CN101003390A - Method for preparing flocculant of ferric chloride of polysilicon acid - Google Patents
Method for preparing flocculant of ferric chloride of polysilicon acid Download PDFInfo
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- CN101003390A CN101003390A CN 200610013081 CN200610013081A CN101003390A CN 101003390 A CN101003390 A CN 101003390A CN 200610013081 CN200610013081 CN 200610013081 CN 200610013081 A CN200610013081 A CN 200610013081A CN 101003390 A CN101003390 A CN 101003390A
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Abstract
This invention discloses a method for preparing a stable inorganic polymer flocculant, polyferric silicate chloride, from industrial acid-washing wastewater and iron scale by high-speed shearing, and its application in tap water purification. The method comprises: adding certain amounts of HCl and iron scale according to the contents of free acid and iron in industrial acid-washing wastewater, adding oxidant and stabilizer, oxidizing and polymerizing, adjusting the alkalinity with CaO (or MgO, or mixed slurry of Mg(OH)2 and Ca(OH)2) to obtain stable polyferric chloride, adding poly(silicic acid), and polymerizing under high speed shearing to obtain stable polyferric silicate chloride flocculant. The method has such advantages as simple process, mild reaction conditions and low investment, and is environmentally friendly. The prepared polyferric silicate chloride has better effect on tap water purification than polyferric chloride, ferric chloride and other iron-containing flocculant.
Description
Technical field
The present invention mainly adopt in the Iron And Steel Industry production process produce hydrochloric acid pickling waste liquor and iron scale prepare a kind of water treatment agent---PFSC, this flocculation agent is particularly useful for waterworks water supply purification, wastewater treatment, low-temperature and low turbidity water treatment.
Background technology
China's water resources critical shortage is preserved the ecological environment at present, protects national resource, and prevents and remedies pollution and other public hazards, and the task that water supply purification is handled is heavy day by day.The pollution level that the water quality of the former water of water factory is subjected to along with the water source and often changing, the influence of the pollution incident that also is subjected to sometimes happening suddenly.Water factory adopts several different treatment processs simultaneously in order to seek cost-effective treatment effect, and the method that adopts mostly is physical method and physico-chemical process usually.Must adopt the multifunctional inorganic polymeric flocculant to carry out flocculation treatment.Just seem particularly important so develop efficient, nontoxic, cheap flocculation agent.
In the water treatment flocculant that reality is used, mainly be organic polymer and inorganic polymer flocculant two big classes at present.Organic polymer coargulator has advantage efficiently, but mostly has toxicity problem, is subjected to strict restriction in tap water; Traditional aluminium system and iron are the low molecular flocculant of salt, and in use speed of reaction is slow, medicine consumption high and low temperature low-cloudy water treatment effect is not good, and therefore developing the polymeric type inorganic flocculating agent becomes the focus that people pay close attention to gradually.And inorganic polymer flocculant mainly contains polymeric aluminum, polymerization iron two big classes, because aluminum ion potential toxicity, so it has been subjected to certain restriction in drinking water treatment is used.Therefore develop the focus that the molysite flocculation agent becomes research.Use more poly-iron at present and mainly contain bodied ferric sulfate.Its production technology is quite ripe.Poly-ferric chloride is owing to exist stability problem, and not by large-scale production and application.Over nearly 20 years, the inorganic polymer flocculant of the poly-silicic acid class of a new generation occurs successively.
The development of aluminium silicate polymer salt starts from the eighties in 20th century abroad, Canada's Chinese enlightening chemical company has at first been reported succeeding in developing of poly aluminium sulfate silicate (PASS), and in operation in 1991,6,000,000 pounds of annual capacities, after this Britain and Japan have also set up respectively and have produced 20000 tons factory per year.Domestic Recent study and patent are also more.
The development of ferric-polysilicate salt starts from phase early 1990s, Japanology more, and all report with the patent form.Domestic many be feedstock production poly-silicic acid iron sulfate (PFSS) with water glass, sulfuric acid and ferric sulfate.Ferric-polysilicate salt is compared with aluminium silicate polymer salt, and it is fast to have flocking settling speed, and sediment weight is few, advantages such as the pH value is applied widely, safety non-toxic, but in water treatment, usually can stay certain color.And cost is higher.
The flocculation agent of molysite has iron trichloride, bodied ferric sulfate, poly-ferric chloride at present, wherein owing to the unstable of poly-ferric chloride, so occupation rate is very low on market, and the technology of iron trichloride and bodied ferric sulfate comparatively speaking, comparative maturity occupies certain share on market.On the market some poly-ferrosilicon compound inorganic high molecular flocculants have also appearred simultaneously.The bodied ferric sulfate complex manufacturing, and sulfuric acid pickling waste liquid is few at present, and adopting industrial sulphuric acid is that raw materials cost is higher; Though iron trichloride has flocculating effect preferably, the free acid content height, serious to equipment corrosion, the water after the processing often needs to regulate the pH value.
In patent CN1266819A, once reported and prepared poly ferric chloride flocculant agent with spent pickle liquor, this patent need be added iron filings, will regulate basicity with acid at last, the source of iron filings is limited, can produce a certain amount of iron filings in the Iron And Steel Industry, but its surface scribbles one deck slushing oil, intractable as not handling, is directly used before use, can give out irritating smell in the production, bring disadvantageous effect to operating environment.The present invention uses the content that iron scale increases iron, can play good effect equally.In patent CN1210818A, poly-ferric chloride and poly-silicic acid are compound, need produce poly-ferric chloride with iron trichloride, produce polymeric silicicacid more in addition, and production cost is higher, and technology is complicated comparatively speaking.
Summary of the invention
With industrial acid-washed waste liquid and iron scale is main raw material, add a certain amount of hydrochloric acid or iron scale according to free acid content, iron level is reached more than 10%, add a certain amount of oxygenant and stablizer then, make it that oxidation, polyreaction take place 30～70 ℃ of quick down stirrings, when oxidation, polyreaction after 15～60 minutes, make basifier with calcium oxide (or magnesium oxide or magnesium hydroxide calcium hydroxide mixed slurry) and regulate basicity to 10～25%, just can prepare stable polyiron chloride.
(15-35 ℃) adds poly-silicic acid under the room temperature in poly-ferric chloride, makes it that further polymerization takes place under shear conditions, then at 30～50 ℃ of following slaking 0.5～2h.Just can obtain stable PFSC.
The invention has the advantages that:
1, raw material all is the waste in the Iron And Steel Industry production process, belongs to utilization of waste material, turns waste into wealth;
2, good, the quality homogeneous of the PFSC product stability produced of utilization High shear device, excellent property;
3, in water supply purification was handled, its effect all was better than poly-ferric chloride, iron trichloride.
Embodiment
Elaborate below in conjunction with specific embodiments of the invention.
Embodiment 1:
The preparation of poly-ferric chloride: get the 200ml hydrochloric acid pickling waste liquor, add the 4g iron scale, stirring 2.5 hours under the following temperature greater than 60 ℃, after the filtration, adding 10g KClO in filtrate
3, 3.2g KH
2PO
4, 2gCaO stirs and promptly got poly-ferric chloride in 1.5 hours.
The preparation of poly-silicic acid: use the 20g water glass,, promptly get and gather silicic acid with 1: 1 hydrochloric acid of 25ml and 120ml water activation 0.5h.
The preparation of PFSC: poly-silicic acid that will prepare under the high-shear agitation condition and poly-ferric chloride mixing and stirring, 40 ℃ of slaking 1h can make.
Embodiment 2:
The preparation of poly-ferric chloride: get the 500ml hydrochloric acid pickling waste liquor, add the 10g iron scale, stirring 2 hours under the following temperature greater than 70 ℃, after the filtration, adding 25g KClO in filtrate
3, 8g KH
2PO
4, 6g MgO stirs and promptly got poly-ferric chloride in 1.7 hours.
The preparation of poly-silicic acid: use the 50g water glass,, promptly get and gather silicic acid with 1: 1 hydrochloric acid of 75ml and 300ml water activation 0.5h.
The preparation of PFSC: poly-silicic acid that will prepare under the high-shear agitation condition and poly-ferric chloride mixing and stirring, 35 ℃ of slaking 1.5h can make.
Embodiment 3:
The preparation of poly-ferric chloride: get the 500ml hydrochloric acid pickling waste liquor, add the 10g iron scale, stirring 2 hours under the following temperature greater than 70 ℃, after the filtration, adding 25g KClO in filtrate
3, 8g KH
2PO
4, 20g Mg (OH)
2Ca (OH)
2Mixed slurry stirs and promptly got poly-ferric chloride in 1.6 hours.
The preparation of poly-silicic acid: use the 50g water glass,, promptly get and gather silicic acid with 1: 1 hydrochloric acid of 75ml and 300ml water activation 0.5h.
The preparation of PFSC: poly-silicic acid that will prepare under the high-shear agitation condition and poly-ferric chloride mixing and stirring, 45 ℃ of slaking 0.5h can make.
Application example 1:
The turbidity removal that is used for former water with the product for preparing in the above example 1 is tested, and does contrast with poly-ferric chloride, raw water turbidity simultaneously: 44.35NTU, and pH:8.63, water temperature: 18 ℃ of results are as shown in Table 1.
Table 1 poly-ferric chloride (PFC) and PFSC (PFSC) flocculation agent are to former water sample flocculation treatment effect
| PFC | PFSC | ||
| Flocculant dosage (ppm) | Residual turbidity (NTU) | Flocculant dosage (ppm) | Residual turbidity (NTU) |
| 40 | 1.28 | 40 | 1.19 |
| 50 | 1.14 | 50 | 0.98 |
| 60 | 1.33 | 60 | 0.52 |
By table 1 result as seen, when identical input amount, the purifying water effect of flocculant of ferric chloride of polysilicon acid is significantly better than poly-ferric chloride, especially when add-on during greater than 40ppm, the purifying water effect of polymeric silicicacid iron(ic) chloride is better than poly-ferric chloride far away, can save pharmaceutical quantities about 20% under the same treatment effect situation.
Application example 2:
The coagulation turbidity removal that is used for former water with the flocculant product for preparing in the above example 2 is handled, while and bodied ferric sulfate, and poly-ferric chloride, iron(ic) chloride contrasts.Raw water turbidity: 38.5NTU, the pH value: 8.63, water temperature: 18 ℃, result sees Table 2.
The turbidity removal effect of the different flocculation agents of table 2
| The flocculation agent kind | Flocculant addition (ppm) | |||
| 30 | 35 | 40 | 45 | |
| Iron trichloride | 1.77 | 1.93 | 2.10 | 2.32 |
| Poly-ferric chloride | 1.81 | 1.58 | 1.43 | 1.45 |
| PFSC | 1.50 | 1.32 | 1.11 | 1.11 |
By above result as seen: the flocculating effect of self-control flocculant of ferric chloride of polysilicon acid obviously is better than the iron(ic) chloride and the poly-ferric chloride of use at present.
Claims (4)
1, the preparation method of flocculant of ferric chloride of polysilicon acid.It is characterized in that described method mainly is: with industrial acid-washed waste liquid and iron scale is main raw material, add a certain amount of hydrochloric acid or iron scale according to free acid content, iron level is reached more than 10%, add a certain amount of oxygenant and stablizer then, make it that oxidation, polyreaction take place 30～70 ℃ of quick down stirrings, when oxidation, polyreaction after 15～60 minutes, make basifier with calcium oxide (or magnesium oxide or magnesium hydroxide calcium hydroxide mixed slurry) and regulate basicity to 10～25%, just can prepare stable polyiron chloride.
2, in poly-ferric chloride under the room temperature (15-35 ℃) add poly-silicic acid, under shear conditions, make it that further polymerization takes place, then at 30～50 ℃ of following slaking 0.5～2h.Just can obtain stable PFSC.
3, as right 1 described preparation technology, raw material adopts industrial acid-washed waste liquid and iron scale; Make oxygenant with Potcrate; Use the potassium primary phosphate used as stabilizers; Poly-silicic acid is made by the activation of service water glass.
4, as described in the right 1,2,3, the flocculant of ferric chloride of polysilicon acid of preparation is applicable to water supply purification, wastewater treatment, low-temperature and low turbidity water treatment.Good effect is especially arranged in the tap water purifying treatment.
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| CN 200610013081 CN101003390A (en) | 2006-01-20 | 2006-01-20 | Method for preparing flocculant of ferric chloride of polysilicon acid |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603015A (en) * | 2012-03-20 | 2012-07-25 | 蓝保(厦门)水处理科技有限公司 | Method for producing polymerized iron chloride by utilizing acid-washing waste liquid of steel |
| CN102774941A (en) * | 2012-08-28 | 2012-11-14 | 艾有年 | Preparation method of solid polymeric ferric chloride silicate flocculant |
| CN102815772A (en) * | 2011-12-05 | 2012-12-12 | 韩晓刚 | Preparation method of composite polyferric chloride coagulant |
| CN102942246A (en) * | 2012-12-10 | 2013-02-27 | 王艳芬 | Process for preparing polyferric flocculant |
| 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 |
| CN103466767A (en) * | 2013-03-19 | 2013-12-25 | 绍兴伊诺环保科技有限公司 | Coagulant for treating printing and dyeing wastewater and production method thereof |
| CN104944549A (en) * | 2015-06-08 | 2015-09-30 | 湖南科技大学 | Preparation method for solid flocculant capable of removing ammonia nitrogen |
| CN106622678A (en) * | 2016-12-28 | 2017-05-10 | 重庆市合川区九峰煤炭有限公司 | Desulfurization inhibitor for flotation of high-sulfur coal |
| CN109626527A (en) * | 2018-12-07 | 2019-04-16 | 江苏永葆环保科技有限公司 | A method of flocculant is prepared using high speed emulsification shearing |
| CN110655156A (en) * | 2019-10-18 | 2020-01-07 | 上海霖动环保科技有限公司 | Catalytic flue gas desulfurization wastewater flocculant and preparation method thereof |
| CN112520774A (en) * | 2021-02-18 | 2021-03-19 | 湖南师范大学 | Preparation method of polyaluminum sulfate solution and alkali-free liquid accelerator |
| CN113930753A (en) * | 2021-09-17 | 2022-01-14 | 武汉钢铁有限公司 | Agent and method for stabilizing rust layer of hot-rolled weather-resistant steel |
| CN115259171A (en) * | 2022-07-08 | 2022-11-01 | 武汉纺织大学 | Polysilicate aluminum ferric flocculant for treating indigo blue wastewater and preparation method and application thereof |
| CN115724472A (en) * | 2021-08-30 | 2023-03-03 | 蓝保(厦门)水处理科技有限公司 | Polysulfide ferric chloride and production method thereof |
| CN115259171B (en) * | 2022-07-08 | 2024-05-03 | 武汉纺织大学 | Poly aluminum ferric silicate flocculant for treating indigo wastewater and preparation method and application thereof |
-
2006
- 2006-01-20 CN CN 200610013081 patent/CN101003390A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815772A (en) * | 2011-12-05 | 2012-12-12 | 韩晓刚 | Preparation method of composite polyferric chloride coagulant |
| CN102603015A (en) * | 2012-03-20 | 2012-07-25 | 蓝保(厦门)水处理科技有限公司 | Method for producing polymerized iron chloride by utilizing acid-washing waste liquid of steel |
| CN102774941A (en) * | 2012-08-28 | 2012-11-14 | 艾有年 | Preparation method of solid polymeric ferric chloride silicate flocculant |
| CN102774941B (en) * | 2012-08-28 | 2015-05-27 | 艾有年 | Preparation method of solid polymeric ferric chloride silicate flocculant |
| CN102942246A (en) * | 2012-12-10 | 2013-02-27 | 王艳芬 | Process for preparing polyferric flocculant |
| 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 |
| CN103466767A (en) * | 2013-03-19 | 2013-12-25 | 绍兴伊诺环保科技有限公司 | Coagulant for treating printing and dyeing wastewater and production method thereof |
| CN104944549B (en) * | 2015-06-08 | 2017-05-17 | 湖南科技大学 | Preparation method for solid flocculant capable of removing ammonia nitrogen |
| CN104944549A (en) * | 2015-06-08 | 2015-09-30 | 湖南科技大学 | Preparation method for solid flocculant capable of removing ammonia nitrogen |
| CN106622678A (en) * | 2016-12-28 | 2017-05-10 | 重庆市合川区九峰煤炭有限公司 | Desulfurization inhibitor for flotation of high-sulfur coal |
| CN109626527A (en) * | 2018-12-07 | 2019-04-16 | 江苏永葆环保科技有限公司 | A method of flocculant is prepared using high speed emulsification shearing |
| CN110655156A (en) * | 2019-10-18 | 2020-01-07 | 上海霖动环保科技有限公司 | Catalytic flue gas desulfurization wastewater flocculant and preparation method thereof |
| CN112520774A (en) * | 2021-02-18 | 2021-03-19 | 湖南师范大学 | Preparation method of polyaluminum sulfate solution and alkali-free liquid accelerator |
| CN115724472A (en) * | 2021-08-30 | 2023-03-03 | 蓝保(厦门)水处理科技有限公司 | Polysulfide ferric chloride and production method thereof |
| CN115724472B (en) * | 2021-08-30 | 2024-04-19 | 蓝保(厦门)水处理科技有限公司 | Poly (ferric sulfide chloride) and production method thereof |
| CN113930753A (en) * | 2021-09-17 | 2022-01-14 | 武汉钢铁有限公司 | Agent and method for stabilizing rust layer of hot-rolled weather-resistant steel |
| CN113930753B (en) * | 2021-09-17 | 2023-09-05 | 武汉钢铁有限公司 | Stabilizing treatment agent and method for hot-rolled weather-resistant steel rust layer |
| CN115259171A (en) * | 2022-07-08 | 2022-11-01 | 武汉纺织大学 | Polysilicate aluminum ferric flocculant for treating indigo blue wastewater and preparation method and application thereof |
| CN115259171B (en) * | 2022-07-08 | 2024-05-03 | 武汉纺织大学 | Poly aluminum ferric silicate flocculant for treating indigo wastewater and preparation method and application thereof |
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