CN105967298A - Method for preparing polyaluminum chloride - Google Patents

Method for preparing polyaluminum chloride Download PDF

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Publication number
CN105967298A
CN105967298A CN201610591956.2A CN201610591956A CN105967298A CN 105967298 A CN105967298 A CN 105967298A CN 201610591956 A CN201610591956 A CN 201610591956A CN 105967298 A CN105967298 A CN 105967298A
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polyaluminium chloride
bentonite
hours
mass fraction
pressure
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韩再满
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Guangxi Chisheng Agricultural Technology Co Ltd
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Guangxi Chisheng Agricultural 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
    • C02F1/5245Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/48Halides, with or without other cations besides aluminium
    • C01F7/56Chlorides

Abstract

The invention discloses a method for preparing polyaluminum chloride. The method is characterized in that polyaluminum chloride is prepared from bentonite and high-aluminum refining slag, and the method comprises the specific steps of 1, pretreatment of the bentonite, 2, pretreatment of the high-aluminum refining slag; 3, one-step reacting; 4, second-step reacting; 5, filtering pressing, 6, heavy metal ion removal and 7, spray drying. The method has the advantages that under the existing two-step technological conditions, the pretreatment steps of the raw materials and the heavy metal removal step are added for reacting, processing equipment is easy to mount and operate and low in replacement frequency, the modification cost of a manufacturing enterprise is greatly reduced, the product quality is improved, meanwhile, the dilemma of greatly modifying equipment to meet the technical standard is avoided, and the product meets the requirement of a new standard.

Description

A kind of method preparing polyaluminium chloride
[technical field]
The present invention relates to water process, chemical field, particularly to a kind of method preparing polyaluminium chloride.
[background technology]
Polyaluminium chloride, is commonly called as water purification agent, has another name called aluminium polychlorid, is called for short poly-aluminum, english name PAC.It is a kind of polyhydroxy, The cationic inorganic polymer flocculant of multinuclear complexation body, solid product outward appearance is bronzing, yellow or white solid powder, Its chemical molecular formula is [Al2(OH)nCl6-n] m. (in formula, 1≤n≤5, m≤10), and soluble in water, there is stronger bridge formation to adsorb Property, with electrochemistry in hydrolytic process, condense, adsorb and the physico change such as precipitation, ultimately generate [Al2(OH)3(OH)3], Thus reach to purify purpose.Polyaluminium chloride is a kind of new and effective inorganic polymer flocculant.It is widely used in former water and Prepared by waste water, and many fields such as papermaking, process hides.
In existing polyaluminium chloride manufacturing enterprise of China, the manufacturing enterprise due to up to 90% use bauxite acid molten and The two step method production technology of calcium aluminate regulation basicity, utilizes the polyaluminium chloride product that this method produces, its content of beary metal Exceed standard, it is impossible to meet the new standard of the polyaluminium chloride of domestic water.If there is pressure to perform by new standard, a lot of companies will Buy less than qualified products, and the problem that purchase cost is to be significantly increased.
[summary of the invention]
The problem that the invention aims to overcome existing for prior art, it is provided that a kind of side preparing polyaluminium chloride Method, it is an advantage of the invention that under the process conditions of existing two step method, adds pre-treatment step and the removing heavy metals of raw material Step reaction, process equipment easily installs, easily operation and replacement frequency low, greatly reduce the improvement cost of manufacturing enterprise, improve Product quality, it also avoid as reaching technical standard and the predicament of significantly reforming equipment simultaneously, makes product meet the requirement of new standard.
For reaching above-mentioned purpose, the technical solution adopted in the present invention is: a kind of method preparing polyaluminium chloride, its feature It is: concretely comprise the following steps:
(1) bentonitic pretreatment: the bentonite of acetum that 5-10Kg mass fraction is 2-8% with 5-8Kg is mixed Close, be then placed within the water-bath of 50-65 DEG C being heated to being dried, put into Muffle furnace little at 500-900 DEG C of roasting 0.5-3 Time, by the bentonite natural cooling after roasting, pulverize, cross 20 mesh sieves, obtain the bentonite handled well;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into formula crusher in crushing 0.5-2 hour, makes Discharging-material size, for reaching 10-20mm, is put into Muffle furnace and is put in cold water cool down in 300-500 DEG C of roasting 0.5-2 hour, taking-up, Further take out and dry, be then placed in infrared baking oven and be dried 12 hours at 50 DEG C, obtain the high alumina refining slag handled well;
(3) single step reaction: by the bentonite handled well that 10-16Kg mass ratio is 1-3:1 and the high alumina refine handled well Slag puts in reactor, first-class reactor manhole cover, then the hydrochloric acid pump that 30-50Kg mass fraction is 20-35% is squeezed into instead Answer still, then open steam and heat up, at a temperature of 100-158 DEG C, carry out reaction 2-4 hour;
(4) two step reactions: after single step reaction terminates, 14-22Kg calcium aluminate is put into dissolution kettle, add 50-100Kg pure Water dissolution, in the calcium aluminate solution that will have dissolved press-in reactor, reacts 4-7 hour at a temperature of 100-115 DEG C further;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters, settle 6-12 hour, by upper Thick end product pool put into by layer clear liquid, obtains rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 5-10 hour, natural sedimentation 6-12 hour, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally with containing active The ultrafiltration membrance filter of charcoal, obtains finished product polyaluminium chloride liquid;
(7) be spray-dried: first by blower fan by the heated dry air of vapor heat exchanger, by the hot blast spiral case at drying tower top and Hot-air distributor uniformly flows into hothouse, then by dry finished product polyaluminium chloride liquid by hopper, is sent into by charging pump Nebulizer, under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, and in hothouse, droplet contacts with hot blast, is dried Become product, packaging, obtain finished product polyaluminium chloride solid.
In the present invention, as further illustrating, alumina content >=55% of the calcium aluminate described in step (4), reaction The pressure of still is 0.15-0.40MPa.
In the present invention, as further illustrating, the feed liquid turbidity described in step (5) is < 200NTU, pressure filter oil pressure pressure Power is 10-20MPa.
In the present invention, as further illustrating, the preparation method of the modified clay mineral described in step (6) is: first will The clay mineral of 10-16Kg is pulverized, and crosses 20 mesh sieves, with the hydrogen peroxide dipping that 15-25Kg mass fraction is 6-20% 5-10 days, then With the soak with hydrochloric acid that 15-25Kg mass fraction is 20-30% 3-5 days, it is finally the carbonic acid of 2-5% with 25-30Kg mass fraction Sodium solution soaks 5-10 days and is also stirred continuously, and filters, and filtering residue is 5-8 with three distilled water washs to filtrate pH, exists at room temperature The vacuum under pressure of 0.05-0.15MPa is dried 6-12 hour, ground 20 mesh sieves, obtains modified clay mineral.
In the present invention, as further illustrating, described clay mineral is montmorillonite, bentonite, Kaolin, Ai Luo One or more in stone, serpentine, pyrophillite, illite, Vermiculitum and meerschaum.
In the present invention, as further illustrating, step (7) is to carry out under condition of negative pressure, and pressure is negative 0.5- 0.8MPa, alumina content >=28%.
In the present invention, as further illustrating, in step (7), the inlet temperature of drying tower is 150-270 DEG C.
In the present invention, as further illustrating, the basicity of described polyaluminium chloride is 60-95%.
Part material effective efficiency is described below:
Bentonite is also bentonite, Bentonite or amargosite.China's application is bentonitic with a long history, the most simply does For a kind of detergent.Colonial is the discovery that in the ancient stratum of the Wyoming State, and in yellowish green clay, after adding water, expansion becomes Pasty state, people were just every clay having this character later, were referred to as bentonite.The most bentonitic main mineral constituent is Montmorillonite, content is at 85-90%, and bentonitic properties is the most all determined by montmorillonite.Montmorillonite can be in various face Color is the most yellowish green, HUANGBAI(sic), ash, white etc..Compact massive can be become, it is possible to for loose earthy, when rubbing mill with the hands with finger, have sliding sense, Small blocks add water after the volume several times that swell to 20-30 times, in suspension in water, when water is few in the pasty state.The character of montmorillonite and Its chemical composition is relevant with internal structure.
The main component of high alumina refining slag is CaO-Al2O3, after referring to mix raw material by a certain percentage with granularity, low Heat in the case of raw material fusing point, make raw material be sintered together, the essence used after being broken into the grain graininess of needs the most again Refining slag.
Hydrochloric acid has another name called hydrochloric acid, is the aqueous solution of hydrogen chloride, belongs to unitary inorganic strong acid, and industrial use is extensive.Hydrochloric acid Character is water white liquid, has strong sharp aroma, has higher corrosivity.(mass fraction is about concentrated hydrochloric acid 37%) there is extremely strong volatility, therefore fill the container of concentrated hydrochloric acid and open afterchlorinate hydrogen and can volatilize, with the water in air Steam combines and produces hydrochloric acid droplet, makes to occur above bottleneck acid mist.Hydrochloric acid is the main component of gastric acid, and it can promote food Digest, resist microorganism infection.
Calcium aluminate is a kind of white solid being insoluble in water, and odorless, tasteless, matter is extremely hard, the easy moisture absorption and not deliquescence.Both sexes oxygen Compound, can be dissolved in mineral acid and alkaline solution, is practically insoluble in water and non-polar organic solvent.Be a series of by calcium oxide and The inorganic compound that aluminium oxide at high temperature sinters, due to the physical property that its hardness is big, fusing point is high, is applied to cement With fire extinguishing material in.Formula is mCaO nAl2O3.Calcium aluminate product is divided into water preparation to use, steel-making deslagging agent, alumina cement three are big Class.
Clay mineral (clay minerals), geology technical term, is composition clay rock and the essential mineral of soil. They are that some contain the hydrosilicate mineral that aluminum, magnesium etc. are master.Layer silicate mineral has tetrahedral sheet and octahedral sheet The crystal structure of composition.The construction unit layer being made up of a tetrahedral sheet and octahedral sheet is referred to as 1: 1 type, such as kaolinite Stone, galapectite and serpentine etc.;The construction unit layer being made up of two tetrahedral sheets one octahedral sheets of folder is referred to as 2: 1 types, as Montmorillonite, pyrophillite, Muscovitum, Vermiculitum etc..The construction unit layer of clay mineral is generally all with electric charge.Due to clay mineral grain Trickle, with electric charge, specific surface area is huge and there is structure interlamination region etc., be allowed to have adsorptivity, dilatancy, plasticity and from The properties such as sub-exchange, these performances make clay mineral material be widely used.
Activated carbon is the solid carbonaceous of a kind of black porous, by coal by pulverize, molding or with uniform coal grain through carbonization, Activation produces.It is mainly composed of carbon, and containing elements such as a small amount of oxygen, hydrogen, sulfur, nitrogen, chlorine.The specific surface area of normal activated carbon is 500 ~1700m2Between/g.There is the strongest absorption property, for a kind of industrial adsorbents that purposes is the widest.
The method have the advantages that
1. bentonite is taked pretreatment mode by the present invention, can break the crystalline structure of bentonitic inside, improves swollen The reactivity of profit soil.Aluminosilicate contained in bentonite occurs the difference of crystal form and mineral structure to change at different temperatures Become, thus make the dissolution rate in acid of the aluminium oxide in ore deposit change the most therewith.The aluminium oxide existed with aluminosilicate form, with salt Acid reactivity is the lowest, it is therefore necessary to processed by certain condition so that it is be turned into the amorphous body that activity is bigger.According to Bentonitic chemical property, when sintering temperature is between 500-750 DEG C, after roasting, the activity with hydrochloric acid reaction is greatly improved; With prior art is announced by bentonite directly and after hydrochloric acid reaction bentonitic reactivity improve 15-30%, make Al2O3 Leaching rate reach 52-86%.
2. the production method of a kind of polyaluminium chloride that the present invention uses, it is possible to effectively reduce the weight produced in production process The content of metal, enables product to meet new national standard.Through the clay mineral that modification is crossed, eliminate the organic matter of self And heavy metal, impurity is removed, and exposes fresh active surface, has the adsorption effect of the heavy metal more excellent than original soil.Its One is specific surface area and the pore volume increasing of modified clay mineral, has supervened huge surface energy, for the table of heavy metal Face absorbability is strengthened;It two is modified clay mineral imbibition, and crystal layer basal spacing strengthens, the interlayer cation after expansion Can also swap with other cation in solution, Adsorption of Heavy Metals ability is higher;It three is the crystalline substance of modified clay mineral The permanent negative charge that interlayer exists, with the form of electrostatic attraction by cation-adsorption therebetween, and remains swap status;This Synergism between three kinds strengthens the adsorptivity of modified clay mineral heavy metal ion, greatly reduces in polyaluminium chloride The content of heavy metal, improve the purity of product.
3. the step of the removing heavy metals ion used in the production method of a kind of polyaluminium chloride that the present invention uses is simple, work Skill equipment easily installs, easily operation and replacement frequency low, greatly reduce the improvement cost of manufacturing enterprise, improve product quality, with Time it also avoid as reaching technical standard and the predicament of significantly reforming equipment, meet the requirement of new standard.
[detailed description of the invention]
Embodiment 1:
1. the preparation of modified clay mineral
First 2Kg bentonite, 3Kg illite and 5Kg meerschaum are pulverized, cross 20 mesh sieves, be 6% with 15Kg mass fraction Hydrogen peroxide dipping 5 days, then with the soak with hydrochloric acid that 15Kg mass fraction is 20% 3 days, is finally the carbon of 2% with 25Kg mass fraction Acid sodium solution soaks 5 days and is also stirred continuously, and filters, and filtering residue is 5 with three distilled water washs to filtrate pH, exists at room temperature The vacuum under pressure of 0.05MPa is dried 12 hours, ground 20 mesh sieves, obtains modified clay mineral.
2. the preparation method of polyaluminium chloride, concretely comprises the following steps:
(1) bentonitic pretreatment: the acetum that 5Kg mass fraction is 2% is mixed, then with the bentonite of 5Kg It is placed on the water-bath of 50 DEG C and is heated to being dried, put into Muffle furnace 500 DEG C of roastings 3 hours, by the Kaolin after roasting Natural cooling, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;Treated bentonitic Al2O3Leaching rate be 52%;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into a formula crusher in crushing 0.5 hour, uses Material granularity, for reaching 20mm, is put into Muffle furnace and is put in cold water and cool down in 300 DEG C of roastings 2 hours, taking-up, further take out and dry, so After put into infrared baking oven at 50 DEG C be dried 12 hours, obtain the high alumina refining slag handled well;
(3) single step reaction: the high alumina refining slag that the bentonite handled well by 5Kg and 5Kg handle well puts in reactor, on Good reactor manhole cover, then the hydrochloric acid pump that 30Kg mass fraction is 20% is squeezed into reactor, then open steam and heat up, in temperature Degree is 100 DEG C, and pressure is to carry out under 0.15MPa reacting 2 hours;
(4) two step reactions: after single step reaction terminates, 14Kg calcium aluminate is put into dissolution kettle, add 50Kg dissolved in purified water, In the calcium aluminate solution press-in reactor that will have dissolved, react 4 hours further at a temperature of 115 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters with oil pressure pressure 10MPa, heavy Drop 6 hours, the supernatant is put into thick end product pool, obtain rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 5 hours, natural sedimentation 6 hours, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally super with containing activated carbon Membrane filtration, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: be first 150 DEG C by blower fan by the heated dry air of vapor heat exchanger, inlet temperature, pass through drying tower The hot blast spiral case at top and hot-air distributor uniformly flow into hothouse, then by dry finished product polyaluminium chloride liquid by expecting Groove, sends into nebulizer by charging pump, and under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, in hothouse, and pressure Contact with hot blast for droplet under conditions of-0.5MPa, be dried to product, packaging, obtain the finished product polychlorostyrene that basicity is 75% Change aluminum solid.
Embodiment 2:
1. the preparation of modified clay mineral
First 5Kg pyrophillite, 1Kg Vermiculitum, 2Kg Kaolin and 2Kg montmorillonite are pulverized, cross 20 mesh sieves, divide by 18Kg mass Number is the hydrogen peroxide dipping 6 days of 8%, then with the soak with hydrochloric acid that 18Kg mass fraction is 21% 3 days, finally uses 25Kg mass fraction Being the soaking in sodium carbonate solution 6 days of 2.5% and be stirred continuously, filter, filtering residue is 5.5 with three distilled water washs to filtrate pH, Vacuum under pressure at 0.07MPa is dried 11 hours at room temperature, ground 20 mesh sieves, obtains modified clay mineral.
2. the preparation method of polyaluminium chloride, concretely comprises the following steps:
(1) bentonitic pretreatment: the acetum that 6Kg mass fraction is 3% is mixed, then with the bentonite of 5Kg It is placed on the water-bath of 55 DEG C and is heated to being dried, put into Muffle furnace 550 DEG C of roastings 3 hours, by the Kaolin after roasting Natural cooling, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;Treated bentonitic Al2O3Leaching rate be 60%;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into a formula crusher in crushing 1 hour, makes discharging Granularity, for reaching 15mm, is put into Muffle furnace and is put in cold water and cool down in 350 DEG C of roastings 2 hours, taking-up, further take out and dry, then Put into infrared baking oven to be dried 12 hours at 50 DEG C, obtain the high alumina refining slag handled well;
(3) single step reaction: the high alumina refining slag that the bentonite handled well by 10Kg and 6Kg handle well puts in reactor, First-class reactor manhole cover, then the hydrochloric acid pump that 35Kg mass fraction is 25% is squeezed into reactor, then open steam and heat up, Temperature is 108 DEG C, and pressure is to carry out under 0.18MPa reacting 2 hours;
(4) two step reactions: after single step reaction terminates, 15Kg calcium aluminate is put into dissolution kettle, add 55Kg dissolved in purified water, In the calcium aluminate solution press-in reactor that will have dissolved, react 4 hours further at a temperature of 112 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters with oil pressure pressure 11MPa, heavy Drop 7 hours, the supernatant is put into thick end product pool, obtain rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 5 hours, natural sedimentation 7 hours, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally super with containing activated carbon Membrane filtration, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: be first 165 DEG C by blower fan by the heated dry air of vapor heat exchanger, inlet temperature, pass through drying tower The hot blast spiral case at top and hot-air distributor uniformly flow into hothouse, then by dry finished product polyaluminium chloride liquid by expecting Groove, sends into nebulizer by charging pump, and under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, in hothouse, and pressure Contact with hot blast for droplet under conditions of-0.55MPa, be dried to product, packaging, obtain the finished product polychlorostyrene that basicity is 85% Change aluminum solid.
Embodiment 3:
1. the preparation of modified clay mineral
First 3Kg galapectite and 10Kg pyrophillite are pulverized, cross 20 mesh sieves, with the dioxygen water logging that 20Kg mass fraction is 10% Steep 7 days, then with the soak with hydrochloric acid that 20Kg mass fraction is 23% 4 days, be finally the sodium carbonate liquor of 3% with 28Kg mass fraction Soaking 7 days and be stirred continuously, filtering, filtering residue is 7 with three distilled water washs to filtrate pH, at room temperature in the pressure of 0.08MPa It is vacuum dried 11 hours under power, ground 20 mesh sieves, obtains modified clay mineral.
2. the preparation method of polyaluminium chloride, concretely comprises the following steps:
(1) bentonitic pretreatment: the acetum that 7Kg mass fraction is 4% is mixed, then with the bentonite of 4Kg It is placed on the water-bath of 55 DEG C and is heated to being dried, put into Muffle furnace 600 DEG C of roastings 2.5 hours.By the kaolinite after roasting Soil natural cooling, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;Treated bentonitic Al2O3Leaching rate be 86%;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into a formula crusher in crushing 1.5 hours, uses Material granularity, for reaching 15mm, is put into Muffle furnace and is put in cold water and cool down in 400 DEG C of roastings 1.5 hours, taking-up, further take out and dry, It is then placed in infrared baking oven to be dried 12 hours at 50 DEG C, obtains the high alumina refining slag handled well;
(3) single step reaction: the high alumina refining slag that the bentonite handled well by 12Kg and 4Kg handle well puts in reactor, First-class reactor manhole cover, then the hydrochloric acid pump that 30Kg mass fraction is 30% is squeezed into reactor, then open steam and heat up, Temperature is 116 DEG C, and pressure is to carry out under 0.18MPa reacting 3 hours;
(4) two step reactions: after single step reaction terminates, 16Kg calcium aluminate is put into dissolution kettle, add 60Kg dissolved in purified water, In the calcium aluminate solution press-in reactor that will have dissolved, react 5 hours further at a temperature of 110 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters with oil pressure pressure 13MPa, heavy Drop 8 hours, the supernatant is put into thick end product pool, obtain rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 8 hours, natural sedimentation 7 hours, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally super with containing activated carbon Membrane filtration, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: be first 180 DEG C by blower fan by the heated dry air of vapor heat exchanger, inlet temperature, pass through drying tower The hot blast spiral case at top and hot-air distributor uniformly flow into hothouse, then by dry finished product polyaluminium chloride liquid by expecting Groove, sends into nebulizer by charging pump, and under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, in hothouse, and pressure Contact with hot blast for droplet under conditions of-0.6MPa, be dried to product, packaging, obtain the finished product polychlorostyrene that basicity is 95% Change aluminum solid.
Embodiment 4:
1. the preparation of modified clay mineral
First 4Kg serpentine, 4Kg montmorillonite, 4Kg illite and 4Kg Vermiculitum are pulverized, cross 20 mesh sieves, divide by 22Kg mass Number is the hydrogen peroxide dipping 7 days of 12%, then with the soak with hydrochloric acid that 22Kg mass fraction is 25% 4 days, finally divides by 30Kg mass The soaking in sodium carbonate solution of several 3.5% 8 days is also stirred continuously, and filters, and filtering residue is 6.5 with three distilled water washs to filtrate pH, Vacuum under pressure at 0.1MPa is dried 10 hours at room temperature, ground 20 mesh sieves, obtains modified clay mineral.
2. the preparation method of polyaluminium chloride, concretely comprises the following steps:
(1) bentonitic pretreatment: the acetum that 8Kg mass fraction is 5% is mixed, then with the bentonite of 6Kg It is placed on the water-bath of 60 DEG C and is heated to being dried, put into Muffle furnace 700 DEG C of roastings 2 hours, by the Kaolin after roasting Natural cooling, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;Treated bentonitic Al2O3Leaching rate be 72%;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into a formula crusher in crushing 2 hours, makes discharging Granularity, for reaching 10mm, is put into Muffle furnace and is put in cold water and cool down in 500 DEG C of roastings 1 hour, taking-up, further take out and dry, then Put into infrared baking oven to be dried 12 hours at 50 DEG C, obtain the high alumina refining slag handled well;
(3) single step reaction: the high alumina refining slag that the bentonite handled well by 10Kg and 6Kg handle well puts in reactor, First-class reactor manhole cover, then the hydrochloric acid pump that 30Kg mass fraction is 35% is squeezed into reactor, then open steam and heat up, Temperature is 124 DEG C, and pressure is to carry out under 0.25MPa reacting 3 hours;
(4) two step reactions: after single step reaction terminates, 17Kg calcium aluminate is put into dissolution kettle, add 65Kg dissolved in purified water, In the calcium aluminate solution press-in reactor that will have dissolved, react 5 hours further at a temperature of 108 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters with oil pressure pressure 14MPa, heavy Drop 6-12 hour, the supernatant is put into thick end product pool, obtain rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 7 hours, natural sedimentation 8 hours, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally super with containing activated carbon Membrane filtration, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: be first 195 DEG C by blower fan by the heated dry air of vapor heat exchanger, inlet temperature, pass through drying tower The hot blast spiral case at top and hot-air distributor uniformly flow into hothouse, then by dry finished product polyaluminium chloride liquid by expecting Groove, sends into nebulizer by charging pump, and under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, in hothouse, and pressure Contact with hot blast for droplet under conditions of-0.65MPa, be dried to product, packaging, obtain the finished product polychlorostyrene that basicity is 69% Change aluminum solid.
Embodiment 5:
1. the preparation of modified clay mineral
First 5Kg bentonite, 4Kg Kaolin and 4Kg galapectite are pulverized, cross 20 mesh sieves, be 14% with 23Kg mass fraction Hydrogen peroxide dipping 8 days, then with the soak with hydrochloric acid that 23Kg mass fraction is 27% 4 days, be finally 4% with 32Kg mass fraction Soaking in sodium carbonate solution 8 days is also stirred continuously, and filters, and filtering residue is 7 with three distilled water washs to filtrate pH, exists at room temperature The vacuum under pressure of 0.11MPa is dried 9 hours, ground 20 mesh sieves, obtains modified clay mineral.
2. the preparation method of polyaluminium chloride, concretely comprises the following steps:
(1) bentonitic pretreatment: the acetum that 8Kg mass fraction is 7% is mixed, then with the bentonite of 7Kg It is placed on the water-bath of 65 DEG C and is heated to being dried, put into Muffle furnace 900 DEG C of roastings 0.5 hour, by the kaolinite after roasting Soil natural cooling, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;Treated bentonitic Al2O3Leaching rate be 80%;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into a formula crusher in crushing 2 hours, makes discharging Granularity, for reaching 10mm, is put into Muffle furnace and is put in cold water and cool down in 500 DEG C of roastings 0.5 hour, taking-up, further take out and dry, so After put into infrared baking oven at 50 DEG C be dried 12 hours, obtain the high alumina refining slag handled well;
(3) single step reaction: the high alumina refining slag that the bentonite handled well by 9Kg and 7Kg handle well puts in reactor, on Good reactor manhole cover, then the hydrochloric acid pump that 40Kg mass fraction is 20% is squeezed into reactor, then open steam and heat up, in temperature Degree is 132 DEG C, and pressure is to carry out under 0.3MPa reacting 2 hours;
(4) two step reactions: after single step reaction terminates, 18Kg calcium aluminate is put into dissolution kettle, add 70Kg dissolved in purified water, In the calcium aluminate solution press-in reactor that will have dissolved, react 6 hours further at a temperature of 106 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters with oil pressure pressure 15MPa, heavy Drop 9 hours, the supernatant is put into thick end product pool, obtain rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 7 hours, natural sedimentation 9 hours, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally super with containing activated carbon Membrane filtration, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: be first 205 DEG C by blower fan by the heated dry air of vapor heat exchanger, inlet temperature, pass through drying tower The hot blast spiral case at top and hot-air distributor uniformly flow into hothouse, then by dry finished product polyaluminium chloride liquid by expecting Groove, sends into nebulizer by charging pump, and under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, in hothouse, and pressure Contact with hot blast for droplet under conditions of-0.7MPa, be dried to product, packaging, obtain the finished product polychlorostyrene that basicity is 76% Change aluminum solid.
Embodiment 6:
1. the preparation of modified clay mineral
First 10Kg pyrophillite, 2Kg serpentine and 2Kg meerschaum are pulverized, cross 20 mesh sieves, be 16% with 24Kg mass fraction Hydrogen peroxide dipping 9 days, then with the soak with hydrochloric acid that 24Kg mass fraction is 28% 4 days, be finally 4.5% with 33Kg mass fraction Soaking in sodium carbonate solution 9 days and be stirred continuously, filter, filtering residue is 7.5 with three distilled water washs to filtrate pH, at room temperature Vacuum under pressure at 0.12MPa is dried 8 hours, ground 20 mesh sieves, obtains modified clay mineral.
2. the preparation method of polyaluminium chloride, concretely comprises the following steps:
(1) bentonitic pretreatment: the acetum that 9Kg mass fraction is 8% is mixed, then with the bentonite of 7Kg It is placed on the water-bath of 65 DEG C and is heated to being dried, put into Muffle furnace 700 DEG C of roastings 2 hours, by the Kaolin after roasting Natural cooling, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;Treated bentonitic Al2O3Leaching rate be 65%;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into a formula crusher in crushing 1.5 hours, uses Material granularity, for reaching 18mm, is put into Muffle furnace and is put in cold water and cool down in 450 DEG C of roastings 1.5 hours, taking-up, further take out and dry, It is then placed in infrared baking oven to be dried 12 hours at 50 DEG C, obtains the high alumina refining slag handled well;
(3) single step reaction: the high alumina refining slag that the bentonite handled well by 6Kg and 5Kg handle well puts in reactor, on Good reactor manhole cover, then the hydrochloric acid pump that 40Kg mass fraction is 35% is squeezed into reactor, then open steam and heat up, in temperature Degree is 138 DEG C, and pressure is to carry out under 0.33MPa reacting 3 hours;
(4) two step reactions: after single step reaction terminates, 19Kg calcium aluminate is put into dissolution kettle, add 80Kg dissolved in purified water, In the calcium aluminate solution press-in reactor that will have dissolved, react 6 hours further at a temperature of 104 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters with oil pressure pressure 17MPa, heavy Drop 11 hours, the supernatant is put into thick end product pool, obtain rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 8 hours, natural sedimentation 10 hours, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally with containing activated carbon Ultrafiltration membrance filter, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: be first 220 DEG C by blower fan by the heated dry air of vapor heat exchanger, inlet temperature, pass through drying tower The hot blast spiral case at top and hot-air distributor uniformly flow into hothouse, then by dry finished product polyaluminium chloride liquid by expecting Groove, sends into nebulizer by charging pump, and under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, in hothouse, and pressure Contacting with hot blast for droplet under conditions of-0.7MPa, be dried to product, packaging, obtaining basicity is that 82% finished product is polychloride Aluminum solid.
Embodiment 7:
1. the preparation of modified clay mineral
First 3Kg montmorillonite, 3Kg bentonite, 3Kg Kaolin and 3Kg galapectite are pulverized, cross 20 mesh sieves, use 25Kg mass Mark is the hydrogen peroxide dipping 9 days of 18%, then with the soak with hydrochloric acid that 25Kg mass fraction is 29% 5 days, finally uses 34Kg mass Mark is the soaking in sodium carbonate solution 9 days of 5% and is stirred continuously, and filters, and filtering residue with three distilled water washs to filtrate pH is 7.5, the vacuum under pressure at 0.14MPa is dried 7 hours at room temperature, and ground 20 mesh sieves obtain modified meerschaum.
2. the preparation method of polyaluminium chloride, concretely comprises the following steps:
(1) bentonitic pretreatment: the acetum that 10Kg mass fraction is 8% is mixed, then with the bentonite of 8Kg It is placed on the water-bath of 65 DEG C and is heated to being dried, put into Muffle furnace 800 DEG C of roastings 2 hours, by the Kaolin after roasting Natural cooling, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;Treated bentonitic Al2O3Leaching rate be 77%;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into a formula crusher in crushing 0.5 hour, uses Material granularity, for reaching 11mm, is put into Muffle furnace and is put in cold water and cool down in 300 DEG C of roastings 2 hours, taking-up, further take out and dry, so After put into infrared baking oven at 50 DEG C be dried 12 hours, obtain the high alumina refining slag handled well;
(3) single step reaction: the high alumina refining slag that the bentonite handled well by 8Kg and 4Kg handle well puts in reactor, on Good reactor manhole cover, then the hydrochloric acid pump that 50Kg mass fraction is 25% is squeezed into reactor, then open steam and heat up, in temperature Degree is 146 DEG C, and pressure is to carry out under 0.36MPa reacting 3 hours;
(4) two step reactions: after single step reaction terminates, 20Kg calcium aluminate is put into dissolution kettle, add 90Kg dissolved in purified water, In the calcium aluminate solution press-in reactor that will have dissolved, react 7 hours further at a temperature of 102 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters with oil pressure pressure 19MPa, heavy Drop 11 hours, the supernatant is put into thick end product pool, obtain rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 9 hours, natural sedimentation 11 hours, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally with containing activated carbon Ultrafiltration membrance filter, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: be first 230 DEG C by blower fan by the heated dry air of vapor heat exchanger, inlet temperature, pass through drying tower The hot blast spiral case at top and hot-air distributor uniformly flow into hothouse, then by dry finished product polyaluminium chloride liquid by expecting Groove, sends into nebulizer by charging pump, and under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, in hothouse, and pressure Contacting with hot blast for droplet under conditions of-0.75MPa, be dried to product, packaging, obtaining basicity is that 60% finished product is polychloride Aluminum solid.
Embodiment 8:
1. the preparation of modified clay mineral
First 16Kg Vermiculitum is pulverized, cross 20 mesh sieves, with the hydrogen peroxide dipping that 25Kg mass fraction is 20% 10 days, then use 25Kg mass fraction is the soak with hydrochloric acid 5 days of 30%, last 35Kg mass fraction be the soaking in sodium carbonate solution 10 days with 5% also Being stirred continuously, filter, filtering residue is 8 with three distilled water washs to filtrate pH, and the vacuum under pressure at 0.15MPa is dry at room temperature Dry 6 hours, ground 20 mesh sieves, obtain modified clay mineral.
2. the preparation method of polyaluminium chloride, concretely comprises the following steps:
(1) bentonitic pretreatment: the acetum that 10Kg mass fraction is 8% is mixed, then with the bentonite of 8Kg It is placed on the water-bath of 55 DEG C and is heated to being dried, put into Muffle furnace 900 DEG C of roastings 0.5 hour, by the kaolinite after roasting Soil natural cooling, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;Treated bentonitic Al2O3Leaching rate be 79%;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into a formula crusher in crushing 2 hours, makes discharging Granularity, for reaching 20mm, is put into Muffle furnace and is put in cold water and cool down in 500 DEG C of roastings 0.5 hour, taking-up, further take out and dry, so After put into infrared baking oven at 50 DEG C be dried 12 hours, obtain the high alumina refining slag handled well;
(3) single step reaction: the high alumina refining slag that the bentonite handled well by 10Kg and 5Kg handle well puts in reactor, First-class reactor manhole cover, then the hydrochloric acid pump that 50Kg mass fraction is 35% is squeezed into reactor, then open steam and heat up, Temperature is 158 DEG C, and pressure is to carry out under 0.4MPa reacting 4 hours;
(4) two step reactions: after single step reaction terminates, 22Kg calcium aluminate is put into dissolution kettle, add 100Kg pure water-soluble Solve, in the calcium aluminate solution press-in reactor that will have dissolved, react 7 hours further at a temperature of 100 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters with oil pressure pressure 20MPa, heavy Drop 12 hours, the supernatant is put into thick end product pool, obtain rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 10 hours, natural sedimentation 12 hours, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally with containing activated carbon Ultrafiltration membrance filter, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: be first 270 DEG C by blower fan by the heated dry air of vapor heat exchanger, inlet temperature, pass through drying tower The hot blast spiral case at top and hot-air distributor uniformly flow into hothouse, then by dry finished product polyaluminium chloride liquid by expecting Groove, sends into nebulizer by charging pump, and under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, in hothouse, and pressure Contact with hot blast for droplet under conditions of-0.8MPa, be dried to product, packaging, obtain the finished product polychlorostyrene that basicity is 77% Change aluminum solid.
Comparative example 1:
Embodiment and the mass fraction of arsenic (As) of embodiment 1-8, the matter of lead (Pb) of removing heavy metals step will not increased Amount mark, the mass fraction of cadmium (Cd), the mass fraction of hydrargyrum (Hg) and Cr VI (Cr+6) mass fraction measure, result It is shown in Table 1.
Table 1:
Table 1 result shows: the mass fraction of arsenic (As) content is arranged as from high to low: for increasing the reality of removing heavy metals step Execute example > embodiment 6 > embodiment 1=embodiment 4 > embodiment 7 > embodiment 8=embodiment 5 > embodiment 2 > embodiment 3;Lead (Pb) The mass fraction of content is arranged as from high to low: for increasing the embodiment of removing heavy metals step > embodiment 2=embodiment 5 > implement Example 7 > embodiment 8=embodiment 4 > embodiment 6 > embodiment 1 > embodiment 3;The mass fraction of cadmium (Cd) content arranges from high to low For: for increasing the embodiment of removing heavy metals step > embodiment 8 > embodiment 1 > embodiment 5 > embodiment 7 > embodiment 6 > embodiment 2 =embodiment 4 > embodiment 3;The mass fraction of arsenic content is arranged as from high to low: for increasing the embodiment of removing heavy metals step > Embodiment 6 > embodiment 1=embodiment 4 > embodiment 7 > embodiment 8=embodiment 5 > embodiment 2 > embodiment 3;Hydrargyrum (Hg) content Mass fraction be arranged as from high to low: for increase removing heavy metals step embodiment > embodiment 4 > embodiment 8 > embodiment 6 > Embodiment 7 > embodiment 1 > embodiment 2 > embodiment 3;Cr VI (Cr+6) mass fraction of content is arranged as from high to low: for increasing Add the embodiment of removing heavy metals step > embodiment 2=embodiment 7 > embodiment 1=embodiment 4=embodiment 8 > embodiment 6=is in fact Execute example 6 > embodiment 3;
A kind of better embodiment in the present invention is:
1. the preparation of modified clay mineral
First 3Kg galapectite and 10Kg pyrophillite are pulverized, cross 20 mesh sieves, with the dioxygen water logging that 20Kg mass fraction is 10% Steep 7 days, then with the soak with hydrochloric acid that 20Kg mass fraction is 23% 4 days, be finally the sodium carbonate liquor of 3% with 28Kg mass fraction Soaking 7 days and be stirred continuously, filtering, filtering residue is 7 with three distilled water washs to filtrate pH, at room temperature in the pressure of 0.08MPa It is vacuum dried 11 hours under power, ground 20 mesh sieves, obtains modified clay mineral.
2. the preparation method of polyaluminium chloride, concretely comprises the following steps:
(1) bentonitic pretreatment: the acetum that 7Kg mass fraction is 4% is mixed, then with the bentonite of 4Kg It is placed on the water-bath of 55 DEG C and is heated to being dried, put into Muffle furnace 600 DEG C of roastings 2.5 hours.By the kaolinite after roasting Soil natural cooling, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;Treated bentonitic Al2O3Leaching rate be 96%;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into a formula crusher in crushing 1.5 hours, uses Material granularity, for reaching 15mm, is put into Muffle furnace and is put in cold water and cool down in 400 DEG C of roastings 1.5 hours, taking-up, further take out and dry, It is then placed in infrared baking oven to be dried 12 hours at 50 DEG C, obtains the high alumina refining slag handled well;
(3) single step reaction: the high alumina refining slag that the bentonite handled well by 12Kg and 4Kg handle well puts in reactor, First-class reactor manhole cover, then the hydrochloric acid pump that 30Kg mass fraction is 30% is squeezed into reactor, then open steam and heat up, Temperature is 116 DEG C, and pressure is to carry out under 0.18MPa reacting 3 hours;
(4) two step reactions: after single step reaction terminates, 16Kg calcium aluminate is put into dissolution kettle, add 60Kg dissolved in purified water, In the calcium aluminate solution press-in reactor that will have dissolved, react 5 hours further at a temperature of 110 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters with oil pressure pressure 13MPa, heavy Drop 8 hours, the supernatant is put into thick end product pool, obtain rough polyaluminium chloride liquid;
(6) removing heavy metals ion: with pump, rough polyaluminium chloride liquid is transported to reaction tank, adds modified clay mineral anti- Answer 8 hours, natural sedimentation 7 hours, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally super with containing activated carbon Membrane filtration, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: be first 180 DEG C by blower fan by the heated dry air of vapor heat exchanger, inlet temperature, pass through drying tower The hot blast spiral case at top and hot-air distributor uniformly flow into hothouse, then by dry finished product polyaluminium chloride liquid by expecting Groove, sends into nebulizer by charging pump, and under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, in hothouse, and pressure Contact with hot blast for droplet under conditions of-0.6MPa, be dried to product, packaging, obtain the finished product polychlorostyrene that basicity is 95% Change aluminum solid.
Described above is the detailed description for the preferable possible embodiments of the present invention, but embodiment is not limited to this Bright patent claim, the equal change completed under the technical spirit suggested by all present invention or modification change, all should belong to In the contained the scope of the claims of the present invention.

Claims (8)

1. the method preparing polyaluminium chloride, it is characterised in that: concretely comprise the following steps:
(1) bentonitic pretreatment: the acetum that 5-10Kg mass fraction is 2-8% is mixed, so with the bentonite of 5-8Kg After be placed on the water-bath of 50-65 DEG C and be heated to being dried, put into Muffle furnace 500-900 DEG C of roasting 0.5-3 hour, will roasting Bentonite natural cooling after burning, pulverizes, and crosses 20 mesh sieves, obtains the bentonite handled well;
(2) pretreatment of high alumina refining slag: 10Kg high alumina refining slag is put into formula crusher in crushing 0.5-2 hour, makes discharging Granularity, for reaching 10-20mm, is put into Muffle furnace and is put in cold water and cool down in 300-500 DEG C of roasting 0.5-2 hour, taking-up, then take Go out to dry, be then placed in infrared baking oven and be dried 12 hours at 50 DEG C, obtain the high alumina refining slag handled well;
(3) single step reaction: the bentonite handled well and the high alumina refining slag handled well that 10-16Kg mass ratio is 1-3:1 are thrown Enter in reactor, first-class reactor manhole cover, then the hydrochloric acid pump that 30-50Kg mass fraction is 20-35% is squeezed into reactor, Then open steam to heat up, at a temperature of 100-158 DEG C, carry out reaction 2-4 hour;
(4) two step reactions: after single step reaction terminates, 14-22Kg calcium aluminate is put into dissolution kettle, add 50-100Kg pure water-soluble Solve, in the calcium aluminate solution press-in reactor that will have dissolved, react 4-7 hour further at a temperature of 100-115 DEG C;
(5) filter pressing: after two step reactions terminate, with pump, feed liquid is pressed onto pressure filter and filters, settle 6-12 hour, upper strata is clear Liquid puts into thick end product pool, obtains rough polyaluminium chloride liquid;
(6) removing heavy metals ion: rough polyaluminium chloride liquid is transported to reaction tank with pump, adds modified clay mineral reaction 5- 10 hours, natural sedimentation 6-12 hour, then with pump, supernatant liquid is pressed onto pressure filter and filters, finally with containing activated carbon Ultrafiltration membrance filter, obtains finished product polyaluminium chloride liquid;
(7) it is spray-dried: first by blower fan by the heated dry air of vapor heat exchanger, by hot blast spiral case and the hot blast at drying tower top Allotter uniformly flows into hothouse, then by dry finished product polyaluminium chloride liquid by hopper, sends into atomization by charging pump Device, under the effect of atomizing disk centrifugal force, material dispersion becomes droplet, and in hothouse, droplet contacts with hot blast, is dried to produce Product, packaging, obtain finished product polyaluminium chloride solid.
A kind of method preparing polyaluminium chloride the most according to claim 1, it is characterised in that: the aluminum described in step (4) Alumina content >=55% of acid calcium, the pressure of reactor is 0.15-0.40MPa.
A kind of method preparing polyaluminium chloride the most according to claim 1, it is characterised in that: the material described in step (5) Liquid turbidity is that < 200NTU, pressure filter oil pressure pressure is 10-20MPa.
A kind of method preparing polyaluminium chloride the most according to claim 1, it is characterised in that changing described in step (6) Property clay mineral preparation method be: first the clay mineral of 10-16Kg is pulverized, crosses 20 mesh sieves, with 15-25Kg mass fraction be The hydrogen peroxide dipping of 6-20% 5-10 days, then with the soak with hydrochloric acid that 15-25Kg mass fraction is 20-30% 3-5 days, finally use 25-30Kg mass fraction is soaking in sodium carbonate solution 5-10 days of 2-5% and is stirred continuously, and filters, and filtering residue is with No. three distilled water Washing is 5-8 to filtrate pH, and the vacuum under pressure at 0.05-0.15MPa is dried 6-12 hour at room temperature, ground 20 mesh Sieve, obtains modified clay mineral.
A kind of method preparing polyaluminium chloride the most according to claim 1, it is characterised in that: described clay mineral is for covering One or more in de-soil, bentonite, Kaolin, galapectite, serpentine, pyrophillite, illite, Vermiculitum and meerschaum.
A kind of method preparing polyaluminium chloride the most according to claim 1, it is characterised in that: step (7) is at negative pressure bar Carrying out under part, pressure is negative 0.5-0.8MPa, alumina content >=28%.
A kind of method preparing polyaluminium chloride the most according to claim 1, it is characterised in that: drying tower in step (7) Inlet temperature is 150-270 DEG C.
8. according to the method for a kind of polyaluminium chloride described in claim 1-7 any one, it is characterised in that: the salt of polyaluminium chloride Base degree is 60-95%.
CN201610591956.2A 2016-07-26 2016-07-26 Method for preparing polyaluminum chloride Pending CN105967298A (en)

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CN107915245A (en) * 2017-12-12 2018-04-17 青岛市昌斯达环保科技有限公司 A kind of production method and technique of high-performance polyaluminium chloride
CN108002416A (en) * 2017-11-27 2018-05-08 沈阳东大东科干燥煅烧工程技术有限公司 A kind of drying and calcining processing technology and equipment for crystallizing Aluminum Chloride Hexahydrate
CN115125446A (en) * 2022-06-28 2022-09-30 浙江伊思灵双第弹簧有限公司 High-fatigue-performance spring for automobile and preparation method thereof

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Application publication date: 20160928