CN102757119A - Preparation method of composite type inorganic polymeric flocculating agent and application thereof - Google Patents
Preparation method of composite type inorganic polymeric flocculating agent and application thereof Download PDFInfo
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- CN102757119A CN102757119A CN2012102527161A CN201210252716A CN102757119A CN 102757119 A CN102757119 A CN 102757119A CN 2012102527161 A CN2012102527161 A CN 2012102527161A CN 201210252716 A CN201210252716 A CN 201210252716A CN 102757119 A CN102757119 A CN 102757119A
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Abstract
The invention discloses preparation of a composite type inorganic polymeric flocculating agent and an application thereof, and belongs to the field of wastewater treatment. The flocculating agent takes ferrous sulfate septihydrate and sodium silicate as main raw materials; and fewer metal ions including Zn<2+>, Mg<2+>, Ca<2+> and the like are added, and steps of activating, mixing, oxidizing, curing and the like are carried out to prepare the composite type inorganic polymeric flocculating agent. A preparation process of the flocculating agent has the advantages of simple preparation process, low cost and excellent flocculating, de-coloring and dephosphorization effects on sewage; a product is liquid and the product stability is good; and the product can be directly added so that the use is convenient.
Description
Technical field
The present invention relates to a kind of preparation and application of flocculation agent, relate in particular to a kind of preparation and application of composite type inorganic polymer flocculation agent, belong to field of waste water treatment.
Background technology
Flocculation sedimentation is a kind of not only economy but also simple sewage water treatment method that generally is used for improving sewage treating efficiency at present both at home and abroad.According to the chemical constitution of flocculation agent, it is divided into inorganic coagulant and organic floculant.
Flocculation agent in the market mainly is aluminium system and iron-based flocculating agent, like Tai-Ace S 150, aluminum chloride, Poly aluminum Chloride (PAC) (PAC), polyaluminium sulfate (PAS), ferric sulfate, iron(ic)chloride, poly-ferric chloride (PFC) and bodied ferric sulfate (PFS) etc.After the aluminium based flocculating agent is disposed of sewage, cause the aluminium content in the water outlet to increase, because the cytogenetic toxicity of aluminium, aluminium causes multiple disease after water cycle gets into tap water, threaten human health.And iron-based flocculating agent uses the back little to environment and human health risk, so iron-based flocculating agent becomes the research heat subject of the scientific domain of flocculating in recent years, and iron-based flocculating agent has the development trend that replaces aluminum salt flocculant at present.Bodied ferric sulfate (PFS) is a kind of well behaved flocculation agent; But it is higher to handle the back effluent color dilution; And the single bodied ferric sulfate polymerization degree is not high; Long-term storage is unstable, is prone to produce deposition, therefore in bodied ferric sulfate, introduces organic and inorganic composition it is carried out the composite modified focus that becomes Recent study.
Disclose a kind of compound method of bodied ferric sulfate in the Chinese patent 200710067347.8, but this method synthetic polymeric ferric sulfate flocculant basicity is higher, and basicity is high more, stability is poor more; Disclose a kind of iron-based compound water treatment agent FPFS-1 and preparation method in the Chinese patent 200910042578.2, but the iron-based composite flocculant of this method preparation is not specifically set forth its decolorizing effect and case history; Disclose a kind of composite water purifying agent of use in waste water treatment in the Chinese patent 200510049584.2, but aluminum chloride content is high in the water purification agent component of this method preparation, therefore is prone to produce secondary pollution.
Summary of the invention
In order to overcome the deficiency of prior art, to the invention reside in a kind of composite type inorganic polymer flocculation agent and preparation method thereof is provided.This flocculation agent good stability, good to flocculation, decolouring, the phosphor-removing effect of sewage, product is liquid, and is easy to use, can be used for high, medium and low concentration wastewater from chemical industry and municipal sewage treatment; Its preparation method technology is simple, and is with low cost, and no poisonous and harmful ion can not cause secondary pollution to environment.
The measuring method of index described in the present invention: full weight of iron mark: adopt dichromate titration (GB14591-2006) to measure; Reducing substances is (with Fe
2+Meter) massfraction: adopt permanganate titration (GB14591-2006) to measure; Basicity: adopt sodium hydroxide volumetry (GB14591-2006) to measure; COD-COD: adopt dichromate titration (GB11914-89) to measure; Colourity: adopt extension rate method (GB11903-1989) to measure; PH value: adopt glass electrode method (GB6920-86) to measure; Total phosphorus: adopt ammonium molybdate spectrophotometry (GB11893-89) to measure.
One of the object of the invention is to disclose a kind of composite type inorganic polymer flocculation agent preparation method; This preparation method is that main raw material is processed bodied ferric sulfate with Producing Titanium Dioxide by product iron vitriol; Make activation with widely used water glass and gather the silicic acid superpolymer; Bodied ferric sulfate and activation gather the silicic acid superpolymer and carry out complexing, form the polymeric novel water treatment flocculant of multinuclear, add Zn simultaneously
2+, Mg
2+, Ca
2+Ion, through the synthetic composite type inorganic polymer flocculation agent of processes such as overactivation, miscible, oxidation, slaking, composite type inorganic polymer flocculation agent preparation method according to the invention comprises following steps:
1) activation: behind the water glass dilute with water, add the vitriol oil, stirring at normal temperature 2.0h carries out activated polymerization, and stirring velocity is 100-120 rev/min, obtains work in-process A;
2) miscible: in work in-process A, add iron vitriol, water, the vitriol oil, Zinc Sulphate Heptahydrate, MAGNESIUM SULPHATE HEPTAHYDRATE 99.5, Calcium Chloride Powder Anhydrous etc. successively, under 40 ℃ of conditions, stir and make the above-mentioned substance dissolving, stirring velocity is 120-150 rev/min, obtains work in-process B;
3) oxidation: in work in-process B, slowly drip VAL-DROP and potassium permanganate, under 55-70 ℃ of condition, be stirred to VAL-DROP and potassium permanganate dropwises, stirring velocity is 120-150 rev/min, obtains work in-process C;
4) slaking: work in-process C continuously stirring 3.0h under 55-60 ℃ of condition is carried out slaking, and stirring velocity is 110-130 rev/min, obtains the composite type inorganic polymer flocculation agent.
The umber of wherein above-mentioned said various supplementary material components is: iron vitriol is 55～65 parts, is preferably 57-60 part, and Zinc Sulphate Heptahydrate is 1.0～1.5 parts, is preferably; 1.2-1.5 part, MAGNESIUM SULPHATE HEPTAHYDRATE 99.5 is 1.5～2.0 parts, is preferably 1.8-2.0 part, Calcium Chloride Powder Anhydrous is 1.0～1.5 parts; Be preferably 1.2-1.5 part, VAL-DROP is 3.0～3.8 parts, is preferably 3.4-3.7 part; Water glass is 0.5～1.0 part, is preferably 0.6-0.8 part, and the vitriol oil is 3.6～5.0 parts; Be preferably 3.9-4.5 part, potassium permanganate is 0.3～0.5 part, is preferably 0.35-0.45 part.Wherein iron vitriol, water glass are the main supplementary materials that generates high molecular polymer; Zinc sulfate, sal epsom, calcium chloride are used to improve decolouring, the phosphor-removing effect of product; VAL-DROP is oxygenant; The vitriol oil is used to regulate acidity, and catalyzer potassium permanganate helps shortening the reaction times, improves polymerization efficiency.Composite type inorganic polymer flocculation agent preparation flow figure of the present invention can be referring to Figure of description 1.
Two of the object of the invention provides a kind of composite type inorganic polymer flocculation agent, and this composite type inorganic polymer flocculation agent adopts the preparation method of the above-mentioned said flocculation agent of the present invention to make.Wherein the appearance character of this composite type inorganic polymer flocculation agent is the reddish-brown thick liquid, and its quality index is shown in table one:
Table one: the quality index of composite type inorganic polymer flocculation agent
| Project | Index |
| The massfraction of full iron | 11.5-13％ |
| Reducing substances is (with Fe 2+Meter) massfraction (<=) | 0.005％ |
| Basicity | 13-16％ |
| Density (20 ℃) | 1.48-1.53g/cm 3 |
| PH (1% aqueous solution) value | 2-3 |
Three of the object of the invention provides a kind of application of above-mentioned composite type inorganic polymer flocculation agent, and promptly above-mentioned composite type inorganic polymer flocculation agent is in Application of Sewage, and wherein said sewage is preferably chemical pharmaceutical waste water and municipal effluent.The embodiment of the invention 4 and 5 adopts the flocculating settling simultaneous test; The inorganic polymer flocculant and the commercially available polymerization ferrous sulfate flocculation agent that use the present invention to prepare are respectively handled chemical pharmaceutical waste water and municipal effluent; Experiment showed, that the inorganic polymer flocculant that the present invention prepares compares with certain commercially available polymerization ferrous sulfate, adding less; The flco that produces is free settling greatly and more, and is more excellent to chroma in waste water, COD, total phosphorus removal effect.
Composite type inorganic polymer flocculation agent of the present invention and preparation method thereof, compared with prior art, its innovation part is described below with the effect that reaches:
1) adopt active silicic acid as coagulant aids, can strengthen the synergistic effect of coagulation, the volume of increase medicament sweeps and net is caught ability, introduces silicate ion simultaneously and improves medicament stability;
2) Zn in the reactant
2+, Mg
2+, Ca
2+Do not participate in polymerization process, exist with free state, the performance synergy obviously improves flocculation, decolouring, phosphor-removing effect;
3) iron vitriol, water glass wide material sources are cheap, and various supplementary materials do not have the poisonous and harmful ion, can not cause secondary pollution to environment;
4) normal temperature for liquid, can directly add use down, and is easy to operate;
5) reasonable compatibility of various supplementary materials make product have flocculating effect good, have decolouring dephosphorization function, advantage such as applied widely concurrently, can be used for COD is 1000-5000mg/l and COD high, medium and low different concns chemical pharmaceutical waste water or the municipal sewage treatment less than 1000mg/l greater than 5000mg/l, COD.
Description of drawings
Fig. 1 is to use the inventive method to prepare the schematic flow sheet of composite type inorganic polymer flocculation agent.
Embodiment
Below will further specify the present invention, but it should be appreciated by those skilled in the art that the specific embodiment of the invention and do not limit the present invention in any way through specific embodiment.Take up an official post on basis of the present invention and how all to fall within protection scope of the present invention with replacement.
Embodiment 1:
5.52 kilograms of usefulness 20 kg of water dilutions of water glass (the water glass massfraction is 57%) back is added in the reaction kettle, add 3.8 kilograms of the vitriol oils, stirring at normal temperature 2h carries out activated polymerization, stirring velocity 100-120 rev/min, obtains work in-process A; In work in-process A, add 116 kilograms of iron vitriols, 34.1 kilograms in water, 3.6 kilograms of the vitriol oils, 3.0 kilograms of Zinc Sulphate Heptahydrates, 4.0 kilograms of MAGNESIUM SULPHATE HEPTAHYDRATE 99.5s, 3.0 kilograms of Calcium Chloride Powder Anhydrouss successively; Temperature of reaction kettle is increased to 40 ℃; Stirring makes the above-mentioned substance dissolving; Stirring velocity is 120-150 rev/min, obtains work in-process B; In work in-process B, drip simultaneously slowly 6.2 kilograms in VAL-DROP, 0.6 kilogram in potassium permanganate, temperature of reaction kettle is increased to and is stirred to VAL-DROP under 60 ℃ of conditions and potassium permanganate dropwises, and stirring velocity is 120-150 rev/min, obtains work in-process C; Continuously stirring 3.0h carries out slaking under 55-60 ℃ of condition of maintenance temperature of reaction kettle, and stirring velocity is 110-130 rev/min, finally obtains the composite type inorganic polymer flocculation agent.
Embodiment 2:
3.46 kilograms of usefulness 15 kg of water dilutions of water glass (the water glass massfraction is 57%) back is added in the reaction kettle, add 3.5 kilograms of the vitriol oils, stirring at normal temperature 2h carries out activated polymerization, stirring velocity 100-120 rev/min, obtains work in-process A; In work in-process A, add 130 kilograms of iron vitriols, 26.1 kilograms in water, 6.3 kilograms of the vitriol oils, 2.0 kilograms of Zinc Sulphate Heptahydrates, 3.0 kilograms of MAGNESIUM SULPHATE HEPTAHYDRATE 99.5s, 2.0 kilograms of Calcium Chloride Powder Anhydrouss successively; Temperature of reaction kettle is increased to 40 ℃; Stirring makes the above-mentioned substance dissolving; Stirring velocity is 120-150 rev/min, obtains work in-process B; In work in-process B, drip simultaneously slowly 7.6 kilograms in VAL-DROP, 0.84 kilogram in potassium permanganate, temperature of reaction kettle is increased to stir under 65 ℃ of conditions and is oxidizing to VAL-DROP and potassium permanganate dropwises, and stirring velocity is 120-150 rev/min, obtains work in-process C; Continuously stirring 3.0h carries out slaking under 60-70 ℃ of condition of maintenance temperature of reaction kettle, and stirring velocity is 110-130 rev/min, finally obtains the composite type inorganic polymer flocculation agent.
Embodiment 3:
4.62 kilograms of usefulness 20 kg of water dilutions of water glass (the water glass massfraction is 57%) back is added in the reaction kettle, add 4.0 jin of the vitriol oils, stirring at normal temperature 2h carries out activated polymerization, stirring velocity 100-120 rev/min, obtains work in-process A; In work in-process A, add 122 kilograms of iron vitriols, 48 kilograms in water, 5.0 kilograms of the vitriol oils, 2.6 kilograms of Zinc Sulphate Heptahydrates, 3.4 kilograms of MAGNESIUM SULPHATE HEPTAHYDRATE 99.5s, 2.4 kilograms of Calcium Chloride Powder Anhydrouss successively; Temperature of reaction kettle is increased to 40 ℃; Stirring makes the above-mentioned substance dissolving; Stirring velocity is 120-150 rev/min, obtains work in-process B; In work in-process B, drip simultaneously slowly 7.1 kilograms in VAL-DROP, 0.77 kilogram in potassium permanganate, temperature of reaction kettle is increased to stir under 55 ℃ of conditions and is oxidizing to VAL-DROP and potassium permanganate dropwises, and stirring velocity is 120-150 rev/min, obtains work in-process C; Continuously stirring 3.0h carries out slaking under 55-60 ℃ of condition of maintenance temperature of reaction kettle, and stirring velocity is 110-130 rev/min, finally obtains the composite type inorganic polymer flocculation agent.
Embodiment 4:
Get the chemical industry pharmacy waste water 1000mL of Shandong a certain chemical pharmaceutical enterprise and place two 1000mL beakers respectively for two parts; The a composite type inorganic polymer flocculation agent that adds present method preparation; A certain the commercially available polymeric ferric sulfate flocculant (Linyi Jin Yuan green technology ltd) that adds; Two parts are all stirred after 5 minutes and form flco, get supernatant behind the standing sedimentation 30min respectively and measure.The result is following:
Table two: to the treatment effect simultaneous test of chemical pharmaceutical waste water
Embodiment 5:
Get a certain municipal sewage plant, Shandong municipal effluent 1000mL and place two 1000mL beakers respectively for two parts; The a composite type inorganic polymer flocculation agent that adds present method preparation; A certain the commercially available polymeric ferric sulfate flocculant (Linyi Jin Yuan green technology ltd) that adds; Two parts are all stirred after 5 minutes and form flco, get supernatant behind the standing sedimentation 30min respectively and measure.The result is following:
Table three: the municipal sewage treatment effect comparison is tested
Claims (9)
1. the preparation method of a composite type inorganic polymer flocculation agent is characterized in that said preparation method may further comprise the steps:
1) activation: behind the water glass dilute with water, add the vitriol oil, stirring at normal temperature 2.0h carries out activated polymerization and gets work in-process A;
2) miscible: in work in-process A, add iron vitriol, water, the vitriol oil, Zinc Sulphate Heptahydrate, MAGNESIUM SULPHATE HEPTAHYDRATE 99.5, Calcium Chloride Powder Anhydrous successively, stir under 40 ℃ of conditions make above-mentioned substance dissolve work in-process B;
3) oxidation: under 55-70 ℃ of condition, in work in-process B, slowly drip VAL-DROP and potassium permanganate, stirring and dissolving gets work in-process C;
4) slaking: work in-process C continuously stirring 3.0h under 55-60 ℃ of condition is promptly obtained the composite type inorganic polymer flocculation agent.
2. the preparation method of composite type inorganic polymer flocculation agent as claimed in claim 1 is characterized in that the umber of each component among the said preparation method is:
Iron vitriol is 55～65 parts, and Zinc Sulphate Heptahydrate is 1.0～1.5 parts, and MAGNESIUM SULPHATE HEPTAHYDRATE 99.5 is 1.5～2.0 parts; Calcium Chloride Powder Anhydrous is 1.0～1.5 parts, and VAL-DROP is 3.0～3.8 parts, and water glass is 0.5～1.0 part; The vitriol oil is 3.6～5.0 parts, and potassium permanganate is 0.3～0.5 part.
3. the preparation method of composite type inorganic polymer flocculation agent as claimed in claim 2 is characterized in that the umber of each component among the said preparation method is:
Iron vitriol is 57-60 part, and Zinc Sulphate Heptahydrate is 1.2-1.5 part, and MAGNESIUM SULPHATE HEPTAHYDRATE 99.5 is 1.8-2.0 part; Calcium Chloride Powder Anhydrous is 1.2-1.5 part, and VAL-DROP is 3.4-3.7 part, and water glass is 0.6-0.8 part; The vitriol oil is 3.9-4.5 part, and potassium permanganate is 0.3～0.4 part.
4. the composite type inorganic polymer flocculation agent for preparing of the preparation method of the said composite type inorganic polymer flocculation agent of claim 1-3.
5. composite type inorganic polymer flocculation agent as claimed in claim 4 is characterized in that its quality index is:
The massfraction of full iron is 11.5-13%, and reducing substances is (with Fe
2+Meter) massfraction is≤0.005%, and basicity is 13-16%, and density (20 ℃) is 1.48-1.53g/cm
3, pH value (1% aqueous solution) is 2-3.
6. composite type inorganic polymer flocculation agent as claimed in claim 4 is characterized in that its appearance character is the reddish-brown thick liquid.
7. the described composite type inorganic polymer flocculation agent of claim 4 is in Application of Sewage.
8. application as claimed in claim 7 is characterized in that said sewage is chemical pharmaceutical waste water or municipal effluent.
9. the application of composite type inorganic polymer flocculation agent as claimed in claim 7 is characterized in that said composite type inorganic polymer flocculation agent has the decolouring dephosphorization function.
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| CN103964555A (en) * | 2014-04-19 | 2014-08-06 | 青岛食之礼中草药研究所 | Compound type water treatment flocculating agent and preparation method thereof |
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| CN105502610A (en) * | 2016-01-28 | 2016-04-20 | 叶君芝 | Efficient sewage dephosphorizing flocculating agent and preparation method thereof |
| CN106865714A (en) * | 2017-03-20 | 2017-06-20 | 天津中瑞水处理剂有限公司 | A kind of composite type polymeric flocculant and preparation method thereof |
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| CN108773891A (en) * | 2018-06-05 | 2018-11-09 | 任丘市佳孚化工有限公司 | A kind of dephosphorization agent and preparation method thereof |
| CN115432789A (en) * | 2022-08-31 | 2022-12-06 | 中国矿业大学 | Method for preparing ferrous sulfate flocculating agent from copper smelting tailing slag |
| CN115671163A (en) * | 2022-11-15 | 2023-02-03 | 江西省蚕桑茶叶研究所(江西省经济作物研究所) | Preparation method of mulberry leaf polyphenol extract |
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| CN103922453A (en) * | 2014-05-14 | 2014-07-16 | 山东盛阳集团有限公司 | Flocculating agent for coking wastewater and preparation method thereof and application thereof |
| CN103922453B (en) * | 2014-05-14 | 2016-03-16 | 山东盛阳集团有限公司 | A kind of coking chemical waste water flocculation agent and preparation method thereof and application |
| CN104495997A (en) * | 2015-01-09 | 2015-04-08 | 刘树芹 | Printing and dyeing wastewater cleaning agent, as well as preparation method and application thereof |
| CN105502610A (en) * | 2016-01-28 | 2016-04-20 | 叶君芝 | Efficient sewage dephosphorizing flocculating agent and preparation method thereof |
| CN106865714A (en) * | 2017-03-20 | 2017-06-20 | 天津中瑞水处理剂有限公司 | A kind of composite type polymeric flocculant and preparation method thereof |
| CN107445276A (en) * | 2017-09-11 | 2017-12-08 | 杨帅 | Composite environment-friendly type flocculant and its preparation method and application |
| CN108128862A (en) * | 2017-12-19 | 2018-06-08 | 东华大学 | A kind of processing dyeing waste water ecotype compound coagulant and its preparation method and application |
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| CN108773891A (en) * | 2018-06-05 | 2018-11-09 | 任丘市佳孚化工有限公司 | A kind of dephosphorization agent and preparation method thereof |
| CN115432789A (en) * | 2022-08-31 | 2022-12-06 | 中国矿业大学 | Method for preparing ferrous sulfate flocculating agent from copper smelting tailing slag |
| CN115671163A (en) * | 2022-11-15 | 2023-02-03 | 江西省蚕桑茶叶研究所(江西省经济作物研究所) | Preparation method of mulberry leaf polyphenol extract |
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