CN109250762A - Method for preparing poly-ferric chloride by using steel hydrochloric acid pickling wastewater - Google Patents
Method for preparing poly-ferric chloride by using steel hydrochloric acid pickling wastewater Download PDFInfo
- Publication number
- CN109250762A CN109250762A CN201710569399.9A CN201710569399A CN109250762A CN 109250762 A CN109250762 A CN 109250762A CN 201710569399 A CN201710569399 A CN 201710569399A CN 109250762 A CN109250762 A CN 109250762A
- Authority
- CN
- China
- Prior art keywords
- acid pickling
- waste water
- pickling waste
- hydrochloric acid
- ferric chloride
- 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
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 239000002351 wastewater Substances 0.000 title claims abstract description 96
- 238000005554 pickling Methods 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 32
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 27
- 239000010959 steel Substances 0.000 title claims abstract description 27
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 title claims description 34
- 229910021578 Iron(III) chloride Inorganic materials 0.000 title claims description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 230000001590 oxidative effect Effects 0.000 claims abstract description 33
- 239000007800 oxidant agent Substances 0.000 claims abstract description 21
- 239000008363 phosphate buffer Substances 0.000 claims abstract description 14
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 69
- 229910052742 iron Inorganic materials 0.000 claims description 35
- 230000005484 gravity Effects 0.000 claims description 16
- 150000002506 iron compounds Chemical class 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical group [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 12
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 8
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 8
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical group [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 8
- 239000002893 slag Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000007788 liquid Substances 0.000 description 6
- 238000007792 addition Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 238000005097 cold rolling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical class [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229940125717 barbiturate Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/10—Halides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention relates to a method for preparing polyferric chloride by using steel hydrochloric acid pickling wastewater, which comprises the steps of pretreating the hydrochloric acid pickling wastewater, quantitatively feeding the filtered hydrochloric acid pickling wastewater into a reaction kettle, adding a phosphate buffer in batches, adding 0.03-0.04 t of phosphate buffer into each ton of concentrated hydrochloric acid pickling wastewater, fully stirring to completely dissolve the hydrochloric acid pickling wastewater, adding an oxidant under stirring and constant-temperature heating conditions to carry out oxidative polymerization, wherein the concentration of the oxidant is 120-150 mg/L, the oxidant is added into each ton of concentrated hydrochloric acid pickling wastewater by 0.7-1.1 kg/h, the rotating speed of a stirrer of the reaction kettle is 200-400 rpm, the reaction temperature is 40-60 ℃, and fully reacting to obtain the polyferric chloride after 14-26 h. The advantages are that: the process flow is simple, only one reaction kettle is needed in the core production process, and the oxidative polymerization reaction is completed in the reaction kettle.
Description
Technical field
The invention belongs to coking technology field more particularly to a kind of poly-ferric chloride is prepared with steel hydrochloric acid pickling waste water
Method.
Background technique
In steel process, need to do degreasing and rust removal processing before steel cold-rolling rolling or before steel surface coating, often
Using hydrochloric acid surface acid-washing method, this method will form acid waste water largely containing iron ion.It is conventional for this acid waste water
Way is that construction neutralizes waste water station, meets environmental emission standard and realizes qualified discharge.Consider for resource recycling angle, steel
Molysite acid pickling waste waters can be used for preparing poly-ferric chloride, and poly-ferric chloride can be used as sewage treatment flocculating agent.
In the prior art, patent publication No. CN1266819A is disclosed a kind of prepared using steel hydrochloric acid pickling waste water and polymerize
The method of chlorination ferric flocculant, using hypochlorite oxidation's technique.After pretreatment, phosphate and chlorine is added in pickling waste waters thereto
Barbiturates compound carries out sufficient oxidative polymerization under stirring and Elevated Temperature Conditions, can obtain product poly-ferric chloride.But it should
The polymeric oxygen agent Chlorates that method uses are inflammable and explosive chemicals, toxic and expensive, and production can be by with buying
To control, thus need to find the raw material medicament of safety, it is in liberal supply, and the alternative of low-cost high-efficiency.
Summary of the invention
In order to overcome the deficiencies of the prior art, the object of the present invention is to provide a kind of with the preparation polymerization of steel hydrochloric acid pickling waste water
The method of iron chloride can get concentration height, the good poly-ferric chloride of stability, and raw materials used pharmacy security is easy to get, cost
Relatively low, process flow is convenient, easy to operate, energy saving, is conducive to engineering popularization.
To achieve the above object, the invention is realized by the following technical scheme:
A method of poly-ferric chloride is prepared with steel hydrochloric acid pickling waste water, comprising the following steps:
1) chlorohydric acid pickling waste water is pre-processed, and is then filtered；
2) filtered chlorohydric acid pickling waste water is quantitatively sent into reaction kettle, phosphate buffer is added in batches, it is per ton dense
Chlorohydric acid pickling waste water after contracting adds 0.03t~0.04t phosphate buffer, is sufficiently stirred and makes it completely dissolved, and is stirring
And oxidant is added under the conditions of heated at constant temperature and carries out oxidative polymerization, oxidant concentration is 120~150mg/L, and oxidant is pressed
Chlorohydric acid pickling waste water after concentration per ton is added 0.7kg/h~1.1kg/h, reaction kettle blender revolving speed be 200rpm~
400rpm, reaction temperature are 40 DEG C~60 DEG C, after 14h~26h, sufficiently react to obtain poly-ferric chloride.
Chlorohydric acid pickling waste water is pre-processed in step 1), comprising the following steps:
1) raw material hydrochloric acid pickling waste waters improves frerrous chloride concentration through 70 DEG C~100 DEG C steam heating concentrations；
2) a small amount of hydrochloric acid and iron compound are added into the chlorohydric acid pickling waste water after concentration, adjust chlorohydric acid pickling waste water,
Make its pH value 1~2, total iron weight percent content is 10% or more, is sufficiently filtered after reaction, the specific gravity of chlorohydric acid pickling waste water
≥1.2g/cm3。
Chlorohydric acid pickling waste water is pre-processed in step 1), comprising the following steps:
1) iron compound is added into chlorohydric acid pickling waste water by with chlorohydric acid pickling wastewater quality ratio 1:0.06~1:0.09, often
After lower reaction 10-30 minutes of temperature, react iron compound sufficiently with pickling waste waters, adjusting waste water specific gravity is 0.9~1.0g/cm3,
PH value is 5~6；
2) the chlorohydric acid pickling waste water sufficiently reacted is sent into distillation process, setting vapo(u)rizing temperature is 70 DEG C~100 DEG C, distillation
The water rate of recovery is up to 90% or more, and residue concentration waste water is as the raw material for preparing poly-ferric chloride.
The iron compound is one or more mixtures of bushel iron slag, iron filings, iron block, iron nail.
The oxidant is ozone.
The phosphate buffer is potassium dihydrogen phosphate.
Compared with prior art, the beneficial effects of the present invention are:
Present invention process process is succinct, and core production process only needs a block response kettle, and oxidative polymerization is in reaction kettle
It completes, production operation is simple, energy saving；Raw material needed for technique is that wasted resources are helped with largely obtaining compared with low-cost
In reduction production and use cost；Pharmacy security needed for technique is easy to get, and does not belong to hazardous chemical, and wherein ozone is as industry
Common oxidant is produced, technology of preparing is more mature；Technological reaction process is simple, and oxidation rate is very fast, acquires concentration
Height, the good product poly-ferric chloride of stability are conducive to engineering popularization.
Meanwhile recyclable partial deionization water, residue concentration waste water can be used as the raw material of production poly-ferric chloride, realizes resource
Full recycling, zero release of pollutant.The demineralized water of recycling is for hydrochloric acid pickling process recycling, the polymerization that subsequent production obtains
Iron chloride can be used as flocculant and utilize for enterprise's Sewage Disposal, the raw material production cost of enterprises be greatly lowered, favorably
Comprehensive utilization of resources is realized inside integrated iron and steel works.
Particularly, for integrated iron and steel works, it is acid that cold rolling production hydrochloric acid pickling process section can discharge a large amount of iron content ions
Waste water, source of oxygen can be used as preparing ozone raw material in factory, poly ferric chloride flocculant agent for the use of enterprises Sewage Disposal,
Be conducive to enterprises and realize comprehensive utilization of resources, saves production cost.
Specific embodiment
The present invention is described in detail below, it should be noted that implementation of the invention embodiment party not limited to the following
Formula.
Embodiment 1
The method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water, comprising the following steps:
1) raw material hydrochloric acid pickling waste waters pre-processes: through 70 DEG C~100 DEG C steam heating concentrations, improving frerrous chloride concentration；
2) a small amount of hydrochloric acid and iron compound are added into the chlorohydric acid pickling waste water after concentration, adjust chlorohydric acid pickling waste water,
Make its pH value 1~2, total iron weight percent content is 10% or more, is sufficiently filtered after reaction, the specific gravity of chlorohydric acid pickling waste water
≥1.2g/cm3；
3) filtered chlorohydric acid pickling waste water is quantitatively sent into reaction kettle, phosphate buffer is added in batches, it is per ton dense
Chlorohydric acid pickling waste water after contracting adds 0.03t~0.04t phosphate buffer, is sufficiently stirred and makes it completely dissolved, and is stirring
And oxidant is added under the conditions of heated at constant temperature and carries out oxidative polymerization, oxidant concentration is 120~150mg/L, and oxidant is pressed
Chlorohydric acid pickling waste water after concentration per ton is added 0.7kg/h~1.1kg/h, reaction kettle blender revolving speed be 200rpm~
400rpm, reaction temperature are 40 DEG C~60 DEG C, after 4h~9h, sufficiently react to obtain poly-ferric chloride.
Wherein, the iron compound in step 2) is the mixing of one or more of bushel iron slag, iron filings, iron block, iron nail
Object.Oxidant is ozone in step 3).Phosphate buffer is potassium dihydrogen phosphate.
Embodiment 2
The method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water, comprising the following steps:
1) iron compound is added into chlorohydric acid pickling waste water by with chlorohydric acid pickling wastewater quality ratio 1:0.06~1:0.09, often
After lower reaction 10-30 minutes of temperature, react iron compound sufficiently with pickling waste waters, adjusting waste water specific gravity is 0.9~1.0g/cm3,
PH value is 5~6；
2) the chlorohydric acid pickling waste water sufficiently reacted is sent into distillation process, setting vapo(u)rizing temperature is 70 DEG C~100 DEG C, distillation
The water rate of recovery is up to 90% or more, and residue concentration waste water is as the raw material for preparing poly-ferric chloride.
3) when preparing poly-ferric chloride, the concentration waste water that step 2) obtains is filtered；Filtered chlorohydric acid pickling is useless
Water is quantitatively sent into reaction kettle, and phosphate buffer is added in batches, the chlorohydric acid pickling waste water after concentration per ton add 0.03t~
0.04t phosphate buffer, is sufficiently stirred and makes it completely dissolved, and oxidant is added under the conditions of stirring and heated at constant temperature and carries out
Oxidative polymerization, oxidant concentration are 120~150mg/L, and oxidant is pressed the chlorohydric acid pickling waste water after concentration per ton and is added
0.7kg/h~1.1kg/h, reaction kettle blender revolving speed are 200rpm~400rpm, and reaction temperature is 40 DEG C~60 DEG C, through 14h
After~26h, poly-ferric chloride is sufficiently reacted to obtain.
Wherein, iron compound is one or more mixtures of bushel iron slag, iron filings, iron block, iron nail.Oxidant is
Ozone.Phosphate buffer is potassium dihydrogen phosphate.
Embodiment 3
Steel hydrochloric acid pickling waste liquid 1100ml is measured, through 85 DEG C of steam heating concentrations, obtaining 175ml specific gravity is 1.2g/cm3
Concentrating spent liquor, pH value 1 moves into four-necked bottle after filtering raw material, weigh potassium dihydrogen phosphate 5.4g as buffer, points 4
Secondary addition, dissolves buffer sufficiently, 45 DEG C of constant temperature is arranged under strong stirring condition, being passed through concentration into concentrating spent liquor is
The ozone of 120mg/L after dosage 150mg/h, oxidative polymerization 4h, can obtain stable polyaluminium iron product.
Embodiment 4
Injection concentration and filtered steel hydrochloric acid pickling waste liquid, specific gravity 1.2g/ into the reaction kettle that capacity is 5t
cm3, pH value 1,45 DEG C of constant temperature of the setting under strong stirring condition, being passed through ozone dosage is 4kg/h, and concentration 120mg/L adds
Enter stabilizer potassium dihydrogen phosphate 0.17t, point 4 additions dissolve it sufficiently, after oxidative polymerization 4h, can obtain stable gather
Close chlorination iron product.
Embodiment 5
The method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water, comprising the following steps:
1) 2000ml chlorohydric acid pickling Wastewater Pretreatment: through 70 DEG C of steam heating concentrations, obtaining 450ml specific gravity is 1.3g/cm3
Concentrating spent liquor；
2) a small amount of hydrochloric acid and bushel iron slag are added into the chlorohydric acid pickling waste water after concentration, are adjusted chlorohydric acid pickling waste water, are made
Its pH value is 1, and total iron weight percent content is 11%, is sufficiently filtered after reaction, and the specific gravity of chlorohydric acid pickling waste water is 1.3g/
cm3；
3) filtered chlorohydric acid pickling waste water is quantitatively sent into reaction kettle, potassium dihydrogen phosphate, biphosphate is added in batches
Points of 4 times additions of potassium, amount to 13.5g, are sufficiently stirred and make it completely dissolved, and be added under the conditions of stirring and heated at constant temperature ozone into
Row oxidative polymerization, ozone concentration 130mg/L, oxidant are added by chlorohydric acid pickling waste water 0.7kg/h~1.1kg/h per ton
Enter, reaction kettle blender revolving speed is 300rpm, and reaction temperature is 50 DEG C, after 5h, sufficiently reacts to obtain poly-ferric chloride.
Embodiment 6
The method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water, comprising the following steps:
1) 10t chlorohydric acid pickling Wastewater Pretreatment: through 100 DEG C of steam heating concentrations, obtaining 1.5t specific gravity is 1.25g/cm3's
Concentrating spent liquor；
2) hydrochloric acid and bushel iron slag are added into the chlorohydric acid pickling waste water after concentration, are adjusted chlorohydric acid pickling waste water, are made its pH
Value is 2, and total iron weight percent content is 10%, is sufficiently filtered after reaction, and the specific gravity of chlorohydric acid pickling waste water is 1.25g/cm3；
3) filtered chlorohydric acid pickling waste water is quantitatively sent into reaction kettle, potassium dihydrogen phosphate, biphosphate is added in batches
Points of 4 times additions of potassium, amount to 50kg, are sufficiently stirred and make it completely dissolved, and be added under the conditions of stirring and heated at constant temperature ozone into
Row oxidative polymerization, ozone concentration 150mg/L, 1.37kg/h addition, reaction kettle blender revolving speed are 400rpm, reaction temperature
Degree is 60 DEG C, after 8h, sufficiently reacts to obtain poly-ferric chloride.
Embodiment 7
When being pre-processed to hydrochloric acid waste water, steel hydrochloric acid pickling waste liquid 260ml is measured, adds 20g bushel iron slag thereto,
Waste water pH value is 6 after room temperature is sufficiently reacted after ten minutes, adjusted.Go scrap iron removing that liquid is sent into distillation still, setting is steamed
Evaporating temperature is 90 DEG C, and distilled water 245ml, pH value 6 can be recycled；Residue concentration waste water 15ml, specific gravity 1.25g/cm3.Then
Remaining concentration waste water carries out the preparation of poly-ferric chloride.
Embodiment 8
When being pre-processed to hydrochloric acid waste water, steel hydrochloric acid pickling waste liquid 5000ml is measured, adds 350g bushel iron thereto
Slag, after room temperature sufficiently reacts 30 minutes, waste water pH value is 6 after being adjusted.Go scrap iron removing that liquid is sent into distillation still, directly
Vapo(u)rizing temperature is 100 DEG C, and distilled water 4735ml, pH value 6 can be recycled；Residue concentration waste water 265ml, specific gravity 1.25g/cm3.It is surplus
Remaining concentration waste water carries out the preparation of poly-ferric chloride.
Final products use titration measuring iron ion, Fe in iron ion3+99.8% is accounted for, remaining is Fe2+.Product pH value
For 1-2, specific gravity is that specific gravity is 1.45g/cm3, product is dark red.
Claims (6)
1. a kind of method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water, which comprises the following steps:
1) chlorohydric acid pickling waste water is pre-processed, and is then filtered；
2) filtered chlorohydric acid pickling waste water is quantitatively sent into reaction kettle, phosphate buffer is added in batches, after concentration per ton
Chlorohydric acid pickling waste water add 0.03t~0.04t phosphate buffer, be sufficiently stirred and make it completely dissolved, and in stirring and permanent
Oxidant is added under warm heating condition and carries out oxidative polymerization, oxidant concentration is 120~150mg/L, and oxidant is by per ton
0.7kg/h~1.1kg/h is added in chlorohydric acid pickling waste water after concentration, and reaction kettle blender revolving speed is 200rpm~400rpm, instead
Answering temperature is 40 DEG C~60 DEG C, after 14h~26h, sufficiently reacts to obtain poly-ferric chloride.
2. a kind of method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water according to claim 1, feature exist
In chlorohydric acid pickling waste water is pre-processed in step 1), comprising the following steps:
1) raw material hydrochloric acid pickling waste waters improves frerrous chloride concentration through 70 DEG C~100 DEG C steam heating concentrations；
2) a small amount of hydrochloric acid and iron compound are added into the chlorohydric acid pickling waste water after concentration, are adjusted chlorohydric acid pickling waste water, are made it
PH value is 1~2, and total iron weight percent content is 10% or more, is sufficiently filtered after reaction, the specific gravity of chlorohydric acid pickling waste water >=
1.2g/cm3。
3. a kind of method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water according to claim 1, feature exist
In chlorohydric acid pickling waste water is pre-processed in step 1), comprising the following steps:
1) iron compound is added into chlorohydric acid pickling waste water by with chlorohydric acid pickling wastewater quality ratio 1:0.06~1:0.09, under room temperature
After reaction 10-30 minutes, react iron compound sufficiently with pickling waste waters, adjusting waste water specific gravity is 0.9~1.0g/cm3, pH value
It is 5~6；
2) the chlorohydric acid pickling waste water sufficiently reacted is sent into distillation process, setting vapo(u)rizing temperature is 70 DEG C~100 DEG C, and distilled water returns
Yield is up to 90% or more, and residue concentration waste water is as the raw material for preparing poly-ferric chloride.
4. a kind of method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water according to claim 2 or 3, feature
It is, the iron compound is one or more mixtures of bushel iron slag, iron filings, iron block, iron nail.
5. a kind of method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water according to claim 1, feature exist
In the oxidant is ozone.
6. a kind of method for preparing poly-ferric chloride with steel hydrochloric acid pickling waste water according to claim 1, feature exist
In the phosphate buffer is potassium dihydrogen phosphate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710569399.9A CN109250762A (en) | 2017-07-13 | 2017-07-13 | Method for preparing poly-ferric chloride by using steel hydrochloric acid pickling wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710569399.9A CN109250762A (en) | 2017-07-13 | 2017-07-13 | Method for preparing poly-ferric chloride by using steel hydrochloric acid pickling wastewater |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109250762A true CN109250762A (en) | 2019-01-22 |
Family
ID=65050952
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710569399.9A Pending CN109250762A (en) | 2017-07-13 | 2017-07-13 | Method for preparing poly-ferric chloride by using steel hydrochloric acid pickling wastewater |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109250762A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109897954A (en) * | 2019-03-27 | 2019-06-18 | 东北师范大学 | A kind of purification process for cold rolling iron cement |
| CN110615485A (en) * | 2019-09-05 | 2019-12-27 | 中信环境技术（广州）有限公司 | Continuous production method and application of polyferric chloride |
| CN111498912A (en) * | 2020-05-14 | 2020-08-07 | 河南佰利联新材料有限公司 | Resource utilization method of waste acid water produced by chlorination process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060100463A1 (en) * | 2003-12-24 | 2006-05-11 | Mahajan Avinash N | Selective hydrogenation of nitrogen containing aromatics |
| CN101462776A (en) * | 2009-01-07 | 2009-06-24 | 金月祥 | Process for preparing poly ferric chloride |
| CN102351252A (en) * | 2011-07-06 | 2012-02-15 | 福建方明环保科技有限公司 | Method for producing flocculant utilizing waste steel pickler |
| CN101891258B (en) * | 2009-05-20 | 2012-08-29 | 北京紫光英力化工技术有限公司 | Novel production process of polyferric chloride |
| CN105502516A (en) * | 2016-02-04 | 2016-04-20 | 天津大学 | Method for preparing polyferric chloride from steel pickling wastewater |
-
2017
- 2017-07-13 CN CN201710569399.9A patent/CN109250762A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060100463A1 (en) * | 2003-12-24 | 2006-05-11 | Mahajan Avinash N | Selective hydrogenation of nitrogen containing aromatics |
| CN101462776A (en) * | 2009-01-07 | 2009-06-24 | 金月祥 | Process for preparing poly ferric chloride |
| CN101891258B (en) * | 2009-05-20 | 2012-08-29 | 北京紫光英力化工技术有限公司 | Novel production process of polyferric chloride |
| CN102351252A (en) * | 2011-07-06 | 2012-02-15 | 福建方明环保科技有限公司 | Method for producing flocculant utilizing waste steel pickler |
| CN105502516A (en) * | 2016-02-04 | 2016-04-20 | 天津大学 | Method for preparing polyferric chloride from steel pickling wastewater |
Non-Patent Citations (4)
| Title |
|---|
| 姚仲鹏: "《空气净化原理、设计与应用》", 30 September 2014, 中国科学技术出版社 * |
| 尹杰等: "酸洗废液制备聚合氯化铁形态及稳定性研究", 《广东化工》 * |
| 林永增等: "轧钢酸洗废液制备聚合氯化铁的工艺条件研究", 《环境保护科学》 * |
| 鲁慧洁等: "钢材盐酸酸洗废液的回收与利用研究进展", 《山东化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109897954A (en) * | 2019-03-27 | 2019-06-18 | 东北师范大学 | A kind of purification process for cold rolling iron cement |
| CN110615485A (en) * | 2019-09-05 | 2019-12-27 | 中信环境技术（广州）有限公司 | Continuous production method and application of polyferric chloride |
| CN110615485B (en) * | 2019-09-05 | 2022-03-25 | 中信环境技术（广州）有限公司 | Continuous production method and application of polyferric chloride |
| CN111498912A (en) * | 2020-05-14 | 2020-08-07 | 河南佰利联新材料有限公司 | Resource utilization method of waste acid water produced by chlorination process |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2019051923A1 (en) | Iron-containing sludge pyrolysis residue-based sludge complex conditioning agent, preparation therefor and use thereof | |
| CN109250762A (en) | Method for preparing poly-ferric chloride by using steel hydrochloric acid pickling wastewater | |
| CN106904807A (en) | A kind of method that phosphorus is reclaimed from dewatered sludge | |
| CN105502516B (en) | A kind of method that poly-iron chloride is prepared by iron and steel pickling waste liquid | |
| CN102120623A (en) | Preparation method of polysilicate aluminium ferric flocculant | |
| CN105366899B (en) | A kind of Fenton oxidation technique of ozone anaerobism iron reduction combination mud decrement | |
| CN105129867A (en) | Method used for preparing polymeric ferric sulfate from sulfuric acid waste liquid | |
| CN105016573B (en) | Method for treating neutral wastewater containing dye and PVA (polyvinyl alcohol) by using UV (ultraviolet) synergistic complexing/Fenton system | |
| CN106746068A (en) | A kind of processing method containing high concentration organism P wastewater | |
| CN102464440B (en) | Method for carrying out decrement on physicochemical and biochemical mixed sludge | |
| CN104709992A (en) | Polymeric phosphorus ferric sulfate flocculating agent as well as preparation method and application thereof | |
| CN103145196A (en) | Method for producing polymerization ferric chloride by utilizing waste hydrochloric acid and waste ferrous mud | |
| CN106830487A (en) | A kind of comprehensive processing technique of the high-concentration ammonia nitrogenous wastewater containing organic matter thiocarbamide | |
| CN106915878A (en) | The recovery method of phosphorus in a kind of phosphorus containing sludge | |
| CN108101307A (en) | A kind of textile printing and dyeing wastewater processing method | |
| CN108892611A (en) | A kind of production technology of sodium acetate solution | |
| CN102838197A (en) | Method for preparing novel composite flocculant PSAFS (poly-silicate aluminum ferrous sulfate) | |
| CN101717123B (en) | Method for preparing modified poly-ferric chloride coagulant | |
| CN104163486B (en) | A kind of bleaching powder waste water processes the method for glyphosate waste water | |
| CN106554140B (en) | A kind of residual active sludge cracks decrement method | |
| CN101759218A (en) | Preparation method of pulping waste water flocculant | |
| CN103833116B (en) | A kind of production method and application that utilizes waste hydrochloric acid, aluminium-containing sludge to prepare defluorinating agent | |
| CN105271435B (en) | Seamless steel pipe pickle liquor prepares the production technology of polyaluminium ferric flocculant | |
| CN101412556A (en) | Poly(zinc aluminum chloride), and preparation thereof and method for treating sewerage by using same | |
| CN108083400A (en) | A kind of preparation method of phosphorous polyiron sulfate and its application for handling coking wastewater |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190122 |
|
| RJ01 | Rejection of invention patent application after publication |