cycles tank adopts nonoxidizing gas sealing, and to maintain tank body internal pressure be 1-10KPa.
In a preferred embodiment of the invention, the soft water adopted in described hollander and washing supplementary feed are all oxygen-free water.
A kind of sulfuric acid method titanium pigment washing process efficiently, this washing process comprises the steps:
(1) hydrolyzation material is put into filter to filter;
(2) filter cake that will fully squeeze out in hydrolyzation material containing the concentrated acid in metatitanic acid and metal ion of filter, filter cake is transported in hollander by filter, and filter is delivered in acid-restoring plant by extruding remaining spent acid in hydrolyzation material;
(3) add in hollander together with filter cake that soft water and filter transport and pull an oar, and by the slurry transferring after making beating to water washing cycles tank;
(4) material of pulling an oar enters water washing cycles tank, the soft water used during washing first also enters water washing cycles tank, making beating material and the foreign ion of pulling an oar in material are diluted, then by the first filtering system, water filtration is gone out, foreign ion in such making beating material just reduces, if soft water continues to enter, the first filtering system clear liquid is constantly discharged, foreign ion in making beating material will constantly reduce, until be reduced to qualified standard;
(5) wash qualified washing material and be transported to the first filtering system, after conveying, next batch making beating material enters water washing cycles tank and continues washing;
Metatitanic acid particle entrapment in the slurry that water washing cycles tank transports by (6) first filtering systems and washing water, again be delivered in water washing cycles tank by what retain containing metatitanic acid particle dope, water washing cycles tank is to again washing containing metatitanic acid particle dope of retaining, and the clear liquid after filtration is delivered in the second filtering system and again filters by the first filtering system;
A clear liquid part for (7) first filtering systems is delivered to reverse osmosis membrane through high-pressure pump and is filtered, a part enters nanofiltration membrane row and filters, reverse osmosis can retain sulfuric acid, ferrous, titanyl sulfate, nanofiltration only retains ferrous iron and titanyl sulfate, clear liquid acidity after nanofiltration membrane produces water and the hydration also of reverse osmosis membrane product maintains proper range, both comparatively can not intake low because of using reverse osmosis membrane completely, also comparatively can not intake high because of using nanofiltration membrane completely, nanofiltration membrane produces the clear liquid ferrous ion concentration after water and the hydration also of reverse osmosis membrane product lower than design load, meet washing water requirement completely, clear liquid is delivered to water washing cycles tank and continues to use by the second filtering system, dope after filtration is delivered to acid-restoring plant reclaim.
(8) add in water washing cycles tank in 10-60 minute before washing terminates and add SYNTHETIC OPTICAL WHITNER on a small quantity or not, the dosage of SYNTHETIC OPTICAL WHITNER is the 0-50% of former technique dosage.
By technique scheme, the invention has the beneficial effects as follows:
Present invention eliminates in existing water wash system bleaching still operation steps, do not distinguish one in traditional water wash system and wash and wash with two, more succinct than traditional water wash system flow process.
The present invention, according to content requirement ferrous in washing accepted stock, adds SYNTHETIC OPTICAL WHITNER on a small quantity or not, does not add sulfuric acid simultaneously, decreases production cost, reduce three wastes discharge amount; Can realize the recycle of washing water, therefore soft water demand reduces greatly, and wastewater treatment capacity also significantly reduces; The loss of metatitanic acid particle can be reduced, thus improve the rate of recovery of titanium dioxide.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is structural representation of the present invention;
Fig. 2 is process flow sheet of the present invention;
Fig. 3 is that the first filtering system coordinates schematic diagram with the second filtering system.
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with concrete diagram, setting forth the present invention further.
See Fig. 1, efficient sulfuric acid method titanium pigment water wash system provided by the invention, it comprises filter 100, acid-restoring plant 200, hollander 300, water washing cycles tank 400, first filtering system 500, second filtering system 600.
Filter 100, it is for filtering hydrolyzation material, and the solid content fully squeezed out in hydrolyzation material containing the concentrated acid in metatitanic acid and metal ion is the filter cake of 40-85%.
Hollander 300, it is connected with filter 100, and it is for pulling an oar to the filter cake after filter 100 filtration, and by the slurry transferring after making beating to water washing cycles tank 400.
The soft water adopted in hollander 300 and washing supplementary feed are all oxygen-free water.
Water washing cycles tank 400, it is connected with hollander 300, it is encloses container, concrete employing nonoxidizing gas sealing, and to maintain tank body internal pressure be 1-10KPa, it can wash material to the slurry that hollander 300 transports, and the slurry after washing and washing water are delivered to the first filtering system 500 and filtered.
First filtering system 500, it is connected with water washing cycles tank 400, it is specially cross-current type microfiltration membrane, precision is 50-1000 nanometer, transmembrane pressure is 0.05-0.8MPa, it is the metatitanic acid particle for retaining in slurry and washing water, and by being again delivered in water washing cycles tank 400 containing metatitanic acid particle dope of retaining, and the clear liquid after filtering is delivered to the second filtering system 600.
Second filtering system 600, it is connected with the first filtering system 500 and water washing cycles tank 400 respectively, it is that clear liquid after the filtration for transporting the first filtering system 500 filters again, be filtered into the washing water meeting water washing cycles tank 400 and wash, such water washing cycles tank 400 does not just need to add washing water.
The concrete nanofiltration membrane of second filtering system 600 and reverse osmosis membrane composition.
Nanofiltration membrane, it is 85-99.8% to the rejection of ferrous ion, is 80-99.8% to the rejection of titanyl sulfate, resistance to sulfuric acid concentration is 0-30%, and working pressure is 1.5-6.5MPa, and its ability mass concentration is the sulfuric acid of 30%, and allow sulfuric acid through, but ferrous ion and titanyl sulfate can be retained;
Reverse osmosis membrane, it is 85-99.8% to the rejection of ferrous ion, be 80-99.8% to the rejection of titanyl sulfate, be 85-99.8% to the rejection of sulfuric acid, resistance to sulfuric acid concentration is 0-15%, working pressure is 1.5-6.5MPa, and its ability mass concentration is the sulfuric acid of 15%, can retain sulfuric acid, ferrous ion and titanyl sulfate.
Like this, by the way, in the water purification that second filtering system 600 produces, sulfuric acid concentration is 0.05-10%, ferrous ion concentration is 0-10ppm, the overall rate of recovery is 75-95%, clear liquid acidity after nanofiltration membrane produces water and the hydration also of reverse osmosis membrane product maintains proper range, both comparatively can not intake low because of using reverse osmosis membrane completely, also comparatively can not intake high because of using nanofiltration membrane completely, nanofiltration membrane produces the clear liquid ferrous ion concentration after water and the hydration also of reverse osmosis membrane product lower than design load, thus can meet washing water requirement completely.
In addition, in order to economize on resources, the soft water water yield being supplemented to water washing cycles tank 400 is equal with the water yield that the second filtering system 600 is disposed to acid-restoring plant 200.
Acid-restoring plant 200, it is connected with filter 100 and the second filtering system 600 respectively, and it is the waste water for reclaiming after filter 100 and the filtration of the second filtering system 600.
See Fig. 2 and Fig. 3, here is the washing process for above-mentioned water wash system, and this washing process comprises the steps:
(1) hydrolyzation material is put into filter 100 to filter;
(2) filter cake that will fully squeeze out in hydrolyzation material containing the concentrated acid in metatitanic acid and metal ion of filter 100, filter cake is transported in hollander 300 by filter, and filter 100 is delivered in acid-restoring plant 200 by extruding remaining spent acid in hydrolyzation material;
(3) add in hollander 300 together with filter cake that soft water and filter 100 transport and pull an oar, and by the slurry transferring after making beating to water washing cycles tank 400;
(4) material of pulling an oar enters water washing cycles tank 400, the soft water used during washing first also enters water washing cycles tank 400, making beating material and the foreign ion of pulling an oar in material are diluted, then by the first filtering system 500, water filtration is gone out, foreign ion in such making beating material just reduces, if soft water continues to enter, the first filtering system 500 clear liquid is constantly discharged, foreign ion in making beating material will constantly reduce, until be reduced to qualified standard;
(5) wash qualified washing material and be transported to the first filtering system 500, after conveying, next batch making beating material enters water washing cycles tank 400 and continues washing;
Metatitanic acid particle entrapment in the slurry that water washing cycles tank 400 transports by (6) first filtering systems 500 and washing water, again be delivered in water washing cycles tank 400 by what retain containing metatitanic acid particle dope, water washing cycles tank 400 is to again washing containing metatitanic acid particle dope of retaining, and the clear liquid after filtration is delivered in the second filtering system 600 and again filters by the first filtering system 500;
A clear liquid part for (7) first filtering systems 500 is delivered to reverse osmosis membrane through high-pressure pump and is filtered, a part enters nanofiltration membrane row and filters, reverse osmosis can retain sulfuric acid, ferrous, titanyl sulfate, nanofiltration only retains ferrous iron and titanyl sulfate, clear liquid acidity after nanofiltration membrane produces water and the hydration also of reverse osmosis membrane product maintains proper range, both comparatively can not intake low because of using reverse osmosis membrane completely, also comparatively can not intake high because of using nanofiltration membrane completely, nanofiltration membrane produces the clear liquid ferrous ion concentration after water and the hydration also of reverse osmosis membrane product lower than design load, meet washing water requirement completely, clear liquid is delivered to water washing cycles tank 400 and continues to use by the second filtering system 600, dope after filtration is delivered to acid-restoring plant 200 reclaim.
(8) add in water washing cycles tank 400 in 10-60 minute before washing terminates and add SYNTHETIC OPTICAL WHITNER on a small quantity or not, the dosage of SYNTHETIC OPTICAL WHITNER is the 0-50% of former technique dosage.
When first making beating material enters water washing cycles tank 400, the second filtering system 600 does not produce water, so washing must use soft water first, when by the time the second filtering system 600 has product water, can reduce soft water consumption.
From water balance, the second filtering system 600 will produce dope, and it is qualified that the clear liquid that the second filtering system 600 produces is not enough to making beating material to be washed till, so making beating material should supplement a part of soft water when washing.
If washed with soft water all the time, the acid concentration in accept can be lower than the acid concentration in making beating material; If washed with the clear liquid of the second filtering system 600, the acid concentration in accept can than only high by the acid concentration in the accept of soft water washing.So introduce reverse osmosis membrane to remove a part of sulfuric acid, to maintain the acid concentration in qualified washing material.
Here is a specific embodiment for above-mentioned technique:
Hydrolyzation material produces the filter cake that solid content is 65% after filter 100 filters, and the making beating material that hollander 300 and oxygen-free water are mixed with solid content 18% delivered to immediately by filter cake; The precision that making beating material enters the employing of water washing cycles tank 400, first filtering system 500 is 500 nanometer tube type filter membrances, and transmembrane pressure is 0.2MPa.Dope containing metatitanic acid after first filtering system 500 processes returns water washing cycles tank 400, and the second filtering system 600 delivered to by clear liquid.In order to reach in the rear accept of washing, ferrous content is lower than 10ppm, and wash one and terminate in water washing cycles tank 400, to add zinc powder in first 25 minutes, dosage is 1.5 ‰ (to material titaniums).The nanofiltration membrane working pressure of the second filtering system 600 is 2MPa, and reverse osmosis working pressure is 3.5MPa, and the clear liquid ferrous ions concentration after two-stage nanofiltration membrane and the process of two steps ro film is 1.2mg/L, and sulfuric acid content is 0.5%.This clear liquid is sent to water washing cycles tank 400 and uses as washing water.The dope amount that second filtering system 600 produces is 8.5% of the first filtering system 500 flooding quantity.
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (6)
1. an efficient sulfuric acid method titanium pigment water wash system, is characterized in that, described sulfuric acid method titanium pigment water wash system comprises:
Filter;
Acid-restoring plant, described acid-restoring plant is connected with the spent acid discharge port of filter;
Hollander, described hollander is connected with the filter cake discharge port of filter;
Water washing cycles tank, described water washing cycles tank is communicated with hollander;
First filtering system, described first filtering system is communicated with water washing cycles tank;
Second filtering system, described second filtering system is communicated with acid-restoring plant with water washing cycles tank, the first filtering system respectively.
2. the efficient sulfuric acid method titanium pigment water wash system of one according to claim 1, is characterized in that, described first filtering system is cross-current type microfiltration membrane, and the precision of described cross-current type microfiltration membrane is 50-1000 nanometer, and transmembrane pressure is 0.05-0.8MPa.
3. the efficient sulfuric acid method titanium pigment water wash system of one according to claim 1, it is characterized in that, described second filtering system is made up of nanofiltration membrane and reverse osmosis membrane, described nanofiltration membrane is 85-99.8% to the rejection of ferrous ion, be 80-99.8% to the rejection of titanyl sulfate, resistance to sulfuric acid concentration is 0-30%, working pressure is 1.0-6.5MPa, described reverse osmosis membrane is 85-99.8% to the rejection of ferrous ion, be 80-99.8% to the rejection of titanyl sulfate, be 85-99.8% to the rejection of sulfuric acid, resistance to sulfuric acid concentration is 0-15%, working pressure is 1.5-6.5MPa.
4. the efficient sulfuric acid method titanium pigment water wash system of one according to claim 1, is characterized in that, described water washing cycles tank is encloses container, and described water washing cycles tank adopts nonoxidizing gas sealing, and to maintain tank body internal pressure be 1-10KPa.
5. the efficient sulfuric acid method titanium pigment water wash system of one according to claim 1, is characterized in that, the soft water adopted in described hollander and washing supplementary feed are all oxygen-free water.
6. an efficient sulfuric acid method titanium pigment washing process, is characterised in that, this washing process comprises the steps:
(1) hydrolyzation material is put into filter to filter;
(2) filter cake that will fully squeeze out in hydrolyzation material containing the concentrated acid in metatitanic acid and metal ion of filter, filter cake is transported in hollander by filter, and filter is delivered in acid-restoring plant by extruding remaining spent acid in hydrolyzation material;
(3) add in hollander together with filter cake that soft water and filter transport and pull an oar, and by the slurry transferring after making beating to water washing cycles tank;
(4) material of pulling an oar enters water washing cycles tank, the soft water used during washing first also enters water washing cycles tank, making beating material and the foreign ion of pulling an oar in material are diluted, then by the first filtering system, water filtration is gone out, foreign ion in such making beating material just reduces, if soft water continues to enter, the first filtering system clear liquid is constantly discharged, foreign ion in making beating material will constantly reduce, until be reduced to qualified standard;
(5) wash qualified washing material and be transported to the first filtering system, after conveying, next batch making beating material enters water washing cycles tank and continues washing;
Metatitanic acid particle entrapment in the slurry that water washing cycles tank transports by (6) first filtering systems and washing water, again be delivered in water washing cycles tank by what retain containing metatitanic acid particle dope, water washing cycles tank is to again washing containing metatitanic acid particle dope of retaining, and the clear liquid after filtration is delivered in the second filtering system and again filters by the first filtering system;
A clear liquid part for (7) first filtering systems is delivered to reverse osmosis membrane through high-pressure pump and is filtered, a part enters nanofiltration membrane row and filters, reverse osmosis can retain sulfuric acid, ferrous, titanyl sulfate, nanofiltration only retains ferrous iron and titanyl sulfate, clear liquid acidity after nanofiltration membrane produces water and the hydration also of reverse osmosis membrane product maintains proper range, both comparatively can not intake low because of using reverse osmosis membrane completely, also comparatively can not intake high because of using nanofiltration membrane completely, nanofiltration membrane produces the clear liquid ferrous ion concentration after water and the hydration also of reverse osmosis membrane product lower than design load, meet washing water requirement completely, clear liquid is delivered to water washing cycles tank and continues to use by the second filtering system, dope after filtration is delivered to acid-restoring plant reclaim.
(8) add in water washing cycles tank in 10-60 minute before washing terminates and add SYNTHETIC OPTICAL WHITNER on a small quantity or not, the dosage of SYNTHETIC OPTICAL WHITNER is the 0-50% of former technique dosage.
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