CN103043714A - 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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- CN103043714A CN103043714A CN2012105922641A CN201210592264A CN103043714A CN 103043714 A CN103043714 A CN 103043714A CN 2012105922641 A CN2012105922641 A CN 2012105922641A CN 201210592264 A CN201210592264 A CN 201210592264A CN 103043714 A CN103043714 A CN 103043714A
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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, relate in particular to a kind of defective that exists 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 are stable is applied to titanium dioxide washing tubular type film device and washing methods.
Background technology
Titanium dioxide is as a kind of white inorganic pigment, has nontoxicly, and best whiteness and luminance brightness are the present best a kind of white pigments of performance in the world, are widely used in the industries such as coating, plastics, papermaking, printing-ink, chemical fibre, rubber and makeup.The Production By Sulfuric Acid Process Technology adopts the vitriol oil decomposition of heat through the ilmenite of selected pulverizing, makes the vitriol mixing solutions of titanium, ferrous iron and other metal take iron powder as reductive agent, is commonly called as titanium liquid.Be under the inducing of nucleus at the titanic acid colloids, dense titanium liquid minute-pressure hydrolysis is generated hydrated titanium dioxide, be commonly called as metatitanic acid.Metatitanic acid after salt is processed is through filtering, and calcining makes coarse particles titanium dioxide, namely gets titanium dioxide through pulverizing, packing.
Industrial employing filter cake washing method is removed various soluble impurities in the metatitanic acid, along with the rising of water washing process pH.Iron is adsorbed in the metatitanic acid with the form of ferric hydroxide precipitate and is difficult to remove.During high-temperature calcination, ironic hydroxide is transformed into the red iron oxide that has with the identical microlitic structure of rutile titanium dioxide type, when the content of iron is higher than 30 * 10
-31 o'clock, rutile titanium dioxide presented yellow, and iron level is higher than 90 * 10
-3, can affect the whiteness of anatase titanium dioxide at 1 o'clock.The iron of trace can form active target spot, affects titanium dioxide as the performance of pigment.In order to remove Fe
2+, also need to carry out secondary or repeatedly washing with adding the vitriol oil and reductive agent after the making beating of metatitanic acid filter cake.
Industrial general employing leaf-type vacuum filter filters, and material forms filter cake at leaf filter, slings and washes into the water washing trough.Shortcoming is that filter cake thickness needs control, excessively thin cause production efficiency to reduce and during washing precipitation by metallic ion accelerate; The too thick filter cake crack performance that then causes, effect is familiar with in impact, if adjacent filter cake links together, then can't washes clean.And because the filter cloth precision is lower, also have the metatitanic acid particle in the filtrate after filtering and washing, it is heavier to cause reclaiming load.
Industrial also have the tubular filter of employing to filter, same, filter in the initial stage filtrate and contain the metatitanic acid particle, and the shortcoming of tubular filter is to be difficult to maintenance when filter cloth breaks.
The industrial method of whizzer that adopts is in addition washed, whizzer each out be contain 40%-50% contain the stereoplasm material, because wherein wrap up by sulfate ion, therefore need to be through making beating washing repeatedly, operation labour intensity is large, and solid content reaches 4%-5% in the washings, larger on the production cost impact, and water loss is large, and the later stage also needs the plain boiled water of a large amount of generations is recycled, and investment is large.
Form this filter type of filter cake also so that being cross-linked with each other of metatitanic acid ion is agglomerating, a small amount of Fe (OH)
3With a small amount of Fe (OH)
2Easily form ol bridge at the metatitanic acid particle, separation efficiency is lower than the crossflow membrane filtration system.
Industrial employing CN strainer concentrates the plain boiled water of washing generation and the spent acid of press filtration generation, and existence is taken up an area large, the facility investment height, and the problem of metatitanic acid particle loss, and need not timing replacing filler.
When using separately membrane separation unit to carry out washing and filtering, separating effect is better, but initial sulfuric acid concentration is higher, causes the subsequent wash water yield larger, 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 defective that exists for existing titanium dioxide washing room device and technique and provides a kind of totally enclosed, treatment capacity large, and titanium dioxide and water lotion separating effect are stable is applied to titanium dioxide washing tubular type film device and washing methods.
A kind of titanium dioxide washing tubular type film device that is applied to, described device adopts plural number level cover to wash mode, and the rear class clear liquid is served as the prime bath water, and described device comprises membrane concentration system and plural groups film washing system.
In specific implementation process of the present invention, 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 also are equipped with the bleaching still between two groups of film washing systems;
Described recycle pump is installed on the pipeline between membrane concentration system storage tank and the membrane concentration assembly;
Described No. 1 recycle pump is installed on the pipeline between No. 1 film washing system storage tank and No. 1 film washing system assembly;
Described No. 2 recycle pumps are installed on the pipeline between No. 2 film washing system storage tanks and No. 2 film washing system assemblies;
On the pipeline between described bleaching still and the second group of film washing system material-handling pump is installed also.
A kind ofly utilize above-mentioned application of installation in the washing methods of titanium dioxide, described method comprises the steps:
A: the hydrolyzed solution after will being hydrolyzed directly enters the membrane concentration system, material is concentrated into 1-4 times of initial value;
B: adopt a plural number level film washing system cover to wash mode, concrete progression is more than 2 grades or 2 grades, rear class is washed clear liquid be used for the prime washing water, and the rear class washing adds pure water, and it is fewer that cover is washed the more multiplex water yield of progression;
C: can be used for the clear liquid water outlet that the prime cover washes in the water washing process and enter respectively the clear liquid storage tank, enter material storage tank through pump or flow by gravity, as bath water washing prime metatitanic acid slurry;
D: when washing Fe to the system
2+Content enters the bleaching of bleaching still when 600-700ppm, continuation was washed to Fe after bleaching was finished
2+Content reaches requirement;
E: the metatitanic acid dope that washs after qualified enters follow-up drying section;
In specific implementation process of the present invention, isolated clear liquid is different according to acid concentration in the waste liquid in described membrane concentration system and No. 1 film washing system, and 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 is used for tail gas to absorb.
In specific implementation process of the present invention, described membrane concentration system and the used mould material of film washing system are acidproof pvdf membrane pipe, and inorganic ceramic film pipe or silicon carbide film pipe, film surface apertures are 0.01-1.0 μ m.
In specific implementation process of the present invention, film washing system and membrane concentration system are the acidproof liner PTFE structure of protection against corrosion.
In specific implementation process of the present invention, to set in metatitanic acid washing film separating system and the spent acid reclamation film separation system, when adopting constant rate filtration, film device pressure reduction begins back flushing when surpassing 0.2MPa; When adopting constant pressure filtration, the film device flux begins back flushing when dropping to set(ting)value, uses pure water as the material of back flushing.
In specific implementation process of the present invention, the recoil pressure reduction in the backwash process is 0.1-0.5MPa.
In specific implementation process of the present invention, crossflow velocity is set as 2-5ms in filtration procedure
-1, transmembrane pressure is set as 0.1-0.3MPa.
In specific implementation process of the present invention, at bleachery, available zinc powder, aluminium powder, titanous bleaching.
Positive progressive effect of the present invention is: the present invention similarly is applied to titanium dioxide washing tubular type film device and washing methods compares with existing, and 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 stable, and titanium dioxide particle rejection can reach more than 99%; The tubular membrane filtering system is simple to operate, and technical process is short, and level of automation is high, and labor savings reduces cost investment; Cleaning interval is long, and tubular membrane flux recovery rate is high after cleaning, and cleans simply, 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 the titanium dioxide particle, improves the titanium dioxide product quality; The catching, solid particles rate is high, reduces cost; Operation can be controlled automatically, and is simple to operate, and labour intensity is low; By the water jacket mode, reduce water consumption, processing power is large, less investment; The recovery of spent acid can improve the reclaim(ed) sulfuric acid quality, improves titanium dioxide output.
Description of drawings
Fig. 1 is the FB(flow block) that is applied to titanium dioxide washing tubular type film device and washing methods provided by the invention.
Embodiment
Provide preferred embodiment of the present invention below in conjunction with accompanying drawing, to describe technical scheme of the present invention in detail.
Fig. 1 is the FB(flow block) that is 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 number level cover to wash mode, and the rear class clear liquid is served as the prime bath water, and described device comprises membrane concentration system and plural groups film washing system.
Particularly, the 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: 6, No. 1 recycle pump 5 of 4, No. 1 film washing system assembly of No. 1 film washing system storage tank;
Second group comprises: bleaching still 7 also is installed between 10, two groups of film washing systems of 11, No. 2 recycle pumps of 9, No. 2 film washing system assemblies of No. 2 film washing system storage tanks;
Recycle pump 2 is installed on the pipeline between membrane concentration system storage tank 1 and the membrane concentration assembly 3;
No. 1 recycle pump 5 is installed 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 installed on the pipeline between No. 2 film washing system storage tanks 9 and No. 2 film washing system assemblies 11;
On the pipeline between bleaching still 7 and the second group of film washing system material-handling pump 8 is installed also.
Washing methods provided by the invention specifically comprises the steps:
A: the hydrolyzed solution after will being hydrolyzed directly enters the membrane concentration system, material is concentrated into 1-4 times of initial value;
B: adopt a plural number level film washing system cover to wash mode, concrete progression is more than 2 grades or 2 grades, rear class is washed clear liquid be used for the prime washing water, and the rear class washing adds pure water, and it is fewer that cover is washed the more multiplex water yield of progression;
C: can be used for the clear liquid water outlet that the prime cover washes in the water washing process and enter respectively the clear liquid storage tank, enter material storage tank through pump or flow by gravity, as bath water washing prime metatitanic acid slurry;
D: when washing Fe to the system
2+Content enters the bleaching of bleaching still when 600-700ppm, continuation was washed to Fe after bleaching was finished
2+Content reaches requirement;
E: the metatitanic acid dope that washs after qualified enters follow-up drying section;
Below be specific embodiment:
Example 1: titanium dioxide washing workshop section washing, concentrated.
In the process of present domestic use Production By Sulfuric Acid Process nano titanium oxide, easily produce a large amount of foreign ions, impurity ion content is too high, can affect the quality of nano-titanium dioxide powder, therefore need to wash to remove wherein foreign ion to titanium dioxide, and conventional method for washing water loss is large, and labour intensity is high.Select membrane separation process, the titanium dioxide particle is concentrated, dilutes washing, it is effective to remove foreign ion, and the washing water consumption is few, and labour intensity is low.
Hydrolyzed solution after the hydrolysis directly enters membrane concentration system storage tank 1, be delivered to membrane concentration assembly 3 through recycle pump 2 and carry out the high precision cross flow filter, clear liquid enters the spent acid recycle section, behind concentrated 1-4 times of material, enter No. 1 film washing system storage tank 4 and thin up to finite concentration, be delivered to No. 1 film washing system assembly 6 through No. 1 recycle pump 5 and carry out the high precision cross flow filter, clear liquid enters downstream section, repeats above-mentioned steps until Fe in the system
2+Content is at 600-700ppm, after enter bleaching still bleaching, add suitable reductive agent and sulfuric acid, bleaching is delivered to film washing system storage tank 9 No. 2 by material-handling pump 8 fully, thin up is to finite concentration, be delivered to No. 2 film washing system assemblies through No. 2 recycle pumps 10 and carry out the high precision cross flow filter, clear liquid is collected into corresponding storage tank for prime washing water, repeats until Fe in the system
2+Content about 40ppm, after enter that salt is processed and calcining workshop section.
The present invention similarly is applied to titanium dioxide washing tubular type film device and washing methods compares with existing, and 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 stable, and titanium dioxide particle rejection can reach more than 99%; The tubular membrane filtering system is simple to operate, and technical process is short, and level of automation is high, and labor savings reduces cost investment; Cleaning interval is long, and tubular membrane flux recovery rate is high after cleaning, and cleans simply, 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 the titanium dioxide particle, improves the titanium dioxide product quality; The catching, solid particles rate is high, reduces cost; Operation can be controlled automatically, and is simple to operate, and labour intensity is low; By the water jacket mode, reduce water consumption, processing power is large, less investment; The recovery of spent acid can improve the reclaim(ed) sulfuric acid quality, improves titanium dioxide output.
More than show and described 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; that describes in above-described embodiment and the 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 the claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. one kind is applied to titanium dioxide washing tubular type film device, it is characterized in that: described device adopts plural number level cover to wash mode, and the rear class clear liquid is served as the prime bath water, and described device comprises membrane concentration system and plural groups film washing system.
2. the titanium dioxide washing tubular type film device that is applied to according to claim 1 is characterized in that: 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 also are equipped with the bleaching still between two groups of film washing systems;
Described recycle pump is installed on the pipeline between membrane concentration system storage tank and the membrane concentration assembly;
Described No. 1 recycle pump is installed on the pipeline between No. 1 film washing system storage tank and No. 1 film washing system assembly;
Described No. 2 recycle pumps are installed on the pipeline between No. 2 film washing system storage tanks and No. 2 film washing system assemblies;
On the pipeline between described bleaching still and the second group of film washing system material-handling pump is installed also.
3. one kind is utilized the described application of installation of claim 1-2 in the washing methods of titanium dioxide, and it is characterized in that: described method comprises the steps:
A: the hydrolyzed solution after will being hydrolyzed directly enters the membrane concentration system, material is concentrated into 1-4 times of initial value;
B: adopt a plural number level film washing system cover to wash mode, concrete progression is more than 2 grades or 2 grades, rear class is washed clear liquid be used for the prime washing water, and the rear class washing adds pure water, and it is fewer that cover is washed the more multiplex water yield of progression;
C: can be used for the clear liquid water outlet that the prime cover washes in the water washing process and enter respectively the clear liquid storage tank, enter material storage tank through pump or flow by gravity, as bath water washing prime metatitanic acid slurry;
D: when washing Fe to the system
2+Content enters the bleaching of bleaching still when 600-700ppm, continuation was washed to Fe after bleaching was finished
2+Content reaches requirement;
E: the metatitanic acid dope that washs after qualified enters follow-up drying section;
4. washing methods according to claim 3 is characterized in that: isolated clear liquid is different according to acid concentration in the waste liquid in described membrane concentration system and No. 1 film washing system, and 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 is used for tail gas to absorb.
5. washing methods according to claim 3, it is characterized in that: described membrane concentration system and the used mould material of film washing system are acidproof pvdf membrane pipe, inorganic ceramic film pipe or silicon carbide film pipe, film surface apertures are 0.01-1.0 μ m.
6. washing methods according to claim 3, it is characterized in that: film washing system and membrane concentration system are the acidproof liner PTFE structure of protection against corrosion.
7. washing methods according to claim 3 is characterized in that: set in metatitanic acid washing film separating system and the spent acid reclamation film separation system, when adopting constant rate filtration, film device pressure reduction begins back flushing when surpassing 0.2MPa; When adopting constant pressure filtration, the film device flux begins back flushing when dropping to set(ting)value, uses pure water as the material of back flushing.
8. washing methods according to claim 3, it is characterized in that: the recoil pressure reduction in the backwash process is 0.1-0.5MPa.
9. washing methods according to claim 3, it is characterized in that: crossflow velocity is set as 2-5ms in filtration procedure
-1, transmembrane pressure is set as 0.1-0.3MPa.
10. washing methods according to claim 3 is characterized in that: at bleachery, and available zinc powder, aluminium powder, titanous bleaching.
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| CN104276600A (en) * | 2014-09-16 | 2015-01-14 | 上海安赐机械设备有限公司 | Device and method applied to washing in post-processing work section of titanium dioxide preparation carried out by adopting chlorination method |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| CN111874945A (en) * | 2020-08-03 | 2020-11-03 | 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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| CN104276600A (en) * | 2014-09-16 | 2015-01-14 | 上海安赐机械设备有限公司 | Device and method applied to washing in post-processing work section of titanium dioxide preparation carried out by adopting chlorination method |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| WO2020082916A1 (en) * | 2018-10-25 | 2020-04-30 | 上海安赐环保科技股份有限公司 | Novel sulfuric acid process titanium oxide water washing process and system |
| CN111874945A (en) * | 2020-08-03 | 2020-11-03 | 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 |
| 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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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. |