CN1524800A - Method for preparing polymeric ferric phosphate sulfate - Google Patents

Method for preparing polymeric ferric phosphate sulfate Download PDF

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Publication number
CN1524800A
CN1524800A CNA031254160A CN03125416A CN1524800A CN 1524800 A CN1524800 A CN 1524800A CN A031254160 A CNA031254160 A CN A031254160A CN 03125416 A CN03125416 A CN 03125416A CN 1524800 A CN1524800 A CN 1524800A
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CN
China
Prior art keywords
aqueous solution
ferrous sulfate
vitriol oil
concentration
phosphate
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Pending
Application number
CNA031254160A
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Chinese (zh)
Inventor
孟 李
李孟
桑稳娇
池波
李翠华
黄功洛
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Application filed by Wuhan University of Technology WUT filed Critical Wuhan University of Technology WUT
Priority to CNA031254160A priority Critical patent/CN1524800A/en
Publication of CN1524800A publication Critical patent/CN1524800A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a process for preparing polyphosphoric acid ferric sesquisulfate comprising the steps of, (1)under normal temperature, reacting the mixture of ferrous sulfate and concentrated sulfuric acid with the aqueous solution of chlorine dioxide for more than 30 minutes, (2) charging inorganic phosphate PO43-Fe into the product yield in (1), (3) obtaining the end product. By employing chlorine dioxide as the oxidation agent in preparing polyphosphoric acid ferric tersulfate, the oxidization efficiency for ferrous iron ions is increased, thus accelerating the generation procedure of molysite polymer.

Description

The preparation method of polymer phosphate ferric sulfate
Technical field
The present invention relates to water purification agent, particularly inorganic polymer flocculant--the preparation method of polymer phosphate ferric sulfate that in the water treatment purification process, uses.
Background technology
Inorganic polymer flocculant is the novel coagulating agent of a class that grows up after 1970, because its water purification performance than traditional inorganic flocculating agent is more excellent, and its production at present and be applied in the whole world and all obtained rapid progress.Wherein polymerize aluminum chloride is the most common coagulating agent.But,, find the surrogate of aluminium salt to become the task of environmentalist's task of top priority along with the understanding that people poison human body and hydrocoles residual aluminum ions in the tap water is more and more deep.
Though traditional molysite has stronger flocculation ability than poly-aluminium, and production cost is lower, but exist, effluent color dilution height handle after strong, handle major defects such as back water body remainder fe ion content exceeds standard, therefore on using, have certain limitation equipment and structures corrodibility.
At present, the method for producing bodied ferric sulfate both at home and abroad has oxygen catalytic oxidation, sodium chlorate oxidation style, sulfurous iron ore calx pressurization acid pasting etc.But some method oxidation efficiency is not high, and some method can be brought environmentally harmful by product in process of production, and then production cost is too high for some, is difficult to suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention is: a kind of inorganic polymer flocculant is provided--polymer phosphate ferric sulfate ([Fe 2(OH) n(PO 4) k(SO 4) (3-n)/2] m, n<2, m>3, k=0.16-0.22), its primary structure unit is Fe 2(OH) n(PO 4) k(SO 4) 6-nMonomer, and the preparation method who connects by hydroxyl shrink polymeric mode.
The present invention solves the problems of the technologies described above the technical scheme that is adopted:
(1) at normal temperatures, react the mixture of the ferrous sulfate and the vitriol oil and the aqueous solution of dioxide peroxide more than 30 minutes; Wherein the concentration of aqueous solution of dioxide peroxide is 1.8-2.2%, and ferrous sulfate is FeSO 4NH 2O, the span of n is between 0-8, and the concentration of the vitriol oil is more than 98%; Mass parts between ferrous sulfate, the vitriol oil, the aqueous solution of chlorine dioxide is than being (5.8-6.1): 1: (3.8-4.0);
(2) in (1) products therefrom, add inorganic phosphate increase poly-, PO 4 3-/ Fe mole ratio is 0.08-0.11;
(3) finished product.
The present invention is in the process of preparation polymer phosphate ferric sulfate, adopted and utilized the method for oxidation of dioxide peroxide under the normal temperature as oxygenant, improved the oxidation efficiency of ferrous ion, use methods such as oxygen high-temperature oxidation and oxymuriate oxidation method to compare with tradition, saved production cost, the generative process of molysite polymkeric substance is rapider, hydroxyl polynuclear complex in its hydrolysate is higher than the relative molecular mass of other inorganic metal salt coagulant, density is bigger, is easy to by the colloidal solid in the former water adsorbed.
The present invention utilizes the phosphatic poly-effect that increases, determined the phosphatic optimal dose that adds by control experiment, make the multinuclear intermediate complex that produces the band phosphate radical of the high electric charge of new class in the poly-iron, further improved aggregation efficiency, improve the hydrolyzation morphology structure of iron ion in water, improved the ratio of active iron polymkeric substance.This coagulating agent has overcome effectively that the corrodibility that the conventional iron salt coagulant has is strong, the water quality colourity height after handling, shortcoming that the remainder fe ion exceeds standard, form density and the big flocs unit of slip resistance after adding Yu Yuanshui, purifying water effect is remarkable, it is little influenced by water temperature, pH value is applied widely, the content (0.08mg/L) of handling remainder fe in the water of back is far below state specified standards (0.3mg/L), and production cost is lower.In addition, owing to contain chlorate anions, hypochlorite plasma in polymer phosphate ferric sulfate product, it has cohesion and germ-resistant dual function simultaneously.With poly-aluminium, among the contrast experiment that traditional coagulating agent such as poly-iron carry out, the product of the inventive method preparation has embodied remarkable advantages on cleaning water, its turbidity removal rate has improved more than 40%, chroma removal rate has improved more than 35%, clearance to COD reaches more than 90%, no matter at the former water (>300 NTU) of handling high turbidity, when still handling the raw water quality (about 10NTU) of low-temperature and low turbidity, it removes turbidity, the effect of colourity is more remarkable, and dosage saves 60-70% than polymerize aluminum chloride, than saving 25-30% with the poly-iron product of traditional method preparation.
Specific embodiments
The step of preparation method embodiment 1 of the present invention is:
(1) at normal temperatures, with 58 kilograms FeSO 47H 2The mixture that O and 10 kilograms of concentration are 98% vitriol oil and 40 kilograms of concentration are 1.8% ClO 2Aqueous solution reaction 30 minutes;
(2) in (1) products therefrom, add 19 kilograms of solid NaH 2PO 4Increase poly-, its PO 4 3-/ Fe mole ratio is 0.08;
(3) finished product.
Utilize above step can make liquid product.
In the product of producing with aforesaid method, all iron content: 220g/L, ferrous ion content<1g/L, heavy metal content<10mg/L, basicity (basicity) is 18%, the pH value when product is made into 1% aqueous solution is 2.7.
The production cost of the liquid product of producing with aforesaid method is about 350 yuan/ton.
The step of preparation method embodiment 2 of the present invention is:
(1) at normal temperatures, with 61 kilograms FeSO 48H 2The mixture that O and 10 kilograms of concentration are 98% vitriol oil and 38 kilograms of concentration are 2% ClO 2Aqueous solution reaction 40 minutes;
(2) in (1) products therefrom, add solid Na 2HPO 417.1 it is poly-that kilogram increases, its PO 4 3-/ Fe mole ratio is 0.11;
(3) oven dry is sent (2) products therefrom into drying cylinder.After in it enters the drying cylinder kerve, contact with red-hot drying cylinder outside surface, service temperature is controlled at 120-140 degree centigrade; Dry in rotation, the place scrapes to scraper;
(4) finished product (solid product).
The production cost of the solid product of producing with aforesaid method is about 970 yuan/ton.
The step of preparation method embodiment 3 of the present invention is:
(1) at normal temperatures, with 61 kilograms FeSO 48H 2The mixture that O and 10 kilograms of concentration are 98% vitriol oil and 38 kilograms of concentration are 2.2% ClO 2Aqueous solution reaction 30 minutes;
(2) in (1) products therefrom, add 14.6 kilograms of solid tripoly phosphate sodium STPPs increase poly-, its PO 4 3-/ Fe mole ratio is 0.08;
(3) finished product (liquid product).
The solid of producing with the inventive method and the using method of liquid product are: solid phase prod directly adds in the dissolving tank between water factory's dosing, stirs with machine mixer can add in the ingress of raw water pipeline or reaction tank with volume pump or impeller pump in 20 minutes; Liquid product adds in raw water pipeline or the ingress of reaction tank with volume pump or impeller pump before use after dissolving tank dilution 2-3 stirs 20 minutes doubly and with machine mixer.The solid phase prod dosage is 1.6-1.9 kilogram/former water of ton (this moment, raw water turbidity was at 5-29NTU), the 2.2-2.8 kilogram/former water of ton (this moment, raw water turbidity was at 30-1500NTU); The liquid product dosage is 5.0-5.7 kilogram/former water of ton (this moment, raw water turbidity was at 5-29NTU), the 5.0-8.4 kilogram/former water of ton (this moment, raw water turbidity was at 30-1500NTU).

Claims (2)

1, the preparation method of polymer phosphate ferric sulfate is characterized in that:
(1) at normal temperatures, react the mixture of the ferrous sulfate and the vitriol oil and the aqueous solution of dioxide peroxide more than 30 minutes; Wherein the concentration of aqueous solution of dioxide peroxide is 1.8-2.2%, and ferrous sulfate is FeSO 4NH 2O, the span of n is between 0-8, and the concentration of the vitriol oil is more than 98%; Mass parts between ferrous sulfate, the vitriol oil, the aqueous solution of chlorine dioxide is than being (5.8-6.1): 1: (3.8-4.0);
(2) in (1) products therefrom, add inorganic phosphate increase poly-, PO 4 3-/ FeMole ratio is 0.08-0.11;
(3) finished product.
2, the method for claim 1 is characterized in that: inorganic phosphate is NaH 2PO 4Or Na 2HPO 4Or tripoly phosphate sodium STPP, inorganic phosphate adds in the solid mode.
CNA031254160A 2003-09-15 2003-09-15 Method for preparing polymeric ferric phosphate sulfate Pending CN1524800A (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
CNA031254160A CN1524800A (en) 2003-09-15 2003-09-15 Method for preparing polymeric ferric phosphate sulfate

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CN1524800A true CN1524800A (en) 2004-09-01

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101805051A (en) * 2010-04-06 2010-08-18 重庆大学 Compound phosphoric polyferric sulfate flocculant and production method thereof
CN104556323A (en) * 2013-10-18 2015-04-29 乔占印 Rare-earth polymeric ferrophosphorus sulfate and preparation method thereof
CN108083400A (en) * 2017-12-21 2018-05-29 上海万狮环保科技有限公司 A kind of preparation method of phosphorous polyiron sulfate and its application for handling coking wastewater
CN110092456A (en) * 2019-04-01 2019-08-06 广西大学 The method for preparing solid phosphoric polyferric sulfate flocculant

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101805051A (en) * 2010-04-06 2010-08-18 重庆大学 Compound phosphoric polyferric sulfate flocculant and production method thereof
CN101805051B (en) * 2010-04-06 2012-07-25 重庆大学 Compound phosphoric polyferric sulfate flocculant and production method thereof
CN104556323A (en) * 2013-10-18 2015-04-29 乔占印 Rare-earth polymeric ferrophosphorus sulfate and preparation method thereof
CN108083400A (en) * 2017-12-21 2018-05-29 上海万狮环保科技有限公司 A kind of preparation method of phosphorous polyiron sulfate and its application for handling coking wastewater
CN110092456A (en) * 2019-04-01 2019-08-06 广西大学 The method for preparing solid phosphoric polyferric sulfate flocculant

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