CN104261525B - The preparation method of aluminium iron polychloride - Google Patents

The preparation method of aluminium iron polychloride Download PDF

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Publication number
CN104261525B
CN104261525B CN201410456974.0A CN201410456974A CN104261525B CN 104261525 B CN104261525 B CN 104261525B CN 201410456974 A CN201410456974 A CN 201410456974A CN 104261525 B CN104261525 B CN 104261525B
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waste acid
aluminium
ferrous waste
iron polychloride
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CN104261525A (en
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朱雪峰
徐晓锋
刘遗松
夏平
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CHANGSHU CITY FOR YU ENVIRONMENT TECHNOLOGY Co Ltd
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CHANGSHU CITY FOR YU ENVIRONMENT TECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/10Halides

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

Abstract

A preparation method for aluminium iron polychloride, belongs to inorganic polymer coagulant preparing technical field.Step: be blended in the ferrous waste acid liquid of 10-14% with dilute hydrochloric acid, until make the concentration of ferrous waste acid liquid be increased to 15-18%, obtains ferrous waste acid liquid; With feeding mode in batches, the ferrous waste acid stoste obtained being dropped in reaction vessel, and drop into aluminium ash, obtain stoste, continuing to make stoste polyreaction under the state stirred, obtaining aluminium iron polychloride first product; First product is released from reaction vessel and introduces in settling tank, readjustment liquid is added in settling tank, precipitation agent and PAM is added again in settling tank, and stir, stratification, end product pool introduced by supernatant liquor, obtains aluminium iron polychloride, and the throw out in settling tank causes filter-pressing device press filtration, the pressing filtering liquid produced during press filtration uses as readjustment liquid.Economize on resources, contribute to the protection to environment; Processing step is brief, processing ease; Energy-saving effect is desirable.

Description

The preparation method of aluminium iron polychloride
Technical field
The invention belongs to inorganic polymer coagulant preparing technical field, be specifically related to a kind of preparation method of aluminium iron polychloride.
Background technology
Why aluminium iron polychloride is widely used in the process to such as Drinking Water, process water, sanitary wastewater and industrial sewage, is because it has the strong point of ten aspects being not limited to conclude below: one be consumption lower than traditional coagulating agent as bodied ferric sulfate, polymerize aluminum chloride; Two be the characteristic of inorganic polymer polymerize aluminum chloride and poly-ferric chloride is held concurrently and it; Three is that flocs unit forms speed and sedimentation speed is fast, and processing power is strong; Four is little to the basicity consumption in water, and water outlet pH value reduces few; Five are that aqueous solution insolubles is low and light transmission good; Six is that applicable pH value range is wide, all can use in the scope of pH5-9; Seven is to turbidity, basicity and organic content change strong adaptability; Eight is that heavy metal content index can meet China standard GB/T 15892-2003 requirement; Nine is that residual free aluminium content is low, and the water quality after purification is excellent; Ten be corrodibility little and be easy to dissolve.
Technical intelligence about the preparation method of aluminium iron polychloride is no lack of and is seen in disclosed patent documentation, as CN100347098C recommendation has " aluminium iron chloride of coagulant agent in polymorphism polymerization and preparation method thereof ", the ultra-fine micropowder that this patent formula adds water glass, calcium aluminate and filled the post of by the clay containing Si modification containing aluminium based on aluminium iron polychloride.Secondary processing category to aluminium iron polychloride is belonged to by reading known its to the full text of this patent specification, to improve aluminium iron polychloride to the absorption effect of flocculant of oil-containing suspended matter (specifically can see the content of last 7 row of the specification sheets page 1 of this patent), thus for preparing aluminium iron polychloride, not there is the enlightenment of referential technology.
Authorization Notice No. CN100554178C provides " a kind of production method of inorganic macromolecule flocculant poly aluminium chloride ferrum ", and this patent formula utilizes the acid waste liquid that contains produced in the process of attapulgite clay production atlapulgite namely to obtain aluminium iron polychloride through alkaline matter as potassium hydroxide, unslaked lime, sodium carbonate or sodium bicarbonate neutralization reaction obtain target product.The positive effect of this patent can see its specification sheets text page 2 the 6th section, and shortcoming is to have limitation to the acquisition of spent acid solution, because cannot be suitable for for the area of no concave-convex rod stone clay resource, that is spent acid solution source is subject to objective restriction.
Authorization Notice No. CN101172684B introduces to be had " method utilizing flyash industrial production of polymeric aluminum ferric chloride water purification agent ", its be by weight part be first 20-30 part flyash drop into reaction vessel, technical hydrochloric acid 30-48 part (weight part) that quality % specific concentration is 10-20% is added again and adds the solubility promoter that weight part is 0.1-0.5 part that (solubility promoter is Repone K in reaction vessel, calcium chloride or sodium-chlor) reaction, after reaction terminates, reactant (patent claims to react feed liquid) is introduced settling pond solid-liquid separation, supernatant liquor solid-liquid separation obtained is introduced polymeric kettle and added parts by weight is that (polymerizing agent is sodium hydroxide to 0.3-1.5 part polymerizing agent, calcium hydroxide, sodium carbonate or ammoniacal liquor) carry out polyreaction, obtain the aluminium iron polychloride of finished product.The 0011st section, the visible specification sheets of technique effect of this patent formula, but owing to needing to consume more technical hydrochloric acid, thus still lose economy.
Authorization Notice No. CN102139943B discloses to be had " a kind of method that Extracting Scandium from Red Mud liquid prepares aluminium iron polychloride ", and visible the 0099 to 0100 section, its specification sheets of achievement part of the method, is short of as the explanation to aforementioned CN100554178C.
Typically as Authorization Notice No. CN102372308B bulletin has " technique that a kind of ferrous waste acid washing lotion produces aluminium iron polychloride coagulating agent ", its step of recommending is followed successively by: the preparation of aluminium iron polychloride mother liquor, polymerize aluminum chloride mother liquor are oxidized and sedimentation, aluminium iron polychloride mother liquor are oxidized and aluminium iron polychloride basicity adjusts, and this patent formula can embody the technique effect that the 0013rd section, its specification sheets is recorded objectively.
The common feature being not limited to the patent formula exemplified above becomes useless (useless: containing acid waste liquid) into precious and utility value that is that embody resource, but still there is common shortcoming, that is exactly still need to rely on industrial raw material, so-called industrial raw material is as the alkaline matter (potassium hydroxide, unslaked lime, sodium carbonate or sodium bicarbonate) mentioned in CN100554178C, the technical hydrochloric acid and for example mentioned in CN101172684B, therefore the maximum using being still not enough to embody resource is worth, and makes the aluminium iron polychloride obtained lose economy.
Known, China is bauxite resource big country, simultaneously Ye Shi aluminum smelting technology big country, and the annual production of aluminium ingot accounts for global about 40% (2010, whole world aluminium ingot output is 4,106 ten thousand tons, and China accounts for 1,390,000 tons).
And then as is known in the industry, in aluminum smelting technology process, more particularly can produce multiple by product in the process manufacturing aluminium ingot, aluminium ash is the one in multiple by product, aluminium ash accounts for the 1-12% of aluminium weight in aluminium melting operation, and previously, aluminium ash was considered as waste residue and abandons it by people, not only cause the waste of bauxite resource, and undermine environment.But along with aluminium ash treatment process and the exploitation of relevant device, by aluminium ash through separating treatment, fragmentation, sieve and melt, until be cast into aluminium ingot, thus bauxite resource is fully utilized.In addition, also can produce a large amount of aluminium ashes in the production process of secondary aluminum, the aluminium ash produced in usually producing secondary aluminum reclaims aluminium in squeezing mode.
No matter be employing aforesaid separating treatment, fragmentation, sieve and melt and be cast as aluminium ingot or reclaim aluminium by squeezing all still there is the waste situation of aluminium component to aluminium ash.
From the above; if metal can be cleaned the ferrous waste acid liquid produced in (pickling) process and the aluminium ash produced in the aluminium ingot course of processing to be used in together and to prepare aluminium iron polychloride; so certainly be able to the maximization effect embodying the utilization of resources ultimate attainmently, and not only can reduce preparation cost but also can protection of the environment.But being showed no in disclosed patent up to now and non-patent literature allly has corresponding report.For this reason, the applicant has done positive and useful exploration and trial, finally defines the technical scheme will introduced below.
Summary of the invention
Task of the present invention is the preparation method providing a kind of aluminium iron polychloride, the method contribute to raising altogether ferrous waste acid liquid and aluminium ash length and with press down affect the short of environment and use the maximum using embodying resource be worth, be conducive to remarkable Simplified flowsheet step and use meet industrial amplification production require, be of value to utilize the spontaneous thermal source of reaction system and use embody energy-conservation.
Task of the present invention has been come like this, and a kind of preparation method of aluminium iron polychloride, comprises the following steps:
A) prepare ferrous waste acid stoste, be blended in the ferrous waste acid liquid of mass percent concentration 10-14% with dilute hydrochloric acid, and until make the mass percent concentration of ferrous waste acid liquid be increased to 15-18%, obtain ferrous waste acid stoste;
B) aluminium iron polychloride first product is prepared, will by steps A with feeding mode in batches) the ferrous waste acid stoste that obtains drops into in the reaction vessel of whipping appts, and equally in reaction vessel, drop into aluminium ash with feeding mode in batches, under the state that whipping appts stirs, make aluminium ash react with ferrous waste acid stoste, control the stirring velocity of whipping appts, control temperature of reaction, control total weight ratio of ferrous waste acid stoste and aluminium ash, control ferrous waste acid stoste that each batch in batches drop into in batches in the weight ratio of aluminium ash that drops into of each batch and reaction times of controlling each batch in batches, obtain stoste, continuing to make stoste polyreaction under the state stirred, and control the speed continuing to stir and the time controlling polyreaction, obtain aluminium iron polychloride first product,
C) precipitate, first by by step B) the aluminium iron polychloride first product that obtains is released and is introduced from described reaction vessel is furnished with in the settling tank of agitator, in settling tank, readjustment liquid is added under the state that agitator is in stirring, adjusted by the density of readjustment liquid to aluminium iron polychloride first product, precipitation agent and PAM is added again in settling tank, to be precipitated dose and PAM add complete and stop the stirring of agitator after stirring, stratification, end product pool introduced by supernatant liquor, obtain aluminium iron polychloride, and the throw out in settling tank causes filter-pressing device press filtration, the pressing filtering liquid produced during press filtration uses as described readjustment liquid.
In a specific embodiment of the present invention, steps A) described in ferrous waste acid liquid be the ferrous waste acid liquid that metal finishing and plating produce, the mass percent concentration of described dilute hydrochloric acid is 35-37%.
In another specific embodiment of the present invention, step B) described in feeding mode in batches refer to described ferrous waste acid stoste and described aluminium ash is respectively divided into first batch, second batch and the 3rd batch drop into described in reaction vessel in.
In another specific embodiment of the present invention, step B) described in the stirring velocity of control whipping appts be that stirring velocity is controlled as 150-200rpm.
In another specific embodiment of the present invention, step B) described in control temperature of reaction be that temperature of reaction is controlled as 85-95 DEG C.
Also have in a specific embodiment of the present invention, step B) described in control ferrous waste acid stoste and total weight ratio of aluminium ash be that total weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be 3.6: 1.
More of the present invention and in a specific embodiment, step B) described in control in batches in the ferrous waste acid stoste that drops into of each batch with in batches in the weight ratio of aluminium ash that drops into of each batch be that the weight ratio of ferrous waste acid stoste and the first batch of aluminium ash dropped into dropped into first batch controls to be 1.6: 0.4, the ferrous waste acid stoste of second batch and the 3rd batch input and the weight ratio of second batch and the 3rd batch aluminium ash dropped into respectively are controlled to be 1: 0.3, the reaction times of each batch in described control is in batches controlled the reaction times of first batch as 170-190min, the reaction times of second batch is 100-140min, the reaction times of the 3rd batch is 160-200min, wherein: in first batch, described ferrous waste acid stoste is in the described reaction vessel of disposable input, and second, 3rd batch then adds in reaction vessel in dropping mode respectively in 170-190min and 100-140min, first, in second batch and the 3rd batch, described aluminium ash is respectively at 170-190min, add complete in 100-140min and 160-200min.
In an of the present invention and then specific embodiment, step B) described in the control speed that continues to stir be 100-120rpm by the speed control that continues to stir; Time of described control polyreaction is 100-140min by the time controling of polyreaction.
Of the present invention again more and in a specific embodiment, step C) described in readjustment liquid be the pressing filtering liquid be press-filtered out in the throw out produced in last reaction; Described is that the density of aluminium iron polychloride first product is adjusted to 1.2-1.25g/cm by the density adjustment of readjustment liquid to aluminium iron polychloride first product 3(adopting specific gravity hydrometer observing and controlling).
In an again of the present invention and then specific embodiment, step C) described in control aluminium iron polychloride first product, precipitation agent and PAM three weight ratio be that the weight ratio of three is controlled to be 1: 0.8: 0.6, the rotating speed of described agitator is 80-120rpm, described precipitation agent and PAM add complete in 10-20min, the described standing time is 120-150min, and described precipitation agent is methyl sodiosul foaliphatate.
One of technique effect of technical scheme provided by the invention, owing to have employed ferrous waste acid liquid and aluminium ash, thus embody and add useless comprehensive utilization effect to useless, the inferior position of ferrous waste acid liquid and aluminium ash is made to be converted into advantage, not only save resource and matched with the energy-saving economic spirit of saving type that the current whole society advocates, and having contributed to the protection to environment; Two, because the processing step of preparation method is brief, processing ease and without extreme harsh technical factor, thus can meet industrial amplification production requirement; Three, due to make use of in reaction process reaction system in-situ reaction heat, thus can embody desirable energy-saving effect.
Embodiment
Embodiment 1:
A) spent acid stoste is prepared, be blended into the dilute hydrochloric acid of mass percent concentration 35% that to come from metal finishing such as the mass percent concentration produced in cleaning metal surface process be in the ferrous waste acid liquid of 14%, until make the mass percent concentration of ferrous waste acid liquid be increased to 15%, obtain ferrous waste acid stoste, in this step, aforesaid ferrous waste acid liquid is deposited in ferrous waste acid liquid storage tank after collecting in advance, release from ferrous waste acid liquid storage tank during use, with adopt mass percent concentration be 35% dilute hydrochloric acid by mass percent concentration be 14% 1000kg ferrous waste acid liquid to convert to mass percent concentration be the account form of 15% that example is: (140+35%X) ÷ (1000+X)=15%, and then be: 140+0.35X=150+0.15X, and then be: 0.2X=10, obtain X=50kg, namely, use 50kg mass percent concentration be 35% dilute hydrochloric acid by mass percent concentration be 14% 1000kg ferrous waste acid liquid be adjusted to the ferrous waste acid liquid that mass percent concentration is 15%, also ferrous waste acid stoste is namely obtained,
B) aluminium iron polychloride first product is prepared, feeding mode (also can be claimed stage by stage) by by steps A with in batches) the ferrous waste acid stoste that obtains drops into whipping appts reaction vessel (the present embodiment is reactor, as follows) in, and equally in reaction vessel, drop into aluminium ash with feeding mode (also can claim feeding mode stage by stage) in batches, under the stirring velocity of whipping appts is the whipped state of 180rpm, make aluminium ash react with ferrous waste acid stoste, wherein: total weight ratio of ferrous waste acid stoste and aluminium ash is 3.6: 1, owing to being feed intake in batches, therefore be divided into three batches and drop into ferrous waste acid stoste and aluminium ash, specifically: when first batch feed intake, the weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be get 1.6: 0.4 in 1.6: 0.4(3.6: 1), in this is first batch, in the disposable input reaction vessel of ferrous waste acid stoste, aluminium ash then slowly adds in 190min, that is the reaction times of first batch is 190min, aluminium ash gradually adds complete in 190min, when second batch feed intake, the weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be get 1: 0.3 in 1: 0.3(3.6: 1), and in this is second batch, ferrous waste acid stoste and aluminium ash are all 100min in the 100min(reaction times) in slowly add complete, when the 3rd batch feed intake, the weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be get 1: 0.3 in 1: 0.3(3.6: 1), and in the 3rd batch, ferrous waste acid stoste and aluminium ash all slowly add in 200min, that is the reaction times of the 3rd batch is 200min, ferrous waste acid stoste slowly adds complete in dropping mode equally in 200min, aluminium ash equally slowly adds.From aforementioned explanation, if the weight of ferrous waste acid stoste is 360kg, and aluminium ash is 100kg, so the add-on of first, second, third batch is respectively 160kg, 100kg and 100kg, and the add-on of aluminium ash in first, second, third batch is respectively 40kg, 30kg and 30kg.In the present embodiment, the temperature of reaction of first, second, third batch is 85 DEG C, when temperature is lower than 85 DEG C, then suitably strengthen the input speed namely accelerating aluminium ash, otherwise with example, through first, second, third batch feed intake and react terminate after obtain stoste, low whipping speed makes stoste realize polyreaction under changing the continuation whipped state of 100rpm into, the time of polyreaction is 140min, obtains aluminium iron polychloride first product;
C) precipitate, by by step B) the aluminium iron polychloride first product that obtains is released and is introduced from reaction vessel is furnished with in the settling tank of agitator, under the state that agitator is in 120rpm, in settling tank, add readjustment liquid, by readjustment liquid, the density of aluminium iron polychloride first product is adjusted to 1.2g/cm 3(adopting specific gravity hydrometer measure and control), precipitation agent and PAM is added again in settling tank, precipitation agent and PAM add complete in 10min, to be precipitated dose and PAM add complete and stop the stirring of agitator after stirring, stratification, end product pool introduced by supernatant liquor, namely aluminium iron polychloride is obtained, throw out in settling tank causes the plate-and-frame filter press press filtration of filter-pressing device, the pressing filtering liquid produced during press filtration uses as the readjustment liquid preparing aluminium iron polychloride next time, in this step, aluminium iron polychloride first product, the weight ratio of precipitation agent and PAM three controls to be 1: 0.8: 0.6, the aforesaid standing time is 150min, aforesaid precipitation agent is methyl sodiosul foaliphatate, aforesaid PAM is polyacrylamide.
Embodiment 2:
A) spent acid stoste is prepared, being blended into the dilute hydrochloric acid of mass percent concentration 37% mass percent concentration come from by plating generation is in the ferrous waste acid liquid of 10%, until make the mass percent concentration of ferrous waste acid liquid be increased to 18%, obtain ferrous waste acid stoste, in this step, aforesaid ferrous waste acid liquid is deposited in ferrous waste acid liquid storage tank after collecting in advance, release from ferrous waste acid liquid storage tank during use, adopt mass percent concentration be 37% dilute hydrochloric acid by mass percent concentration be 10% 1000kg ferrous waste acid liquid to convert to mass percent concentration be that the account form of 18% is as the description (account form is with embodiment 1) to embodiment 1,
B) aluminium iron polychloride first product is prepared, feeding mode (also can be claimed stage by stage) by by steps A with in batches) the ferrous waste acid stoste that obtains drops into whipping appts reaction vessel (the present embodiment is reactor, as follows) in, and (also can claim feeding mode stage by stage) with in batches drops into aluminium ash in reaction vessel equally, under the stirring velocity of whipping appts is the whipped state of 150rpm, make aluminium ash react with ferrous waste acid stoste, wherein: total weight ratio of ferrous waste acid stoste and aluminium ash is 3.6: 1, owing to being feed intake in batches, therefore be divided into three batches and drop into ferrous waste acid stoste and aluminium ash, specifically: when first batch feed intake, the weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be get 1.6: 0.4 in 1.6: 0.4(3.6: 1), in this is first batch, in the disposable input reaction vessel of ferrous waste acid stoste, aluminium ash then slowly adds in 170min, that is the reaction times of first batch is 170min, aluminium ash gradually adds complete in 170min, when second batch feed intake, the weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be get 1: 0.3 in 1: 0.3(3.6: 1), and in this is second batch, ferrous waste acid stoste and aluminium ash are all 140min in the 140min(reaction times) in slowly add complete, when the 3rd batch feed intake, the weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be get 1: 0.3 in 1: 0.3(3.6: 1), and in the 3rd batch, ferrous waste acid stoste and aluminium ash all slowly add in 160min, that is the reaction times of the 3rd batch is 160min, ferrous waste acid stoste slowly adds complete in dropping mode equally in 160min, aluminium ash slowly adds complete equally in 160min.In the present embodiment, the temperature of reaction of first, second, third batch is 95 DEG C, when temperature is lower than 95 DEG C, then suitably strengthen the input speed namely accelerating aluminium ash, otherwise with example, through first, second, third batch feed intake and react terminate after obtain stoste, low whipping speed makes stoste realize polyreaction under changing the continuation whipped state of 120rpm into, the time of polyreaction is 100min, obtains aluminium iron polychloride first product;
C) precipitate, change the speed of agitator into 80rpm, change the density of aluminium iron polychloride first product into 1.25g/cm 3, precipitation agent and PAM are changed into and add complete in 20min, change the standing time into 120min.In the present embodiment 2, NM content is all with the description to embodiment 1.
Embodiment 3:
A) spent acid stoste is prepared, be blended into the dilute hydrochloric acid of mass percent concentration 36% that to come from the mass percent concentration that Plate Production manufacturer produces cleaning steel plate and pickling be in the ferrous waste acid liquid of 12%, until make the mass percent concentration of ferrous waste acid liquid be increased to 16.5%, obtain ferrous waste acid stoste, in this step, aforesaid ferrous waste acid liquid is deposited in ferrous waste acid liquid storage tank after collecting in advance, release from ferrous waste acid liquid storage tank during use, adopt mass percent concentration be 36% dilute hydrochloric acid by mass percent concentration be 12% 1000kg ferrous waste acid liquid to convert to mass percent concentration be that the account form of 16.5% is as the description to embodiment 1,
B) aluminium iron polychloride first product is prepared, feeding mode (also can be claimed stage by stage) by by steps A with in batches) the ferrous waste acid stoste that obtains drops into whipping appts reaction vessel (the present embodiment is reactor, as follows) in, and (also can claim feeding mode stage by stage) with in batches drops into aluminium ash in reaction vessel equally, under the stirring velocity of whipping appts is the whipped state of 200rpm, make aluminium ash react with ferrous waste acid stoste, wherein: total weight ratio of ferrous waste acid stoste and aluminium ash is 3.6: 1, owing to being feed intake in batches, therefore be divided into three batches and drop into ferrous waste acid stoste and aluminium ash, specifically: when first batch feed intake, the weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be get 1.6: 0.4 in 1.6: 0.4(3.6: 1), in this is first batch, in the disposable input reaction vessel of ferrous waste acid stoste, aluminium ash then slowly adds in 180min, that is the reaction times of first batch is 180min, aluminium ash gradually adds complete in 180min, when second batch feed intake, the weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be get 1: 0.3 in 1: 0.3(3.6: 1), and in this is second batch, ferrous waste acid stoste and aluminium ash are all 120min in the 120min(reaction times) in slowly add complete, when the 3rd batch feed intake, the weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be get 1: 0.3 in 1: 0.3(3.6: 1), and in the 3rd batch, ferrous waste acid stoste and aluminium ash all slowly add complete in 180min, that is the reaction times of the 3rd batch is 180min, ferrous waste acid stoste slowly adds complete in dropping mode equally in 180min, aluminium ash also slowly adds complete in 180min.In the present embodiment, the temperature of reaction of first, second, third batch is 90 DEG C, when temperature is lower than 90 DEG C, then suitably strengthen the input speed namely accelerating aluminium ash, otherwise with example, through first, second, third batch feed intake and react terminate after obtain stoste, low whipping speed makes stoste realize polyreaction under changing the continuation whipped state of 110rpm into, the time of polyreaction is 120min, obtains aluminium iron polychloride first product;
C) precipitate, change the speed of agitator into 100rpm, change the density of aluminium iron polychloride first product into 1.22g/cm 3, precipitation agent and PAM are changed into and add complete in 15min, change the standing time into 135min.In the present embodiment 3, NM content is all with the description to embodiment 1.
The dilute hydrochloric acid that the mass percent concentration mentioned in above-described embodiment 1 to 3 is respectively 35%, 37% and 36% selects the by-product hydrochloric acid with being produced in process of production by Jiangsu Province, China Changshu City three Ai Fuzhonghao new chemical materials company limited, and this by-product hydrochloric acid is in fact also acid waste liquid.Ferrous waste acid liquid in embodiment 1 to 3 all refers to waste hydrochloric acid containing iron liquid.

Claims (10)

1. a preparation method for aluminium iron polychloride, is characterized in that comprising the following steps:
A) prepare ferrous waste acid stoste, be blended in the ferrous waste acid liquid of mass percent concentration 10-14% with dilute hydrochloric acid, and until make the mass percent concentration of ferrous waste acid liquid be increased to 15-18%, obtain ferrous waste acid stoste;
B) aluminium iron polychloride first product is prepared, will by steps A with feeding mode in batches) the ferrous waste acid stoste that obtains drops into in the reaction vessel of whipping appts, and equally in reaction vessel, drop into aluminium ash with feeding mode in batches, under the state that whipping appts stirs, make aluminium ash react with ferrous waste acid stoste, control the stirring velocity of whipping appts, control temperature of reaction, control total weight ratio of ferrous waste acid stoste and aluminium ash, control ferrous waste acid stoste that each batch in batches drop into in batches in the weight ratio of aluminium ash that drops into of each batch and reaction times of controlling each batch in batches, obtain stoste, continuing to make stoste polyreaction under the state stirred, and control the speed continuing to stir and the time controlling polyreaction, obtain aluminium iron polychloride first product,
C) precipitate, first by by step B) the aluminium iron polychloride first product that obtains is released and is introduced from described reaction vessel is furnished with in the settling tank of agitator, in settling tank, readjustment liquid is added under the state that agitator is in stirring, adjusted by the density of readjustment liquid to aluminium iron polychloride first product, precipitation agent and PAM is added again in settling tank, to be precipitated dose and PAM add complete and stop the stirring of agitator after stirring, stratification, end product pool introduced by supernatant liquor, obtain aluminium iron polychloride, and the throw out in settling tank causes filter-pressing device press filtration, the pressing filtering liquid produced during press filtration uses as described readjustment liquid.
2. the preparation method of aluminium iron polychloride according to claim 1, is characterized in that steps A) described in ferrous waste acid liquid be metal finishing and plating produce ferrous waste acid liquid, the mass percent concentration of described dilute hydrochloric acid is 35-37%.
3. the preparation method of aluminium iron polychloride according to claim 1, is characterized in that step B) described in feeding mode in batches refer in the reaction vessel described in described ferrous waste acid stoste and described aluminium ash being respectively divided into first batch, second batch and the 3rd batch drops into.
4. the preparation method of aluminium iron polychloride according to claim 1, is characterized in that step B) described in the stirring velocity of control whipping appts be that stirring velocity is controlled as 150-200rpm.
5. the preparation method of aluminium iron polychloride according to claim 1, is characterized in that step B) described in control temperature of reaction be that temperature of reaction is controlled as 85-95 DEG C.
6. the preparation method of aluminium iron polychloride according to claim 1, is characterized in that step B) described in control ferrous waste acid stoste and total weight ratio of aluminium ash be that total weight ratio of ferrous waste acid stoste and aluminium ash is controlled to be 3.6: 1.
7. the preparation method of aluminium iron polychloride according to claim 1, it is characterized in that step B) described in control in batches in the ferrous waste acid stoste that drops into of each batch with in batches in the weight ratio of aluminium ash that drops into of each batch be that the weight ratio of ferrous waste acid stoste and the first batch of aluminium ash dropped into dropped into first batch controls to be 1.6: 0.4, the ferrous waste acid stoste of second batch and the 3rd batch input and the weight ratio of second batch and the 3rd batch aluminium ash dropped into respectively are controlled to be 1: 0.3, the reaction times of each batch in described control is in batches controlled the reaction times of first batch as 170-190min, the reaction times of second batch is 100-140min, the reaction times of the 3rd batch is 160-200min, wherein: in first batch, described ferrous waste acid stoste is in the described reaction vessel of disposable input, and second, 3rd batch then adds in reaction vessel in dropping mode respectively in 170-190min and 100-140min, first, in second batch and the 3rd batch, described aluminium ash is respectively at 170-190min, add complete in 100-140min and 160-200min.
8. the preparation method of aluminium iron polychloride according to claim 1, is characterized in that step B) described in control continue stir speed be by continue stir speed control be 100-120rpm; Time of described control polyreaction is 100-140min by the time controling of polyreaction.
9. the preparation method of aluminium iron polychloride according to claim 1, is characterized in that step C) described in readjustment liquid be the pressing filtering liquid be press-filtered out in the throw out produced in last reaction; Described is that the density of aluminium iron polychloride first product is adjusted to 1.2-1.25g/cm by the density adjustment of readjustment liquid to aluminium iron polychloride first product 3.
10. the preparation method of aluminium iron polychloride according to claim 1, it is characterized in that step C) described in control aluminium iron polychloride first product, precipitation agent and PAM three weight ratio be that the weight ratio of three is controlled to be 1: 0.8: 0.6, the rotating speed of described agitator is 80-120rpm, described precipitation agent and PAM add complete in 10-20min, the described standing time is 120-150min, and described precipitation agent is methyl sodiosul foaliphatate.
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CN109761323A (en) * 2019-01-26 2019-05-17 山东铝晖环保科技有限公司 By the method for aluminium ash, the water purification agent of hydrochloric acid and the preparation of optional red mud containing aluminium polychloride
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CN112110465A (en) * 2020-08-28 2020-12-22 宁夏中宁县兴日晟环保科技有限公司 Preparation method of polyaluminium chloride for polyaluminium chloride flocculating agent
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