CN102101711A - Method for preparing metal polysilicate flocculant - Google Patents
Method for preparing metal polysilicate flocculant Download PDFInfo
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- CN102101711A CN102101711A CN 201010595216 CN201010595216A CN102101711A CN 102101711 A CN102101711 A CN 102101711A CN 201010595216 CN201010595216 CN 201010595216 CN 201010595216 A CN201010595216 A CN 201010595216A CN 102101711 A CN102101711 A CN 102101711A
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- sodium silicate
- aqueous solution
- silicate aqueous
- ferric sulfate
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- Silicates, Zeolites, And Molecular Sieves (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention relates to a method for preparing a metal polysilicate flocculant. At present, the metal polysilicate flocculant is higher in production cost. The method comprises the following steps of: adding green vitriol and waste acid which are produced during production of titanium white into a reaction vessel together with industrial potassium chlorate and stirring to obtain viscous polymeric ferric sulfate; adding water to dilute sodium silicate into sodium silicate aqueous solution, wherein the weight content of SiO2 in the sodium silicate aqueous solution is 2 to 3 percent; adding the waste acid which is produced during the production of the titanium white into the sodium silicate aqueous solution, adjusting pH value of the sodium silicate aqueous solution to be between 3.5 and 4.5, and stirring at normal temperature to obtain polysilicate solution; and adding the polymeric ferric sulfate into the polysilicate solution, uniformly stirring, standing and activating for 10 to 24 hours to obtain the metal polysilicate flocculant. A byproduct produced by the production of the titanium white is low in cost; and the prepared flocculant has the characteristics of high stability, wide application range and good flocculation effect.
Description
Technical field
The invention belongs to water-treatment technology field, relate to a kind of preparation method of polysilics acid metal salt flocculation agent.
Background technology
Polysilics acid metal salt is the novel compound inorganic high molecular flocculant of a class, and it is the poly-silicic acid that grows up on the basis of flocculation agents such as poly-silicic acid and traditional aluminium salt, molysite and the combination product of metal-salt.Because such flocculation agent combines the charge neutrality ability of metal ion simultaneously and the adsorption bridging net of poly-silicic acid is caught effect, compare with traditional inorganic flocculating agent (as Tai-Ace S 150, iron(ic) chloride, ferrous sulfate, polymerize aluminum chloride (PAC) and bodied ferric sulfate (PFS) etc.) and to have the advantage that alumen ustum generates early, alumen ustum is big, settling velocity is fast, under the low-temperature and low turbidity condition, still have flocculating effect preferably, caused the very big concern of field of water treatment.Zhang Li adds inorganic aluminate in the polymeric silicicacid, stirs post curing and makes aluminium silicate polymer flocculation agent (patent of invention CN1162345C); Wu Youming invents a kind of polymerization alkali formula aluminium silicon flocculation agent and preparation method (CN1173893C), adds Tai-Ace S 150 and the formation of sodium hydroxide polyreaction in activated silicic acid; Li Suqin adds ferric sulfate, Tai-Ace S 150, the static slaking 1-2 of sodium tetraborate and days prepares a kind of boracic polymeric aluminium ferrum silicate composite flocculation agent (CN100500589C) in activated silicic acid.Yet the cost of these polysilics acid metal salt flocculation agents is higher.
Summary of the invention
The purpose of this invention is to provide the preparation method that a kind of by product that utilizes titanium white production prepares cheap polysilics acid metal salt flocculation agent.
Titanium dioxide is a kind of inorganic white pigment most widely used, that consumption is maximum, and its output accounts for 80% of world's white pigment ultimate production.In recent years, the yearly capacity of China's titanium white powder has reached 200,000 tons, and wherein the overwhelming majority is to adopt Production By Sulfuric Acid Process.In the Titanium White Production By Sulfuric Acid Process process, 1 ton of white powder product of every production can produce 7～8 tons in 3.5～4.0 tons of by product hydration ferrous sulfate (being commonly called as green vitriol) and spent acid.The composition of spent acid is generally: H
2SO
418～22%, FeSO
45～8%, TiOSO
41～2%, Al
2SO
41.5～2.5%, MgSO
41～2%, TiO
2Deng.These by products if can utilize rightly can not only reduce the environmental pollution degree, and can also improve economic benefit of enterprises.
The concrete steps of the inventive method are as follows:
Step 1. will be produced the green vitriol that produces in the titanium dioxide process and spent acid and industrial Potcrate and be joined in the reaction vessel, stir down at 35～50 ℃ and obtain the heavy-gravity bodied ferric sulfate in 2～3 hours;
The green vitriol that adds and the weight ratio of industrial Potcrate are 0.5～1: 1, and the spent acid of adding and the weight ratio of industrial Potcrate are 1～2: 1;
Step 2. becomes sodium silicate aqueous solution with the water glass thin up, SiO in the sodium silicate aqueous solution
2Weight content be 2～3%; Add to produce the spent acid that produces in the titanium dioxide process at sodium silicate aqueous solution, the pH value of sodium silicate aqueous solution is adjusted to 3.5～4.5, sodium silicate aqueous solution was stirred 10～30 minutes at normal temperatures, promptly obtain gathering silicate solution;
The bodied ferric sulfate that step 3. obtains step 1 joins in the poly-silicate solution, and the static activation in back that stirs promptly got polysilics acid metal salt flocculation agent, SiO in the bodied ferric sulfate of adding and the sodium silicate aqueous solution in 10～24 hours
2Weight ratio be 1～2: 1.
Among the preparation method of polysilics acid metal salt flocculation agent of the present invention, utilized the by product of titanium white production, cheap, simultaneously owing in spent acid, also contain metal ion and TiO such as Al, Ti, Mg
2Micro mist, they have participated in the polymerization of silicic acid, have optimized the structure of polysilics acid metal salt inorganic polymer, and the gained flocculation agent has good stability, and is applied widely, the characteristics that flocculating effect is good.
Embodiment
Further specify the inventive method below in conjunction with embodiment.
Embodiment 1
Preparation polysilics acid metal salt flocculation agent, concrete steps are:
1) respectively with 20 gram green vitriol (FeSO
47H
2O), 40 the gram titanium dioxide spent acid and 40 the gram industrial Potcrate join in the reaction vessel, obtained the heavy-gravity bodied ferric sulfate in 3 hours at 35 ℃ of following stirring reactions;
2) take by weighing 203 gram water glass (Na
2SiO
3, contain 100 gram SiO
2) thin up becomes SiO
2Weight content is 2% sodium silicate aqueous solution, is 3.5 with the pH value of spent acid regulator solution, and normal temperature stirs polymerization down and obtained poly-silicate solution in 10 minutes;
3) get the above-mentioned bodied ferric sulfate of 100 grams and join in the poly-silicate solution, the static activation in back that stirs promptly got the polysilics acid metal salt flocculation agent in 10 hours.
Embodiment 2
Preparation polysilics acid metal salt flocculation agent, concrete steps are:
1) respectively with 50 gram green vitriol (FeSO
47H
2O), 100 the gram titanium dioxide spent acid and 50 the gram industrial Potcrate join in the reaction vessel, obtained the heavy-gravity bodied ferric sulfate in 2 hours at 50 ℃ of following stirring reactions;
2) take by weighing 203 gram water glass (Na
2SiO
3, contain 100 gram SiO
2) thin up becomes SiO
2Weight content is 3% sodium silicate aqueous solution, is 4.5 with the pH value of spent acid regulator solution, and normal temperature stirs polyase 13 down and obtained poly-silicate solution in 0 minute;
3) get the above-mentioned bodied ferric sulfate of 200 grams and join in the poly-silicate solution, the static activation in back that stirs promptly got the polysilics acid metal salt flocculation agent in 24 hours.
Embodiment 3
Preparation polysilics acid metal salt flocculation agent, concrete steps are:
1) respectively with 45 gram green vitriol (FeSO
47H
2O), 90 the gram titanium dioxide spent acid and 60 the gram industrial Potcrate join in the reaction vessel, obtained the heavy-gravity bodied ferric sulfate in 2.5 hours at 45 ℃ of following stirring reactions;
2) take by weighing 473 gram water glass (Na
2SiO
39H
2O contains 100 gram SiO
2) thin up becomes SiO
2Weight content is 2.5% sodium silicate aqueous solution, is 4 with the pH value of spent acid regulator solution, and normal temperature stirs polymerization down and obtained poly-silicate solution in 20 minutes;
3) take by weighing the above-mentioned bodied ferric sulfate of 150 grams and join in the poly-silicate solution, the static activation in back that stirs promptly got the polysilics acid metal salt flocculation agent in 18 hours.
Embodiment 4
Preparation polysilics acid metal salt flocculation agent, concrete steps are:
1) respectively with 30 gram green vitriol (FeSO
47H
2O), 50 the gram titanium dioxide spent acid and 40 the gram industrial Potcrate join in the reaction vessel, obtained the heavy-gravity bodied ferric sulfate in 3 hours at 40 ℃ of following stirring reactions;
2) take by weighing 353 gram water glass (Na
2SiO
35H
2O contains 100 gram SiO
2) thin up becomes SiO
2Weight content is 2% sodium silicate aqueous solution, is 3.5 with the pH value of spent acid regulator solution, and normal temperature stirs polymerization down and obtained poly-silicate solution in 15 minutes;
3) get the above-mentioned bodied ferric sulfate of 120 grams and join in the poly-silicate solution, the static activation in back that stirs promptly got the polysilics acid metal salt flocculation agent in 15 hours.
Embodiment 5
Preparation polysilics acid metal salt flocculation agent, concrete steps are:
1) respectively with 50 gram green vitriol (FeSO
47H
2O), 90 the gram titanium dioxide spent acid and 60 the gram industrial Potcrate join in the reaction vessel, obtained the heavy-gravity bodied ferric sulfate in 2.5 hours at 45 ℃ of following stirring reactions;
2) taking by weighing 206 gram moduluses is 2.4 water glass (Na
2O2.4SiO
2, contain 144 gram SiO
2) thin up becomes SiO
2Weight content is 2.5% sodium silicate aqueous solution, is 4 with the pH value of spent acid regulator solution, and normal temperature stirs polymerization down and obtained poly-silicate solution in 10 minutes;
3) get the above-mentioned bodied ferric sulfate of 200 grams and join in the poly-silicate solution, the static activation in back that stirs promptly got the polysilics acid metal salt flocculation agent in 20 hours.
Claims (1)
1. the preparation method of a polysilics acid metal salt flocculation agent is characterized in that the concrete steps of this method are:
Step (1) will be produced the green vitriol that produces in the titanium dioxide process and spent acid and industrial Potcrate and be joined in the reaction vessel, stir down at 35～50 ℃ and obtain the heavy-gravity bodied ferric sulfate in 2～3 hours;
The green vitriol that adds and the weight ratio of industrial Potcrate are 0.5～1: 1, and the spent acid of adding and the weight ratio of industrial Potcrate are 1～2: 1;
Step (2) becomes sodium silicate aqueous solution with the water glass thin up, SiO in the sodium silicate aqueous solution
2Weight content be 2～3%; Add to produce the spent acid that produces in the titanium dioxide process at sodium silicate aqueous solution, the pH value of sodium silicate aqueous solution is adjusted to 3.5～4.5, sodium silicate aqueous solution was stirred 10～30 minutes at normal temperatures, promptly get and gather silicate solution;
The bodied ferric sulfate that step (3) obtains step (1) joins in the poly-silicate solution, and the static activation in back that stirs promptly got polysilics acid metal salt flocculation agent, SiO in the bodied ferric sulfate of adding and the sodium silicate aqueous solution in 10～24 hours
2Weight ratio be 1～2: 1.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838197A (en) * | 2012-10-09 | 2012-12-26 | 重庆理工大学 | Method for preparing novel composite flocculant PSAFS (poly-silicate aluminum ferrous sulfate) |
| CN103030200A (en) * | 2013-01-09 | 2013-04-10 | 杨祺 | Method for producing poly-silicon rare earth chloride sulfate aluminum iron by using rare earth-containing sludge and electroplated and pickled acid-containing sewage |
| CN103073100A (en) * | 2013-02-08 | 2013-05-01 | 河北大学 | Dextrin-modified polysilicon ferric sulfate composite flocculating agent and preparation method thereof |
| CN104016460A (en) * | 2014-06-26 | 2014-09-03 | 云南梓康廷环保科技有限公司 | Stable polyferrosilite production method |
| CN104085969A (en) * | 2014-07-17 | 2014-10-08 | 广西平果锋华科技有限公司 | Method for preparing compound type multi-element flocculating agent aluminum ferric sulfate chloride polysilicate by utilizing waste acid |
| CN104261529A (en) * | 2014-09-19 | 2015-01-07 | 句容亿格纳米材料厂 | Nano titanium dioxide coating flocculant and preparation method thereof |
| CN104817148A (en) * | 2015-04-10 | 2015-08-05 | 济南大学 | Poly ferro-silicon-titanium coagulant used for treating low-sludge amount water and preparation technology thereof |
| CN107235543A (en) * | 2017-07-17 | 2017-10-10 | 山西大学 | A kind of coagulation method of low temperature muddy water |
| CN108751371A (en) * | 2018-06-20 | 2018-11-06 | 昆明理工大学 | It is a kind of to combine the method for preparing polysilicon acid ferrotianium flocculant and application using titanium plate pickle liquor and iron and steel pickling waste liquid |
| CN110818048A (en) * | 2019-11-25 | 2020-02-21 | 广西大学 | Polysilicate iron/cationic starch composite flocculant and preparation method thereof |
| CN110862131A (en) * | 2019-11-25 | 2020-03-06 | 广西大学 | Method for treating nitrogen and phosphorus-containing wastewater by applying polysilicate iron/cationic starch composite flocculant |
| CN111689559A (en) * | 2020-06-05 | 2020-09-22 | 山西大学 | Preparation method and application of polysilicate ferrotitanium composite flocculant |
| CN112479329A (en) * | 2020-11-17 | 2021-03-12 | 安徽瑞和新材料有限公司 | Preparation method of polysilicate iron composite flocculant |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838197A (en) * | 2012-10-09 | 2012-12-26 | 重庆理工大学 | Method for preparing novel composite flocculant PSAFS (poly-silicate aluminum ferrous sulfate) |
| CN103030200A (en) * | 2013-01-09 | 2013-04-10 | 杨祺 | Method for producing poly-silicon rare earth chloride sulfate aluminum iron by using rare earth-containing sludge and electroplated and pickled acid-containing sewage |
| CN103073100A (en) * | 2013-02-08 | 2013-05-01 | 河北大学 | Dextrin-modified polysilicon ferric sulfate composite flocculating agent and preparation method thereof |
| CN103073100B (en) * | 2013-02-08 | 2014-04-30 | 河北大学 | Dextrin-modified polysilicon ferric sulfate composite flocculating agent and preparation method thereof |
| CN104016460A (en) * | 2014-06-26 | 2014-09-03 | 云南梓康廷环保科技有限公司 | Stable polyferrosilite production method |
| CN104085969B (en) * | 2014-07-17 | 2016-03-30 | 广西平果锋华科技有限公司 | Spent acid is utilized to produce the method for compound polynary flocculant poly silicic acid chloro sulphuric acid ferro-aluminum |
| CN104085969A (en) * | 2014-07-17 | 2014-10-08 | 广西平果锋华科技有限公司 | Method for preparing compound type multi-element flocculating agent aluminum ferric sulfate chloride polysilicate by utilizing waste acid |
| CN104261529A (en) * | 2014-09-19 | 2015-01-07 | 句容亿格纳米材料厂 | Nano titanium dioxide coating flocculant and preparation method thereof |
| CN104817148A (en) * | 2015-04-10 | 2015-08-05 | 济南大学 | Poly ferro-silicon-titanium coagulant used for treating low-sludge amount water and preparation technology thereof |
| CN107235543A (en) * | 2017-07-17 | 2017-10-10 | 山西大学 | A kind of coagulation method of low temperature muddy water |
| CN107235543B (en) * | 2017-07-17 | 2020-09-29 | 山西大学 | Coagulation method of low-temperature turbid water |
| CN108751371A (en) * | 2018-06-20 | 2018-11-06 | 昆明理工大学 | It is a kind of to combine the method for preparing polysilicon acid ferrotianium flocculant and application using titanium plate pickle liquor and iron and steel pickling waste liquid |
| CN110818048A (en) * | 2019-11-25 | 2020-02-21 | 广西大学 | Polysilicate iron/cationic starch composite flocculant and preparation method thereof |
| CN110862131A (en) * | 2019-11-25 | 2020-03-06 | 广西大学 | Method for treating nitrogen and phosphorus-containing wastewater by applying polysilicate iron/cationic starch composite flocculant |
| CN111689559A (en) * | 2020-06-05 | 2020-09-22 | 山西大学 | Preparation method and application of polysilicate ferrotitanium composite flocculant |
| CN112479329A (en) * | 2020-11-17 | 2021-03-12 | 安徽瑞和新材料有限公司 | Preparation method of polysilicate iron composite flocculant |
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Application publication date: 20110622 |