CN101786708A - Iron-based flocculating agent and preparation method thereof - Google Patents
Iron-based flocculating agent and preparation method thereof Download PDFInfo
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- CN101786708A CN101786708A CN 201010116600 CN201010116600A CN101786708A CN 101786708 A CN101786708 A CN 101786708A CN 201010116600 CN201010116600 CN 201010116600 CN 201010116600 A CN201010116600 A CN 201010116600A CN 101786708 A CN101786708 A CN 101786708A
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Abstract
The invention provides a kind of iron-based flocculating agent and preparation method thereof, the chemical formula of this iron-based flocculating agent is [Fe
2(OH)
n(SO
4)
3-n/2]
mAlkaline ferrum sulfuricum oxydatum solutum, n 〉=1 wherein, and m is below 100, concentration of iron is 50g/l～200g/l, SO
4 2-With the molar ratio of Fe greater than 0.5 and less than 1.5.Iron-based flocculating agent of the present invention and preparation method thereof has solved the defective of prior art, obtains high force of flocculation, and makes simply iron-based flocculating agent with low cost.
Description
Technical field
The embodiment of the invention relates to iron-based flocculating agent and preparation method thereof, relates in particular to a kind of cheaply and simply preparation method who is used for iron-based flocculating agent and this iron-based flocculating agent of sewage disposal use.
Background technology
Be used for water, following water, the no material flocculation agent that plant drainage is handled has Tai-Ace S 150, the poly aluminium chloride (PAC) of aluminium system, and ferrous sulfate, iron(ic) chloride and the polyiron sulfate etc. of iron system.
Tai-Ace S 150 is represented aluminium system, and its history is the longest, but force of flocculation is weak and mud (sludge) that produce is many, is difficult to handle.Developed poly aluminium chloride (PAC) for improvement, force of flocculation is improved, but the mud problem is not resolved.
On the other hand, the flocculation PH of ferrous sulfate is very high more than 9, and the usage quantity of alkali is many, the processing cost height.
Iron(ic) chloride is the representative of iron-based flocculating agent, and is serious to equipment corrosion, and the sludge high temperature that is found Cl and generation produces Dioxins when handling, and uses hardly now.
Polyiron sulfate is that the present inventor propose for No. 842085 in patent, through what the copperas solution oxidation was obtained, is expressed as [Fe
2(OH) n (SO
4)
2-n/2] m, O＜n＜l, m=f (n).
Its shortcoming is owing to being to utilize oxidation to import the OH base in ferrous sulfate, so n can not can't improve force of flocculation greater than 1.
In addition, the present inventor has studied again and has used iron filings, and iron powder has proposed special permission 11-292546 number as raw material.This is to be the center with the sulfuric acid dissolution iron material, rather than considers to import the OH base.
Summary of the invention
The embodiment of the invention provides a kind of iron-based flocculating agent and preparation method thereof, in order to solve the defective of above-mentioned prior art, obtains high force of flocculation, and makes simply iron-based flocculating agent with low cost.
The invention provides a kind of iron-based flocculating agent in order to achieve the above object, its chemical formula is [Fe
2(OH)
n(SO
4)
3-n/2]
mAlkaline ferrum sulfuricum oxydatum solutum, n 〉=1 wherein, and m is below 100, concentration of iron is 50g/l～200g/l, SO
4 2-With the molar ratio of Fe greater than 0.5 and less than 1.5.
The present invention also provides a kind of preparation method of iron-based flocculating agent in order to achieve the above object, comprising:
Step 1, preparation contain the above ferrous iron of 50g/L, SO
4 2-With the molar ratio of Fe greater than 0.5 and less than 1.5 the sulphuric acid soln that contains ferrous sulfate;
Step 2, under PH is condition below 0.5, carrying out oxidation below 80 ℃.
The preparation method of above-mentioned iron-based flocculating agent in the wherein said step 2, carries out oxidation under 50 ℃～60 ℃ temperature ranges.
The preparation method of above-mentioned iron-based flocculating agent, the sulphuric acid soln that contains ferrous sulfate described in the wherein said step 1 is iron filings or iron powder are dissolved in sulfuric acid and get.
The preparation method of above-mentioned iron-based flocculating agent in the wherein said step 2, carries out oxidation by hydrogen peroxide.
The present invention who obtains by all research has following beneficial effect and advantage:
1, by with iron filings, iron powder etc. below 80 ℃, preferably oxidation under 60 ℃～50 ℃ temperature has realized dissolving fully SO
4The molar ratio of/Fe is lower than the effect of 1.0 supersaturated solution;
2, by also quantitatively splashing into the method that the vitriol oil slowly dilutes the vitriol oil of iron on a small quantity, simple realization the maintenance solvent temperature below 80 ℃, preferably 60 ℃～50 ℃ effect, avoided rapid temperature variation to cause detrimentally affect, and do not need special control heating refrigerative device, method is simple, and with low cost.
3, under certain condition, promptly PH under the condition below 0.5, is carrying out below 80 ℃, dissolves and oxidation in preferred 60 ℃～50 ℃ scopes, has obtained the force of flocculation more increased compared to existing technology, has improved sewage treatment capacity.
4, utilize hydrogen peroxide as oxygenant, can cause the reaction of hydrogen peroxide and iron, produce the oxygen (O) of OH free radical and status nascendi (nascent state), because the two response capacity is all strong, particularly the oxygen of status nascendi can activate other oxygen, quickens the oxidation of iron.
Embodiment
For the purpose, technical scheme and the advantage that make the embodiment of the invention is clearer, below the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that is obtained under the creative work prerequisite.
By research to prior art, the contriver think can not make n value (with basicity, overlap ratio is relevant) surpass 1 be because, the cause of ferrous sulfate being carried out oxidation.Such as immediately using iron filings, iron powder during blast-furnace slag, is also handled with sulfuric acid, makes ferrous sulfate, then it is carried out oxidation.Therefore, among the present invention, emphatically at SO
4The molar ratio of/Fe improves the n value.
Of the present inventionly contain ferrous iron more than the 50g/L, SO by preparation
4 2-With the molar ratio of Fe greater than 0.5 and less than 1.5 the sulphuric acid soln that contains ferrous sulfate, and under PH is condition below 0.5, carrying out oxidation below 80 ℃, having obtained chemical formula is [Fe
2(OH)
n(SO
4)
3-n/2]
mAlkaline ferrum sulfuricum oxydatum solutum, n 〉=1 wherein, and m is below 100, concentration of iron is 50g/l～200g/l, SO
4 2-With the molar ratio of Fe greater than 0.5 and less than 1.5.
The method of prior art is an oxidation sulfuric acid ferrous sulphuric acid soln, so T-SO
4The molar ratio of/T-Fe can't be lower than 1.
The present invention owing to adopted metallic irons such as iron filings, iron powder, therefore can regulate SO when dissolving
4Concentration and the concentration of Fe, realized 0.5＜SO
4The molar ratio of/Fe＜1.5.Because can produce the precipitation of alkaline ferric sulfate, this value can not be lower than 0.5.
Also having, temperature is fixed on below 80 ℃, also is because can produce the sedimentary cause of alkaline ferric sulfate more than 80 ℃.
In addition, ferric existence can make the dissolving of iron accelerate, and can obtain the iron liquid of high density, the easy polymerization of oxidation in this state.
The present invention uses hydrogen peroxide, when making oxidation not pure component sneak into, the control of temperature of reaction is easy.
The present invention adopts the vitriol oil, can effectively utilize the solution heat of the vitriol oil, controls solvent temperature easily.Particularly, the intermittent interpolation vitriol oil is temperature controlled a kind of mode.
Below, with specific embodiment and comparative experiments, further specify effect of the present invention.
Embodiment 1:
Adding iron powder 320g to the vitriol oil and water, to mix the concentration that obtains be among the sulphuric acid soln 1.8L of 100g/L, dissolves at 60 ℃, and then, each a small amount of vitriol oil that adds makes temperature be no more than 60 ℃, makes SO
4The molar ratio of/Fe reaches 0.75; After testing, the Fe of the solution that obtains is 160g/L, SO
4Be 207g/L; With above-mentioned solution H
2O
2Obtain the polyiron sulfate of 2L after the oxidation.
In order to compare, use the draining of chemical oxygen demand (COD) (COD), result such as following table 1 as 3000ppm with existing product:
| Addition | ??(ppm) | ??300 | ??1000 | ??2000 | ??5000 |
| Existing product | ??COD | ??1000 | ??200 | ??100 | ??10 |
| The present invention | ??COD | ??900 | ??150 | ??60 | ??5 |
Embodiment 2
Adding iron filings 320g to the vitriol oil and water, to mix the concentration that obtains be among the concentrated sulfuric acid solution 1.8L of 100g/L, and this moment, temperature was 55 ℃.Then, add that a certain amount of (2～5cc) the vitriol oil keeps 60 ℃.All after the dissolving, measurement result is that Fe is 160g/L, and SO4 is 270g/L (molar ratio of SO4/Fe is 0.98).With above-mentioned solution H
2O
2Obtain the polyiron sulfate of 2L after the oxidation.
Use COD to handle and carry out than hinge result such as following table 2 as the draining retrogradation of 3000ppm.
| Addition | ??(ppm) | ??0 | ??300 | ??1000 | ??2000 | ??5000 |
| Existing product | ??COD | ??3000 | ??1000 | ??200 | ??100 | ??10 |
| The present invention's product | ??COD | ??3000 | ??800 | ??170 | ??50 | ??4 |
Embodiment 3
Adding iron filings 320g to the vitriol oil and water, to mix the concentration that obtains be among the concentrated sulfuric acid solution 1.8L of 150g/L, and this moment, temperature was 58 ℃.Add vitriol oil 2cc/ branch, keep 67 ℃.Fe is 160g/L in the solution that obtains, SO
4Be 400g/L (molar ratio of SO4/Fe is 1.46).With above-mentioned solution H
2O
2Obtain the polyiron sulfate of 2L after the oxidation.
Use draining retrogradation result such as the following table 3 of COD as 3000ppm.
| Addition | ??(ppm) | ??0 | ??300 | ??1000 | ??2000 | ??5000 |
| Existing product | ??COD | ??3000 | ??1000 | ??200 | ??100 | ??10 |
| The present invention's product | ??COD | ??3000 | ??850 | ??170 | ??55 | ??5 |
Embodiment 4
Adding iron filings 320g to the vitriol oil and water, to mix the concentration that obtains be among the concentrated sulfuric acid solution 1.8L of 150g/L, is heated to temperature and reaches 78 ℃.Add vitriol oil 2cc/ branch, keep 78 ℃.Fe is 160g/L in the solution that obtains, SO
4Be 400g/L (molar ratio of SO4/Fe is 1.46).With above-mentioned solution H
2O
2Obtain the polyiron sulfate of 2L after the oxidation.
Use draining retrogradation result such as the following table 4 of COD as 3000ppm.
| Addition | ??(ppm) | ??0 | ??300 | ??1000 | ??2000 | ??5000 |
| Existing product | ??COD | ??3000 | ??1000 | ??200 | ??100 | ??10 |
| The present invention's product | ??COD | ??3000 | ??870 | ??180 | ??60 | ??6 |
It should be noted that at last: above embodiment only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that: it still can be made amendment to the technical scheme that aforementioned each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution break away from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (5)
1. iron-based flocculating agent, its chemical formula is [Fe
2(OH)
n(SO
4)
3-n/2]
mAlkaline ferrum sulfuricum oxydatum solutum, n 〉=1 wherein, and m is below 100, concentration of iron is 50g/l～200g/l, SO
4 2-With the molar ratio of Fe greater than 0.5 and less than 1.5.
2. the preparation method of an iron-based flocculating agent comprises:
Step 1, preparation contain the above ferrous iron of 50g/L, SO
4 2-With the molar ratio of Fe greater than 0.5 and less than 1.5 the sulphuric acid soln that contains ferrous sulfate;
Step 2, carrying out oxidation below 80 ℃.
3. the preparation method of iron-based flocculating agent according to claim 2 in the wherein said step 2, carries out oxidation under 50 ℃～60 ℃ temperature ranges.
4. the preparation method of iron-based flocculating agent according to claim 2, the sulphuric acid soln that contains ferrous sulfate described in the wherein said step 1 is iron filings or iron powder are dissolved in sulfuric acid and get.
5. the preparation method of iron-based flocculating agent according to claim 2 in the wherein said step 2, carries out oxidation by hydrogen peroxide.
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|---|---|---|---|
| CN 201010116600 CN101786708A (en) | 2010-03-01 | 2010-03-01 | Iron-based flocculating agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010116600 CN101786708A (en) | 2010-03-01 | 2010-03-01 | Iron-based flocculating agent and preparation method thereof |
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| CN101786708A true CN101786708A (en) | 2010-07-28 |
Family
ID=42530109
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111675295A (en) * | 2020-04-28 | 2020-09-18 | 西北矿冶研究院 | Preparation method of efficient flocculant for purifying acid mine wastewater |
| CN114466824A (en) * | 2019-09-30 | 2022-05-10 | 日铁矿业株式会社 | High-concentration iron-series flocculant and production 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 |
| CN117542997A (en) * | 2024-01-04 | 2024-02-09 | 河南师范大学 | Preparation method of carbon-coated basic ferric potassium sulfate ion battery anode material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000016816A (en) * | 1998-06-30 | 2000-01-18 | Nittetsu Mining Co Ltd | Efficient production of high-purity ferric polysulfate |
-
2010
- 2010-03-01 CN CN 201010116600 patent/CN101786708A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000016816A (en) * | 1998-06-30 | 2000-01-18 | Nittetsu Mining Co Ltd | Efficient production of high-purity ferric polysulfate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114466824A (en) * | 2019-09-30 | 2022-05-10 | 日铁矿业株式会社 | High-concentration iron-series flocculant and production method thereof |
| CN111675295A (en) * | 2020-04-28 | 2020-09-18 | 西北矿冶研究院 | Preparation method of efficient flocculant for purifying acid mine wastewater |
| 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 |
| CN117542997A (en) * | 2024-01-04 | 2024-02-09 | 河南师范大学 | Preparation method of carbon-coated basic ferric potassium sulfate ion battery anode material |
| CN117542997B (en) * | 2024-01-04 | 2024-04-16 | 河南师范大学 | Preparation method of carbon-coated basic ferric potassium sulfate ion battery anode material |
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Effective date of abandoning: 20100728 |