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 PDFInfo
- 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
- Authority
- CN
- China
- Prior art keywords
- waste liquid
- silicon
- silicon sludge
- iron
- sludge
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000010802 sludge Substances 0.000 title claims abstract description 32
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 31
- 239000010703 silicon Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000002699 waste material Substances 0.000 title claims abstract description 24
- 239000007788 liquid Substances 0.000 title claims abstract description 22
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 20
- 239000010959 steel Substances 0.000 title claims abstract description 20
- 238000005554 pickling Methods 0.000 title claims abstract description 18
- 238000001914 filtration Methods 0.000 title claims abstract description 7
- 230000003472 neutralizing effect Effects 0.000 title abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 61
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052742 iron Inorganic materials 0.000 claims abstract description 25
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims abstract description 11
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract 2
- 238000004064 recycling Methods 0.000 abstract 1
- 230000001172 regenerating effect Effects 0.000 abstract 1
- 235000011167 hydrochloric acid Nutrition 0.000 description 10
- 239000002253 acid Substances 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- CUXQLKLUPGTTKL-UHFFFAOYSA-M microcosmic salt Chemical compound [NH4+].[Na+].OP([O-])([O-])=O CUXQLKLUPGTTKL-UHFFFAOYSA-M 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 235000021110 pickles Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Treatment Of Sludge (AREA)
- 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
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104118974A true CN104118974A (en) | 2014-10-29 |
Family
ID=51764646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410279961.0A Pending CN104118974A (en) | 2014-06-20 | 2014-06-20 | Method for treating silicon sludge obtained by neutralizing steel pickling waste liquid, removing silicon and filtering |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104118974A (en) |
Citations (4)
| 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 |
-
2014
- 2014-06-20 CN CN201410279961.0A patent/CN104118974A/en active Pending
Patent Citations (4)
| 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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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141029 |