CN1559917A - Process of synthesizing high titanate and application as dehydrator for algas thereby - Google Patents
Process of synthesizing high titanate and application as dehydrator for algas thereby Download PDFInfo
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- CN1559917A CN1559917A CNA2004100218525A CN200410021852A CN1559917A CN 1559917 A CN1559917 A CN 1559917A CN A2004100218525 A CNA2004100218525 A CN A2004100218525A CN 200410021852 A CN200410021852 A CN 200410021852A CN 1559917 A CN1559917 A CN 1559917A
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Abstract
The invention is a ferrate synthesizing method and its application as algae dehydrator, uniformly mixing ferric salt with ultra peroxide in a mixer, placing the mixture in a reaction kettle and arranging the kettle in a resonant cavity, using an infrared thermometer to measure temperature, regulating the anode current of a microwave source and the cavity short-circuiting piston to control the field strength in the resonant cavity, maintaining reaction temperature to bake reacting mixture, vacuum-cooling and obtaining the crude ferrate product. It is easy, convenient and safe to develop and the ferrate added to algae in forms of final product, basic solution, ferrate-containing solution in production oxidizes and flocculates the algae, implementing the dehydration and effective separation of residues from water.
Description
Affiliated technical field:
The present invention relates to a kind of novel method of synthesized high iron hydrochlorate and used as the application of algae dewatering agent.
Background technology: high ferro acid group (FeO
4 2-) having the space tetrahedral structure, its redox potential in acid-alkali medium is respectively 2.20V and 0.72V (R.H.Wood, J.Am.Chem.Soc., Vol.80, p.2038-2041 (1957)).Its four Sauerstoffatom equivalences in water, and at leisure with water molecules in Sauerstoffatom exchange (J.Gump, W.Wagner, and E.Hart, Anal.Chem., Vol.24., p.1497-1498 (1952)).
Because ferrate is a kind of strong oxidizer also stronger than the oxidation capacity of potassium permanganate, ozone and chlorine, in whole pH scope, all have oxidisability, can with many inorganic and organic reducing agent reactions, and high ferro acid group (FeO
4 2-) Fe that generates of reaction reduction
3+Can produce the polymerization throwing out, so ferrate has fine application prospect aspect organic synthesis and the water treatment.Because the high ferro acid group is in all oxidizing reactions, final product is avirulent Fe
3+, thereby have the feature of environmental friendliness oxygenant.
Ferrate is found first by Germany's chemistry and physicist Geor Stahl that as far back as 1720 its laboratory is synthetic to start from 1897.The someone is engaged in laboratory vegetation and suitability for industrialized production research thereof always since finding, but do not form the maturation process of everybody approval so far yet, this mainly is because preparation method's more complicated of ferrate, operational condition is relatively harsher, product recovery rate is on the low side, poor stability, the large-scale industrial production of being unrealized eventually, this has also seriously limited its application.
The method of known three kinds of synthesized high iron hydrochlorates is at present: hypochlorite oxidation style, electrolytic process and scorification.
The hypochlorite oxidation style was proposed by Hrostowski and Scott in nineteen fifty, and product purity can reach 96.9%, but productive rate is extremely low, is no more than 10～15%.People such as Thomposn improve from preparation and two processes of purifying aforesaid method, and productive rate can be brought up to 44～76% (Thomposn G.W., Ockerman L.T., and Schreyer J.M., J.Am.Chem.Soc., Vol.73., p.1379-1381 (1951)).At present, both at home and abroad about the report of the preparation of ferrate mostly based on the preparation method of propositions such as Thomposn, proposed some improvement at the particular problem of some link, but this method still is difficult to realize heavy industrialization.
It is that anodic alkaline hydrated oxide solution is realized with iron by electrolysis that electrolytic process prepares ferrate.This method is simple to operate, and raw materials consumption is few, but the power consumption height, byproduct is more, the purge process complexity, and efficient is low.
Scorification adopts the oxide compound of superoxide high temperature oxidation iron to prepare ferrate.Because this method sets off an explosion easily, the operational condition harshness, relatively more dangerous, be difficult to realize suitability for industrialized production, so there be limited evidence currently of adopts.
In addition, the invention still further relates to the application of ferrate as the algae dewatering agent.
Algae is to distribute the extensivelyst, also is one of biology the most able to bear hardships, no matter be the two poles of the earth of the earth, near the ebullient hot spring, or on more salty than seawater in ten times the salina, it can both be grown.Even in the desert, it also can be survived.In lake and river, algae relies on dirt and multiplies procreation.Along with society, rapid development of economy, human pollution and destruction to water source environment is also serious day by day, and increasing of nitrogen, phosphorus content causes the source water eutrophication in the water body, thereby causes a large amount of breedings of algae.
The surface pond is adopted in domestic most of waterworks more, takes from rivers, lake and reservoir respectively.Along with the expansion of eutrophic water area and increasing the weight of of degree, algae becomes day by day with face of land unhurried current waters, is that the waterworks at water source is the problem of headache deeply as the lake.The floatation algal residue of waterworks is the residue that produces in the air floatation alga removing technological process, and it and water form a kind of dope of colloidal, swims in formation industrial residue waterborne.
Long term studies shows that algae-residue is more difficult, and reason has 2 points: the water ratio of (1) wet algae-residue is about 97%, and algae-residue and water form a more stable system, is difficult to separate.(2) amount of algae-residue is very big, is difficult to find rational processing approach.
Some water factory at will throws aside it outside factory, and stink is very big, influences environmental health; Some water factory then simply passes back into the lake with it, but the consequence of doing like this is to have formed an algae circulation, has increased the algae amount that contains in lake, and may make algae produce certain resistance, has increased the difficulty of algae processing from now on.
Find that in application algae-residue is better with sheet frame filter dehydrating effect.Processings of will offeing medicine before the dehydration, generally medicament adds iron trichloride or lime addition polymerization aluminium with lime, and comparatively speaking, the filter cake moisture content after the latter dewaters is lower, is about 78%.The final outlet of algae-residue generally is producing methane, brickmaking or composting.But present three kinds of ways all have certain problem.
Direct processing aspect: though take off algae-residue water effect better with the sheet frame filter, the processing of will offeing medicine before the dehydration, and also dehydration rate is low, only has about 22%.In addition, institute's with medicament is generally lime and adds iron trichloride or lime addition polymerization aluminium, and chloride thing be added in carcinogenic by products such as being easy to generate halohydrocarbon in the water, the adding of poly-aluminium flocculating agent will be detrimental to health because of aluminum ions residual accumulation, thereby brings secondary pollution.
Composting aspect: mainly be that to utilize the algae-residue of water treatment and mud that is produced from the municipal sewage plant be main fertilizer raw material, be equipped with inorganic fertilizer and make the special-purpose mixed fertilizer of various crops, as CN 1 155 529A, CN 1 158 328A, the method that CN 1 097 409A etc. propose because the water ratio of used algae-residue is 5～30%, adopts desiccating method usually, so both caused the waste of water, again contaminate environment.
Because the algae-residue of waterworks belongs to the non-degradable thing, toxic organic compound such as trichloromethane content are higher, and present treatment process can not the mass treatment that this serious harm is healthy be fallen and do not caused secondary pollution.
Summary of the invention: the novel method that the invention discloses a kind of synthesized high iron hydrochlorate, be in mixing tank, molysite and superoxide or super-oxide to be mixed, the reactor of packing into places in the resonator cavity, measure temperature with infrared thermometer, regulate field intensity in microwave source anodic current and the cavity short-circuit plunger control resonator cavity, keep temperature of reaction roasting reaction mixture, vacuum cooling obtains the thick product of ferrate, easy, convenient, the safety of this synthetic method exploitation; Can also prepare sodium salt, sylvite and other cationic salts.
The invention also discloses the method for purifying ferrate.
A kind of synthetic method of ferrate, synthesis step is as follows:
A. in mixing tank with molysite and superoxide or super-oxide by mass ratio=(0.5～2.0): (1.5～6.0) mix;
B. pack into reactor and placing in the resonator cavity of mixture, be not less than under the 50W microwave radiation at microwave output power, keep temperature of reaction roasting reaction mixture, with superoxide or super-oxide molysite is oxidized to ferrate, the mixture reaction temperature is 300 ± 50～1000 ± 50 ℃, and roasting time is 2min～15h;
C. vacuum cooling obtains the thick product of ferrate;
D. by thick product (g): 6M potassium hydroxide aqueous solution (ml): saturated potassium hydroxide aqueous solution (ml)=(2.0～8.0): (20～60): (20～60), wash thick product with the 6M potassium hydroxide aqueous solution; Washing lotion is filtered in the saturated potassium hydroxide solution that joins in the ice bath; Under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solids and filtrate to saturated; Potassium hydroxide aqueous solution rinsing solids with 6M; Washing lotion is filtered in the saturated potassium hydroxide aqueous solution that joins in the ice bath; Under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solid potassium ferrate and filtrate to saturated;
E. with the purification product of drying solid potassium ferrate under the ether vacuum, vacuum is preserved then.
Above-mentioned molysite mixes with solid-state with superoxide or super-oxide.
Above-mentioned superoxide is sodium peroxide or Potassium peroxide or potassium hydrogen peroxymonosulfate; Super-oxide is a potassium superoxide.
Above-mentioned molysite be contain+2 and the compound of the iron atom of+3 valency oxidation state; Ferrate is that iron atom is the wustite that the above oxidation state of+4 valencys exists.
Above-mentioned microwave source power is adjustable continuously.
Another object of the present invention is to provide a kind of environmental friendliness algae dewatering agent, and the energy degree of depth is deviate from the water in the algae-residue, and with organic substance oxidation in the algae-residue, and can not cause secondary pollution to environment.Be about to ferrate and add algae with its oxidizing, flocculating with final product form or with the basic solution form or with the solution form that contains ferrate that produces in thick product form or the production process, realization dehydration and slag effectively separate with water.The ferrate consumption is 10～5000ppm, and moderate stirring 2～15min leaves standstill 5～30min after the stirring, filters.
Embodiment: the present invention further specifies by following examples and application example.
Embodiment one:
A. uniform mixing 2.0g ferric sulfate and 10.0g potassium hydrogen peroxymonosulfate;
B. pack into and place in the resonator cavity in the reactor;
C. measure temperature with infrared thermometer, regulating microwave output power is field intensity in 700W and the cavity short-circuit plunger control resonator cavity, and keeping temperature of reaction is 700 ± 50 ℃, roasting reaction mixture 10min;
D. vacuum cooling c obtains the thick product of ferrate;
E. with 25ml 6M potassium hydroxide aqueous solution washing d crude product;
F. washing lotion is filtered the saturated potassium hydroxide solution of 25ml that enters in ice bath;
G. under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solids and filtrate to saturated;
H. use the potassium hydroxide aqueous solution rinsing g solids of 15ml 6M;
I. washing lotion is filled in the saturated potassium hydroxide aqueous solution of 25ml in ice bath;
J. repeat g and obtain solid potassium ferrate and filtrate;
K. use drying solid potassium ferrate under the ether vacuum, vacuum is preserved then.
Embodiment two:
A. 3.0g ferric oxide and 6.0g sodium peroxide are mixed;
B. pack into and place in the resonator cavity in the reactor;
C. measure temperature with infrared thermometer, regulating microwave output power is field intensity in 800W and the cavity short-circuit plunger control resonator cavity, and keeping temperature of reaction is 800 ± 50 ℃, roasting reaction mixture 6min;
D. vacuum cooling c obtains the thick product of ferrate;
E. with 50ml 6M potassium hydroxide aqueous solution washing d crude product;
F. washing lotion is filtered the saturated potassium hydroxide solution of 50ml that enters in ice bath;
G. under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solids and filtrate to saturated;
H. use the potassium hydroxide aqueous solution rinsing g solids of 30ml 6M;
I. washing lotion is filled in the saturated potassium hydroxide aqueous solution of 50ml in ice bath;
J. repeat g and obtain solid potassium ferrate and filtrate;
K. use drying solid potassium ferrate under the ether vacuum, vacuum is preserved then.
Embodiment three:
A. 3.0g ferric oxide and 7.0g Potassium peroxide are mixed;
B. pack into and place in the resonator cavity in the reactor;
C. measure temperature with infrared thermometer, regulating microwave output power is field intensity in 500W and the cavity short-circuit plunger control resonator cavity, and keeping temperature of reaction is 400 ± 50 ℃, roasting reaction mixture 10h;
D. vacuum cooling c obtains the thick product of ferrate;
E. with 50ml 6M potassium hydroxide aqueous solution washing d crude product;
F. washing lotion is filtered the saturated potassium hydroxide solution of 50ml that enters in ice bath;
G. under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solids and filtrate to saturated;
H. use the potassium hydroxide aqueous solution rinsing g solids of 30ml 6M;
I. washing lotion is filled in the saturated potassium hydroxide aqueous solution of 50ml in ice bath;
J. repeat g and obtain solid potassium ferrate and filtrate;
K. use drying solid potassium ferrate under the ether vacuum, vacuum is preserved then.
Embodiment four:
A. 1.5g ferric oxide and 4.0g potassium superoxide are mixed;
B. pack into and place in the resonator cavity in the reactor;
C. measure temperature with infrared thermometer, regulating microwave output power is field intensity in 550W and the cavity short-circuit plunger control resonator cavity, and keeping temperature of reaction is 500 ± 50 ℃ of roasting reaction mixture 6h;
D. vacuum cooling c obtains the thick product of ferrate;
E. with 30ml 6M potassium hydroxide aqueous solution washing d crude product;
F. washing lotion is filtered the saturated potassium hydroxide solution of 30ml that enters in ice bath;
G. under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solids and filtrate to saturated;
H. use the potassium hydroxide aqueous solution rinsing g solids of 20ml 6M;
I. washing lotion is filled in the saturated potassium hydroxide aqueous solution of 30ml in ice bath;
J. repeat g and obtain solid potassium ferrate and filtrate;
K. use drying solid potassium ferrate under the ether vacuum, vacuum is preserved then.
Embodiment five:
A. 2.0g iron protoxide and 4.0g Potassium peroxide are mixed;
B. pack into and place in the resonator cavity in the reactor;
C. measure temperature with infrared thermometer, regulating microwave output power is field intensity in 700W and the cavity short-circuit plunger control resonator cavity, and keeping temperature of reaction is 800 ± 50 ℃ of roasting reaction mixture 8min;
D. vacuum cooling c obtains the thick product of ferrate;
E. with 40ml 6M potassium hydroxide aqueous solution washing d crude product;
F. washing lotion is filtered the saturated potassium hydroxide solution of 40ml that enters in ice bath;
G. under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solids and filtrate to saturated;
H. use the potassium hydroxide aqueous solution rinsing g solids of 20ml 6M;
I. washing lotion is filled in the saturated potassium hydroxide aqueous solution of 40ml in ice bath;
J. repeat g and obtain solid potassium ferrate and filtrate;
K. use drying solid potassium ferrate under the ether vacuum, vacuum is preserved then.
Embodiment six:
A. 3.0g ferrous sulfate and 4.0g sodium peroxide are mixed;
B. pack into and place in the resonator cavity in the reactor;
C. measure temperature with infrared thermometer, regulating microwave output power is field intensity in 600W and the cavity short-circuit plunger control resonator cavity, and keeping temperature of reaction is 500 ± 50 ℃ of roasting reaction mixture 6h;
D. vacuum cooling c obtains the thick product of ferrate;
E. with 30ml 6M potassium hydroxide aqueous solution washing d crude product;
F. washing lotion is filtered the saturated potassium hydroxide solution of 30ml that enters in ice bath;
G. under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solids and filtrate to saturated;
H. use the potassium hydroxide aqueous solution rinsing g solids of 20ml 6M;
I. washing lotion is filled in the saturated potassium hydroxide aqueous solution of 30ml in ice bath;
J. repeat g and obtain solid potassium ferrate and filtrate;
K. use drying solid potassium ferrate under the ether vacuum, vacuum is preserved then.
Application example one:
Get the floatation algal residue 100g of the water ratio about 97% of certain waterworks, add the g step filtrate of 50ml embodiment one, stir 2min, static 5min filters and obtains about 120ml liquid.Dehydration rate about 72.2%.
Application example two:
Get the floatation algal residue 100g of the water ratio about 97% of certain waterworks, add the solid product of 10mg embodiment one, stir 5min, static 10min filters and obtains about 77ml liquid.Dehydration rate about 79.4%.
Application example three:
Get the floatation algal residue 100g of the water ratio about 97% of certain waterworks, the d that adds 100mg embodiment two goes on foot thick product, stirs 2min, and static 5min filters and obtains about 74ml liquid.Dehydration rate about 76.3%.
Application example four:
Get the floatation algal residue 100g of the water ratio about 97% of certain waterworks, add the solid product of 10mg embodiment two, stir 5min, static 10min filters and obtains about 80ml liquid.Dehydration rate about 82.5%.
Application example five:
Get the floatation algal residue 100g of the water ratio about 97% of certain waterworks, add the g step filtrate of 50ml embodiment three, stir 2min, static 5min filters and obtains about 126ml liquid.Dehydration rate about 78.4%.
Application example six:
Get the floatation algal residue 100g of the water ratio about 97% of certain waterworks, add the j step filtrate of 50ml embodiment three, stir 2min, static 5min filters and obtains about 128ml liquid.Dehydration rate about 80.4%.
Application example seven:
Get the floatation algal residue 100g of the water ratio about 97% of certain waterworks, add the solid product of 10mg embodiment four, stir 5min, static 10min filters and obtains about 82ml liquid.Dehydration rate about 84.5%.
Application example eight:
Get the floatation algal residue 100g of the water ratio about 97% of certain waterworks, add the solid product of 10mg embodiment five, stir 5min, static 10min filters and obtains about 80ml liquid.Dehydration rate about 82.5%.
Application example nine:
Get the floatation algal residue 100g of the water ratio about 97% of certain waterworks, add the solid product of 10mg embodiment six, stir 5min, static 10min filters and obtains about 79ml liquid.Dehydration rate about 81.4%.
Claims (6)
1. the synthetic method of a ferrate, synthesis step is as follows:
A. in mixing tank with molysite and superoxide or super-oxide by mass ratio=(0.5～2.0): (1.5～6.0) mix;
B. pack into reactor and placing in the resonator cavity of mixture, be not less than under the 50W microwave radiation at microwave output power, keep temperature of reaction roasting reaction mixture, with superoxide or super-oxide molysite is oxidized to ferrate, the mixture reaction temperature is 300+50～1000 ± 50 ℃, and roasting time is 2min～15h;
C. vacuum cooling obtains the thick product of ferrate;
D. by thick product (g): 6M potassium hydroxide aqueous solution (ml): saturated potassium hydroxide aqueous solution (ml)=(2.0～8.0): (20～60): (20～60), wash thick product with the 6M potassium hydroxide aqueous solution; Washing lotion is filtered in the saturated potassium hydroxide solution that joins in the ice bath; Under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solids and filtrate to saturated; Potassium hydroxide aqueous solution rinsing solids with 6M; Washing lotion is filtered in the saturated potassium hydroxide aqueous solution that joins in the ice bath; Under 20 ℃ of the holding temperatures, add solid potassium hydroxide, continue to be refrigerated to precipitation and finish, filter and obtain solid potassium ferrate and filtrate to saturated;
E. with the purification product of drying solid potassium ferrate under the ether vacuum, vacuum is preserved then.
2. method according to claim 1 is characterized in that: molysite mixes with solid-state with superoxide or super-oxide.
3. method according to claim 1 is characterized in that: superoxide is sodium peroxide or Potassium peroxide or potassium hydrogen peroxymonosulfate; Super-oxide is a potassium superoxide.
4. method according to claim 1 is characterized in that: molysite be contain+2 and the compound of the iron atom of+3 valency oxidation state; Ferrate is that iron atom is the wustite that the above oxidation state of+4 valencys exists.
5. method according to claim 1 is characterized in that: microwave source power is adjustable continuously.
6. application that ferrate is used as the algae dewatering agent, it is characterized in that: ferrate adds algae with its oxidizing, flocculating with final product form or with the solution form that contains ferrate that produces in the building-up process or with thick product form, the ferrate consumption is 10～5000ppm, moderate stirring 2～15min, leave standstill 5～30min after the stirring, filter.
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| CNA2004100218525A CN1559917A (en) | 2004-02-15 | 2004-02-15 | Process of synthesizing high titanate and application as dehydrator for algas thereby |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497461B (en) * | 2009-03-16 | 2013-06-05 | 黄河水利职业技术学院 | Method for rapidly preparing ferrate solution by microwave radiation |
| CN113667823A (en) * | 2021-07-15 | 2021-11-19 | 江西理工大学 | Method for comprehensively recovering rare earth and iron from neodymium iron boron waste |
-
2004
- 2004-02-15 CN CNA2004100218525A patent/CN1559917A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497461B (en) * | 2009-03-16 | 2013-06-05 | 黄河水利职业技术学院 | Method for rapidly preparing ferrate solution by microwave radiation |
| CN113667823A (en) * | 2021-07-15 | 2021-11-19 | 江西理工大学 | Method for comprehensively recovering rare earth and iron from neodymium iron boron waste |
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