CN103626274A - Method for preparing flocculating agent - Google Patents
Method for preparing flocculating agent Download PDFInfo
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- CN103626274A CN103626274A CN201310709577.5A CN201310709577A CN103626274A CN 103626274 A CN103626274 A CN 103626274A CN 201310709577 A CN201310709577 A CN 201310709577A CN 103626274 A CN103626274 A CN 103626274A
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- Prior art keywords
- rust
- rust cleaning
- iron
- filtrate
- aging
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- Treatment Of Water By Oxidation Or Reduction (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a method for preparing a flocculating agent. The method comprises the following steps of (a) collecting aged rust-oil removing agents; (b) adding ferric oxide powder or waste iron rust in the aged rust-oil removing agents, reacting for 1-2 hours, and then filtering; (c) adding iron chips to filter liquor obtained from the step (b), reacting for 1-2 hours, then filtering, and measuring the content of ferrous ions contained in the filter liquor; (d) adding an oxidizing agent, increasing temperature to 50-70 DEG C to oxidize for 1-2 hours, then reducing the temperature to room temperature, and filtering to obtain the flocculating agent. The method disclosed by the invention can be used for processing the aged rust-oil removing agents into the flocculating agent; the method disclosed by the invention can not only be used for harmlessly treating the aged rust-oil removing agents, but also be used for recycling the resources because other raw materials used for the method can be the waste iron rust and the waste iron chips in industrial production, thereby achieving higher environmental benefit and economic benefit.
Description
Technical field
The present invention relates to a kind of preparation method of flocculation agent, specifically utilize aging salt acid type rust cleaning degreaser to prepare the method for flocculation agent.
Background technology
Ferrous materials, due to the airborne oxygen of Long Term Contact and moisture, very easily gets rusty, and the application of rust cleaning degreaser is necessary very much.Conventional rust cleaning degreaser is salt acid type or sulfuric acid type rust cleaning degreaser, iron rust composition is mainly ferric oxide or Z 250, hydrochloric acid reacts with iron rust, generate iron(ic) chloride or iron protochloride, therefore how but the discharge meeting of aging rust cleaning degreaser causes severe contamination to environment, the rust cleaning degreaser for the treatment of of aged becomes comparison stubborn problem.
Poly-ferric chloride claims again alkali formula iron(ic) chloride, is called for short PFC, is a kind of novel efficient inorganic molecular flocculant, and chemical formula is [Fe
2(OH)
ncl
6-n]
m.Poly-ferric chloride is mainly liquid product at present, and outward appearance is that sorrel is opaque, has soluble in waterly, and flocculating property is good, to the advantage such as the subject range of temperature, water quality and pH is wide.The applicable pH value scope of poly-ferric chloride is 9～11, and the flco density of formation is large, easily precipitates, and when low temperature or high turbidity, effect is still fine.The flocculation mechanism of poly-ferric chloride is identical with polymerize aluminum chloride, and the Polyferric Sulfate hydroxyl coordination ion providing in water has very strong adsorptive power to the particle being suspended in water, and ultra's flocculating effect is better than to other Polyferric Sulfates, and mud is had to strong dehydration.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of flocculation agent, the aging salt acid type rust cleaning degreaser of mainly take is raw material, not only can the aging rust cleaning degreaser of harmless treatment, and make resource obtain cycling and reutilization, make the flocculation agent that can be used for sewage disposal, there is higher environmental benefit and economic benefit.
The technical scheme that the present invention takes is to provide a kind of preparation method of flocculation agent, comprises the following steps:
A) collect aging rust degreaser;
B) in aging rust cleaning degreaser, add brown iron oxide or scrap iron rust, react 1～2 hour, filter, collect filtrate;
C) in the filtrate of step b), add excessive iron filings, after completion of the reaction, filter, collect filtrate, measure filtrate Central Asia iron ion content;
D) according to the ferrous ion content recording, in the filtrate of step c), add oxygenant, the mol ratio of oxygenant and ferrous ion is (1～1.5): (2～6), be warming up to 50～70 ℃, react after 1～2 hour and be cooled to room temperature, filter and obtain flocculation agent.
Described aging rust cleaning degreaser refers to the salt acid type rust cleaning degreaser that loses effective rust cleaning oil removing ability, aging rust cleaning degreaser can not meet the requirement of producing upper rust cleaning oil removing process again, if directly resource is not only wasted in discharge, also can be to environment.
Described brown iron oxide can be commercially available brown iron oxide, can be also the spent ferric oxide producing in industrial production.
Described iron filings are the waste iron filing producing in the iron and steel course of processing.
Described oxygenant is KClO
3, hydrogen peroxide or ozone.
First collect aging salt acid type rust cleaning degreaser, wherein mainly contain FeCl
2, FeCl
3, hydrochloric acid and water, add after brown iron oxide, brown iron oxide can with hydrochloric acid reaction wherein, in and hydrochloric acid, product is FeCl
3and FeCl
2, reaction equation is as follows:
Fe
2O
3?＋?6HCl?＝?2FeCl
3?＋?3H
2O
FeO?＋?2HCl?＝?FeCl
2?＋?H
2O
But, prepare flocculation agent, just need FeCl
3there is enough concentration, depend merely on aging rust cleaning degreaser and can't meet concentration demand, can first use fe (iron filings) by FeCl
3be reduced to FeCl
2, meanwhile, iron can also react with unnecessary hydrochloric acid, also generates FeCl
2, like this, FeCl
2content will increase, then with oxygenant by Fe
2+be oxidized to Fe
3+, meanwhile, Fe
3+partial hydrolysis occurs, and polymerization generates poly-ferric chloride.
Iron and FeCl
3or the equation of hydrochloric acid reaction is as follows:
Fe＋?2HCl?＝?FeCl
2?＋?H
2
2FeCl
3?＋?Fe?＝?3?FeCl
2
FeCl
2with oxygenant (KClO
3, hydrogen peroxide, ozone) react and be hydrolyzed, polymerization generates poly-ferric chloride ([Fe
2(OH)
ncl
6-n]
m) equation as follows:
6FeCl
2?+?KClO
3?+?6HCl=6FeCl
3?+?KCl+?3H
2O
2FeCl
2?+?H
2O
2?+?2HCl=2FeCl
3?+?2H
2O
2FeCl
2?+?O
3?+?2HCl=2FeCl
3?+?H
2O?+O
2
mFeCl
3?+nH
2O=[Fe
2(OH)
nCl
6-n]
m
The present invention makes poly-ferric chloride solution (flocculation agent) by aging rust cleaning degreaser, the reaction raw materials of using in preparation method can be industrial scrap iron rust, waste iron filing, both made the flocculation agent that can be used for sewage disposal, again can the aging rust cleaning degreaser of harmless treatment, make resource obtain cycling and reutilization, there is higher environmental benefit and economic benefit.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment mono-:
The preparation method of flocculation agent, comprises the following steps:
A) collect in salt acid type rust cleaning degreaser to the first reactor aging in steel derusting oil removing process;
B) to adding scrap iron rust in the first reactor, (main component is Fe
2o
3and FeO), in aging rust cleaning degreaser, remaining HCl reacts with iron rust 1 hour, and temperature of reaction is 80 ℃, generates FeCl
3and FeCl
2, after completion of the reaction, to filter, filtrate adds in the second reactor;
C) in the second reactor, add waste iron filing (composition is Fe), the FeCl in solution
3with iron generation redox reaction, generate FeCl
2, meanwhile, remaining HCl also reacts with iron and generates FeCl
2, after completion of the reaction, filter, filtrate is added in the 3rd reactor, measure the content of ferrous ion in the 3rd reactor;
D) according to the content of the ferrous ion recording, by the speed of every 5 minutes 1 g/L, in the 3rd reactor, add oxygenant KClO
3, the amount of oxygenant is 1:6 with the mol ratio of the ferrous ion recording, and is warming up to 60 ℃, reacts 1.5 hours, makes Fe
2+by KClO
3be oxidized to Fe
3+, while Fe
3+there is partial hydrolysis, and aggregate into flocculation agent, then, be cooled to room temperature, filter and obtain flocculant poly iron(ic) chloride.
Adopt aforesaid method can obtain sewage disposal flocculant poly iron(ic) chloride, transformation efficiency is 76%.
Embodiment bis-:
The preparation method of flocculation agent, comprises the following steps:
A) collect in salt acid type rust cleaning degreaser to the first reactor aging in steel derusting oil removing process;
B) to adding scrap iron rust in the first reactor, (main component is Fe
2o
3and FeO), in aging rust cleaning degreaser, remaining HCl reacts with iron rust 2 hours, and temperature of reaction is 60 ℃, generates FeCl
3and FeCl
2, after completion of the reaction, to filter, filtrate adds in the second reactor;
C) in the second reactor, add waste iron filing (composition is Fe), the FeCl in solution
3with iron generation redox reaction, generate FeCl
2, meanwhile, remaining HCl also reacts with iron and generates FeCl
2, after completion of the reaction, filter, filtrate is added in the 3rd reactor, measure the content of ferrous ion in the 3rd reactor;
D) according to the content of the ferrous ion recording, by the speed of every 5 minutes 1 g/L, in the 3rd reactor, add oxidant hydrogen peroxide, the amount of oxygenant is 1:2 with the mol ratio of the ferrous ion recording, and is warming up to 50 ℃, reacts 2 hours, makes Fe
2+by hydrogen peroxide oxidation, be Fe
3+, while Fe
3+there is partial hydrolysis, and aggregate into flocculation agent, then, be cooled to room temperature, filter and obtain flocculant poly iron(ic) chloride.
Adopt aforesaid method can obtain trade effluent flocculant poly iron(ic) chloride, transformation efficiency is 68%.
Embodiment tri-:
The preparation method of flocculation agent, comprises the following steps:
A) collect in salt acid type rust cleaning degreaser to the first reactor aging in steel derusting oil removing process;
B) to adding brown iron oxide in the first reactor, (main component is Fe
2o
3), in aging rust cleaning degreaser, remaining HCl reacts with iron rust 1.5 hours, and temperature of reaction is 70 ℃, generates FeCl
3and FeCl
2, after completion of the reaction, to filter, filtrate adds in the second reactor;
C) in the second reactor, add waste iron filing (composition is Fe), the FeCl in solution
3with iron generation redox reaction, generate FeCl
2, meanwhile, remaining HCl also reacts with iron and generates FeCl
2, after completion of the reaction, filter, filtrate is added in the 3rd reactor, measure the content of ferrous ion in the 3rd reactor;
D) according to the content of the ferrous ion recording, by the speed of every 5 minutes 1 g/L, in the 3rd reactor, pass into oxidant, ozone, the amount of oxygenant is 1.5:2 with the mol ratio of the ferrous ion recording, and is warming up to 70 ℃, reacts 1 hour, makes Fe
2+by ozone oxidation, be Fe
3+, while Fe
3+there is partial hydrolysis, and aggregate into flocculation agent, then, be cooled to room temperature, filter and obtain flocculant poly iron(ic) chloride.
Adopt aforesaid method can obtain trade effluent flocculation agent, transformation efficiency is 90%.
Claims (2)
1. the preparation method of flocculation agent, comprises the following steps:
A) collect aging rust cleaning degreaser;
B) in aging rust cleaning degreaser, add brown iron oxide or scrap iron rust, react 1～2 hour, filter, collect filtrate;
C) in the filtrate of step b), add excessive iron filings, after completion of the reaction, filter, collect filtrate, measure filtrate Central Asia iron ion content;
D) according to the ferrous ion content recording, in the filtrate of step c), add oxygenant, the mol ratio of oxygenant and ferrous ion is (1～1.5): (2～6), be warming up to 50～70 ℃, react after 1～2 hour and be cooled to room temperature, filter and obtain flocculation agent;
Described aging rust cleaning degreaser refers to the salt acid type rust cleaning degreaser that loses rust cleaning oil removing ability.
2. rust cleaning degreaser method for treating waste liquid according to claim 1, is characterized in that: the oxygenant described in step d) is KClO
3, hydrogen peroxide or ozone.
Priority Applications (1)
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|---|---|---|---|
| CN201310709577.5A CN103626274A (en) | 2013-12-21 | 2013-12-21 | Method for preparing flocculating agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310709577.5A CN103626274A (en) | 2013-12-21 | 2013-12-21 | Method for preparing flocculating agent |
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| Publication Number | Publication Date |
|---|---|
| CN103626274A true CN103626274A (en) | 2014-03-12 |
Family
ID=50207773
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|---|---|---|---|
| CN201310709577.5A Pending CN103626274A (en) | 2013-12-21 | 2013-12-21 | Method for preparing flocculating agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115771991A (en) * | 2022-12-12 | 2023-03-10 | 安徽省通源环境节能股份有限公司 | Polymeric aluminum ferric silicate sludge conditioner and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000264640A (en) * | 1999-03-17 | 2000-09-26 | Tsurumi Soda Co Ltd | Treatment of waste liquor of hydrochloric acid |
| CN101172727A (en) * | 2007-10-16 | 2008-05-07 | 中冶南方工程技术有限公司 | Waste hydrochloric acid liquid cleaning treatment technique |
| CN101717123A (en) * | 2009-12-01 | 2010-06-02 | 浙江温州轻工研究院 | Method for preparing modified poly-ferric chloride coagulant |
| CN103073067A (en) * | 2013-02-02 | 2013-05-01 | 梁锡明 | Method for producing ferric chloride by using pickle liquor |
-
2013
- 2013-12-21 CN CN201310709577.5A patent/CN103626274A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000264640A (en) * | 1999-03-17 | 2000-09-26 | Tsurumi Soda Co Ltd | Treatment of waste liquor of hydrochloric acid |
| CN101172727A (en) * | 2007-10-16 | 2008-05-07 | 中冶南方工程技术有限公司 | Waste hydrochloric acid liquid cleaning treatment technique |
| CN101717123A (en) * | 2009-12-01 | 2010-06-02 | 浙江温州轻工研究院 | Method for preparing modified poly-ferric chloride coagulant |
| CN103073067A (en) * | 2013-02-02 | 2013-05-01 | 梁锡明 | Method for producing ferric chloride by using pickle liquor |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115771991A (en) * | 2022-12-12 | 2023-03-10 | 安徽省通源环境节能股份有限公司 | Polymeric aluminum ferric silicate sludge conditioner and preparation method thereof |
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Application publication date: 20140312 |