CN108975475A - A kind of preparation method of bodied ferric sulfate - Google Patents

A kind of preparation method of bodied ferric sulfate Download PDF

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Publication number
CN108975475A
CN108975475A CN201811208396.3A CN201811208396A CN108975475A CN 108975475 A CN108975475 A CN 108975475A CN 201811208396 A CN201811208396 A CN 201811208396A CN 108975475 A CN108975475 A CN 108975475A
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ferric sulfate
bodied ferric
preparation
sulfate
ferrous
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CN108975475B (en
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璧典匠
赵佳
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Xuzhou Clean Water Environmental Protection Technology Co Ltd
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Xuzhou Clean Water Environmental Protection Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/14Sulfates
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/12Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/14Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The invention belongs to water treatment agent preparation field more particularly to a kind of preparation methods of bodied ferric sulfate.A kind of preparation method of bodied ferric sulfate, includes the following steps, under the conditions of catalyst and cocatalyst, bodied ferric sulfate is made in ferrous sulfate mixed solution and oxidant reaction.The invention has the advantages that (1) present invention is that under the action of catalyst, bodied ferric sulfate is made in ferrous sulfate mixed solution and oxidant single step reaction, and production stage is simple, strong operability;(2) production cost of product is substantially reduced, good productivity effect and economic benefit can be achieved;(3) cocatalyst is added during the preparation process is sodium phosphate, so that bodied ferric sulfate prepared by the present invention has stable state and preferable product coagulation effect, and product characteristic obtained complies with the national standard requirements;(4) pickle liquor of steel tube factory or trombone slide factory is prepared into production bodied ferric sulfate, turned waste into wealth, not will cause secondary pollution, be conducive to environmental protection.

Description

A kind of preparation method of bodied ferric sulfate
Technical field
The invention belongs to water treatment agent preparation field more particularly to a kind of preparation methods of bodied ferric sulfate.
Background technique
The inorganic coagulant being commonly used is broadly divided into two major classes: aluminium salt and molysite.With polyaluminium chloride, sulphur in aluminium salt Based on sour aluminium, aluminium chloride.And molysite is then based on bodied ferric sulfate.Since the sixties in last century, polyaluminium chloride is only with it To advantage occupy one seat in the market, but the progress of science and technology also makes it expose certain deficiency.Polyaluminum sulfate Iron is most pioneering by Japan earlier than nineteen seventies, and China develops in the 1980s and puts into industrialized production Using.After especially Environmental Protection in China portion in 2015 announces " ten, water ", application of the bodied ferric sulfate in sewage treatment is obtained More sufficient development.
Prior art data disclosed in Chinese patent publication: (1) CN1043292A- technology for making polyiron sulfate;(2) A kind of production method of ferrous system of polymerized water purifier of CN1034909A-;(3) CN1043484A- high-effective sewage purifying agent and its device; (4) production method of GK87104053- ferrous system of polymerized water purifier.The maximum feature of the prior art (1) is not have to any oxidant Or catalyst, directly make raw material with the industrial residue containing iron oxide, manufactures polymeric ferrous sulphate solution with sulfuric acid reaction one-step method.It is existing Technology (2) is to utilize hydrochloric acid pickling waste liquor: ferrous chloride solution, and sodium hypochlorite is added, then prepares a kind of mother liquor, and three reacts system Obtain ferrous system of polymerized water purifier.The prior art (3) is using the ferrous sulfate by 55%-60%, the sulfuric acid of 5%-10%, 3%- 5% sodium chlorate and the water of 28%-35% form cleanser, are produced using chemical oxidization method.The prior art (4) is to utilize sulphur Mother liquor is made in sour ferrous iron waste liquid, and oxidant is reacted with mother liquor, ferrous system of polymerized water purifier is made.
But the production technology of bodied ferric sulfate is complicated, production cost is higher.How the production work of bodied ferric sulfate is simplified Skill reduces the major issue that production cost is always contained enterprise development.
Summary of the invention
It is an object of the invention to overcome the defect of the production technology of prior art bodied ferric sulfate complexity, provide a kind of poly- Close the preparation method of ferric sulfate.
A kind of preparation method of bodied ferric sulfate, includes the following steps, under the conditions of catalyst and cocatalyst, sulfuric acid Bodied ferric sulfate is made in ferrous mixed solution and oxidant reaction.
Preferentially, the cocatalyst is sodium phosphate, and the catalyst is sulfuric acid, and the mass fraction of the sulfuric acid is 98%, the working solution for being 1 ‰~2 ‰ at mass fraction by the catalyst preparation.
Preferentially, the dosage of the working solution is that finished product per ton uses 1~2 kilogram, the cocatalyst dosage 1~2g is used for finished product per ton.
Preferentially, the oxidant is oxygen or ozone.
Preferentially, the ferrous sulfate mixed solution is the mixed solution of pickle liquor, ferrous sulfate, and wherein pickling is useless The mass ratio of liquid and ferrous sulfate is 1:1~1.2.
Preferentially, the pickle liquor is the pickle liquor of steel tube factory or trombone slide factory.
Preferentially, ferrous iron mass fraction in terms of Fe2+ is 10~15% in the pickle liquor, and acid is with H2SO4Count quality Score is 8~10%.
In addition, being obtained the present invention also provides a kind of Polymerization ferric sulfate water treatment agent by the preparation method of the bodied ferric sulfate It arrives.
In addition, Polymerization ferric sulfate water treatment agent of the present invention is applied in wastewater treatment and sludge treatment technique.
Beneficial effects of the present invention: (1) present invention is ferrous sulfate mixed solution and oxidant one under the action of catalyst Step, which is reacted, is made bodied ferric sulfate, and production stage is simple, strong operability;(2) present invention substantially reduces the production cost of product, Good productivity effect and economic benefit can be achieved;(3) cocatalyst sodium phosphate is added in preparation process of the present invention, So that bodied ferric sulfate prepared by the present invention has stable state and preferable product coagulation effect, and product characteristic obtained Comply with the national standard requirements;(4) present invention is that the pickle liquor of steel tube factory or trombone slide factory is prepared into production bodied ferric sulfate, is become Waste be changed into values, not will cause secondary pollution, is conducive to environmental protection.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.
Embodiment 1
The pickle liquor that the steel tube factory 2kg is added in the experiment kettle of 5L is (wherein ferrous with Fe2+Counting mass fraction is 10%, Acid is with H2SO4Counting mass fraction is 8%), the titanium powder plant ferrous sulfate by-product of 2kg to be then added, and 98% sulfuric acid of catalyst is added Working solution and cocatalyst sodium phosphate, are passed through oxygen, are then turned on stirring or circulating pump, and a sample was taken every five minutes PFS-1# measures remaining ferrous content.It is molten that 98% sulfuric acid of catalyst is wherein configured to the work that mass fraction is 1 ‰ Liquid, finished product per ton use 1 kilogram of working solution, and the cocatalyst dosage is that finished product per ton uses 1g.
Embodiment 2
The pickle liquor that 2kg trombone slide factory is added in the experiment kettle of 5L is (wherein ferrous with Fe2+Counting mass fraction is 13%, Acid is with H2SO4Counting mass fraction is 9%), the titanium powder plant ferrous sulfate by-product of 2.2kg to be then added, and 98% sulphur of catalyst is added Sour working solution and cocatalyst sodium phosphate, are passed through ozone, are then turned on stirring or circulating pump, and a sample was taken every five minutes PFS-2# measures remaining ferrous content.It is molten that 98% sulfuric acid of catalyst is wherein configured to the work that mass fraction is 2 ‰ Liquid, finished product per ton use 2 kilograms of working solutions, and the cocatalyst dosage is that finished product per ton uses 2g.
Embodiment 3
The pickle liquor that 2kg trombone slide factory is added in the experiment kettle of 5L is (wherein ferrous with Fe2+Counting mass fraction is 15%, Acid is with H2SO4Counting mass fraction is 10%), the titanium powder plant ferrous sulfate by-product of 2.4kg to be then added, and catalyst 98% is added Sulfuric acid working solution and cocatalyst sodium phosphate, are passed through ozone, are then turned on stirring or circulating pump, take every five minutes primary Sample PFS-3# measures remaining ferrous content.98% sulfuric acid of catalyst is wherein configured to the work that mass fraction is 2 ‰ Solution, finished product per ton use 2 kilograms of working solutions, and the cocatalyst dosage is that finished product per ton uses 2g.
Comparative example 1
Cocatalyst sodium phosphate in embodiment 1 is removed, other are the same as embodiment 1.
Comparative example 2
Cocatalyst sodium phosphate in embodiment 1 is replaced with to the potassium iodide of equivalent, other are the same as embodiment 1.
Table 1 is Examples 1 to 3 and 1~2 different process of comparative example each period remaining ferrous iron amount/%
Note: "-" indicates that reaction terminates no longer to sample.
Table 2 is the specificity analysis of product made from Examples 1 to 3 and comparative example 1~2
Basicity is one of most important index in polyaluminum sulfate iron product, is had very closely with water process flocculating effect Relationship.Bodied ferric sulfate basicity is higher, then water process flocculating effect is better.As can be seen from Table 2, Examples 1 to 3 product In basicity be higher than the basicity in 1~2 product of comparative example, then the water process flocculating effect of Examples 1 to 3 product can be more preferable And product characteristic obtained complies with the national standard requirements.
Table 3 is the data of the flocculating effect of product made from Examples 1 to 3 and comparative example 1~2
Note: "-" expression no longer provides turbidity.
From table 3 it can be seen that the coagulation effect of bodied ferric sulfate prepared by the embodiment of the present invention 1~3 is substantially better than comparison The coagulation effect of bodied ferric sulfate prepared by example 1~2.
When water turbidity reaches 1.0NTU, bodied ferric sulfate dosage prepared by the embodiment of the present invention 1 is 20mg/L, and When water turbidity reaches 1.0NTU, bodied ferric sulfate dosage prepared by comparative example 2 is 30mg/L, can save dosage (30-20)/20*100%=50% substantially reduces the production cost of product and improves product coagulation effect, can achieve good Good productivity effect and economic benefit.
Bodied ferric sulfate, commercially available prepared by bodied ferric sulfate prepared by Examples 1 to 3 in the present invention, comparative example 1~2 Bodied ferric sulfate (be purchased from Zibo sky and water new material Co., Ltd) be respectively put into beaker, be respectively separated 1h, 5h, 10h, for 24 hours, 2d, 5d, 10d, 30d, 50d and 70d observe phenomenon, record such as table 4.
The phenomenon that 4 various bodied ferric sulfates of table, compares
From table 4, it can be seen that the bodied ferric sulfate and commercially available bodied ferric sulfate of Examples 1 to 3 preparation are stable State, and the state labile of bodied ferric sulfate prepared by comparative example 1~2.Specifically, meeting when placing 1~10 hour There is the phenomenon that thick liquid, without mobility, stability declines significantly.With the increase of experimental period, when place for 24 hours~ When 10d, it may appear that the phenomenon that yellowish-brown lotion;When placing 30d~70d, it may appear that the phenomenon that g., jelly-like solid.
It should be appreciated that described above, the specific embodiments are only for explaining the present invention, is not intended to limit the present invention.By The obvious changes or variations that spirit of the invention is extended out are still in the protection scope of this invention.

Claims (9)

1. a kind of preparation method of bodied ferric sulfate, it is characterised in that: include the following steps, in catalyst and cocatalyst item Under part, bodied ferric sulfate is made in ferrous sulfate mixed solution and oxidant reaction.
2. the preparation method of bodied ferric sulfate according to claim 1, it is characterised in that: the cocatalyst is phosphoric acid Sodium, the catalyst are sulfuric acid, and the mass fraction of the sulfuric acid is 98%, are at mass fraction by the catalyst preparation 1 ‰~2 ‰ working solution.
3. the preparation method of bodied ferric sulfate according to claim 2, it is characterised in that: the dosage of the working solution is Finished product per ton uses 1~2 kilogram, and the cocatalyst dosage is that finished product per ton uses 1~2g.
4. the preparation method of bodied ferric sulfate according to claim 1, it is characterised in that: the oxidant be oxygen or Ozone.
5. the preparation method of bodied ferric sulfate according to claim 1, it is characterised in that: the ferrous sulfate mixing is molten Liquid is the mixed solution of pickle liquor, ferrous sulfate, and wherein the mass ratio of pickle liquor and ferrous sulfate is 1:1~1.2.
6. the preparation method of bodied ferric sulfate according to claim 5, it is characterised in that: the pickle liquor is steel pipe The pickle liquor of factory or trombone slide factory.
7. the preparation method of bodied ferric sulfate according to claim 6, it is characterised in that: ferrous in the pickle liquor With Fe2+Counting mass fraction is 10~15%, and acid is with H2SO4Counting mass fraction is 8~10%.
8. a kind of Polymerization ferric sulfate water treatment agent is obtained by preparation method according to any one of claims 1 to 8.
9. Polymerization ferric sulfate water treatment agent according to claim 8 is applied in wastewater treatment and sludge treatment technique.
CN201811208396.3A 2018-10-17 2018-10-17 Preparation method of polymeric ferric sulfate Active CN108975475B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110228932A (en) * 2019-07-18 2019-09-13 广州晓橙环保科技有限公司 A kind of sludge conditioner and its application method
CN111995027A (en) * 2020-07-07 2020-11-27 广西夏阳环保科技有限公司 Metallurgical coking wastewater treatment agent and preparation method thereof
CN113247960A (en) * 2021-05-07 2021-08-13 河南师范大学 Production method of nano composite solid polymeric ferric sulfate
CN115382503A (en) * 2022-09-14 2022-11-25 岳阳天河环保科技有限公司 Preparation method of special phosphorus removal agent based on modified attapulgite

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CN105906019A (en) * 2016-06-23 2016-08-31 江门市江海区炜洁净水材料有限公司 Preparing method for polymeric ferric phosphoric sulfate water purifying agent
CN108046335A (en) * 2017-11-29 2018-05-18 兰州理工大学白银新材料研究院 A kind of solid ferric polysulfate preparation method

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CN105906019A (en) * 2016-06-23 2016-08-31 江门市江海区炜洁净水材料有限公司 Preparing method for polymeric ferric phosphoric sulfate water purifying agent
CN108046335A (en) * 2017-11-29 2018-05-18 兰州理工大学白银新材料研究院 A kind of solid ferric polysulfate preparation method

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110228932A (en) * 2019-07-18 2019-09-13 广州晓橙环保科技有限公司 A kind of sludge conditioner and its application method
CN111995027A (en) * 2020-07-07 2020-11-27 广西夏阳环保科技有限公司 Metallurgical coking wastewater treatment agent and preparation method thereof
CN113247960A (en) * 2021-05-07 2021-08-13 河南师范大学 Production method of nano composite solid polymeric ferric sulfate
CN115382503A (en) * 2022-09-14 2022-11-25 岳阳天河环保科技有限公司 Preparation method of special phosphorus removal agent based on modified attapulgite

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