CN104118974A - Method for treating silicon sludge obtained by neutralizing steel pickling waste liquid, removing silicon and filtering - Google Patents

Method for treating silicon sludge obtained by neutralizing steel pickling waste liquid, removing silicon and filtering Download PDF

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Publication number
CN104118974A
CN104118974A CN201410279961.0A CN201410279961A CN104118974A CN 104118974 A CN104118974 A CN 104118974A CN 201410279961 A CN201410279961 A CN 201410279961A CN 104118974 A CN104118974 A CN 104118974A
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China
Prior art keywords
waste liquid
silicon
silicon sludge
iron
sludge
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Pending
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CN201410279961.0A
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Chinese (zh)
Inventor
熊天庆
熊新宇
唐胜卫
远洋
石入峰
陈志海
蒯勇
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MAANSHAN HUAQING ENVIRONMENTAL ENGINEERING Co Ltd
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MAANSHAN HUAQING ENVIRONMENTAL ENGINEERING Co Ltd
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Priority to CN201410279961.0A priority Critical patent/CN104118974A/en
Publication of CN104118974A publication Critical patent/CN104118974A/en
Pending legal-status Critical Current

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  • Removal Of Specific Substances (AREA)

Abstract

The invention discloses a method for treating silicon sludge obtained by neutralizing steel pickling waste liquid, removing silicon and filtering. The method comprises the following steps: firstly, throwing silicon sludge and industrial hydrochloric acid into a reactor, wherein the mass ratio of silicon sludge to industrial hydrochloric acid is 1: 2, heating while stirring and controlling the temperature at 50-65 DEG C; secondly, after the reaction in the first step is completed, cooling to room temperature, and putting sodium chlorate according to the condition that a mass ratio of the silicon sludge to sodium chlorate is 1:0.017 into the reactor; thirdly, adjusting the pH value of the entire reaction and controlling the content of the HCl at less than or equal to 0.5%; fourthly, cooling and filtering to remove crystallized impurities and recycling ferric chloride and ammonium chloride. The method is a relatively effective method of regenerating silicon-removal sludge from steel pickling waste liquid, available iron and total iron are not only utilized and but also the problem of the treatment of sludge waste liquid is solved, no secondary waste solid is generated, the content of available iron in produced liquid ferric chloride is above 8%, the method can be widely applied in the wastewater treatment industry and the cost of the product is 40% of that of the commercially available products.

Description

A kind of iron and steel pickling waste liquid is except the treatment process of silicon sludge
Technical field
The present invention relates to a kind of process field of mud, particularly a kind of iron and steel pickling waste liquid is except the treatment process of silicon sludge.
Background technology
Iron and steel pickling waste liquid removes silicon sludge and refers in pickle solution and desiliconization, and the silicon sludge obtaining after filtration is called for short silicon sludge.
The major ingredient of silicon sludge is Fe (OH) 3, Fe (OH) 2, FeCl 2, NH 4cl etc., all iron content 40%-50%, it is yellow that color is.Domestic basic employing landfill disposal, expense is high, and the wasting of resources easily produces secondary pollution, and this mud and alkaline ashes are mixed into steel sintering system by some unit in addition, on-the-spot irritant smell, and also fire bars has latch up phenomenon.
Application number: 201110278314.4, denomination of invention is a kind of waste sludge recycle and the technological method that reclaims Z 250 again after dehydration utilizing after pickling iron and steel Industrial Wastewater Treatment for " regeneration of mud and recovery Z 250 technology after steel pickling waste liquor neutralizing treatment " discloses.Present method is the industrial waste mud that the acid-washing waste acid waste water of pickling iron and steel industry is produced after sewage disposal, after dehydration, again as basic agent, spent acid waste water is carried out neutralizing treatment and remove the free acid in waste acid water, after making sour water pH value reach the neutrality of 6-7 and mud synthetic Fe 3 O 4 magnetic sludge settling under the condition of heating, precipitation, with obtaining the above nano level Z 250 of metallic iron iron-holder 50% filter cake after the liquid-solid separation of pressure filter, is used for to the breeze raw material of smelting iron and steel as recovery.
But the method also cannot be removed the silicon in spent acid, and waste liquid, still to environment, also can produce secondary solid waste simultaneously.
The mud of currently available technology after for iron and steel pickling waste liquid desiliconization does not have good treatment process.
Summary of the invention
For solving the problems of the technologies described above, the invention provides following technical scheme:
Iron and steel pickling waste liquid is except a treatment process for silicon sludge, and its step is as follows:
Step 1, drop into silicon sludge and technical hydrochloric acid to reactor, the mass ratio of silicon sludge and technical hydrochloric acid is 1:2, and stir on intensification limit, limit, and temperature is controlled at 50-65 DEG C;
After step 2, step 1 react completely, be cooled to normal temperature, drop into sodium chlorate according to silicon sludge and sodium chlorate mass ratio 1:0.017;
Step 3, regulate the acid-basicity of whole reactant, control HCl content≤0.5%;
Step 4, cold filtration are removed crystalline impurities, reclaim iron(ic) chloride, ammonium chloride.
Normal temperature in step 2 is 25 DEG C;
While dropping into sodium chlorate in step 2, temperature of reaction is no more than 60 DEG C.
In step 3, control the method for HCl content for adding alkali lye neutralization.
The method of controlling HCl content in step 3 is to control the injected volume of technical hydrochloric acid.
Present method is that iron and steel pickling waste liquid acid regeneration is except comparatively effective means of silicon sludge, effectively full Fe has been done and utilized, solve again the handling problems of this mud waste liquid, produce without secondary solid waste, the liquid iron(ic) chloride DTPA-Fe of producing is more than 8%, energy widespread use in sewage treatment industry, product cost is 40% of market sale product.
Brief description of the drawings
Fig. 1 method route figure
Embodiment
Be described further below in conjunction with accompanying drawing.
Fig. 1 is process flow sheet of the present invention, adds technical hydrochloric acid by outsourcing hydrochloric acid trough to reactor.
The present invention first drops into mud to reactor, then drops into wherein technical hydrochloric acid, and the mass ratio of silicon sludge and technical hydrochloric acid is 1:2, intensification limit, limit stirring reaction, and temperature is controlled at 50-65 DEG C, after question response is complete, i.e. Fe in system (OH) 3, Fe (OH) 2change FeCl into 3, FeCl 2for having reacted, be cooled to afterwards normal temperature, optimum temps is 25 DEG C, then starts silicon sludge and sodium chlorate mass ratio 1:0.017 and drops into sodium chlorate (utilize the type of cooling, temperature of reaction is no more than 60 DEG C), by FeCl 2be oxidized to FeCl 3, Fe in system 2+content≤0.1% is complete for oxidation, and then regulation system material acid-basicity, controls HCl content≤0.5%, and the mode of controlling content of hydrochloric acid has one, and a kind of is the input amount of controlling technical hydrochloric acid, and another kind is to neutralize with alkali lye.Carrying out cold filtration removal crystalline impurities etc., filtrate is iron(ic) chloride product, and filter residue further reclaims the products such as ammonium chloride.
Present method is that iron and steel pickling waste liquid acid regeneration removes comparatively effective means of silicon sludge, effectively full Fe has been done and has been utilized, and has solved again the handling problems of this mud waste liquid, produces without secondary solid waste.
According to silicon sludge 200g, 400 grams of technical hydrochloric acids, 3.29 grams of sodium chlorate, the amount that microcosmic salt acid is 6 grams is reacted, and after end reaction, total mass is 609.29 grams, and DTPA-Fe is 9.83%, HCl0.3%, and ferrous iron 0% reclaims without crystallization.The liquid iron(ic) chloride DTPA-Fe of producing, can widespread use in sewage treatment industry more than 8%, and product cost is 40% of market sale product.

Claims (5)

1. iron and steel pickling waste liquid is except a treatment process for silicon sludge, and its step is as follows:
Step 1, drop into silicon sludge and technical hydrochloric acid to reactor, the mass ratio of silicon sludge and technical hydrochloric acid is 1:2, and stir on intensification limit, limit, and temperature is controlled at 50-65 DEG C;
After step 2, step 1 react completely, be cooled to normal temperature, drop into sodium chlorate according to silicon sludge and sodium chlorate mass ratio 1:0.017;
Step 3, regulate the acid-basicity of whole reactant, control HCl content≤0.5%;
Step 4, cold filtration are removed crystalline impurities, reclaim iron(ic) chloride, ammonium chloride.
2. a kind of iron and steel pickling waste liquid according to claim 1 is except the treatment process of silicon sludge, and the normal temperature in step 2 is 25 DEG C.
3. a kind of iron and steel pickling waste liquid according to claim 1 is except the treatment process of silicon sludge, and while dropping into sodium chlorate in step 2, temperature of reaction is no more than 60 DEG C.
4. a kind of iron and steel pickling waste liquid according to claim 1, except the treatment process of silicon sludge, is controlled the method for HCl content for adding alkali lye neutralization in step 3.
5. a kind of iron and steel pickling waste liquid according to claim 1 is except the treatment process of silicon sludge, and the method for controlling HCl content in step 3 is to control the injected volume of technical hydrochloric acid.
CN201410279961.0A 2014-06-20 2014-06-20 Method for treating silicon sludge obtained by neutralizing steel pickling waste liquid, removing silicon and filtering Pending CN104118974A (en)

Priority Applications (1)

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CN201410279961.0A CN104118974A (en) 2014-06-20 2014-06-20 Method for treating silicon sludge obtained by neutralizing steel pickling waste liquid, removing silicon and filtering

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CN201410279961.0A CN104118974A (en) 2014-06-20 2014-06-20 Method for treating silicon sludge obtained by neutralizing steel pickling waste liquid, removing silicon and filtering

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CN104118974A true CN104118974A (en) 2014-10-29

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1067867A (en) * 1991-06-18 1993-01-13 金强 The non-pollution producing technology of iron trichloride
CN1356406A (en) * 2000-11-30 2002-07-03 黄卓林 Process for removing Si and Al from solution of ferrous chloride
WO2003045851A1 (en) * 2001-11-29 2003-06-05 Corporation Biolix Method for stabilizing and conditioning town and industrial wastewater sludge
CN103073067A (en) * 2013-02-02 2013-05-01 梁锡明 Method for producing ferric chloride by using pickle liquor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1067867A (en) * 1991-06-18 1993-01-13 金强 The non-pollution producing technology of iron trichloride
CN1356406A (en) * 2000-11-30 2002-07-03 黄卓林 Process for removing Si and Al from solution of ferrous chloride
WO2003045851A1 (en) * 2001-11-29 2003-06-05 Corporation Biolix Method for stabilizing and conditioning town and industrial wastewater sludge
CN103073067A (en) * 2013-02-02 2013-05-01 梁锡明 Method for producing ferric chloride by using pickle liquor

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Application publication date: 20141029