CN103172152B - Preparation method of modified polymerized ferric sulfate - Google Patents
Preparation method of modified polymerized ferric sulfate Download PDFInfo
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- CN103172152B CN103172152B CN201310116419.9A CN201310116419A CN103172152B CN 103172152 B CN103172152 B CN 103172152B CN 201310116419 A CN201310116419 A CN 201310116419A CN 103172152 B CN103172152 B CN 103172152B
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- ferric sulfate
- silicic acid
- preparation
- active silicic
- modified poly
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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, it is all the inorganic coagulant that is the most extensively used as in the world at present industrial sewage wastewater treatment, it is under the jurisdiction of respectively iron system and aluminium system, bodied ferric sulfate has the suspended substance of removing in waste water, effect of removing the organism such as COD and BOD, removal phenol benzene and other detrimental impurity (as: sulfide, prussiate and part phosphide) and heavy metal because of it, therefore bodied ferric sulfate is widely adopted in the multiple industry wastewater treatments of China.But, in the technique of every profession and trade sewage and waste water processing, bodied ferric sulfate is much relatively narrower than the employing scope of polymerize aluminum chloride, trace it to its cause: except the character feature and the decision of effect difference of product self, one of them important choice factor is exactly due in the time 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, affect the application prospect of Polyferric Sulfate.
Processing for bodied ferric sulfate the reason that occurs water outlet color after treatment yellowing after trade effluent, study discovery through 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.In the time that pH value is less than 3, this hydrated iron ion will be Main Morphology, and less its hydrated iron ion content of pH value is higher, and the yellowish brown of water also can lightlyer even disappear.Along with pH value raises, will there is the hydrolytic process (i.e. the reversing process of hydrolysis and polycondensation) of coordinated water molecule in a large amount of hydrated iron ions wherein, 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, the sewage and waste water of wish processing is mostly commonplace in the situation of weak acid or alkaline range, 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 in too high the presenting in alkaline water of PH, ferric ion can directly be separated out bulky ferric hydroxide precipitate; Meanwhile, 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 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 absorption peak afterbody entered visible region, present yellow.Therefore the yellow overwhelming majority that, we see is conventionally 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 when trivalent iron salt is water-soluble, obtain is all yellow-brownish solution, must make water present " yellowing look " phenomenon.
Therefore, in the time processing trade effluent, suppress the hydrolysis of Polyferric Sulfate in water, make iron ion residual in solution as often as possible with trivalent hydrated iron ion [Fe6H
2o]
3+form exist in solution, 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, in processing the suspended substance that has when trade effluent in quick removal waste water, decolouring, except effects such as COD and BOD, removal organism and other objectionable impuritiess and heavy metals, and no longer there is " yellowing " phenomenon in water outlet color after treatment.
In order to achieve the above object, the invention provides following technical scheme:
A preparation method for 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 for subsequent usely at 85: 2.5: 1, and flower bulb alkali water glass is diluted with water to SiO
2content 2%-3%, adds the dilution heat of sulfuric acid of concentration 2%-3% to stir, in the time that viscosity reaches Tu Shi viscometer and records viscosity and be 1 ' 30 " 1 ' 40 " ", add iron trichloride and Resorcinol to mix fully and stir, make 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 and stirred, under 110 DEG C of conditions of normal pressure, in generation and polyreaction, react 3 hours-4 hours, make its fully occur in and polyreaction after, cooling-sedimentation.
3) filter progress, utilizes strainer step 2) impurity of not participating in reaction in the mixed solution of gained filters out, and obtains 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 is 200ppm.
Step 2) in, by weight, preferred ratio is 1: 52 for active silicic acid and polymeric ferrous sulphate solution.
Step 2) in, under 110 DEG C of conditions of normal pressure, react 3.5 hours.
The invention has the beneficial effects as follows: in the time processing trade effluent, add and use the prepared modified poly ferric sulfate of the present invention, turbidity removal effect is obviously better than bodied ferric sulfate, and floc settling velocity is faster; Process the coking chemical waste water after biochemical treatment, under equal conditions, its decolorizing effect is obviously better than bodied ferric sulfate, and under same texts, consumption reduces 20%-35% compared with 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, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
A preparation method for 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 for subsequent usely at 85: 2.5: 1, 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 the dilution heat of sulfuric acid of concentration 2%-3% to stir, in the time that viscosity reaches Tu Shi viscometer and records viscosity and be 1 ' 30 " 1 ' 40 " ", add iron trichloride and Resorcinol (concentration 200ppm) to mix fully and stir, 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, object is to delay silicic acid to form gel, the active silicic acid making can be preserved 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 general polymerization degree is got, and recording limit viscosity by 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 1: the ratio of 45-55, active silicic acid is joined to polymeric ferrous sulphate solution, and (solution degree Beaume is 55, density is 1.6g/l) middle stirring, in generation and polyreaction, under 110 DEG C of conditions of normal pressure, react 3.5 hours, make its fully occur in and polyreaction after, cooling-sedimentation;
Chemical formula is: [Fe
2(OH)
n(SO
4)
3-n/2]
m+ nH
2siO
3→ [Fe
2(OH)
n(SO
4)
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
-, also make the flocculation ability of bodied ferric sulfate weaken, 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 not participating in reaction in the mixed solution of gained filters out, and obtains qualified modified poly ferric sulfate liquid, and the degree Beaume of the modified poly ferric sulfate liquid making is 50, and density is 1.5g/l; Strainer can use plate filter, if filter require can be by step 2) in do not participate in reaction material filter out.
The polymeric ferrous sulphate solution using 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, any be familiar with those skilled in the art the present invention disclose technical scope in; 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 described be as the criterion with the protection domain of claim.
Claims (1)
1. a preparation method for modified poly ferric sulfate, is characterized in that, comprises the steps:
1) preparation section of active silicic acid, takes out flower bulb alkali water glass, iron trichloride, Resorcinol according to weight ratio for subsequent usely at 85: 2.5: 1, and flower bulb alkali water glass is diluted with water to SiO
2content 2%-3%, adding concentration is that the dilution heat of sulfuric acid of 2%-3% stirs, and in the time that viscosity reaches Tu Shi viscometer and records viscosity and be 1 ' 30 " 1 ' 40 ", adds iron trichloride and Resorcinol to mix fully and stirs, and makes 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, object is to delay silicic acid to form gel, the active silicic acid making can be preserved the long period, soak time 1.5h, the polymerization degree of active silicic acid is 0.5, and recording limit viscosity by 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 1: the ratio of 45-55, active silicic acid is joined in polymeric ferrous sulphate solution and stirred, in generation and polyreaction, under 110 DEG C of conditions of normal pressure, react 3.5 hours, make its fully occur in and polyreaction after, cooling-sedimentation;
Chemical formula is: [Fe
2(OH)
n(SO
4)
3-n/2]
m+ nH
2siO
3→ [Fe
2(OH)
n(SO
4)
3-n/2]
mnSiO
2+ nH
2o;
3) filter progress, utilizes strainer step 2) material of not participating in reaction in the mixed solution of gained filters out, and obtains qualified modified poly ferric sulfate liquid, and the degree Beaume of the modified poly ferric sulfate liquid making is 50, and density is 1.5g/l.
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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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|---|---|---|---|
| CN201310116419.9A CN103172152B (en) | 2013-04-07 | 2013-04-07 | Preparation method of modified polymerized ferric sulfate |
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| CN103172152A CN103172152A (en) | 2013-06-26 |
| CN103172152B true CN103172152B (en) | 2014-08-13 |
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| 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 |
|---|
| 聚硅硫酸铁絮凝剂的制备与性能;郑怀礼 等;《华东理工大学学报》;20030630;第29卷(第3期);1实验部分和2结果与讨论 * |
| 聚硅酸硫酸铁的研究和制备;徐天有 等;《浙江工业大学学报》;20031030;第31卷(第5期);0前言和1实验部分 * |
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