CN103172152A - Preparation method of modified polymerized ferric sulfate - Google Patents
Preparation method of modified polymerized ferric sulfate Download PDFInfo
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- CN103172152A CN103172152A CN2013101164199A CN201310116419A CN103172152A CN 103172152 A CN103172152 A CN 103172152A CN 2013101164199 A CN2013101164199 A CN 2013101164199A CN 201310116419 A CN201310116419 A CN 201310116419A CN 103172152 A CN103172152 A CN 103172152A
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- China
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- ferric sulfate
- preparation
- silicic acid
- modified poly
- active silicic
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Abstract
The invention provides a preparation method of a modified polymerized ferric sulfate. The preparation method comprises the steps of: step 1) preparation of active silicic acid: mixing sodium metasilicate silicate, ferric trichloride and hydroquinone according to a weight ratio of 85:2.5:1; and step 2) preparation of modified polymerized ferric sulfate: mixing active silicic acid with the polymerized ferric sulfate solution according to a weight ratio of 1:(45-55), and then preparing the modified polymerized ferric sulfate after a filtration step in step 3). In treatment of industrial waste water, by adding the modified polymerized ferric sulfate prepared by the method, the turbidity removal effect is obviously better than that of polymer ferric sulfate and the sedimentation speed of flocculating constituent is faster; the decoloring effect of the waste coking water generated after biological treatment is obviously better than that of the polymer ferric sulfate under the same condition; and the dosage is reduced by 20%-35% than that of the polymer ferric sulfate under the effect.
Description
Technical field
The present invention relates to inorganic water treatment coagulant technical field, especially relate to a kind of preparation method of modified poly ferric sulfate.
Background technology
As everyone knows, bodied ferric sulfate (being called for short " Polyferric Sulfate ") is the same with polymerize aluminum chloride, all the most extensively to be used as in the world at present the inorganic coagulant of industrial sewage wastewater treatment, it is under the jurisdiction of respectively iron system and aluminium is, bodied ferric sulfate because of its have the suspended substance removed in waste water, except the effect of the organism such as COD and BOD, removal phenol benzene and other detrimental impurity (as: sulfide, prussiate and part phosphide) and heavy metal, therefore bodied ferric sulfate is widely adopted in a plurality of industry wastewater treatments of China.But, in the technique that the every profession and trade sewage and waste water is processed, bodied ferric sulfate is much relatively narrower than the employing scope of polymerize aluminum chloride, trace it to its cause: except the character characteristics and the decision of effect difference of product self, one of them important choice factor is exactly due to when processing waste water, because the color that adds bodied ferric sulfate and process rear water outlet can produce " yellowing " drawback, give people's vision directly perceived bad, affected the application prospect of Polyferric Sulfate.
The reason of the water outlet color yellowing after occurring after processing trade effluent for bodied ferric sulfate processing, study discovery through the contriver, the coagulation mechanism of purifying waste water according to Polyferric Sulfate: the ferric ion in Polyferric Sulfate does not exist with single ionic condition in the aqueous solution, but with trivalent hydrated iron ion [Fe6H
2O]
3+State exist.Less than 3 the time, this hydrated iron ion will be Main Morphology, and less its hydrated iron ion content of pH value is higher when the pH value, and the yellowish brown of water also can lightlyer even disappear.Along with pH value raises, wherein the hydrolytic process (i.e. the reversing process of hydrolysis and polycondensation) of coordinated water molecule will occur in a large amount of hydrated iron ions, generates various hydroxyl hydration coordination ion [Fe (H
2O)
5(OH)]
2+, [Fe (H
2O)
4(OH)
2Fe (H
2O)
4]
4+, due in the production practice of water treatment, it is commonplace that the sewage and waste water that wish is processed is in the situation of weak acid or alkaline range mostly, so hydroxyl hydration coordination ion [Fe (H wherein
2O) 5 (OH)]
2+, [Fe (H
2O) 4 (OH)
2Fe (H
2O) 4]
4+A large amount of existences of ferric ion because PH too high present alkaline water, ferric ion can directly be separated out bulky ferric hydroxide precipitate; Simultaneously, find trivalent hydrated iron ion [Fe6H through X-ray diffraction studies
2O]
3+With various hydroxyl hydration coordination ion [Fe (H
2O) 5 (OH)]
2+, [Fe (H
2O) 4 (OH)
2Fe (H
2O)
4]
4+Different Deng the absorption peak position to light in water, [Fe6H
2O]
3+Absorption peak in the ultraviolet region, present lilac or colourless, and hydroxyl hydration coordination ion [Fe (H
2O) 5 (OH)]
2+, [Fe (H
2O) 4 (OH)
2Fe (H
2O) 4]
4+Deng the absorption peak afterbody entered the visible region, present yellow.Therefore, our the yellow overwhelming majority usually seen is by due to the hydrolysate hydroxyl hydration coordination ion of trivalent iron salt.Secondly, the organism water soluble contaminants such as the soil ulmin in water form humic acids can with iron salt coagulant in ferric ion form trivalent iron salt, what obtain when trivalent iron salt is water-soluble is all yellow-brownish solution, must make water present " yellowing look " phenomenon.
Therefore, suppress the hydrolysis of Polyferric Sulfate in water when processing trade effluent, make iron ion residual in solution as often as possible with trivalent hydrated iron ion [Fe6H
2O]
3+Form exist in solution, namely can solve the drawback problem of the water outlet " yellowing look " after Industrial Wastewater Treatment.
Summary of the invention
The object of the present invention is to provide the preparation method of modified poly ferric sulfate, when suspended substance, decolouring have quick removal waste water when processing trade effluent in, removing COD and BOD, removal organism and the effects such as other objectionable impuritiess and heavy metal, and " yellowing " phenomenon no longer appears in the water outlet color after processing.
In order to achieve the above object, the invention provides following technical scheme:
A kind of preparation method of modified poly ferric sulfate, it comprises the steps:
1) preparation section of active silicic acid takes out flower bulb alkali water glass, iron trichloride, Resorcinol according to weight ratio standbyly at 85: 2.5: 1, and flower bulb alkali water glass is diluted with water to SiO
2Content 2%-3% adds dense dilution heat of sulfuric acid for degree 2%-3% to stir, and when viscosity reaches the Tu Shi viscometer and records concentration and be 1 ' 30 " 1 ' 40 ", adds iron trichloride and Resorcinol to mix fully and stirs, and namely makes active silicic acid.
2) modified poly ferric sulfate preparation section, active silicic acid and polymeric ferrous sulphate solution are by weight 1: the ratio of 45-55, active silicic acid is joined in polymeric ferrous sulphate solution stir, under 110 ℃ of conditions of normal pressure, in generation and polyreaction, reacted 3 hours-4 hours, make its fully occur in and polyreaction after, cooling-sedimentation.
3) filter progress utilizes strainer step 2) impurity of participating in reaction in the mixed solution of gained filters out, and namely gets qualified modified poly ferric sulfate liquid.
Step 1) in, the modulus M of described flower bulb alkali water glass is 3.0-3.2, SiO
2Content 〉=28%, the concentration of Resorcinol are 200ppm.
Step 2) in, active silicic acid and polymeric ferrous sulphate solution by weight, preferred ratio is 1: 52.
Step 2) in, reaction is 3.5 hours under 110 ℃ of conditions of normal pressure.
The invention has the beneficial effects as follows: when processing trade effluent, add and use the prepared modified poly ferric sulfate of the present invention, turbidity removal effect obviously is better than bodied ferric sulfate, and floc settling velocity is faster; The coking chemical waste water of processing after biochemical treatment, under equal conditions, its decolorizing effect obviously is better than bodied ferric sulfate, and with under texts, consumption reduces 20%-35% than bodied ferric sulfate.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, rather than whole embodiment.Based on the embodiment in the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
A kind of preparation method of modified poly ferric sulfate, it comprises the steps:
1) preparation section of active silicic acid, with flower bulb alkali water glass, iron trichloride, Resorcinol according to weight ratio 85: 2.5: l takes out standby, and (modulus M is 3.0-3.2 to flower bulb alkali water glass, SiO
2Content 〉=28%) be diluted with water to SiO
2Content 2%-3%, add dense dilution heat of sulfuric acid for degree 2%-3% to stir, when viscosity reaches the Tu Shi viscometer and records concentration and be 1 ' 30 " 1 ' 40 ", add iron trichloride and Resorcinol (concentration 200ppm) to mix fully and stir, namely make active silicic acid; The reacted resultant of flower bulb alkali water glass and dilute sulphuric acid is silicic acid, iron trichloride and Resorcinol have been mainly the effects of stopper, purpose is to delay silicic acid to form gel, make the active silicic acid that makes to preserve the long period, soak time 1.5h, the polymerization degree of active silicic acid is higher adds the coagulation performance in bodied ferric sulfate also better, but can not be too high, too high easy generation gelling, it is 0.5 more suitable that the general polymerization degree is got, and namely recording limit viscosity by the Tu Shi viscometer is 1 ' 30 " 1 ' 40 ".
2) modified poly ferric sulfate preparation section, active silicic acid and polymeric ferrous sulphate solution are by weight the ratio of l: 45-55, active silicic acid is joined polymeric ferrous sulphate solution, and (the solution degree Beaume is 55, density is 1.6g/l) the middle stirring, in generation and polyreaction, under 110 ℃ of conditions of normal pressure the reaction 3.5 hours, make its fully occur in and polyreaction after, cooling-sedimentation;
Chemical formula is: [Fe
2(OH)
n(SO4)
3-n/2] m+nH
2SiO
3→ [Fe
2(OH)
n(SO4)
3-n/2]
mNSiO
2+ nH
2O。
In the present invention, do not use flower bulb alkali water glass directly to add bodied ferric sulfate, because industrial metasilicate alkalescence is stronger, directly adds membership and introduce a large amount of OH
-, the flocculation ability of bodied ferric sulfate is weakened, adopt active silicic acid can reduce OH
-Concentration, improve the flocculation ability of bodied ferric sulfate.
3) filter progress utilizes strainer step 2) material of participating in reaction in the mixed solution of gained filters out, and namely gets qualified modified poly ferric sulfate liquid, and the degree Beaume of the modified poly ferric sulfate liquid that makes is 50, and density is 1.5g/l; Strainer can use plate filter, can be with step 2 as long as filter to require) in participate in reaction material filter out.
The polymeric ferrous sulphate solution that uses in the present invention can adopt the solution of buying on market, also can be voluntarily according to textbook or the disclosed method preparation of other relevant preparation technologies.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; can expect easily changing or replacing, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion by described protection domain with claim.
Claims (4)
1. the preparation method of a modified poly ferric sulfate, it is characterized in that: it comprises the steps:
1) preparation section of active silicic acid takes out flower bulb alkali water glass, iron trichloride, Resorcinol according to weight ratio standbyly at 85: 2.5: 1, and flower bulb alkali water glass is diluted with water to SiO
2Content 2%-3% adds dense dilution heat of sulfuric acid for degree 2%-3% to stir, and when viscosity reaches the Tu Shi viscometer and records concentration and be 1 ' 30 " 1 ' 40 ", adds iron trichloride and Resorcinol to mix fully and stirs, and namely makes active silicic acid.
2) modified poly ferric sulfate preparation section, active silicic acid and polymeric ferrous sulphate solution are by weight 1: the ratio of 45-55, active silicic acid is joined in polymeric ferrous sulphate solution stir, under 110 ℃ of conditions of normal pressure, in generation and polyreaction, reacted 3 hours-4 hours, make its fully occur in and polyreaction after, cooling-sedimentation.
3) filter progress utilizes strainer step 2) impurity of participating in reaction in the mixed solution of gained filters out, and namely gets qualified modified poly ferric sulfate liquid.
2. the preparation method of a kind of modified poly ferric sulfate according to claim 1, is characterized in that: step 1) in, the modulus M of described flower bulb alkali water glass is 3.0-3.2, SiO
2Content 〉=28%, the concentration of Resorcinol are 200ppm.
3. the preparation method of a kind of modified poly ferric sulfate according to claim 1, is characterized in that: step 2) in, active silicic acid and polymeric ferrous sulphate solution by weight, preferred ratio is 1: 52.
4. the preparation method of a kind of modified poly ferric sulfate according to claim 1, is characterized in that: step 2) in, reaction is 3.5 hours under 110 ℃ of conditions of normal pressure.
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|---|---|---|---|
| CN201310116419.9A CN103172152B (en) | 2013-04-07 | 2013-04-07 | Preparation method of modified polymerized ferric sulfate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310116419.9A CN103172152B (en) | 2013-04-07 | 2013-04-07 | Preparation method of modified polymerized ferric sulfate |
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| CN103172152A true CN103172152A (en) | 2013-06-26 |
| CN103172152B CN103172152B (en) | 2014-08-13 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104973668A (en) * | 2015-06-10 | 2015-10-14 | 天津大港油田滨港集团博弘石油化工有限公司 | Preparation method of organically modified polymeric ferric sulfate water purification agent |
| CN105152293A (en) * | 2015-09-08 | 2015-12-16 | 海南宜净环保有限公司 | Preparation method for polymeric ferric sulfate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04250883A (en) * | 1990-12-27 | 1992-09-07 | Kurita Water Ind Ltd | Treatment of waste water |
| CN1243099A (en) * | 1998-07-28 | 2000-02-02 | 周毅 | Active polysilicate flocculating agent and preparation method thereof |
| JP2000154013A (en) * | 1998-11-17 | 2000-06-06 | Ebara Corp | Production of activated silica |
-
2013
- 2013-04-07 CN CN201310116419.9A patent/CN103172152B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04250883A (en) * | 1990-12-27 | 1992-09-07 | Kurita Water Ind Ltd | Treatment of waste water |
| CN1243099A (en) * | 1998-07-28 | 2000-02-02 | 周毅 | Active polysilicate flocculating agent and preparation method thereof |
| JP2000154013A (en) * | 1998-11-17 | 2000-06-06 | Ebara Corp | Production of activated silica |
Non-Patent Citations (2)
| Title |
|---|
| 徐天有 等: "聚硅酸硫酸铁的研究和制备", 《浙江工业大学学报》 * |
| 郑怀礼 等: "聚硅硫酸铁絮凝剂的制备与性能", 《华东理工大学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104973668A (en) * | 2015-06-10 | 2015-10-14 | 天津大港油田滨港集团博弘石油化工有限公司 | Preparation method of organically modified polymeric ferric sulfate water purification agent |
| CN105152293A (en) * | 2015-09-08 | 2015-12-16 | 海南宜净环保有限公司 | Preparation method for polymeric ferric sulfate |
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| Publication number | Publication date |
|---|---|
| CN103172152B (en) | 2014-08-13 |
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Granted publication date: 20140813 Termination date: 20200407 |