CN105314687A - Preparation method of polymeric ferric sulfate - Google Patents
Preparation method of polymeric ferric sulfate Download PDFInfo
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- CN105314687A CN105314687A CN201510857714.9A CN201510857714A CN105314687A CN 105314687 A CN105314687 A CN 105314687A CN 201510857714 A CN201510857714 A CN 201510857714A CN 105314687 A CN105314687 A CN 105314687A
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- Prior art keywords
- sulfate
- preparation
- ferric sulfate
- sodium hydroxide
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- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 title claims abstract description 21
- 229910000360 iron(III) sulfate Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 23
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 18
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 18
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 14
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 14
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 63
- 239000012065 filter cake Substances 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- 239000000047 product Substances 0.000 claims description 7
- 239000006227 byproduct Substances 0.000 claims description 6
- 229940056729 sodium sulfate anhydrous Drugs 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- -1 hydrogen sodium oxide Chemical class 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 5
- 229960003010 sodium sulfate Drugs 0.000 claims description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 235000011149 sulphuric acid Nutrition 0.000 claims 2
- 239000001117 sulphuric acid Substances 0.000 claims 2
- 229910052742 iron Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 3
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 abstract description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 abstract description 2
- 229960004887 ferric hydroxide Drugs 0.000 abstract 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 abstract 2
- 239000007789 gas Substances 0.000 abstract 1
- 150000007529 inorganic bases Chemical class 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 231100000331 toxic Toxicity 0.000 abstract 1
- 230000002588 toxic effect Effects 0.000 abstract 1
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a preparation method of polymeric ferric sulfate, belonging to the technical field of flocculant preparation. The method adopts ferrous sulfate and ferric sulfate as raw materials and inorganic base as a reactant. Firstly, the characteristic that ferrous hydroxide is easily oxidized into ferric hydroxide by air under the alkaline condition is utilized to convert ferrous sulfate into ferric hydroxide, and then a proper amount of sulfuric acid is added for polymerization reaction for a certain time to obtain the polymeric ferric sulfate. Compared with the existing common preparation method of polymeric ferric sulfate, the method has the advantages of less time-consuming process flow, good process repeatability, no emission of toxic and harmful gases, simple equipment, controllable cost and obvious economic value.
Description
Technical field
The invention belongs to flocculation agent preparing technical field.Be specifically related to a kind of preparation method of aggretion type ferric sulfate.
Background technology
Bodied ferric sulfate (PFS) is a kind of New Inorganic High Polymer Coagulant, has the features such as hydrolysis rate is fast, floc density is large, pH is applied widely, little to equipment corrosion, production cost is low.In PFS and suspended particle electric charge very capable, specific surface area is large, high adsorption capacity, the impurity such as suspended substance, microorganism, organism, sulfide, heavy metal ion in water can be removed well, and the functions such as decolouring, deodorizing, breakdown of emulsion and sludge dewatering are comparatively strong, are widely used in the process of service water, municipal effluent and tap water.
According to the difference of mode of oxidizing, the preparation method of bodied ferric sulfate is mainly divided into direct oxidation method and catalytic oxidation.The preparation of industrial most of bodied ferric sulfate adopts direct oxidation method, and this method operational path is comparatively simple, can reduce facility investment and production link for industrial production, reduce equipment cost, but this production technique must depend on oxygenant, as: H
2o
2, KClO
3, HNO
3deng inorganic oxidizer.If select H in direct oxidation method
2o
2for catalyzer, then cost compare is high; Select KClO
3for remaining higher chlorion and chloranion in catalyzer then product, be unsuitable for drinking water treatment, Potcrate is expensive simultaneously; Select HNO
3for can NO be generated in reaction during catalyzer
2, processed for avoiding causing environmental pollution need increase special absorption unit.Catalytic oxidation is generally oxygenant with air, production cost is relatively low, but need carry out at higher temperature and certain pressure, the simultaneous reactions time is longer, also need waste gas purification apparatus to be installed to slough a large amount of oxides of nitrogen gas produced in reaction process, technical process is complicated, higher to equipment requirements, invests larger.In summary it can be seen in existing method and all have obvious deficiency, therefore, the poly ferric sulfate preparation method finding the environmental issues such as a kind of technique is simple, cost is controlled, emission-free purification has obvious economic benefit and social benefit.
Summary of the invention
The present invention is directed to the problems referred to above existed in current poly ferric sulfate preparation method, propose a kind of new aggretion type ferric sulfate preparation method.Present method selects ferrous sulfate and ferric sulfate to be raw material, and mineral alkali is reagent.First utilize ferrous hydroxide under alkaline condition to be easily oxidised with air to the feature of ironic hydroxide, make ferrous sulfate change ironic hydroxide into, then add moderate amount of sulfuric acid polyreaction certain hour, obtain molecular formula for [Fe
2(OH)
n(SO
4)
3-n/2]
mbodied ferric sulfate.Do not use expensive oxygenant relative in present method direct oxidation method, and release without obnoxious flavour; Relative catalytic oxidation style present method effectively shortens the reaction times and releases without obnoxious flavour; Present method also by-product Sodium sulfate anhydrous.min(99), effectively improves economic value added simultaneously.According to 2013 yearly correlation price of chemical products measuring and calculating, total raw material cost about 870 yuan/ton, corresponding generation about 2000 yuan of value products, thus present method has obvious economic worth.
Concrete steps of the present invention are as follows:
(1) corresponding amount ferrous sulfate and sodium hydroxide is taken respectively by amount of substance 1:2,50% sodium hydroxide is configured to the sodium hydroxide solution of certain mass mark, in sodium hydroxide solution, add ferrous sulfate and residual hydrogen sodium oxide under blowing air agitation condition simultaneously, reaction certain hour, filtering separation, and with a small amount of hot wash filter cake, obtain filter cake and filtrate;
(2) filter cake adds a small amount of water and is modulated into thickness pulpous state, adds moderate amount of sulfuric acid under strong stirring condition, and reaction certain hour, namely obtains polyaluminum sulfate iron product;
(3) filtrate that step (1) obtains makes wherein sodium sulfate separate out by crystallisation by cooling, obtains byproduct Sodium sulfate anhydrous.min(99).
embodiment:
embodiment 1:corresponding amount ferrous sulfate 278g and sodium hydroxide 80g is taken respectively by amount of substance 1:2,40g sodium hydroxide is configured to the sodium hydroxide solution 200g that massfraction is 20%, in sodium hydroxide solution, add ferrous sulfate and residual hydrogen sodium oxide under blowing air agitation condition simultaneously, evenly add in 10min, continue stirring reaction 50min, filtering separation, and with a small amount of hot wash filter cake, obtain filter cake and filtrate; Filter cake adds 200mL and is modulated into thickness pulpous state, adds the vitriol oil of 60mL mass concentration 98% under strong stirring condition, and reaction 20min, namely obtains bodied ferric sulfate.The filtrate that said process obtains makes wherein sodium sulfate separate out by crystallisation by cooling, obtains byproduct Sodium sulfate anhydrous.min(99).
embodiment 2:corresponding amount ferrous sulfate 278g and sodium hydroxide 80g is taken respectively by amount of substance 1:2,40g sodium hydroxide is configured to the sodium hydroxide solution 400g that massfraction is 10%, in sodium hydroxide solution, add ferrous sulfate and residual hydrogen sodium oxide under blowing air agitation condition simultaneously, evenly add in 10min, continue stirring reaction 30min, filtering separation, and with a small amount of hot wash filter cake, obtain filter cake and filtrate; Filter cake adds 200mL and is modulated into thickness pulpous state, adds the vitriol oil of 70mL mass concentration 98% under strong stirring condition, and reaction 20min, namely obtains polyaluminum sulfate iron product.The filtrate that said process obtains makes wherein sodium sulfate separate out by crystallisation by cooling, obtains byproduct Sodium sulfate anhydrous.min(99).
embodiment 3:corresponding amount ferrous sulfate 278g and sodium hydroxide 80g is taken respectively by amount of substance 1:2,40g sodium hydroxide is configured to the sodium hydroxide solution 267g that massfraction is 15%, in sodium hydroxide solution, add ferrous sulfate and residual hydrogen sodium oxide under blowing air agitation condition simultaneously, evenly add in 10min, continue stirring reaction 40min, filtering separation, and with a small amount of hot wash filter cake, obtain filter cake and filtrate; Filter cake adds 200mL and is modulated into thickness pulpous state, adds the vitriol oil of 54mL mass concentration 98% under strong stirring condition, and reaction 20min, namely obtains polyaluminum sulfate iron product.The filtrate that said process obtains makes wherein sodium sulfate separate out by crystallisation by cooling, obtains byproduct Sodium sulfate anhydrous.min(99).
Claims (5)
1. a preparation method for aggretion type ferric sulfate, is characterized in that the method concrete steps are as follows:
(1) corresponding amount ferrous sulfate and sodium hydroxide is taken respectively by amount of substance 1:2,50% sodium hydroxide is configured to the sodium hydroxide solution of certain mass mark, in sodium hydroxide solution, add ferrous sulfate and residual hydrogen sodium oxide under blowing air agitation condition simultaneously, reaction certain hour, filtering separation, and with a small amount of hot wash filter cake, obtain filter cake and filtrate;
(2) filter cake adds a small amount of water and is modulated into thickness pulpous state, adds moderate amount of sulfuric acid under strong stirring condition, and reaction certain hour, namely obtains polyaluminum sulfate iron product;
(3) filtrate that step (1) obtains makes wherein sodium sulfate separate out by crystallisation by cooling, obtains byproduct Sodium sulfate anhydrous.min(99).
2. according to claim 1, a kind of preparation method of aggretion type ferric sulfate, is characterized in that: the mass fraction of the sodium hydroxide solution described in step (1) is 10 ~ 20%.
3. according to claim 1, a kind of preparation method of aggretion type ferric sulfate, is characterized in that: the reaction times described in step (1) is 30 ~ 50min.
4. according to claim 1, a kind of preparation method of aggretion type ferric sulfate, is characterized in that: the sulfuric acid described in step (2) is the industrial sulphuric acid of mass concentration 98%.
5. according to claim 1, a kind of preparation method of aggretion type ferric sulfate, is characterized in that: the sulfuric acid described in step (2) is the industrial sulphuric acid of mass concentration 98%, and the amount adding sulfuric acid can just regulate the amount of substance ratio of sulfuric acid and iron between 1 ~ 1.3:1.
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CN201510857714.9A CN105314687A (en) | 2015-11-30 | 2015-11-30 | Preparation method of polymeric ferric sulfate |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109502655A (en) * | 2019-01-25 | 2019-03-22 | 杭州秀澈环保科技有限公司 | A kind of production technology of bodied ferric sulfate |
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CN102070198A (en) * | 2011-02-28 | 2011-05-25 | 湖南科技大学 | Method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron |
CN103864154A (en) * | 2014-03-27 | 2014-06-18 | 李科 | Production method of liquid polymeric ferric sulfate water purifying agent |
CN104891537A (en) * | 2015-05-20 | 2015-09-09 | 南阳东方应用化工研究所 | Comprehensive utilization method of silicate minerals |
CN104986838A (en) * | 2015-07-02 | 2015-10-21 | 季红军 | Preparation method for water treatment agent |
-
2015
- 2015-11-30 CN CN201510857714.9A patent/CN105314687A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102070198A (en) * | 2011-02-28 | 2011-05-25 | 湖南科技大学 | Method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron |
CN103864154A (en) * | 2014-03-27 | 2014-06-18 | 李科 | Production method of liquid polymeric ferric sulfate water purifying agent |
CN104891537A (en) * | 2015-05-20 | 2015-09-09 | 南阳东方应用化工研究所 | Comprehensive utilization method of silicate minerals |
CN104986838A (en) * | 2015-07-02 | 2015-10-21 | 季红军 | Preparation method for water treatment agent |
Non-Patent Citations (2)
Title |
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阮复昌等: ""各种聚合硫酸铁生产方法的评比"", 《化学工业与工程》 * |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109502655A (en) * | 2019-01-25 | 2019-03-22 | 杭州秀澈环保科技有限公司 | A kind of production technology of bodied ferric sulfate |
CN109502655B (en) * | 2019-01-25 | 2023-08-08 | 杭州秀澈环保科技有限公司 | Production process of polymeric ferric sulfate |
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