CN109133293A - A kind of preparation process of use in waste water treatment bodied ferric sulfate crystal - Google Patents
A kind of preparation process of use in waste water treatment bodied ferric sulfate crystal Download PDFInfo
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- CN109133293A CN109133293A CN201811234816.5A CN201811234816A CN109133293A CN 109133293 A CN109133293 A CN 109133293A CN 201811234816 A CN201811234816 A CN 201811234816A CN 109133293 A CN109133293 A CN 109133293A
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- sulfate
- solution
- ferric sulfate
- ferrous
- water treatment
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- 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
Abstract
The present invention relates to industrial waste water treatment, specially a kind of preparation process of use in waste water treatment bodied ferric sulfate crystal, it is intended to solve the problems, such as that tradition is prepared in bodied ferric sulfate production process and be easy to appear ferric hydroxide precipitate.Its preparation step mainly includes S1: the concentrated sulfuric acid being diluted with deionized water, prepares sulfuric acid solution；S2: ferrous sulfate solid powder is added into sulfuric acid solution, ferrous sulfate solution is prepared；S3: oxidant and modifying agent chavicol being added into ferrous sulfate solution, make ferrous sulfate that oxidation, hydrolysis and polymerization reaction occur, polymeric ferrous sulphate solution is made；S4: polymeric ferrous sulphate solution is cooled down, and prepares bodied ferric sulfate crystal.Chavicol is added in the present invention in the solution, makes to form pi bond effect between chavicol and iron hydroxide, successively avoids ferric hydroxide precipitate.
Description
Technical field
The present invention relates to industrial waste water treatment, specially a kind of system of use in waste water treatment bodied ferric sulfate crystal
Standby technique.
Background technique
Bodied ferric sulfate has been developed in recent years a kind of inorganic polymer flocculant, with traditional flocculant such as three
Iron chloride, aluminum sulfate, chloro sulphuric acid iron etc. are compared, low with production cost and purification process adding less, applicable pH range
Extensively, impurity (turbidity, COD, suspended matter etc.) removal rate is high, debris concentration is low, alumen ustum sinking speed is fast, and good decolorizing effect etc. is excellent
Point.The production method of bodied ferric sulfate can be divided mainly into two major class: (1) direct oxidation method, that is, use strong oxidizer (such as H2O2、
NaClO、KClO3And MnO2Deng) it is directly iron ion by ferrous ions, then hydrolyzed and polymerize and obtain bodied ferric sulfate；
(2) that is, under the effect of the catalyst ferrous ions are iron ion using air or oxygen by catalytic oxidation, same to pass through
Hydrolysis and polymerization obtain bodied ferric sulfate.
Publication No. is that the patent of invention of CN1109027 discloses a kind of production new technique of bodied ferric sulfate, with sulfuric acid
Ferrous iron is primary raw material, and bodied ferric sulfate stoste is made under conditions of temperature-pressure and oxygenation, and liquid is made through diluting in stoste
Polyaluminum sulfate iron product, then through dry obtained solid ferric polysulfate product.
But the technical solution of above-mentioned disclosure is in the actual production process, and it is heavy often to occur iron hydroxide in product mixture
It forms sediment, influences product purity.
Summary of the invention
The object of the present invention is to provide a kind of preparation processes of use in waste water treatment bodied ferric sulfate crystal, can be preferably
It solves the problems, such as that tradition is prepared in bodied ferric sulfate production process and is easy to appear ferric hydroxide precipitate.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of preparation process of use in waste water treatment bodied ferric sulfate crystal, comprising the following steps:
S1: the concentrated sulfuric acid is diluted with deionized water, prepares sulfuric acid solution；
S2: ferrous sulfate solid powder is added into sulfuric acid solution, ferrous sulfate solution is prepared；
S3: oxidant and modifying agent being added into ferrous sulfate solution, make ferrous sulfate that oxidation, hydrolysis and polymerization occur anti-
It answers, polymeric ferrous sulphate solution is made；
S4: polymeric ferrous sulphate solution is cooled down, and prepares bodied ferric sulfate crystal.
Further, oxidant described in S3 is permanganic acid chromium.
Further, modifying agent described in S3 is chavicol.
Further, in S4 while cooling down to polymeric ferrous sulphate solution, chromium sulfate, manganese sulfate and nitre are added thereto
At least two in sour iron, it stirs evenly.
Further, the molar concentration of sulfuric acid is 0.5-3moL/L in the sulfuric acid solution prepared in S1.
Further, the molar concentration of ferrous sulfate is 5-10moL/L in the ferrous sulfate solution prepared in S2.
Further, polymeric ferrous sulphate solution is cooled as 5 DEG C or less in S4.
The invention has the following advantages:
1. improving the phenomenon that iron hydroxide easily precipitates by the way that modifying agent chavicol is added in the solution.Iron hydroxide
Because its solubility product is very small, the solubility product at 20 DEG C is about 4*10-33, therefore, it is very easy to sink in the solution
It forms sediment.Modifying agent chavicol is added in the solution, contains a large amount of double bonds in chavicol, the d orbital electron of iron ion with
The pi bond effect that d-p form is formed between chavicol, makes iron hydroxide in conjunction with chavicol, formation is dissolved each other, to keep away
Exempt from ferric hydroxide precipitate, improves the purity of finished product.
2. promoting to gather by the way that chromium sulfate, manganese sulfate and ferric nitrate are added thereto in bodied ferric sulfate crystallisation step
Close the crystallization of ferric sulfate.The intramolecular nuclear separation of chromium sulfate and manganese sulfate is all larger than the intramolecular nuclear separation of ferric sulfate, and the two
Molecular bond energy is respectively less than ferric sulfate, and therefore, when chromium sulfate, manganese sulfate and ferric sulfate exist simultaneously, manganese sulfate is electric in aqueous solution
From more thoroughly, sulfate radical increases in solution；Meanwhile ferric nitrate ionizes in aqueous solution, increases iron concentration in aqueous solution,
According to common-ion effect, the ionization equilibrium of ferric sulfate is carried out to the direction of ferric sulfate crystalline deposit, to promote the knot of ferric sulfate
It is brilliant.On the other hand, after chromium sulfate, manganese sulfate and ferric nitrate being added in solution, ionic species and quantity in entire reaction system
Increase that (chromium sulfate, manganese sulfate and ferric nitrate ionize out sulfate radical, chromium ion, manganese ion, nitrate ion and iron in aqueous solution
Ion), the electrolyte concentration in reaction system increases, and the ionization equilibrium of ferric sulfate is destroyed, the solubility of ferric sulfate is reduced, thus
The crystallization for further strengthening ferric sulfate is precipitated.
Specific embodiment
Technical solution is clearly and completely described below in conjunction with the embodiment of the present invention.Obviously, described implementation
Example is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiment of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention discloses a kind of preparation process of use in waste water treatment bodied ferric sulfate crystal, it is each that specific preparation process is as follows
Shown in embodiment.
Embodiment 1
S1: taking mass concentration is the 98% industrial concentrated sulfuric acid, is added into 100mL deionized water, makes sulphur
Acid concentration is the sulfuric acid solution of 0.5moL/L.
S2: taking ferrous sulfate solid powder 13.9g, is added into the sulphur that the sulfuric acid concentration prepared into S1 is 0.5moL/L
It in acid solution, is uniformly mixed, the molar concentration for preparing ferrous sulfate is the ferrous sulfate solution of 5moL/L.
S3: oxidant permanganic acid chromium 0.5g, modifying agent chavicol are added in the ferrous sulfate solution prepared into S2
3mL is stirred, and is uniformly mixed.Ferrous ion is oxidized to ferric ion；Ferric ion hydrolyzes later, generates hydrogen-oxygen
Change iron；Later, polymerization reaction occurs, obtains polymeric ferrous sulphate solution.
Since the solubility product of iron hydroxide is very small, the solubility product at 20 DEG C is about 4*10-33, therefore, in solution
In be very easy to precipitate.In the present embodiment, modifying agent chavicol is added in the solution, contains in chavicol big
Double bond is measured, the pi bond effect of d-p form is formed between the d orbital electron and chavicol of iron ion, makes iron hydroxide and allyl
Base phenol combines, and formation is dissolved each other, to avoid ferric hydroxide precipitate, improves the purity of finished product.
S4: by the polymeric ferrous sulphate solution prepared in S3 as cooling down in 5 DEG C of cold water, meanwhile, total matter is added thereto
Amount is the chromium sulfate of 0.5g and the mixture of manganese sulfate, and the two mass ratio is 1:1, and stirring prepares bodied ferric sulfate crystal.
The intramolecular nuclear separation of chromium sulfate and manganese sulfate is all larger than the intramolecular nuclear separation of ferric sulfate, the molecular bond energy of the two
Respectively less than ferric sulfate, therefore, when chromium sulfate, manganese sulfate and ferric sulfate three exist simultaneously, chromium sulfate and manganese sulfate are in aqueous solution
Middle ionization is more thorough, and sulfate radical increases in solution, and according to common-ion effect, the ionization equilibrium of ferric sulfate is to ferric sulfate crystalline deposit
Direction carry out, to promote the crystallization of ferric sulfate.On the other hand, entire to react after chromium sulfate and manganese sulfate being added in solution
Ionic species and quantity in system increase (chromium sulfate and manganese sulfate ionize out in aqueous solution sulfate radical, chromium ion, manganese from
Son), the electrolyte concentration in reaction system increases, and the ionization equilibrium of ferric sulfate is destroyed, the solubility of ferric sulfate is reduced, thus into
The crystallization that one step reinforces ferric sulfate is precipitated.
Embodiment 2
S1: taking mass concentration is the 95% industrial concentrated sulfuric acid, is added into 100mL deionized water, makes sulphur
Acid concentration is the sulfuric acid solution of 2moL/L.
S2: taking ferrous sulfate solid powder 22.3g, is added into the sulfuric acid that the sulfuric acid concentration prepared into S1 is 2moL/L
It in solution, is uniformly mixed, the molar concentration for preparing ferrous sulfate is the ferrous sulfate solution of 8moL/L.
S3: oxidant permanganic acid chromium 0.5g, modifying agent chavicol are added in the ferrous sulfate solution prepared into S2
3mL is stirred, and is uniformly mixed.Ferrous ion is oxidized to ferric ion；Ferric ion hydrolyzes later, generates hydrogen-oxygen
Change iron；Later, polymerization reaction occurs, obtains polymeric ferrous sulphate solution.
Since the solubility product of iron hydroxide is very small, the solubility product at 20 DEG C is about 4*10-33, therefore, in solution
In be very easy to precipitate.In the present embodiment, modifying agent chavicol is added in the solution, contains in chavicol big
Double bond is measured, the pi bond effect of d-p form is formed between the d orbital electron and chavicol of iron ion, makes iron hydroxide and allyl
Base phenol combines, and formation is dissolved each other, to avoid ferric hydroxide precipitate, improves the purity of finished product.
S4: by the polymeric ferrous sulphate solution prepared in S3 as cooling down in 0 DEG C of ice water, meanwhile, total matter is added thereto
Amount is the manganese sulfate of 0.8g and the mixture of ferric nitrate, and the two mass ratio is 1:1, and stirring prepares bodied ferric sulfate crystal.
The intramolecular nuclear separation of manganese sulfate is greater than the intramolecular nuclear separation of ferric sulfate, and molecular bond energy is less than ferric sulfate, because
This, when manganese sulfate and ferric sulfate exist simultaneously, manganese sulfate ionizes more thoroughly in aqueous solution, and sulfate radical increases in solution；Meanwhile
Ferric nitrate ionizes in aqueous solution, increases iron concentration in aqueous solution, according to common-ion effect, the ionization equilibrium of ferric sulfate
It is carried out to the direction of ferric sulfate crystalline deposit, to promote the crystallization of ferric sulfate.On the other hand, manganese sulfate and nitre are added in solution
After sour iron, ionic species and quantity in entire reaction system increase that (manganese sulfate and ferric nitrate ionize out sulfuric acid in aqueous solution
Root, manganese ion, nitrate ion and iron ion), the electrolyte concentration in reaction system increases, and the ionization for destroying ferric sulfate is flat
Weighing apparatus, reduces the solubility of ferric sulfate, so that the crystallization for further strengthening ferric sulfate is precipitated.
Embodiment 3
S1: taking mass concentration is the 98% industrial concentrated sulfuric acid, is added into 100mL deionized water, makes sulphur
Acid concentration is the sulfuric acid solution of 3moL/L.
S2: taking ferrous sulfate solid powder 27.8g, is added into the sulfuric acid that the sulfuric acid concentration prepared into S1 is 3moL/L
It in solution, is uniformly mixed, the molar concentration for preparing ferrous sulfate is the ferrous sulfate solution of 10moL/L.
S3: oxidant permanganic acid chromium 0.8g, modifying agent chavicol are added in the ferrous sulfate solution prepared into S2
5mL is stirred, and is uniformly mixed.Ferrous ion is oxidized to ferric ion；Ferric ion hydrolyzes later, generates hydrogen-oxygen
Change iron；Later, polymerization reaction occurs, obtains polymeric ferrous sulphate solution.
Since the solubility product of iron hydroxide is very small, the solubility product at 20 DEG C is about 4*10-33, therefore, in solution
In be very easy to precipitate.In the present embodiment, modifying agent chavicol is added in the solution, contains in chavicol big
Double bond is measured, the pi bond effect of d-p form is formed between the d orbital electron and chavicol of iron ion, makes iron hydroxide and allyl
Base phenol combines, and formation is dissolved each other, to avoid ferric hydroxide precipitate, improves the purity of finished product.
S4: by the polymeric ferrous sulphate solution prepared in S3 as cooling down in 1 DEG C of ice water, meanwhile, total matter is added thereto
Amount is the mixture of the chromium sulfate of 1.2g, manganese sulfate and ferric nitrate, and three's mass ratio is 1:1:1, and stirring prepares bodied ferric sulfate
Crystal.
The intramolecular nuclear separation of chromium sulfate and manganese sulfate is all larger than the intramolecular nuclear separation of ferric sulfate, and the two molecular bond energy
Respectively less than ferric sulfate, therefore, when chromium sulfate, manganese sulfate and ferric sulfate exist simultaneously, manganese sulfate ionizes more thoroughly in aqueous solution,
Sulfate radical increases in solution；Meanwhile ferric nitrate ionizes in aqueous solution, increases iron concentration, according to from
The ionization equilibrium of sub- effect, ferric sulfate is carried out to the direction of ferric sulfate crystalline deposit, to promote the crystallization of ferric sulfate.Another party
Face, after chromium sulfate, manganese sulfate and ferric nitrate is added in solution, ionic species and quantity in entire reaction system increase (sulfuric acid
Chromium, manganese sulfate and ferric nitrate ionize out sulfate radical, chromium ion, manganese ion, nitrate ion and iron ion in aqueous solution), instead
It answers the electrolyte concentration in system to increase, destroys the ionization equilibrium of ferric sulfate, reduce the solubility of ferric sulfate, to further add
The crystallization of strength sulfuric acid iron is precipitated.
Experimental result: according to water treatment agent, the standard GB/T 14591-2006 of bodied ferric sulfate is to obtained by each embodiment
Polymeric ferrous sulphate solution or crystalline solid are detected, specific testing result such as following table.
As seen from the above table, the bodied ferric sulfate indices prepared using technical solution provided by the present invention meet country
Standard, especially insolubles content, hence it is evident that be not higher than 0.5% lower than requirements of the national standard, illustrate in the present invention using modification
Agent chavicol handles iron hydroxide, can be effectively improved the precipitating of iron hydroxide.
Claims (7)
1. a kind of preparation process of use in waste water treatment bodied ferric sulfate crystal, which comprises the following steps:
S1: the concentrated sulfuric acid is diluted with deionized water, prepares sulfuric acid solution；
S2: ferrous sulfate solid powder is added into sulfuric acid solution, ferrous sulfate solution is prepared；
S3: oxidant and modifying agent being added into ferrous sulfate solution, make ferrous sulfate that oxidation, hydrolysis and polymerization reaction occur,
Polymeric ferrous sulphate solution is made；
S4: polymeric ferrous sulphate solution is cooled down, and prepares bodied ferric sulfate crystal.
2. a kind of preparation process of use in waste water treatment bodied ferric sulfate crystal according to claim 1, it is characterised in that: S3
Described in oxidant be permanganic acid chromium.
3. a kind of preparation process of use in waste water treatment bodied ferric sulfate crystal according to claim 1, it is characterised in that: S3
Described in modifying agent be chavicol.
4. a kind of preparation process of use in waste water treatment bodied ferric sulfate crystal according to claim 1, it is characterised in that: S4
In while cooling down to polymeric ferrous sulphate solution, chromium sulfate, at least two in manganese sulfate and ferric nitrate are added thereto, stirs
It mixes uniformly.
5. a kind of preparation process of use in waste water treatment bodied ferric sulfate crystal according to claim 1, it is characterised in that: S1
The molar concentration of sulfuric acid is 0.5-3moL/L in the sulfuric acid solution of middle preparation.
6. a kind of preparation process of use in waste water treatment bodied ferric sulfate crystal according to claim 1, it is characterised in that: S2
The molar concentration of ferrous sulfate is 5-10moL/L in the ferrous sulfate solution of middle preparation.
7. a kind of preparation process of use in waste water treatment bodied ferric sulfate crystal according to claim 1, it is characterised in that: S4
It is middle that polymeric ferrous sulphate solution cools as 5 DEG C or less.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362242A (en) * | 2020-03-19 | 2020-07-03 | 王敏 | Preparation method of anhydrous iron phosphate with large specific surface area |
| CN111517535A (en) * | 2020-04-20 | 2020-08-11 | 生态环境部华南环境科学研究所 | Method for treating chemical copper plating waste liquid by utilizing autocatalytic reaction |
| CN114160555A (en) * | 2021-11-25 | 2022-03-11 | 赛恩斯环保股份有限公司 | Wet mineralization and detoxification treatment method for arsenic sulfide slag |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111362242A (en) * | 2020-03-19 | 2020-07-03 | 王敏 | Preparation method of anhydrous iron phosphate with large specific surface area |
| CN111362242B (en) * | 2020-03-19 | 2021-09-24 | 王敏 | Preparation method of anhydrous iron phosphate with large specific surface area |
| CN111517535A (en) * | 2020-04-20 | 2020-08-11 | 生态环境部华南环境科学研究所 | Method for treating chemical copper plating waste liquid by utilizing autocatalytic reaction |
| CN114160555A (en) * | 2021-11-25 | 2022-03-11 | 赛恩斯环保股份有限公司 | Wet mineralization and detoxification treatment method for arsenic sulfide slag |
| CN114160555B (en) * | 2021-11-25 | 2022-09-16 | 赛恩斯环保股份有限公司 | Wet mineralization and detoxification treatment method for arsenic sulfide slag |
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Denomination of invention: Preparation process of polymeric iron sulfate crystals for wastewater treatment Effective date of registration: 20230913 Granted publication date: 20210924 Pledgee: Agricultural Bank of China Limited Qianjiang Branch Pledgor: HUBEI YONG SHAO POLYTRON TECHNOLOGIES Inc. Registration number: Y2023980056462 |