CN102424418A - Method for continuous filtration washing of hydrated titanium dioxide - Google Patents
Method for continuous filtration washing of hydrated titanium dioxide Download PDFInfo
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- CN102424418A CN102424418A CN2011102643261A CN201110264326A CN102424418A CN 102424418 A CN102424418 A CN 102424418A CN 2011102643261 A CN2011102643261 A CN 2011102643261A CN 201110264326 A CN201110264326 A CN 201110264326A CN 102424418 A CN102424418 A CN 102424418A
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Abstract
The invention discloses a method for continuous filtration washing of hydrated titanium dioxide, which comprises the following steps: filtering hydrated titanium dioxide obtained by hydrolysis to remove most ferrous sulphate, beating to prepare slurry with a certain concentration, continuously adding the slurry into a multistage continuous filtration washing device, adding washing water at the last stage of the continuous filtration washing device. The method has the characteristics of high flux of washing filtration, high washing efficiency, no flocculant addition, less washing water using amount, continuous process operations, and easy realization of automatic control, and the method is also applicable to washing of other fine or superfine particles.
Description
Technical field
The present invention relates to a kind of method of ultra-fine or subparticle continuous filtration washing.Particularly about the continuous filtration washing methods of hydrated titanium dioxide.
Background technology
In the sulfate process titanium dioxide production process, the hydrated titanium dioxide that the titanyl sulfate hydrolysis obtains contains a large amount of impurity such as ferrous sulfate, because the hydrated titanium dioxide particle is superfine, washing and filtering efficient is very low.Commercial run adopts leaf filter to carry out filtration washing mostly, and this method facility investment is big, and labour intensity is big, the washing periodical operation, and detersive efficiency is low, and the washing water loss is big, and washing process white titanium pigment per ton produces 40~70 tons of washess.Chinese patent CN1032925A discloses a kind of continuous washing method and equipment of titanium dioxide hydrates; This method is in order to improve the settling property of hydrated titanium dioxide; Quicken the particulate sedimentation through adding flocculation agent; Because the adding of flocculation agent has reduced the quality of product, therefore do not see in industry and apply.Chinese patent CN1248969C discloses and has a kind ofly adopted membrane sepn washer washing to remove the ferrous sulfate impurity in the hydrated titanium dioxide, and this method is periodical operation, and production efficiency is low, and filtration procedure is unstable.
Summary of the invention
The purpose of this invention is to provide the method that a kind of continuous high-efficient, washing water consume little, as to need not to add flocculation agent hydrated titanium dioxide continuous filtration washing.
The objective of the invention is to realize through following mode:
The hydrated titanium dioxide that hydrolysis obtains is after removing by filter most of ferrous sulfate, and being made into solid content by the making beating of hydrated titanium dioxide suspension-s is 5%~30% slip to be washed; Slip to be washed is continued to have joined the multistage continuous filtration washing device of solid-liquid separation effect; Said continuous filtration washing device is in series by 2~12 grades of continuous filtration washing devices; Describedly wait to wash slip and add at the 1st grade of continuous filtration washing device; Washing is with the last 1 grade adding of clear water at the continuous filtration washer; Washing clear liquid part after the 1st grade of filtration is gone wastewater treatment, and the circulation of another part washing clear liquid is used for the making beating of hydrated titanium dioxide suspension-s, and last 1 grade of washing that obtains is accomplished slip and gone aftertreatment through filtering after concentrating; The washing clear liquid that all the other continuous filtration washers at different levels except that the 1st grade of continuous filtration washing device come out is all reached the last one-level continuous filtration washer as washings through pump step by step; Then following current is mobile step by step for slip, and washing water and slip are counter-current flow between continuous filtration washers at different levels.
The present invention preferably waits to wash slip solid content (being the particulate mass percent concentration) between 30%~50%.
The continuous filtration washing device preferably is made up of 4~10 grades of continuous filtration washing device series connection.
The solid content of slip can change in 5%~30% scope in the continuous filtration washers at different levels.
Every grade of continuous filtration washing device is made up of shurry pump and continous way filter washing equipment except that the 1st grade of continuous filtration washing device; The 1st grade of continuous filtration washing device is made up of the continous way filter washing equipment.
The continuous filtration washing plant is selected from membrane filtration washer, disk filtration washer or plate-sheet-type continuous filtration washing machine etc., and other has the continuous filtration equipment of better filtration washing effect to white titanium pigment.
The continuous filtration washing device also can be the one or more combination in the equipment such as membrane filtration washer, disk filtration washer, plate-sheet-type continuous filtration washing machine.
The contriver is through discovering, clear water with wait that the volume ratio of washing slip is preferably 1~20: 1, most preferably 3~10: 1 o'clock, can obtain good washing and preferable water and combine effect.
The high efficiency filter multistage continuous filtration washing device of the present invention through adopting series combination to form can be realized the continuous filtration washing of hydrated titanium dioxide.Owing to adopt membrane filtration washer, disk filtration washer, plate-sheet-type continuous filtration washing machine, can the less slip of particle separation diameter, have higher filtration flux simultaneously.
The present invention has following beneficial effect; 1, can realize the continuous filtration washing of hydrated titanium dioxide; That washing water consume is little, the more important thing is and need not to add flocculation agent, when effectively improving the settling property of hydrated titanium dioxide, has guaranteed the quality of product preferably; 2, adopt the multi-stage countercurrent filtration washing, realized the counter current contact of washing water and solid materials, can make the consumption of washing water reduce by 30%~70%, greatly reduced the discharging of washing process waste water; 3, the solid content of filtration washing is low, and detersive efficiency is high, and filtration flux is big, has reduced facility investment; 4, the filtration washing process is operate continuously, can realize that whole process controls automatically, has reduced working strength of workers, has greatly improved labour productivity, and this method also is suitable for the filtration washing of other ultra-fine grain, subparticle.
Description of drawings
Accompanying drawing is the schematic flow sheet of 4 grades of continuous filtration washings of the present invention's employing.The increase of washing progression can increase the quantity of continuous filtration washer and the quantity of recycle pump successively like figure behind 3rd level.
Below be the figure number explanation.
1,2,3,4-is respectively the 1st grade, the 2nd grade, 3rd level, the 4th grade of continuous filtration washing device;
5,6,7-is respectively the 2nd grade, 3rd level, the recycle pump of the 4th grade of washing clear liquid (promptly filtrating is as follows);
8,9,10,11-is respectively the 1st grade, the 2nd grade, the filtrate outlet of 3rd level, the 4th grade of continous way filter washing equipment;
The filtrating of the 4th grade of continuous filtration washing device of 12-gets into the circulating line of 3rd level continuous filtration washer;
The filtrating of 13-3rd level continuous filtration washer gets into the circulating line of the 2nd grade of continuous filtration washing device;
The filtrating of the 2nd grade of continuous filtration washing device of 14-gets into the circulating line of the 1st grade of continuous filtration washing device;
The slip connecting tube of the 1st grade of continuous filtration washing device of 15-and the 2nd grade of continuous filtration washing device;
The slip connecting tube of the 2nd grade of continuous filtration washing device of 16-and 3rd level continuous filtration washer;
The slip connecting tube of 17-3rd level continuous filtration washer and the 4th grade of continuous filtration washing device;
The slurry outlet of the 4th grade of continous way filter washing equipment of 18-;
The clear water inlet of the 4th grade of continous way filter washing equipment of 19-;
A-slip to be washed;
Slip is accomplished in the B-washing;
C-washs clear liquid;
The D-clear water.
Embodiment
Below in conjunction with embodiment the present invention is further specified, the invention is not restricted to embodiment, its embodiment can be described any mode of summary of the invention.
The metatitanic acid slip that hydrolysis obtains contains titanium oxide 176g/L; Free sulfuric acid 250g/L, ferrous sulfate 120g/L is after removing by filter most ferrous sulfate; Being made into solid content with the clear liquid after 10kg/h water or the 1st grade of filtration is 30% slip; Join the 1st grade of disk filtration washer that is connected into by 4 grades of disk filtration washers continuously, clear water joins the 4th grade of disk filtration washer continuously with 80kg/h, and the filtering clear liquid of back one-level disk filtration washer is reached the last one-level filtration washing device as washings step by step through pump; Then following current is mobile step by step for slip, and washing water and slip are counter-current flow between disk filtration washers at different levels.Most of clear liquid after the 1st grade of disk filtration washer filters goes wastewater treatment, and the circulation of part clear liquid is used for making beating, after further concentrating, goes aftertreatment by the 4th grade of slip that the disk filtration washer comes out.The hydrated titanium dioxide solid phase iron-holder that this method obtains is less than 120ppm.
The metatitanic acid slip that hydrolysis obtains contains titanium oxide 176g/L; Free sulfuric acid 250g/L, ferrous sulfate 120g/L is after removing by filter most ferrous sulfate; Being made into solid content with the clear liquid after 10kg/h water or the 1st grade of filtration is 15% slip; Join the 1st grade of membrane filtration washer that is connected into by 8 grades of membrane filtration washers continuously, clear water joins the 8th grade of membrane filtration washer continuously with 30kg/h, and the filtering clear liquid of back one-level membrane filtration washer is reached the last one-level membrane filtration washer as washings step by step through pump; Then following current is mobile step by step for slip, and washing water and slip are counter-current flow between membrane filtration washers at different levels.Most of clear liquid after the 1st grade of membrane filtration washer filters goes wastewater treatment; The circulation of part clear liquid is used for making beating; After further concentrating, go aftertreatment by the 8th grade of slip that the membrane filtration washer comes out, the hydrated titanium dioxide solid phase iron-holder that this method obtains is less than 50ppm.
The metatitanic acid slip that hydrolysis obtains contains titanium oxide 176g/L; Free sulfuric acid 250g/L, ferrous sulfate 120g/L is after removing by filter most ferrous sulfate; Being made into solid content with the clear liquid after 10kg/h water or the 1st grade of filtration is 20% slip; Join the 1st grade of membrane filtration washer that is in series by 10 grades of membrane filtration washers continuously, clear water joins the 10th grade of membrane filtration washer continuously with 10kg/h, and the filtering clear liquid of back one-level membrane filtration washer is reached the last one-level membrane filtration washer as washings step by step through pump; Then following current is mobile step by step for slip, and washing water and slip are counter-current flow between membrane filtration washers at different levels.Most of clear liquid after the 1st grade of membrane filtration washer filters goes wastewater treatment; The circulation of part clear liquid is used for making beating; After further concentrating, go aftertreatment by the 10th grade of slip that the membrane filtration washer comes out, the hydrated titanium dioxide solid phase iron-holder that this method obtains is less than 80ppm.
The metatitanic acid slip that hydrolysis obtains contains titanium oxide 176g/L; Free sulfuric acid 250g/L; Ferrous sulfate 120g/L; After removing by filter most ferrous sulfate, being made into solid content with the clear liquid after 10kg/h water or the 1st grade of filtration is 5% slip, joins the 1st grade of plate-sheet-type continuous filtration washing machine that is connected into by 6 grades of plate-sheet-type continuous filtration thickners continuously; Clear water joins the 6th grade of plate-sheet-type continuous filtration washing machine continuously with 100kg/h; The filtering clear liquid of back one-level plate-sheet-type continuous filtration washing machine is reached the last one-level plate-sheet-type continuous filtration washing machine as washings step by step through pump, and then following current is mobile step by step for slip, and washing water and slip are counter-current flow between plate-sheet-type continuous filtration washing machines at different levels.Most of clear liquid after the 1st grade of plate-sheet-type continuous filtration washing machine filters goes wastewater treatment; The circulation of part clear liquid is used for making beating; The slip that is come out by the 6th grade of plate-sheet-type continuous filtration washing machine goes aftertreatment after concentrating, the hydrated titanium dioxide solid phase iron-holder that this method obtains is less than 60ppm.
Embodiment 5
The metatitanic acid slip that hydrolysis obtains contains titanium oxide 176g/L; Free sulfuric acid 250g/L, ferrous sulfate 120g/L is after removing by filter most ferrous sulfate; Being made into solid content with the clear liquid after 10kg/h water or the 1st grade of filtration is 10% slip; Join continuously by 1 grade of membrane filtration washer and 4 grades of disk filtration washers or 4 grades of continuous filtration washing devices that the plate-sheet-type strainer is connected into, slip adds at the 1st grade of membrane filtration washer, and clear water joins the 5th grade of disk filtration washer continuously with 80kg/h; The filtering clear liquid of back one-level disk filtration washer is reached the last one-level disk filtration washer as washings step by step through pump; Get into the 1st grade of membrane filtration washer at last, then following current is mobile step by step for slip, and washing water and slip are counter-current flow between continuous filtration washers at different levels.Most of clear liquid after the 1st grade of membrane filtration washer filters goes wastewater treatment, and the circulation of part clear liquid is used for making beating, after further concentrating, goes aftertreatment by the 4th grade of slip that the disk filtration washer comes out.The hydrated titanium dioxide solid phase iron-holder that this method obtains is less than 120ppm.
Claims (8)
1. the method for hydrated titanium dioxide continuous filtration washing, it is characterized in that: the hydrated titanium dioxide that hydrolysis obtains is after removing by filter most of ferrous sulfate, and being made into solid content by the making beating of hydrated titanium dioxide suspension-s is 5%~30% slip to be washed; Slip to be washed is continued to have joined the multistage continuous filtration washing device of solid-liquid separation effect; Said continuous filtration washing device is in series by 2~12 grades of continuous filtration washing devices; Describedly wait to wash slip and add at the 1st grade of continuous filtration washing device; Washing is with the last 1 grade adding of clear water at the continuous filtration washer; Washing clear liquid part after the 1st grade of filtration is gone wastewater treatment, and the circulation of another part washing clear liquid is used for the making beating of hydrated titanium dioxide suspension-s, and last 1 grade of washing that obtains is accomplished slip and gone aftertreatment through filtering after concentrating; The washing clear liquid that all the other continuous filtration washers at different levels except that the 1st grade of continuous filtration washing device come out is all reached the last one-level continuous filtration washer as washings through pump step by step; Then following current is mobile step by step for slip, and washing water and slip are counter-current flow between continuous filtration washers at different levels.
2. method according to claim 1 is characterized in that: the solid content of hydrated titanium dioxide suspension-s is between 30%~50%.
3. method according to claim 1 is characterized in that: the continuous filtration washing device is in series by 4~10 grades of continuous filtration washing devices.
4. according to each described method of claim 1-3, it is characterized in that: every grade of continuous filtration washing device except that the 1st grade of continuous filtration washing device is made up of shurry pump and continous way filter washing equipment; The 1st grade of continuous filtration washing device is made up of the continous way filter washing equipment.
5. method according to claim 4 is characterized in that: said continous way filter washing equipment is selected from membrane filtration washer, disk filtration washer or plate-sheet-type continuous filtration washing machine.
6. method according to claim 4 is characterized in that: the continuous filtration washing device adopts one or both in disk filtration washer, the plate-sheet-type continuous filtration washing machine, makes up with the membrane filtration washer.
7. method according to claim 1 is characterized in that: clear water is 1~20: 1 with the volume ratio of waiting to wash slip.
8. method according to claim 7 is characterized in that: clear water is 3~10: 1 with the volume ratio of waiting to wash slip.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103030175A (en) * | 2012-12-29 | 2013-04-10 | 上海安赐机械设备有限公司 | Device and method applied to metatitanic acid washing room |
CN103043714A (en) * | 2012-12-31 | 2013-04-17 | 上海安赐机械设备有限公司 | Tubular membrane device applicable to titanium dioxide washing and washing method |
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 |
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 |
CN108178188B (en) * | 2018-03-08 | 2020-02-11 | 四川龙蟒钛业股份有限公司 | Method for effectively improving disc filtration efficiency and titanium liquid concentration |
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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CN1032925A (en) * | 1988-11-30 | 1989-05-17 | 核工业部北京第五研究所 | The continuous washing method and apparatus of titanium dioxide hydrates |
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103030175A (en) * | 2012-12-29 | 2013-04-10 | 上海安赐机械设备有限公司 | Device and method applied to metatitanic acid washing room |
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 |
CN103043714A (en) * | 2012-12-31 | 2013-04-17 | 上海安赐机械设备有限公司 | Tubular membrane device applicable to titanium dioxide washing and washing method |
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 |
CN108178188B (en) * | 2018-03-08 | 2020-02-11 | 四川龙蟒钛业股份有限公司 | Method for effectively improving disc filtration efficiency and titanium liquid concentration |
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 |
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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