CN108675418A - A kind of polysilicate aluminium ferric flocculant and preparation method thereof - Google Patents
A kind of polysilicate aluminium ferric flocculant and preparation method thereof Download PDFInfo
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- CN108675418A CN108675418A CN201810473172.9A CN201810473172A CN108675418A CN 108675418 A CN108675418 A CN 108675418A CN 201810473172 A CN201810473172 A CN 201810473172A CN 108675418 A CN108675418 A CN 108675418A
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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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Abstract
The invention discloses a kind of polysilicate aluminium ferric flocculant and preparation method thereof, the preparation method of the polysilicate aluminium ferric flocculant includes the following steps：(1) ferrous sulfate heptahydrate and by-product sulfuric acid liquid are mixed and heated to 60~75 DEG C, obtain mixed liquor；(2) mixed liquor is added in reaction kettle, then passes to oxygen, and by-product nitric acid liquid is added and is reacted；Wherein, the ferrous sulfate heptahydrate is titanium dioxide industry by-product；The by-product sulfuric acid liquid is industrial aluminium foil surface sulfuric acid washing by-product；The by-product nitric acid liquid is industrial aluminium foil surface nitric acid acidwashing by-product.The present invention is using titanium dioxide industry by-product ferrous sulfate and industrial aluminium foil surface acid-washing by-product as the primary raw material for preparing polysilicate aluminium ferric flocculant, not only considerably reduce production cost, and the comprehensive utilization of titanium dioxide industry by-product ferrous sulfate and industrial aluminium foil surface acid-washing by-product is realized, reduce environmental pollution.
Description
Technical field
The present invention relates to water-treatment technology fields, in particular to a kind of polysilicate aluminium ferric flocculant and its preparation
Method.
Background technology
Currently, common water treatment inorganic coagulant includes mainly two major classes agent, that is, molysite and aluminium salt in the market.Molysite has
There are the advantages such as hydrolysis is fast, alumen ustum volume is big, closely knit, fast, the intensity height of sedimentation, however remaining coloration is big to be lacked there is also being discharged
It falls into.And the advantage that aluminium salt has the remaining coloration of water outlet small, but at the same time in the presence of hydrolysis is slow, alumen ustum is small, water oil repellency is slow
The defects of.Polysilicate aluminium ferric flocculant is because of the advantage that the purifying water effect for having both aluminium salt is excellent and the sinking speed of molysite is fast, together
When also overcome aluminium salt using harmful in rear excess of aluminum remaining water, molysite easy tos produce the deficiency of yellowing and blackening, and
It is widely used in the purified treatment of the water bodys such as industrial water, municipal sewage and industrial wastewater.
However, at present in the production of polysilicate aluminium ferric flocculant, main preparation process has direct oxidation method and catalysis oxygen
Change method.Catalytic oxidation has the advantages such as at low cost, the reaction time is short and is applied in the industrial production extensively.However aluminium is next
Source is essentially all the compound containing aluminium using industrial agent.In addition, common catalyst is also using industry in catalytic oxidation
Agent such as sodium nitrite, potassium chlorate etc..This has increased considerably the production cost of polysilicate aluminium ferric flocculant, not big using carrying out
Technical scale produces.Therefore, how using further preparing polysilicate aluminium ferric flocculant water purification agent using the by-product of aluminium,
Turn waste into wealth to realize, becomes the hot spot studied now.
Acid cleaning process is that one kind being widely used in metal surface such as steel and iron industry, foil industry etc. to clean metal surface oxygen
Change layer and then realizes the processing technologys such as metallic surface structures optimization.However the processing technology will produce a large amount of volume metal ions
Strongly acid wastewater.Processing method traditional at present is mainly to be neutralized using direct plus alkali method, however this method is deposited
In waste of resource, cost of disposal it is high and the defects of generate a large amount of sludge.Therefore, it explores how to maximize and recycles its metal
Surface acid-washing waste water is significant.
Titanium dioxide accounts for about world's white face as a kind of current application amount maximum also most wide inorganic white pigment, yield
Expect the 80% of total output.And sulfuric acid process is to produce the main method of titanium dioxide at present, this method produces 1 ton of titanium dioxide and will will produce
About 3.5~4.0 tons of by-product ferrous sulfate heptahydrates contain plurality of impurities in the ferrous sulfate, are unable to direct reuse and everywhere heap
It puts, therefore, the comprehensive utilization and environmental pollution of titanium dioxide industry by-product ferrous sulfate are also that current technical field to be solved
Problem.So far, it has not seen and is prepared using titanium dioxide industry by-product ferrous sulfate and industrial aluminium foil surface acid-washing by-product
The report of polymeric ferric sulfate.
Invention content
In view of this, a kind of polysilicate aluminium ferric flocculant provided by the invention and preparation method thereof, preferably overcomes
The above-mentioned problems of the prior art and defect, the present invention utilize titanium dioxide industry by-product ferrous sulfate and industrial aluminium foil surface
Pickling by-product is as the primary raw material for preparing polysilicate aluminium ferric flocculant, wherein industrial aluminium foil surface nitric acid acidwashing by-product
The source of aluminium during aluminum nitrate in object is not only produced as the source of catalyst but also as polysilicate aluminium ferric flocculant, and industrial aluminum
Aluminum sulfate in the sulfuric acid washing by-product of foil surface is also the important sources of aluminium in polysilicate aluminium ferric flocculant production, this is not only
Production cost is considerably reduced, and realizes titanium dioxide industry by-product ferrous sulfate and industrial aluminium foil surface acid-washing by-product
The comprehensive utilization of object saves the commission handling of industrial aluminium foil surface acid-washing by-product and efficiently solves titanium dioxide industry pair
The problem of product ferrous sulfate is unable to direct reuse and stores up everywhere, reduces environmental pollution.
A kind of preparation method of polysilicate aluminium ferric flocculant, includes the following steps：
(1) ferrous sulfate heptahydrate and by-product sulfuric acid liquid are mixed and heated to 60~75 DEG C, obtain mixed liquor；
(2) mixed liquor is added in reaction kettle, then passes to oxygen, and by-product nitric acid liquid is added and is reacted；
Wherein, the ferrous sulfate heptahydrate is titanium dioxide industry by-product；
The by-product sulfuric acid liquid is industrial aluminium foil surface sulfuric acid washing by-product, and includes dilute sulfuric acid and aluminum sulfate；
The by-product nitric acid liquid is industrial aluminium foil surface nitric acid acidwashing by-product, and includes dust technology and aluminum nitrate.
Further, the mass ratio of the ferrous sulfate heptahydrate, by-product sulfuric acid liquid, oxygen and by-product nitric acid liquid be 35~
42：14~21：0.95~1：4~5.
Further, the by-product sulfuric acid liquid is the by-product sulfuric acid liquid after being concentrated using membrane distillation concentration technology, institute
The mass fraction for stating dilute sulfuric acid in by-product sulfuric acid liquid is 15~25%, and the mass fraction of aluminum sulfate is 10~15%.
Further, the by-product nitric acid liquid is the by-product nitric acid liquid after being concentrated using membrane distillation concentration technology, institute
The mass fraction for stating dust technology in by-product nitric acid liquid is 15~25%, and the mass fraction of aluminum nitrate is 10~15%.
Further, in step (1), the process of the Hybrid Heating includes：By ferrous sulfate heptahydrate and by-product sulfuric acid liquid
After mixing, high-temperature vapor is passed through into the mixed liquor of ferrous sulfate heptahydrate and by-product sulfuric acid liquid while stirring and is heated.
Further, further include that co-catalyst is added in step (2).
Further, the co-catalyst and the mass ratio of by-product nitric acid liquid are 1~2：50~80.
Further, the co-catalyst is sodium iodide.
Further, in step (2), in the reaction process：Reaction pressure in reaction kettle is 0.3~0.4Mpa, instead
It is 70~120 DEG C to answer temperature, and the reaction time is 60~120min.
A kind of polysilicate aluminium ferric flocculant, the polysilicate aluminium ferric flocculant are flocculated by above-mentioned polymeric aluminum sulfate iron
The preparation method of agent.
Compared with prior art, the advantageous effect of a kind of polysilicate aluminium ferric flocculant of the invention and preparation method thereof
It is：
(1) present invention is using titanium dioxide industry by-product ferrous sulfate and industrial aluminium foil surface acid-washing by-product as preparation
The primary raw material of polysilicate aluminium ferric flocculant, wherein the aluminum nitrate in industrial aluminium foil surface nitric acid acidwashing by-product is as portion
The source of divided catalyst and part aluminium, the aluminum sulfate in industrial aluminium foil surface sulfuric acid washing by-product are wadded a quilt with cotton as polymeric aluminum sulfate iron
The source of part aluminium, not only considerably reduces production cost, but also realize titanium dioxide industry by-product sulphur in solidifying agent production
The comprehensive utilization of sour ferrous and industrial aluminium foil surface acid-washing by-product, at the commission for saving industrial aluminium foil surface acid-washing by-product
Reason takes and solves the problems, such as that titanium dioxide industry by-product ferrous sulfate is unable to direct reuse and stores up everywhere, reduces ring
It pollutes in border.
(2) preparation method of polysilicate aluminium ferric flocculant of the invention is simple for process, and raw material is easy to get, and low energy consumption, operation
Simply.
To enable the above objects, features and advantages of the present invention to be clearer and more comprehensible, preferred embodiment cited below particularly is made detailed
It is described as follows.
Specific implementation mode
To facilitate the understanding of the present invention, it elaborates to technical scheme of the present invention with reference to the mode of embodiment,
Many details are elaborated in the following description in order to fully understand the present invention.
But the invention can be embodied in many other ways as described herein, those skilled in the art can be with
Similar improvement is done without violating the connotation of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
Unless otherwise defined, all technologies used herein and scientific terminology have and the common skill of fields of the present invention
The normally understood identical meaning of art personnel.When there is a conflict, the definition in this specification shall prevail.
Term as used herein：
Term "comprising" used herein, " comprising ", " having ", " containing " or its any other deformation, it is intended that covering
Non-exclusionism includes.For example, composition, step, method, product or device comprising listed elements are not necessarily limited to those and want
Element, but may include not expressly listed other elements or such composition, step, method, product or device it is intrinsic
Element.
Conjunction " by ... form " exclude any element that do not point out, step or component.If in claim,
This phrase will make claim be closed, so that it is not included the material in addition to the material of those descriptions, but relative
Except customary impurities.When phrase " by ... form " be rather than immediately following theme in the clause that appears in claim main body after
When, only it is limited to the element described in the clause；Other elements be not excluded the claim as a whole it
Outside.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this, which should be understood as, specifically discloses by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1~5 ", described range should be interpreted as including range " 1~4 ", " 1~3 ", " 1~2 ", " 1~2 and 4~
5 ", " 1~3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise range intention includes its end
Value and all integers and score in the range.
"and/or" is used to indicate that one of illustrated situation or both may to occur, for example, A and/or B includes (A
And B) and (A or B).
A kind of preparation method of polysilicate aluminium ferric flocculant, includes the following steps：
(1) ferrous sulfate heptahydrate and by-product sulfuric acid liquid are mixed and heated to 60~75 DEG C such as 60 DEG C, 65 DEG C 70 DEG C or 75 DEG C,
Obtain mixed liquor；
(2) mixed liquor is added in reaction kettle, then passes to oxygen, and by-product nitric acid liquid is added and is reacted.
Wherein, the ferrous sulfate heptahydrate is titanium dioxide industry by-product.
The by-product sulfuric acid liquid is industrial aluminium foil surface sulfuric acid washing by-product, and includes dilute sulfuric acid and aluminum sulfate；
The by-product nitric acid liquid is industrial aluminium foil surface nitric acid acidwashing by-product, and includes dust technology and aluminum nitrate.
Preferably, the mass ratio of the ferrous sulfate heptahydrate, by-product sulfuric acid liquid, oxygen and by-product nitric acid liquid is 35~42：
14~21：0.95~1：4~5.
Preferably, the by-product sulfuric acid liquid is the by-product sulfuric acid liquid after being concentrated using membrane distillation concentration technology, described
The mass fraction of dilute sulfuric acid is 15~25% in by-product sulfuric acid liquid, and the mass fraction of aluminum sulfate is 10~15%.
Preferably, the by-product nitric acid liquid is the by-product nitric acid liquid after being concentrated using membrane distillation concentration technology, described
The mass fraction of dust technology is 15~25% in by-product nitric acid liquid, and the mass fraction of aluminum nitrate is 10~15%.
Above-mentioned ferrous sulfate heptahydrate, by-product sulfuric acid liquid, oxygen and by-product nitric acid liquid mass ratio it is specific enumerable be 35：
14：0.95：4、38：18：0.98：4.5、40：14：1：4.8、42：21：1：5 or 36：20：0.97：4.6 waiting.
Preferably, in step (1), the process of the Hybrid Heating includes：Ferrous sulfate heptahydrate and by-product sulfuric acid liquid are mixed
After conjunction, high-temperature vapor is passed through into the mixed liquor of ferrous sulfate heptahydrate and by-product sulfuric acid liquid while stirring and is heated.
Wherein, the mass ratio of the quality and ferrous sulfate heptahydrate that are passed through high-temperature vapor is 4~5：35~42.
The specific enumerable mass ratio of above-mentioned high-temperature vapor and ferrous sulfate heptahydrate is 4：35、4.2：37、4.5：37、4：
38、4.8：40 or 5：42 etc..It is preferable to use the vapor that temperature is 150~170 DEG C for high-temperature vapor.
Preferably, further include that co-catalyst is added in step (2)；The mass ratio of the co-catalyst and by-product nitric acid liquid
It is 1~2：50~80.
The specific enumerable mass ratio of co-catalyst and by-product nitric acid liquid is 1~2：50~80 such as 1：50、1.2：55、1.5：
60、1.5：65、1.8：70 or 2：80 etc..It should be noted that the addition of co-catalyst NaI, when can further shorten reaction
Between, production efficiency is improved, is more advantageous to and meets the needs of large-scale industrial production.
Preferably, the co-catalyst is sodium iodide.But the present invention is not intended to limit the type of co-catalyst, described help is urged
Agent can also be potassium iodide (KI) etc..
Preferably, in step (2), in the reaction process：Reaction pressure in reaction kettle be 0.3~0.4Mpa such as
0.3Mpa, 0.32Mpa, 0.35Mpa, 0.38Mpa or 0.40Mpa etc.；Reaction temperature is 70~120 DEG C；Reaction time be 60~
120min such as 60min, 70min, 80min, 90min, 100min, 110min or 120min etc..
A kind of polysilicate aluminium ferric flocculant, the polysilicate aluminium ferric flocculant are flocculated by above-mentioned polymeric aluminum sulfate iron
The preparation method of agent.
The present invention is poly- as preparing using titanium dioxide industry by-product ferrous sulfate and industrial aluminium foil surface acid-washing by-product
Close the primary raw material of aluminium iron sulfate flocculant, wherein the aluminum nitrate in industrial aluminium foil surface nitric acid acidwashing by-product is as part
The source of catalyst and part aluminium, the aluminum sulfate in industrial aluminium foil surface sulfuric acid washing by-product flocculate as polymeric aluminum sulfate iron
The source of part aluminium in agent production, this not only considerably reduces production cost, but also realizes titanium dioxide industry by-product sulphur
The comprehensive utilization of sour ferrous and industrial aluminium foil surface acid-washing by-product, at the commission for saving industrial aluminium foil surface acid-washing by-product
Reason takes and solves the problems, such as that titanium dioxide industry by-product ferrous sulfate is unable to direct reuse and stores up everywhere, reduces ring
It pollutes in border.
In addition, the preparation method of the polysilicate aluminium ferric flocculant of the present invention is simple for process, raw material is easy to get, and low energy consumption, behaviour
Make simple.
To facilitate the understanding of the present invention, the technical solution further illustrated the present invention with reference to embodiment.Applicant
Statement, the present invention are illustrated by the following examples detailed process equipment and the technological process of the present invention, but the present invention not office
It is limited to following detailed process equipments and technological process, that is, does not mean that the present invention should rely on above-mentioned detailed process equipment and technique stream
Cheng Caineng is implemented.Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, to each original of product of the present invention
The equivalence replacement of material and the addition of auxiliary element, the selection of concrete mode etc. all fall within protection scope of the present invention and open model
Within enclosing.
Embodiment 1
(1) 5.9t titanium dioxide industry byproduct ferrous sulfate heptahydrates are placed in dissolving tank, then warp is added into reactive tank
(mass fraction of wherein dilute sulfuric acid is industrial aluminium foil surface sulfuric acid washing by-product by-product sulfuric acid liquid 2.4t after membrane distillation concentration
25%, aluminum sulfate mass fraction 15%), and open agitating device and be stirred mixing, so that ferrous sulfate heptahydrate is completely dissolved in
By-product sulfuric acid liquid obtains uniform mixed liquor, and high-temperature water vapor is at the same time passed through into dissolving tank is heated, until mixing
Liquid temperature reaches 70 DEG C and stops leading to high-temperature vapor and close agitating device, and at this moment the intake of high-temperature water vapor is 0.7t.
(2) mixed liquor obtained in step (1) is pumped into 10m immediately3Closed reactor in and ON cycle pumping unit
It is stirred, at the same time, opens oxygen valve (oxygen sources are in liquid oxygen gasifier), oxygen, oxygen are passed through in reaction kettle
Flow control in 150kg/h (in terms of liquid zmount of oxygen consumption), and be pumped into 0.80t dissolving cocatalyst sodium iodide industrial aluminum
(wherein dust technology mass fraction is 25% to foil surface sulfuric acid washing by-product by-product nitric acid liquid, and the mass fraction of aluminum nitrate is
15%), wherein the content of co-catalyst sodium iodide is 8.5kg.In entire reaction process, the pressure control of reaction kettle for 0.3~
0.4Mpa, reaction temperature maintain 70~120 DEG C with the progress entirely reacted, and the reaction time needed for end reaction is
70min；Liquid is obtained after reaction shows brownish red and thick polysilicate aluminium ferric flocculant.
Embodiment 2
(1) 5.2t titanium dioxide industry byproduct ferrous sulfate heptahydrates are placed in dissolving tank, then warp is added into reactive tank
Industrial aluminium foil surface sulfuric acid washing by-product by-product sulfuric acid liquid 2.50t (the wherein mass fractions of dilute sulfuric acid after membrane distillation concentration
It is 20%, aluminum sulfate mass fraction 14%), and open agitating device and be stirred mixing, so that ferrous sulfate heptahydrate is fully dissolved
Uniform mixed liquor is obtained in by-product sulfuric acid liquid, high-temperature water vapor is at the same time passed through into dissolving tank is heated, until mixed
It closes liquid temperature to reach the logical high-temperature vapor of 70 DEG C of stoppings and close agitating device, at this moment the intake of high-temperature water vapor is 0.6t.
(2) mixed liquor obtained in step (1) is pumped into 10m immediately3Closed reactor in and ON cycle pumping unit
It is stirred, at the same time, opens oxygen valve (oxygen sources are in liquid oxygen gasifier), oxygen, oxygen are passed through in reaction kettle
Flow control in 130kg/h (in terms of liquid zmount of oxygen consumption), and be pumped into 0.52t dissolving cocatalyst sodium iodide industrial aluminum
(wherein dust technology mass fraction is 20% to foil surface sulfuric acid washing by-product by-product nitric acid liquid, and the mass fraction of aluminum nitrate is
13%), wherein the content of co-catalyst sodium iodide is 6.3kg.In entire reaction process, the pressure control of reaction kettle for 0.3~
0.4Mpa, reaction temperature maintain 70~120 DEG C with the progress entirely reacted, and the reaction time needed for end reaction is
65min；Liquid is obtained after reaction shows brownish red and thick polysilicate aluminium ferric flocculant.
Embodiment 3
(1) 5.8t titanium dioxide industry byproduct ferrous sulfate heptahydrates are placed in dissolving tank, then warp is added into reactive tank
(mass fraction of wherein dilute sulfuric acid is industrial aluminium foil surface sulfuric acid washing by-product by-product sulfuric acid liquid 2.9t after membrane distillation concentration
22%, aluminum sulfate mass fraction 12%), and open agitating device and be stirred mixing, so that ferrous sulfate heptahydrate is completely dissolved in
By-product sulfuric acid liquid obtains uniform mixed liquor, and high-temperature water vapor is at the same time passed through into dissolving tank is heated, until mixing
Liquid temperature reaches 70 DEG C and stops leading to high-temperature vapor and close agitating device, and at this moment the intake of high-temperature water vapor is 0.69t.
(2) mixed liquor obtained in step (1) is pumped into 10m immediately3Closed reactor in and ON cycle pumping unit
It is stirred, at the same time, opens oxygen valve (oxygen sources are in liquid oxygen gasifier), oxygen, oxygen are passed through in reaction kettle
Flow control in 120kg/h (in terms of liquid zmount of oxygen consumption), and be pumped into 0.7t dissolving cocatalyst sodium iodide industrial aluminum
(wherein dust technology mass fraction is 25% to foil surface sulfuric acid washing by-product by-product nitric acid liquid, and the mass fraction of aluminum nitrate is
15%), wherein the content of co-catalyst sodium iodide is 8.5kg.In entire reaction process, the pressure control of reaction kettle for 0.3~
0.4Mpa, reaction temperature maintain 70~120 DEG C with the progress entirely reacted, and the reaction time needed for end reaction is
70min；Liquid is obtained after reaction shows brownish red and thick polysilicate aluminium ferric flocculant.
Embodiment 4
(1) 3.9t titanium dioxide industry byproduct ferrous sulfate heptahydrates are placed in dissolving tank, then warp is added into reactive tank
Industrial aluminium foil surface sulfuric acid washing by-product by-product sulfuric acid liquid 1.85t (the wherein mass fractions of dilute sulfuric acid after membrane distillation concentration
It is 15%, aluminum sulfate mass fraction 10%), and open agitating device and be stirred mixing, so that ferrous sulfate heptahydrate is fully dissolved
Uniform mixed liquor is obtained in by-product sulfuric acid liquid, high-temperature water vapor is at the same time passed through into dissolving tank is heated, until mixed
It closes liquid temperature to reach the logical high-temperature vapor of 70 DEG C of stoppings and close agitating device, at this moment the intake of high-temperature water vapor is 0.46t.
(2) mixed liquor obtained in step (1) is pumped into 10m immediately3Closed reactor in and ON cycle pumping unit
It is stirred, at the same time, opens oxygen valve (oxygen sources are in liquid oxygen gasifier), oxygen, oxygen are passed through in reaction kettle
Flow control in 100kg/h (in terms of liquid zmount of oxygen consumption), and be pumped into 0.46t dissolving cocatalyst sodium iodide industrial aluminum
(wherein dust technology mass fraction is 25% to foil surface sulfuric acid washing by-product by-product nitric acid liquid, and the mass fraction of aluminum nitrate is
15%), wherein the content of co-catalyst sodium iodide is 8.5kg.In entire reaction process, the pressure control of reaction kettle for 0.3~
0.4Mpa, reaction temperature maintain 70~120 DEG C with the progress entirely reacted, and the reaction time needed for end reaction is
60min；Liquid is obtained after reaction shows brownish red and thick polysilicate aluminium ferric flocculant.
Embodiment 5
Embodiment 5 difference from example 1 is that：Remove co-catalyst sodium iodide；It is the time required to end reaction
100min。
Embodiment 6
Embodiment 6 with embodiment 1 the difference is that：In step (1), it is passed through high-temperature water vapor and is heated, until
Mixeding liquid temperature, which reaches 60 DEG C, to be stopped leading to high-temperature vapor and closes agitating device；It is 100min the time required to end reaction.
Embodiment 7
Embodiment 7 with embodiment 1 the difference is that：In step (1), it is passed through high-temperature water vapor and is heated, until
Mixeding liquid temperature, which reaches 65 DEG C, to be stopped leading to high-temperature vapor and closes agitating device；It is 90min the time required to end reaction.
Embodiment 8
Embodiment 8 with embodiment 1 the difference is that：The industrial aluminium foil surface sulphur of cocatalyst sodium iodide will be dissolved
The amount of being pumped into of pickling by-product by-product nitric acid liquid is adjusted to 0.71t；It is 100min the time required to end reaction.
Embodiment 9
Embodiment 9 with embodiment 1 the difference is that：The industrial aluminium foil surface sulphur of cocatalyst sodium iodide will be dissolved
The amount of being pumped into of pickling by-product by-product nitric acid liquid is adjusted to 0.60t；It is 120min the time required to end reaction.
Embodiment 10
Embodiment 10 and embodiment 2 the difference is that：Remove co-catalyst sodium iodide；It is the time required to end reaction
95min。
When embodiment 2 and the comparison of embodiment 10 can be obtained by embodiment 1 and embodiment 5, co-catalyst iodate is added
Sodium is than being added without the reaction time of co-catalyst sodium iodide faster.
It can be obtained by the comparison of embodiment 1, embodiment 6 and embodiment 7, in step (1), the mixed liquor in dissolving tank is heated
Reaction time nuclear reaction efficiency is influenced to different temperature, the temperature that the mixed liquor heating in dissolving tank is reached is higher, reaction
Time is shorter, and reaction efficiency is higher.
It can be obtained by the comparison of embodiment 1, embodiment 8 and embodiment 9, dissolve the industrial aluminium foil table of cocatalyst sodium iodide
The amount of being pumped into of face sulfuric acid washing by-product by-product nitric acid liquid is higher, and the reaction time is shorter, and reaction efficiency is higher.
To Examples 1 to 4 prepare indices include：Al2O3, full iron and basicity content and 1% polyaluminum sulfate
The pH of the aqueous solution of ferro-aluminum is detected, and testing result is as shown in table 1.
Table 1
Bodied ferric sulfate that polysilicate aluminium ferric flocculant and market prepared by the embodiment of the present invention 1~4 are sold and
Flocculant of polymeric aluminium chloride is as shown in table 2 below to the flocculating setting Contrast on effect of the COD in waste water.Wherein, wastewater sample is derived from
Certain sanitary sewage, the content of total COD is 97.5mg/L before handling.
Table 2
It can be obtained by upper table 1, the flocculation to the COD in waste water of polymeric ferric sulfate prepared by the embodiment of the present invention 1~4
Flocculating setting to COD in waste water of the effect of settling than commercially available polymeric ferric sulfate flocculant and commercially available flocculant of polymeric aluminium chloride
Effect is more preferable.
The preferred embodiment of the present invention is above are only, is not intended to restrict the invention, for those skilled in the art
For member, inventive formulation and preparation process can have various modifications and variations.All within the spirits and principles of the present invention, institute
Any modification, equivalent substitution, improvement and etc. of work, should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of polysilicate aluminium ferric flocculant, it is characterised in that：Include the following steps：
(1) ferrous sulfate heptahydrate and by-product sulfuric acid liquid are mixed and heated to 60~75 DEG C, obtain mixed liquor；
(2) mixed liquor is added in reaction kettle, then passes to oxygen, and by-product nitric acid liquid is added and is reacted；
Wherein, the ferrous sulfate heptahydrate is titanium dioxide industry by-product；
The by-product sulfuric acid liquid is industrial aluminium foil surface sulfuric acid washing by-product, and includes dilute sulfuric acid and aluminum sulfate；
The by-product nitric acid liquid is industrial aluminium foil surface nitric acid acidwashing by-product, and includes dust technology and aluminum nitrate.
2. the preparation method of polysilicate aluminium ferric flocculant according to claim 1, it is characterised in that：The seven water sulfuric acid
The mass ratio of ferrous iron, by-product sulfuric acid liquid, oxygen and by-product nitric acid liquid is 35~42：14~21：0.95~1：4~5.
3. the preparation method of polysilicate aluminium ferric flocculant according to claim 2, it is characterised in that：The by-product sulfuric acid
Liquid is the by-product sulfuric acid liquid after being concentrated using membrane distillation concentration technology, the mass fraction of dilute sulfuric acid in the by-product sulfuric acid liquid
It is 15~25%, the mass fraction of aluminum sulfate is 10~15%.
4. the preparation method of polysilicate aluminium ferric flocculant according to claim 2, it is characterised in that：The by-product nitric acid
Liquid is the by-product nitric acid liquid after being concentrated using membrane distillation concentration technology, the mass fraction of dust technology in the by-product nitric acid liquid
It is 15~25%, the mass fraction of aluminum nitrate is 10~15%.
5. the preparation method of polysilicate aluminium ferric flocculant according to claim 1, it is characterised in that：In step (1), institute
The process for stating Hybrid Heating includes：After ferrous sulfate heptahydrate and by-product sulfuric acid liquid are mixed, while stirring to ferrous sulfate heptahydrate
It is heated with high-temperature vapor is passed through in the mixed liquor of by-product sulfuric acid liquid.
6. the preparation method of polysilicate aluminium ferric flocculant according to claim 1, it is characterised in that：In step (2), also
Including co-catalyst is added.
7. the preparation method of polysilicate aluminium ferric flocculant according to claim 6, it is characterised in that：The co-catalyst
Mass ratio with by-product nitric acid liquid is 1~2：50~80.
8. the preparation method of polysilicate aluminium ferric flocculant according to claim 6, it is characterised in that：The co-catalyst
For sodium iodide.
9. the preparation method of polysilicate aluminium ferric flocculant according to claim 1, it is characterised in that：In step (2), institute
It states in reaction process：Reaction pressure in reaction kettle is 0.3~0.4Mpa, and reaction temperature is 70~120 DEG C, the reaction time 60
~120min.
10. a kind of polysilicate aluminium ferric flocculant, it is characterised in that：The polysilicate aluminium ferric flocculant is by claim 1~9
The preparation method of any one of them polysilicate aluminium ferric flocculant.
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