CN104828885A - Preparation method of liquid ferrate - Google Patents
Preparation method of liquid ferrate Download PDFInfo
- Publication number
- CN104828885A CN104828885A CN201510250048.2A CN201510250048A CN104828885A CN 104828885 A CN104828885 A CN 104828885A CN 201510250048 A CN201510250048 A CN 201510250048A CN 104828885 A CN104828885 A CN 104828885A
- Authority
- CN
- China
- Prior art keywords
- liquid
- ferrate
- reaction
- preparation
- pickle liquor
- 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
Landscapes
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention belongs to the technical field of sewage treatment, and particularly relates to a preparation method of liquid ferrate. The whole reaction process is carried out at normal temperature. The method comprises the following steps: (1) regulating the total iron content with ferrous chloride according to the iron content in hydrochloric acid pickle liquor, putting in a reaction kettle, and stirring uniformly; (2) adding an oxidizer 1 to perform oxidation reaction with the liquid; (3) adding a reaction stabilizer to perform reaction conversion on the liquid and coproduce the stabilizer; and (4) adding a strong alkali and an oxidizer 2 into the solution to perform oxidation reaction, thereby obtaining the ferrate solution. The method for producing the liquid ferrate has the advantages of high liquid ferrate quality, low production cost, high operational safety, low equipment investment and short production time, is convenient for production, can reutilize the pickle liquor by 100%, achieves the goal of zero discharge of three wastes, and can implement large-scale production.
Description
Technical field
The invention belongs to technical field of sewage, particularly relate to a kind of preparation method of liquid ferrate.
Background technology
Iron And Steel Industry, metal product industry need remove steel surface iron scale and use acid to carry out pickling in process of production, can produce a large amount of spent acid solutions in acid cleaning process.The corrodibility serious because of it and hazardness, be put into " National Hazard refuse register ".The direct discharge not only serious environment pollution of such waste liquid, and cause the great wasting of resources.Therefore by technical renovation, utilize spent pickle liquor, direct production goes out the liquid ferrate water conditioner needed for market, both the environmental pollution of company had been solved, again for society has saved a large amount of resources, really accomplish the treatment of wastes with processes of wastes against one another, there is huge economic benefit and social benefit.The major cause that spent acid solution production ferrate water conditioner fails to find broad application there is following shortcoming:
1, utilize waste iron filing and hydrochloric acid reaction to carry out supplementary total iron content to need to carry out under Boiler Steam heating condition, waste iron filing and hydrochloric acid reaction produce hydrogen, bring danger to production, and to environment.
2, ferrous oxidising is in ferric iron process, and 1. catalytic oxidation produces nitrogen protoxide, nitrogen dioxide waste gas in process of production, causes serious harm to human body.And need of production adds at condition of negative pressure and carries out, operative employee is unskilled or careless in process of production, very easily causes pipe explosion, causes significant consequences.2. the use of an one-step chlorination method not only material chlorine is restricted, and inevitably produces the leakage of chlorine in process of production, and considerably increases the danger of production.
3, the highly basic added in production process is sodium hydroxide, adds production cost.
4, the use cost of potassium hypochlorite, clorox or sodium peroxide that adopts of last oxidation stage is high.
5, high price iron has unstable, needs to add stablizer and finished product just can be made to preserve for a long time.
Summary of the invention
Main purpose of the present invention is to solve problems of the prior art, provide that a kind of low production cost, spent pickle liquor 100% regeneration, production process are simple and safe, zero emission, stable performance liquid ferrate preparation method.
Problem solved by the invention realizes by the following technical solutions:
A kind of preparation method of liquid ferrate, comprise: 1. integral production process is carried out at normal temperatures, known iron and steel pickling waste liquid composition is free hydrochloric acid content 2-7%, total iron content is 8-14%, spent pickle liquor is dropped in reactor and carry out ingredient analysis and stir, free hydrochloric acid content need not regulate, by the method adding iron protochloride spent pickle liquor total iron content is transferred to and is greater than 10%, obtain (iron protochloride, iron(ic) chloride, hydrochloric acid, water) solution after dissolving, chemical formula is FeCl2+FeCl3+HCL+H2O; 2. oxygenant sodium chlorate is slowly added, 15 minutes reaction times, reaction equation is NaClO3+6FeCl2+6HCl=NaCl+6FeCl3+3H2O, because hydrochloric acid is a small amount of, so hydrochloric acid exhaust rear generation reaction NaClO3+6FeCl2+3H2O=4FeCl3+NaCl+2Fe (OH) below 3 ↓, obtain (iron(ic) chloride, sodium-chlor, ironic hydroxide, water) solution.3. the waste residue calcium hydroxide of discharging in acetylene gas production process is slowly added again in the solution, chemical formula is Ca (OH) 2,15 minutes reaction times, react with iron(ic) chloride in liquid, reaction equation is 3Ca (OH) 2+2FeCl3=3CaCl2+2Fe (OH) 3, obtain (calcium chloride, ironic hydroxide, sodium-chlor, water) solution, the calcium chloride that reaction generates serves as stablizer in the solution, plays stabilization to cationic high price iron.4. in solution, slowly add waste residue calcium hydroxide and the sodium chlorate that discharge produced by acetylene gas successively, make ironic hydroxide under the effect of alkaline medium calcium hydroxide with sodium chlorate generation oxidizing reaction, reaction times 30-60 minute, reaction equation is that 2NaClO3+4Fe (OH) 3+4Ca (OH) 2=Na2FeO4+3CaFeO4+CaCl2+10H2O generates Na2Fe04, calcium ferrate and calcium chloride solution, stop stirring, reaction completes, and obtains the liquid ferrate containing Na2Fe04, calcium ferrate, calcium chloride.
Beneficial effect of the present invention is:
1, the present invention's spent pickle liquor does raw material, spent pickle liquor 100% regeneration, really accomplishes to turn waste into wealth.
2, the present invention's iron protochloride is as total iron supplementary material, makes production process simple, pollution-free.
3, the present invention sodium chlorate, as ferrous oxidising dose, makes production process simple, pollution-free.
4, the calcium chloride that the waste residue discharged in the present invention's acetylene gas production process and solution reaction generate is as stablizer, and waste residue obtains utilization, reduces production cost.
5, the waste residue discharged in the present invention's acetylene gas production process replaces sodium hydroxide as reagent, and waste residue obtains utilization, reduces production cost.
6, the waste residue discharged in the present invention's acetylene gas production process replaces sodium hydroxide as highly basic, and waste residue obtains utilization, reduces production cost.
7, the present invention sodium chlorate replaces hypochlorite, sodium peroxide etc. as oxygenant, and oxidant production cost reduces by 1/3.
8, the reaction times of the present invention short (60-90 minute), equipment is established into few (primary device only has reactor), and production cost is low, and production technique is simple, and production process environmental protection, can accomplish scale production.
Accompanying drawing explanation
Fig. 1 is production scheme of the present invention.
In figure: the stirring and dissolving of stirring and dissolving-in corrosion-resistant reactor, oxygenant 1-sodium chlorate, reaction stabilizer-acetylene discharge waste residue (sodium hydroxide), highly basic-acetylene discharge waste residue (calcium hydroxide), oxygenant 2-sodium chlorate.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described further:
Embodiment 1
As shown in Figure 1, the present embodiment comprises spent pickle liquor, iron protochloride, stirring and dissolving, oxygenant 1 sodium chlorate, oxidation conversion, reaction stabilizer acetylene discharge waste residue (calcium hydroxide), reaction conversion, highly basic acetylene discharge waste residue (calcium hydroxide), oxygenant 2 sodium chlorate, oxidation conversion, product liquid ferrate.
During work, spent pickle liquor 1T is added in corrosion-resistant reactor, (detecting its composition is hydrochloric acid 4.5%, total iron content is 9.6%), add the ferrous 20kg of solid chlorine of content 50%, start stirring and dissolving (rotating speed is 300 revs/min), slowly add oxygenant 1 sodium chlorate 20kg after dissolving completes and carry out oxidation conversion, slowly add reaction stabilizer acetylene discharge waste residue (calcium hydroxide) 10kg after 15 minutes and carry out reaction conversion, slowly add highly basic acetylene discharge waste residue (calcium hydroxide) 35kg and oxygenant 2 sodium chlorate 12kg after 15 minutes successively and carry out oxidation conversion, stop after 30 minutes stirring, generate the liquid ferrate product containing stablizer.After taking out reaction, liquid carries out next production process again.
Embodiment 2
As shown in Figure 1, the present embodiment comprises spent pickle liquor, iron protochloride, stirring and dissolving, oxygenant 1 sodium chlorate, oxidation conversion, reaction stabilizer acetylene discharge waste residue (calcium hydroxide), reaction conversion, highly basic acetylene discharge waste residue (calcium hydroxide), oxygenant 2 sodium chlorate, oxidation conversion, product liquid ferrate.
During work, spent pickle liquor 1T is added in corrosion-resistant reactor, (detecting its composition is hydrochloric acid 5.35%, total iron content is 11.6%), iron protochloride need not be added, start to stir (rotating speed is 300 revs/min), slowly add oxygenant 1 sodium chlorate 29kg and carry out oxidation conversion, add reaction stabilizer acetylene discharge waste residue (calcium hydroxide) 15kg after 15 minutes and carry out reaction conversion, within 15 minutes, add highly basic acetylene discharge waste residue (calcium hydroxide) 40kg and oxygenant 2 sodium chlorate 13kg and carry out oxidation conversion, stop after 50 minutes stirring, generate the liquid ferrate product containing stablizer.After taking out reaction, liquid carries out next production process again.
Utilize technical solutions according to the invention, or those skilled in the art being under the inspiration of technical solution of the present invention, designing similar technical scheme, and reach above-mentioned technique effect, is all fall into protection scope of the present invention.
Claims (8)
1. a preparation method for liquid ferrate, is characterized in that: W-response carries out at normal temperatures, 1. according to the iron level in hydrochloric acid pickling waste liquor, adjusts the content of total iron with iron protochloride, puts into reactor and stir; 2. add oxygenant 1 and carry out oxidizing reaction with liquid material; 3. add reaction stabilizer and liquid material to carry out reaction and transform, reaction by-product goes out stablizer; 4. in solution, add highly basic and oxygenant 2 carries out oxidizing reaction, react complete and namely obtain ferrate solution.
2. the preparation method of a kind of liquid ferrate according to claim 1, is characterized in that: described under normal temperature condition for react at normal temperatures, oxidation reaction solution heat up can not more than 60 DEG C, heating and cooling process that it goes without doing.
3. the preparation method of a kind of liquid ferrate according to claim 1, is characterized in that: described iron protochloride is to be transferred to by spent pickle liquor total iron content with iron protochloride to be greater than 10% to adjust the content of total iron.
4. the preparation method of a kind of liquid ferrate according to claim 1, is characterized in that: described oxygenant 1 is sodium chlorate, and addition is 0.2-0.3 times of total iron content in spent pickle liquor.
5. the preparation method of a kind of liquid ferrate according to claim 1, it is characterized in that: described stable reagent is that acetylene gas produces discharge waste residue (major ingredient calcium hydroxide) or calcium hydroxide, addition is 0.1-0.2 times of total iron content in spent pickle liquor.
6. the preparation method of a kind of liquid ferrate according to claim 1, it is characterized in that: described highly basic is that acetylene gas produces discharge waste residue (major ingredient calcium hydroxide) or calcium hydroxide, addition is 0.2-0.4 times of total iron content in spent pickle liquor.
7. the preparation method of a kind of liquid ferrate according to claim 1, is characterized in that: described oxymuriate is sodium chlorate, and addition is 0.12-0.16 times of total iron content in spent pickle liquor.
8. the preparation method of a kind of liquid ferrate according to claim 1, is characterized in that: described ferrate solution is Na2Fe04, calcium ferrate and calcium chloride mixing solutions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510250048.2A CN104828885A (en) | 2015-05-18 | 2015-05-18 | Preparation method of liquid ferrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510250048.2A CN104828885A (en) | 2015-05-18 | 2015-05-18 | Preparation method of liquid ferrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104828885A true CN104828885A (en) | 2015-08-12 |
Family
ID=53807145
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510250048.2A Pending CN104828885A (en) | 2015-05-18 | 2015-05-18 | Preparation method of liquid ferrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104828885A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105441950A (en) * | 2015-02-13 | 2016-03-30 | 叶涛 | Regeneration and recycling technology for acid copper chloride etching waste liquid |
| CN107055643A (en) * | 2017-05-03 | 2017-08-18 | 陈雷 | A kind of preparation method of river lake effluent purifier |
| CN115893506A (en) * | 2022-12-28 | 2023-04-04 | 江苏永葆环保科技股份有限公司 | Method for preparing ferric chloride by using steel pickling waste liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013056328A (en) * | 2011-08-18 | 2013-03-28 | Kurita Water Ind Ltd | Treatment method and treatment apparatus of cyanide-containing water |
| CN103449527A (en) * | 2013-08-09 | 2013-12-18 | 华南理工大学 | Method for preparing ferrate through hydraulic power cavitation and activation |
| CN103723772A (en) * | 2014-01-15 | 2014-04-16 | 哈尔滨工业大学 | Preparation method of composite ferrate reagent |
-
2015
- 2015-05-18 CN CN201510250048.2A patent/CN104828885A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013056328A (en) * | 2011-08-18 | 2013-03-28 | Kurita Water Ind Ltd | Treatment method and treatment apparatus of cyanide-containing water |
| CN103449527A (en) * | 2013-08-09 | 2013-12-18 | 华南理工大学 | Method for preparing ferrate through hydraulic power cavitation and activation |
| CN103723772A (en) * | 2014-01-15 | 2014-04-16 | 哈尔滨工业大学 | Preparation method of composite ferrate reagent |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105441950A (en) * | 2015-02-13 | 2016-03-30 | 叶涛 | Regeneration and recycling technology for acid copper chloride etching waste liquid |
| CN107055643A (en) * | 2017-05-03 | 2017-08-18 | 陈雷 | A kind of preparation method of river lake effluent purifier |
| CN115893506A (en) * | 2022-12-28 | 2023-04-04 | 江苏永葆环保科技股份有限公司 | Method for preparing ferric chloride by using steel pickling waste liquid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103073067B (en) | A kind of method utilizing spent pickle liquor to produce iron(ic) chloride | |
| CN104828885A (en) | Preparation method of liquid ferrate | |
| CN104817118A (en) | Simple and quick method for preparing polyferric chloride | |
| WO2021088459A1 (en) | Method for producing amino trimethylene phosphonic acid as water treatment agent | |
| CN110627131A (en) | Method for recycling waste liquid containing iron and nitric acid | |
| CN103723772A (en) | Preparation method of composite ferrate reagent | |
| CN105369266A (en) | Steel acid washing liquid based on Fenton oxidation reaction and acid washing process | |
| CN101285196B (en) | Processing technology for surface oxide skin of aviation tubes | |
| CN102275947A (en) | Method for preparing potassium fluoborate by using mixed acid containing hydrogen fluoride | |
| CN104495809B (en) | A kind of micro crystal graphite purifying method | |
| CN108339374B (en) | Treatment method for realizing zero emission of HCl gas absorption cycle | |
| CN101780986B (en) | Method for producing iron chloride by using steel pickling waste liquor | |
| CN109369053A (en) | Utilize the process of aluminium ash manufacture accelerator and flocculant | |
| CN103449425B (en) | Method for preparing high-purity graphite through purifying natural high-carbon flake graphite by using alkaline-acid complexing method | |
| CN104828920A (en) | Preparation method of poly ferric perchloride flocculant | |
| CN102583294A (en) | Method for producing sodium tripolyphosphate by replacing ammonium nitrate with sodium nitrate taken as catalyst | |
| CN201722149U (en) | Magnesium tail water recycling device in production of concentrated nitric acid | |
| CN114804426A (en) | Iron-containing waste hydrochloric acid treatment process | |
| CN109279631A (en) | A kind of preparation method of magnesium chloride and the purposes of magnesium chloride as made from it | |
| CN203976418U (en) | A kind ofly take Repone K, Sweet natural gas and realize the production system of comprehensive utilization of resources as raw material | |
| CN103896761A (en) | Method for composite oxidation and synthesis of glyoxalic acid | |
| CN103466586A (en) | Method for producing sodium tripolyphosphate by taking mixture of sodium nitrate and ammonium nitrate as catalyst | |
| CN102399294A (en) | Method for producing low-substituted hydroxypropylcellulose | |
| CN218841716U (en) | Recovery unit of industrial waste salt in hydrazine hydrate production process | |
| TW201518202A (en) | Apparatus for the decomposition of hydrogen peroxide included in sulfuric acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150812 |