CN104803460A - Method for preparing PAFS (polymeric aluminum ferric sulfate) by adopting acid self-coupling balance and near-dry method - Google Patents
Method for preparing PAFS (polymeric aluminum ferric sulfate) by adopting acid self-coupling balance and near-dry method Download PDFInfo
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- CN104803460A CN104803460A CN201510133663.5A CN201510133663A CN104803460A CN 104803460 A CN104803460 A CN 104803460A CN 201510133663 A CN201510133663 A CN 201510133663A CN 104803460 A CN104803460 A CN 104803460A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/04—Surfactants, used as part of a formulation or alone
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- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a method for preparing PAFS (polymeric aluminum ferric sulfate) by adopting an acid self-coupling balance and near-dry method. According to the method, Al2(SO4)3*18H2O, FeSO4*7H2O and NaClO3 are taken as raw materials, the acid self-coupling balance and near-dry method is adopted to prepare the PAFS. The preparation conditions are as follows: the ratio of n(Al<3+>)/n(Fw<2+>) is 2.0, the temperature is 60 DEG C, the reaction time is 50 min, the oxidizing agent NaClO3 exceeds by 4% when accounted in terms of Fe<2+>, and the PAFS is prepared. The quality of the PAFS product meets the national standard requirement, the ferrous conversion rate of the product is reduced by 0.17% when the product is stored at the room temperature for 3 months, the basicity is reduced by 1.02%, the precipitation amount is increased by 2.78%, but all the indexes still meet the national standard requirements, accordingly, the indexes of the product are more stable, and the storage effect is better.
Description
Technical field
The present invention relates to chemical technology field, be specifically related to a kind of method that sour self coupling balances accurate dry process PAFS.
Background technology
Inorganic polymer coagulant is the novel coagulant grown up after the sixties in last century, and it has the advantage such as nontoxicity, low price, thus replaces organic polymer coagulating agent, is widely used in feeding water, the various flow processs of trade effluent and municipal effluent.At present, the inorganic polymer flocculant generally used mainly contains polymerize aluminum chloride (PAC) and bodied ferric sulfate (PFS) two kinds.Wherein polymerize aluminum chloride has the advantages such as remaining colourity is little, but is hydrolyzed weak, and flocculation volume is little, loose, the slow and Al of sedimentation
3+remain, be unfavorable for applying in water treatment.And bodied ferric sulfate has product performance and stablizes, not containing Al
3+and the objectionable impurities such as heavy metal, higher to the clearance of COD, turbidity, easily easy in water, dosage is little, hydrolysis is strong, and flocculation volume is large, advantages such as sedimentation is fast and being used widely, but also there is the deficiencies such as the remaining colourity of water outlet, limits its use.And the new and effective water conditioner of one that PFAS (PFAS) flocculation agent is comprehensive PFS and PAC advantage and develops, it is excellent that it has aluminium salt purifying water effect concurrently, the advantage that molysite settling velocity is fast, cost of water treatment is low; Also overcome that aluminium salt cost is higher, sedimentation effect is undesirable, excess of aluminum remains in water harmful, molysite easily produces the deficiency of yellowing and blackening, is a kind of desirable water treatment composite flocculant simultaneously.
A lot of to the research of PAFS in recent years, the method preparing PAFS is also various.Such as, Zhang Minquan, Jia-Q ianJiang and N igel J.D.Graham is with ferrous sulfate (FeSO
47H
2and Tai-Ace S 150 [Al O)
2(SO
4)
318H
2o] be main raw material, synthesize PAFS; Bodied ferric sulfate and polyaluminium sulfate mix by the people such as Mo Binglu according to a certain percentage, prepare PAFS, and these preparation methods need to add a large amount of acid or alkali.Meanwhile, if acidity is excessively strong in these preparation process, polymerization not exclusively; If acidity is excessively weak, easily emanate again, produce indissoluble material, therefore usually need to maintain the stable of reaction material liquid acidity in preparation process by the mode of outer acid adding or alkali, not only increase the control difficulty of technique, and affect quality product, increase the consumption of production process material and energy, be unfavorable for cleaner production.
The Atom economy and the clean-up performance that control, improve preparation process is easy in order to make preparation technology simple, I once proposed the novel method of sour self coupling balance Liquid preparation methods PAFS, but obtained product is also liquid, be unfavorable for storing and long-distance transport.For this reason, how applying polyaluminium sulfate iron product that easy, clean technique prepares dry state is those skilled in the art's technical problems urgently to be resolved hurrily.
Summary of the invention
The object of the present invention is to provide a kind of technique simple and be easy to control, Atom economy and the clean-up performance of preparation process are higher, directly can preparing the preparation method of dry state polyaluminium sulfate iron product, in order to realize object of the present invention, intending adopting following technical scheme:
The present invention relates to a kind of method that sour self coupling balances accurate dry process PAFS, it is characterized in that comprising the steps: to take a certain amount of solid iron vitriol and aluminum sulfate octadecahydrate, be placed in mortar, then quantitative sodium chlorate saturated solution is added, being ground to the specified time obtains tenne cream solid, is product PAFS (PAFS).Preparation condition is: n (Al
3+)/n (Fe
2+) proportioning is 0.8 to 2.0, temperature of reaction room temperature to 60 DEG C, reaction times 40 to 60min, oxygenant NaClO
3consumption presses Fe
2+the stoichiometries such as meter are to excessive 4%.The general preferably optional n (Al of preparation condition
3+)/n (Fe
2+) proportioning 1.4, temperature of reaction 50 DEG C, oxygenant NaClO
3consumption presses Fe
2+stoichiometry meter excessive 4%, reaction times 60min.
In a preferred embodiment of the present invention, the not outer acid adding/of described preparation method or alkali.
In a preferred embodiment of the present invention, except preparation sodium chlorate saturated solution adds except limited amount water in preparation process, do not add water again in addition, therefore the product that obtains is cream solid and on-liquid.
In a preferred embodiment of the present invention, in preparation process by adjustment reaction mass n (Al
3+)/n (Fe
2+) proportioning adjusts the basicity of product.
The invention enables the sour self coupling of PAFS (PAFS) product balance preparation method can when carrying out close to when dry state.Both the sour self coupling null readings preparation process having maintained my invention does not need outer acid adding, technique is simply easy to the advantage controlled, achieve again in preparation process and be only preparation sodium chlorate saturated solution and add outside limited amount water, do not add water again in addition, making obtained product be transport and the storage that cream solid facilitates product, providing possibility for expanding product radiation radius.Preparation method of the present invention meets the green production of low-carbon (LC), low consumption, reduces production cost, has certain realistic meaning, and solve the problem that in existing technique, PAFS liquid product radiation radius is narrower.
Embodiment
If not specified, the conventional means that technique means used in embodiment is well known to those skilled in the art.
Embodiment 1:
1 laboratory apparatus
Glass beaker (50mL 100mL 200mL 500mL 1000mL), (scale value is 0.001g/cm for electric magnetic agitator, digital display electric-heated thermostatic water bath, PH-2 type acidometer, densometer
3), graduated cylinder, drop-burette, triangular flask etc.
2 experimental drugs
Iron vitriol (analytical pure), ferric sulfate, sodium chlorate, aluminum sulfate octadecahydrate (analytical pure), distilled water, disodium ethylene diamine tetraacetate, ZnO, vulkacit H, phenolphthalein, concentrated hydrochloric acid, xylenol orange, A.R sterling sulfosalicylic acid, anhydrous sodium sulphate, Potassium monofluoride, Potassium Hydrogen Phthalate, 95% ethanol, NaOH.
3 experimental techniques
3.1 preparation method
Take a certain amount of sodium chlorate and be placed in mortar, add specified amount distilled water to dissolve, then solid iron vitriol, aluminum sulfate octadecahydrate is added, ceaselessly grind, being ground to the specified time obtains sorrel polyaluminium sulfate transparent liquid, is product PAFS (PAFS).With basicity, Fe
2+transformation efficiency and precipitation capacity are that index is to inquire into the feasibility of experiment.
3.2 detection method
(1) Fe is surveyed
2+transformation efficiency, detect and undertaken by Polyferric Sulfate product standard GB/T 14591-93.
(2) survey the basicity of product, detect and press polyaluminum sulfate iron product standard GB/T 14591-93.Measure ferro-aluminum content Continuous Titration method.
(3) survey the precipitation capacity of product, take and place slaking at normal temperatures (product is stablized) the product m of 7 days
1, add a certain amount of water and make it dissolve, then make its solid-liquid separation.Being placed on by the solid obtained in baking oven dries to constant weight, then claims its weight m
2, calculate precipitation capacity (%)=m
2/ m
1
Embodiment 1: preparation during different milling time
Take sodium chlorate 0.5308g (by Fe
2+the stoichiometric excess 4% such as oxidation) be dissolved in 6ml water and be made into saturated solution, add and be equipped with solid iron vitriol 8g, in the mortar of aluminum sulfate octadecahydrate 13.4g, at 50 DEG C, be ground to setting-up time, products obtained therefrom the results are shown in Table 1.
The index of the different milling time products made thereby of table 1
From table, Fe within the system
2+oxidation and the hydrolysis of ferric iron aluminium be easier to carry out with being polymerized, be oxidized in combined reaction, hydrolysis, polymerization and ferro-aluminum the impact of multiple factor such as segregation, the reaction times is to control to be advisable at about 50min.
Embodiment 2: preparation during different oxygenant consumption
By embodiment 1 preparation condition, change oxygenant consumption griding reaction 50min, the results are shown in table 2.
Product prepared by the different oxygenant consumption of table 2
Table 2 data show, because reaction mass is relatively dry, for the oxygen in air participates in Fe
2+oxidation provides possibility, thus the Fe when amount owed by oxygenant
2+also higher oxidation ratio can be reached.In general, but for guaranteeing Fe
2+completely, oxygenant dosage is still advisable with excessive 4% in oxidation.
Embodiment 3: preparation during differential responses temperature
By the preparation condition of embodiment 2, oxygenant dosage is excessive 4%, and for preparing at differential responses temperature the results are shown in table 3.
Preparation during table 3 differential responses temperature
As can be seen from Table 3, it is not very high for reacting the requirement of temperature, the Fe of product between room temperature to 60 DEG C
2+transformation efficiency and basicity two indexs all can reach comparatively ideal value.But temperature obviously can affect the carrying out of ferro-aluminum hydrolysis, polymerization, is oxidized in combined reaction, hydrolysis, polymerization and ferro-aluminum the impact of multiple factor such as segregation, temperature of reaction selects 50 to 60 DEG C to be advisable.
Embodiment 4: assistant ingredients than time preparation
By the condition of embodiment 3, temperature of reaction changes 60 DEG C into, n (Al in adjustment material
3+)/n (Fe
2+) ratio of components, preparation the results are shown in table 4.
Table 4 assistant ingredients than time preparation
As can be seen from Table 4, the basicity index of product depends primarily on the proportioning n (Al of ferro-aluminum in reaction mass
3+)/n (Fe
2+), product basicity B/% and ratio of components N has good funtcional relationship, and this can be product basicity index Design and provides foundation.
Embodiment 5: ratio of components N is 1.8, reaction times 50min, and prepared by repeating under temperature of reaction 60 DEG C of conditions, the results are shown in table 5
Preparation result under table 5 the same terms
Can find out that this technology stability is relatively good from lower 3 results repeating sample of table 5 the same terms, carry out deisgn product basicity by ratio of components basic or reliable.
The investigation of 4.6 product memory properties
Obtained PAFS (PAFS) at room temperature stores 3 months, and after 3 months, the contrast of the indices of product is in table 6.
The contrast of table 63 months front and back product indices
Known according to table 6, after 3 months, the ferrous transformation efficiency of product have dropped 0.17%, and the basicity of product have dropped 1.02%, and the precipitation capacity of product adds 2.78%, because along with the increase of curing time, and Fe
3+there occurs slight hydrolysis, so the ferrous transformation efficiency of product has slight decline, and the basicity of product depends on Fe
3+hydrolysis, therefore basicity also declines thereupon, and along with the increase of curing time, the polymerization degree between monomer is carried out more abundant, so precipitation capacity increases thereupon.But the indices of product all meets the standard-required of country.Illustrate that the index of product is more stable, the storage effect of product is better.
The above is the preferred embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from principle of the present invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (4)
1. a sour self coupling balances the method for accurate dry process PAFS, it is characterized in that: comprise the steps: to take a certain amount of solid iron vitriol and aluminum sulfate octadecahydrate, be placed in mortar, then quantitative sodium chlorate saturated solution is added, being ground to the specified time obtains tenne cream solid, be product PAFS, PAFS; Preparation condition is: n (Al
3+)/n (Fe
2+) proportioning is 0.8 to 2.0, temperature of reaction room temperature to 60 DEG C, reaction times 40 to 60min, oxygenant NaClO
3consumption presses Fe
2+the stoichiometries such as meter are to excessive 4%; The general preferably optional n (Al of preparation condition
3+)/n (Fe
2+) proportioning 1.4, temperature of reaction 50 DEG C, oxygenant NaClO
3consumption presses Fe
2+stoichiometry meter excessive 4%, reaction times 60min.
2. method according to claim 1, is characterized in that: the not outer acid adding of described preparation method and/or alkali.
3. method according to claim 1, is characterized in that: except configuration sodium chlorate saturated solution adds except limited amount water in preparation process, do not add water in addition again, therefore the product that obtains is cream solid and on-liquid.
4. method according to claim 1, is characterized in that: by adjustment reaction mass n (Al in preparation process
3+)/n (Fe
2+) proportioning adjusts the basicity of product.
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| CN201510133663.5A CN104803460B (en) | 2015-03-26 | 2015-03-26 | The method that sour self coupling balances quasi- dry process polymeric aluminum sulfate iron |
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| CN201510133663.5A CN104803460B (en) | 2015-03-26 | 2015-03-26 | The method that sour self coupling balances quasi- dry process polymeric aluminum sulfate iron |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052295A (en) * | 1989-12-08 | 1991-06-19 | 樊冠球 | Basic ferric sulfate coagulant for water treatment |
| CN1486938A (en) * | 2003-07-29 | 2004-04-07 | 东华理工学院 | Prepn process of polymerized iron phosphosulfate |
| CN1504415A (en) * | 2002-12-04 | 2004-06-16 | 中国科学院广州能源研究所 | Method for producing composite polyaluminium ferric sulfate water-purifying agent |
| CN102120623A (en) * | 2011-01-28 | 2011-07-13 | 重庆大学 | Preparation method of polysilicate aluminium ferric flocculant |
| KR20120043832A (en) * | 2010-10-27 | 2012-05-07 | 고재석 | Inorganic coagulants for water treatment method |
| CN103224256A (en) * | 2013-04-09 | 2013-07-31 | 华南理工大学 | Polymerization ferric sulfate water treatment agent and preparation method thereof |
| CN103803662A (en) * | 2013-12-19 | 2014-05-21 | 广西大学 | Method for preparing solid polymeric aluminum ferric sulfate by use of bauxite oxide |
-
2015
- 2015-03-26 CN CN201510133663.5A patent/CN104803460B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1052295A (en) * | 1989-12-08 | 1991-06-19 | 樊冠球 | Basic ferric sulfate coagulant for water treatment |
| CN1504415A (en) * | 2002-12-04 | 2004-06-16 | 中国科学院广州能源研究所 | Method for producing composite polyaluminium ferric sulfate water-purifying agent |
| CN1486938A (en) * | 2003-07-29 | 2004-04-07 | 东华理工学院 | Prepn process of polymerized iron phosphosulfate |
| KR20120043832A (en) * | 2010-10-27 | 2012-05-07 | 고재석 | Inorganic coagulants for water treatment method |
| CN102120623A (en) * | 2011-01-28 | 2011-07-13 | 重庆大学 | Preparation method of polysilicate aluminium ferric flocculant |
| CN103224256A (en) * | 2013-04-09 | 2013-07-31 | 华南理工大学 | Polymerization ferric sulfate water treatment agent and preparation method thereof |
| CN103803662A (en) * | 2013-12-19 | 2014-05-21 | 广西大学 | Method for preparing solid polymeric aluminum ferric sulfate by use of bauxite oxide |
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