CN103043714B - Tubular membrane device applicable to titanium dioxide washing and washing method - Google Patents
Tubular membrane device applicable to titanium dioxide washing and washing method Download PDFInfo
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- CN103043714B CN103043714B CN201210592264.1A CN201210592264A CN103043714B CN 103043714 B CN103043714 B CN 103043714B CN 201210592264 A CN201210592264 A CN 201210592264A CN 103043714 B CN103043714 B CN 103043714B
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Abstract
The invention relates to a tubular membrane device applicable to titanium dioxide washing and a washing method. The tubular membrane device structurally and mainly comprises storage tanks, pumps, a membrane separation system, a bleaching kettle and the like. The tubular membrane device adopts a plural-stage new washing method and uses the post-stage clear liquid as the water for pre-stage washing. The tubular membrane device comprises a membrane concentration system and multiple groups of membrane washing systems. The washing method comprises the following steps: enabling the metatitanic acid serum after hydrolyzation to directly enter the membrane concentration system, removing a large part of sulfuric acid of the metatitanic acid serum and enabling the metatitanic acid serum to enter a No.1 membrane washing system; adding water to wash metatitanic acid, and when the content of Fe<2+> in the No.1 membrane washing system is up to a certain degree, enabling the metatitanic acid serum to enter the bleaching kettle for bleaching; and after bleaching, enabling the metatitanic acid serum to enter a No.2 membrane washing system and adding water to continue washing till the content of Fe<2+> in the No.2 membrane washing system meets the requirement. According to the invention, a membrane separation method is adopted, so that contents of impurities in metatitanic acid particles are effectively reduced, the quality of the titanium dioxide product is improved, the retention rate of solid particles is high, the cost is low, the operation is simple, and the water consumption is low.
Description
Technical field
The present invention relates to a kind of device and method, particularly relate to a kind of defect of existing for existing titanium dioxide washing room device and technique and provide a kind of totally enclosed, treatment capacity large, titanium dioxide and water lotion separating effect stable be applied to titanium dioxide washing tubular type film device and washing methods.
Background technology
Titanium dioxide, as a kind of white inorganic pigment, has nontoxic, best whiteness and luminance brightness, is a kind of white pigment that performance is best in the world at present, is widely used in the industries such as coating, plastics, papermaking, printing-ink, chemical fibre, rubber and makeup.Production By Sulfuric Acid Process Technology adopts the vitriol oil of heat to decompose through the selected ilmenite pulverized, and take iron powder as the vitriol mixing solutions that reductive agent obtains titanium, ferrous iron and other metal, is commonly called as titanium liquid.Be under the induction of nucleus at titanic acid colloids, dense titanium liquid minute-pressure hydrolysis generated hydrated titanium dioxide, is commonly called as metatitanic acid.Metatitanic acid after Ficus caricaL is through filtering, and the obtained coarse particles titanium dioxide of calcining, through pulverizing, packing and obtain titanium dioxide.
Various soluble impurity in industrial employing filter cake washing method removing metatitanic acid, along with the rising of water washing process pH.Iron is adsorbed in metatitanic acid with the form of ferric hydroxide precipitate and is difficult to removing.During high-temperature calcination, ironic hydroxide is transformed into the red iron oxide with microlitic structure identical with rutile titanium dioxide type, when the content of iron is higher than 30 × 10
-3when ‰, rutile titanium dioxide presents yellow, and iron level is higher than 90 × 10
-3when ‰, the whiteness of anatase titanium dioxide can be affected.The iron of trace can form active target spot, affects the performance of titanium dioxide as pigment.In order to can Fe be removed
2+, after also needing metatitanic acid filter cake to pull an oar, add the vitriol oil and reductive agent carries out secondary or repeatedly washes.
Industrial general employing leaf-type vacuum filter filters, and material forms filter cake on leaf filter, slings into water washing trough and washes.Shortcoming be filter cake thickness need control, excessively thin cause production efficiency reduce and washing time precipitation by metallic ion accelerate; Too thick, cause filter cake crack performance, effect is familiar with in impact, if adjacent filter cake links together, then and cannot washes clean.And because filter cloth precision is lower, in the filtrate after filtering and washing, also have metatitanic acid particle, cause reclaiming load heavier.
Industrial also have employing tubular filter to filter, and equally, filter containing metatitanic acid particle in initial stage filtrate, and the shortcoming of tubular filter is, is difficult to maintenance when filter cloth breaks.
Industrial also have the method for employing whizzer to wash, whizzer each out be containing 40%-50% containing stereoplasm material, because wherein wrap up by sulfate ion, therefore need through making beating washing repeatedly, operation labour intensity is large, and in washings, solid content reaches 4%-5%, larger on production cost impact, and water loss is large, the later stage also needs to recycle a large amount of plain boiled water produced, and investment is large.
This filter type forming filter cake also makes being cross-linked with each other of metatitanic acid ion agglomerating, a small amount of Fe (OH)
3with a small amount of Fe (OH)
2easily on metatitanic acid particle, form ol bridge, comparatively crossflow membrane filtration system is lower for separation efficiency.
Industrial employing CN strainer concentrates the spent acid that the plain boiled water of washing generation and press filtration produce, and existence is taken up an area large, and facility investment is high, the problem of metatitanic acid particle loss, and needs not timing to change filler.
Be used alone membrane separation unit when carrying out washing and filtering, separating effect is better, but initial sulfuric acid concentration is higher, causes the subsequent wash water yield comparatively large, and is not easy to the recovery of sulfuric acid.
Summary of the invention
For the problems referred to above, main purpose of the present invention is to provide a kind of defect of existing for existing titanium dioxide washing room device and technique and provides a kind of totally enclosed, treatment capacity large, titanium dioxide and water lotion separating effect stable be applied to titanium dioxide washing tubular type film device and washing methods.
One is applied to titanium dioxide washing tubular type film device, and described device adopts plural level cover to wash mode, and rear class clear liquid is served as prime bath water, and described device comprises membrane concentration system and plural groups film washing system.
In specific embodiment of the invention process, described membrane concentration system comprises membrane concentration system storage tank, recycle pump and membrane concentration assembly, and described film washing system is two groups,
Wherein first group comprises: No. 1 film washing system storage tank, No. 1 film washing system assembly, No. 1 recycle pump;
Second group comprises: No. 2 film washing system storage tanks, No. 2 film washing system assemblies, No. 2 recycle pumps, be also provided with bleaching still between two groups of film washing systems;
Described recycle pump is arranged on the pipeline between membrane concentration system storage tank and membrane concentration assembly;
Described No. 1 recycle pump is arranged on the pipeline between No. 1 film washing system storage tank and No. 1 film washing system assembly;
Described No. 2 recycle pumps are arranged on the pipeline between No. 2 film washing system storage tanks and No. 2 film washing system assemblies;
Pipeline between described bleaching still and second group of film washing system is also provided with material-handling pump.
Utilize above-mentioned application of installation in a washing methods for titanium dioxide, described method comprises the steps:
A: the hydrolyzed solution after hydrolysis is directly entered membrane concentration system, is concentrated into the 1-4 of initial value doubly by material;
B: adopt plural level film washing system cover to wash mode, concrete progression is more than 2 grades or 2 grades, rear class is washed clear liquid and is used for prime washing water, rear class washing adds pure water, and it is fewer that the more multiplex water yield of progression washed by cover;
C: can be used for the clear liquid water outlet that prime cover washes in water washing process and enter clear liquid storage tank respectively, enter material storage tank through pump or flow by gravity, as bath water washing prime metatitanic acid slurry;
D: when washing is to Fe in system
2+content, when 600-700ppm, enters the bleaching of bleaching still, has bleached rear continuation washing to Fe
2+content reaches requirement;
E: wash qualified after metatitanic acid dope enter follow-up drying section;
In specific embodiment of the invention process, in described membrane concentration system and No. 1 film washing system, isolated clear liquid is different according to acid concentration in waste liquid, the desulfuration acid subsequent disposal that concentration is higher, reclaims this part of sulfuric acid; The part that concentration is lower goes wastewater treatment or for tail gas absorption.
In specific embodiment of the invention process, described membrane concentration system and film washing system mould material used are acidproof pvdf membrane pipe, inorganic ceramic film pipe or silicon carbide film pipe, and film surface apertures is 0.01-1.0 μm.
In specific embodiment of the invention process, film washing system and membrane concentration system are the acidproof liner PTFE structure of protection against corrosion.
In specific embodiment of the invention process, setting metatitanic acid washs in film separating system and waste acidity recovery film separating system, and when adopting constant rate filtration, film device pressure reduction starts back flushing more than during 0.2MPa; When adopting constant pressure filtration, when film device flux drops to set(ting)value, start back flushing, use pure water as the material of back flushing.
In specific embodiment of the invention process, the recoil pressure reduction in backwash process is 0.1-0.5MPa.
In specific embodiment of the invention process, in filtration procedure, crossflow velocity is set as 2-5ms
-1, transmembrane pressure is set as 0.1-0.3MPa.
In specific embodiment of the invention process, at bleachery, available zinc powder, aluminium powder, titanous are bleached.
Positive progressive effect of the present invention is: the present invention and existing similar be applied to titanium dioxide washing tubular type film device and washing methods compare, film separating system of the present invention is closed, can not introduce other impurity; Tubular membrane clear liquid lateral flux format high throughput is large, and titanium dioxide and water lotion separating effect are stablized, and titanium dioxide particle entrapment rate can reach more than 99%; Tubular membrane filtering system is simple to operate, and technical process is short, and level of automation is high, saves labor force, reduces costs investment; Cleaning interval is long, and after cleaning, tubular membrane flux recovery rate is high, and cleaning is simple, and the recovery rate of flux can reach more than 90%.
The present invention adopts the mode of membrane sepn, can effectively reduce foreign matter content in titanium dioxide particle, improves titanium dioxide product quality; Catching, solid particles rate is high, reduces costs; Operation can control automatically, simple to operate, and labour intensity is low; By water jacket mode, reduce water consumption, processing power is large, less investment; The recovery of spent acid can improve reclaim(ed) sulfuric acid quality, improves titanium dioxide output.
Accompanying drawing explanation
Fig. 1 is the FB(flow block) being applied to titanium dioxide washing tubular type film device and washing methods provided by the invention.
Embodiment
Present pre-ferred embodiments is provided, to describe technical scheme of the present invention in detail below in conjunction with accompanying drawing.
Fig. 1 is the FB(flow block) being applied to titanium dioxide washing tubular type film device and washing methods provided by the invention.As shown in Figure 1: device of the present invention adopts plural level cover to wash mode, and rear class clear liquid is served as prime bath water, described device comprises membrane concentration system and plural groups film washing system.
Particularly, membrane concentration system comprises membrane concentration system storage tank 1, recycle pump 2 and membrane concentration assembly 3, and described film washing system is two groups,
Wherein first group comprises: No. 1 film washing system storage tank 4, No. 1 film washing system assembly 6, No. 1 recycle pump 5;
Second group comprises: be also provided with bleaching still 7 between No. 2 film washing system storage tanks 9, No. 2 film washing system assemblies 11, No. 2 recycle pumps 10, two groups of film washing systems;
Recycle pump 2 is arranged on the pipeline between membrane concentration system storage tank 1 and membrane concentration assembly 3;
No. 1 recycle pump 5 is arranged on the pipeline between No. 1 film washing system storage tank 4 and No. 1 film washing system assembly 6;
No. 2 recycle pumps 10 are arranged on the pipeline between No. 2 film washing system storage tanks 9 and No. 2 film washing system assemblies 11;
Pipeline between bleaching still 7 and second group of film washing system is also provided with material-handling pump 8.
Washing methods provided by the invention specifically comprises the steps:
A: the hydrolyzed solution after hydrolysis is directly entered membrane concentration system, is concentrated into the 1-4 of initial value doubly by material;
B: adopt plural level film washing system cover to wash mode, concrete progression is more than 2 grades or 2 grades, rear class is washed clear liquid and is used for prime washing water, rear class washing adds pure water, and it is fewer that the more multiplex water yield of progression washed by cover;
C: can be used for the clear liquid water outlet that prime cover washes in water washing process and enter clear liquid storage tank respectively, enter material storage tank through pump or flow by gravity, as bath water washing prime metatitanic acid slurry;
D: when washing is to Fe in system
2+content, when 600-700ppm, enters the bleaching of bleaching still, has bleached rear continuation washing to Fe
2+content reaches requirement;
E: wash qualified after metatitanic acid dope enter follow-up drying section;
Below specific embodiment:
Example 1: titanium dioxide washing workshop section washs, concentrates.
In the process of current domestic use Production By Sulfuric Acid Process nano titanium oxide, the a large amount of foreign ion of easy generation, impurity ion content is too high, the quality of nano-titanium dioxide powder can be affected, therefore need to wash to titanium dioxide the foreign ion removed wherein, and conventional water wash method water loss is large, labour intensity is high.Select membrane separation process, concentrate titanium dioxide particle, dilute washing, remove foreign ion effective, washing water consumption is few, and labour intensity is low.
Hydrolyzed solution after hydrolysis directly enters membrane concentration system storage tank 1, be delivered to membrane concentration assembly 3 through recycle pump 2 and carry out high precision cross flow filter, clear liquid enters waste acidity recovery workshop section, after material being concentrated 1-4 times, enter No. 1 film washing system storage tank 4 and be diluted with water to finite concentration, be delivered to No. 1 film washing system assembly 6 through No. 1 recycle pump 5 and carry out high precision cross flow filter, clear liquid enters downstream section, repeats above-mentioned steps until Fe in system
2+content is at 600-700ppm, after enter bleaching still bleaching, add suitable reductive agent and sulfuric acid, No. 2 film washing system storage tanks 9 are delivered to through material-handling pump 8 after bleaching completely, be diluted with water to finite concentration, be delivered to No. 2 film washing system assemblies through No. 2 recycle pumps 10 and carry out high precision cross flow filter, clear liquid is collected into corresponding storage tank for prime water scouring water, repeats until Fe in system
2+content at about 40ppm, after enter Ficus caricaL and calcining workshop section.
The present invention and existing similar be applied to titanium dioxide washing tubular type film device and washing methods compare, film separating system of the present invention is closed, can not introduce other impurity; Tubular membrane clear liquid lateral flux format high throughput is large, and titanium dioxide and water lotion separating effect are stablized, and titanium dioxide particle entrapment rate can reach more than 99%; Tubular membrane filtering system is simple to operate, and technical process is short, and level of automation is high, saves labor force, reduces costs investment; Cleaning interval is long, and after cleaning, tubular membrane flux recovery rate is high, and cleaning is simple, and the recovery rate of flux can reach more than 90%.
The present invention adopts the mode of membrane sepn, can effectively reduce foreign matter content in titanium dioxide particle, improves titanium dioxide product quality; Catching, solid particles rate is high, reduces costs; Operation can control automatically, simple to operate, and labour intensity is low; By water jacket mode, reduce water consumption, processing power is large, less investment; The recovery of spent acid can improve reclaim(ed) sulfuric acid quality, improves titanium dioxide output.
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; these changes and improvements all fall in the claimed scope of the invention, and application claims protection domain is defined by appending claims and equivalent thereof.
Claims (5)
1. the washing methods of a titanium dioxide, device used adopts plural level cover to wash mode, rear class clear liquid is served as prime bath water, described device comprises membrane concentration system and plural groups film washing system, described membrane concentration system comprises membrane concentration system storage tank, recycle pump and membrane concentration assembly, and described recycle pump is arranged on the pipeline between membrane concentration system storage tank and membrane concentration assembly; Described film washing system is two groups,
Wherein first group comprises: No. 1 film washing system storage tank, No. 1 film washing system assembly, No. 1 recycle pump;
Second group comprises: No. 2 film washing system storage tanks, No. 2 film washing system assemblies, No. 2 recycle pumps, be also provided with bleaching still between two groups of film washing systems;
Described No. 1 recycle pump is arranged on the pipeline between No. 1 film washing system storage tank and No. 1 film washing system assembly;
Described No. 2 recycle pumps are arranged on the pipeline between No. 2 film washing system storage tanks and No. 2 film washing system assemblies;
Pipeline between described bleaching still and second group of film washing system is also provided with material-handling pump, it is characterized in that: described method comprises the steps:
A: the hydrolyzed solution after hydrolysis is directly entered membrane concentration system, is concentrated into the 1-4 of initial value doubly by material;
B: adopt plural groups film washing system cover to wash mode, concrete progression is more than 2 grades or 2 grades, rear class is washed clear liquid and is used for prime washing water, and rear class washing adds pure water, it is fewer that the more multiplex water yield of progression washed by cover;
C: can be used for the clear liquid water outlet that prime cover washes in water washing process and enter clear liquid storage tank respectively, enter material storage tank through pump or flow by gravity, as bath water washing prime metatitanic acid slurry;
D: when washing is to Fe in system
2+content, when 600-700ppm, enters the bleaching of bleaching still, has bleached rear continuation washing to Fe
2+content reaches requirement;
E: wash qualified after metatitanic acid dope enter follow-up drying section;
Recoil pressure reduction in backwash process is 0.1-0.5MPa;
In filtration procedure, crossflow velocity is set as 2-5ms
-1, transmembrane pressure is set as 0.1-0.3MPa.
2. washing methods according to claim 1, is characterized in that: described membrane concentration system and film washing system mould material used are acidproof pvdf membrane pipe, inorganic ceramic film pipe, and film surface apertures is 0.01-1.0 μm.
3. washing methods according to claim 1, is characterized in that: film washing system and membrane concentration system are the acidproof liner PTFE structure of protection against corrosion.
4. washing methods according to claim 1, is characterized in that: setting metatitanic acid washs in film separating system and waste acidity recovery film separating system, and when adopting constant rate filtration, film device pressure reduction starts back flushing more than during 0.2MPa; When adopting constant pressure filtration, when film device flux drops to set(ting)value, start back flushing, use pure water as the material of back flushing.
5. washing methods according to claim 1, is characterized in that: at bleachery, and available zinc powder, aluminium powder, titanous are bleached.
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| CN103043714B true CN103043714B (en) | 2015-05-27 |
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| CN104276600B (en) * | 2014-09-16 | 2016-05-18 | 上海安赐环保科技股份有限公司 | A kind of device and method that is applied to the washing of preparing titanium white through chlorination process powder treatment and finishing section |
| CN106587121A (en) * | 2016-12-21 | 2017-04-26 | 上海安赐环保科技股份有限公司 | Water washing device and water washing method applied to washing process of aluminum hydroxide powder |
| CN108658270A (en) * | 2017-11-27 | 2018-10-16 | 江苏久吾高科技股份有限公司 | A kind of processing method and processing device of titanium white production waste water |
| CN109092060A (en) * | 2018-08-24 | 2018-12-28 | 中国科学院青海盐湖研究所 | A kind of solid-liquid continuously washs and isolated method and system |
| CN109011819A (en) * | 2018-08-24 | 2018-12-18 | 中国科学院青海盐湖研究所 | A kind of automation, the method and system that continuously separate of serialization solid-liquid |
| CN109133124A (en) * | 2018-08-24 | 2019-01-04 | 中国科学院青海盐湖研究所 | A kind of magnesium hydroxide continuously washs and isolated method and system |
| CN109045841A (en) * | 2018-08-24 | 2018-12-21 | 中国科学院青海盐湖研究所 | A kind of automation solid-liquid continuously washs and isolated method and system |
| CN109133163A (en) * | 2018-10-25 | 2019-01-04 | 上海安赐环保科技股份有限公司 | A kind of novel sulfuric acid method titanium pigment washing process and system |
| CN111874945B (en) * | 2020-08-03 | 2022-08-16 | 上海安赐环保科技股份有限公司 | Sulfuric acid process titanium dioxide washing system, purification system and process |
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| CN1170775C (en) * | 2002-09-29 | 2004-10-13 | 南京工业大学 | Membrane-integrated hydrothermal reaction ultrafine nano-titanium dioxide production method |
| CN1248969C (en) * | 2003-10-28 | 2006-04-05 | 南宁一泓环境工程有限公司 | Filterpressing, washing, cleansing processes for manufacturing hydration titania |
| CN102424418A (en) * | 2011-09-08 | 2012-04-25 | 湘潭大学 | Method for continuous filtration and washing of hydrated titanium dioxide |
| CN203079706U (en) * | 2012-12-29 | 2013-07-24 | 上海安赐机械设备有限公司 | Device applied to metatitanic acid washing working section |
| CN103030175B (en) * | 2012-12-29 | 2014-12-31 | 上海安赐机械设备有限公司 | Device and method applied to metatitanic acid washing room |
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Address after: 201201 Shanghai, Pudong New Area Jin Tang Road, No. 2, block B, 145 Patentee after: SHANGHAI ANHORN ENVIRONMENTAL TECHNOLOGY CO., LTD. Address before: 201201 Shanghai, Pudong New Area Jin Tang Road, No. 2, block B, 145 Patentee before: Shanghai Anhorn Mechanical Equipment Co., Ltd. |