CN104556182A - Method for preparing solid high-efficiency flocculant polyaluminum chloride from fly ash - Google Patents

Method for preparing solid high-efficiency flocculant polyaluminum chloride from fly ash Download PDF

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CN104556182A
CN104556182A CN201510026731.8A CN201510026731A CN104556182A CN 104556182 A CN104556182 A CN 104556182A CN 201510026731 A CN201510026731 A CN 201510026731A CN 104556182 A CN104556182 A CN 104556182A
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solid
flyash
reaction
product
fly ash
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CN104556182B (en
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王晖
温龙英
孙忠
红艳
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Inner Mongolia University
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Inner Mongolia University
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Abstract

The invention discloses a method for preparing a solid high-efficiency flocculant polyaluminum chloride from fly ash. According to the method, by using the fly ash as the raw material, an intermediate product alpha-Al(OH)3 is adopted to prepare the solid high-efficiency flocculant polyaluminum chloride 13 [Al13(OH)24(H2O)24Cl15.13H2O] (P-Al13 for short) crystal. The method comprises the following steps: reacting an aluminiferous solution, which is prepared by carrying out acid dipping on clinker prepared by carrying out high-temperature solid-phase reaction on sodium carbonate and fly ash, with sodium hydroxide to obtain the alpha-Al(OH)3 intermediate product, carrying out hydrolysis-polymerization reaction with hydrochloric acid under the conditions of high temperature and normal pressure until a certain degree of alkalization, naturally crystallizing to precipitate the P-Al13 solid product, and merging the residual mother solution with the acid dipping solution to implement reutilization, thereby achieving the goal of zero discharge of aluminum ions. The flocculation test indicates that the method has the advantages of low loss rate of aluminum ions and high conversion rate of P-Al13; the obtained solid product P-Al13 has obviously better flocculation effects than Keggin-Al13([AlO4Al12(OH)24(H2O)12]7+); and the solid high-efficiency flocculant polyaluminum chloride conforms to the specifications for premium grades in national standard (GB15892-2009).

Description

A kind of method taking flyash as raw material and develop solid-state efficient flocculant aluminium polychloride
Technical field
The present invention relates to total utilization of PCA and solid-state High-purity Polyaluminum Chloride preparation method, refer in particular to a kind of method taking flyash as raw material and develop solid-state efficient flocculant aluminium polychloride.
Background technology
Flyash is the complicated multiphase solid refuse that left behind after coal burns in burning boiler.The dominant phase composition of flyash is mullite, and primary chemical composition is SiO 2, Al 2o 3.At present, many domestic and international experts and scholars are engaged in the comprehensive development and utilization of flyash, achieve flyash and are widely used in the fields such as construction material, agricultural (plantation) cultivation, concrete construction, chemical; Also good economic benefit, environmental benefit and social benefit is created while turning waste into wealth.Taking flyash as the process that raw material prepares that efficient flocculant realizes sewage, waste water, is one of method of flyash high value added utilization.At present, realization to have with flyash be that raw material prepares alumina silicate flocculant, silicate aluminium ferric flocculating agent, aluminium iron polychloride floculant.And utilize coal ash for manufacturing for being considered to the most effective flocculation morphology in polymeric aluminum, there is the Al of superior water purification performance 13but report is had no.
Al 13because of its nano molecular size and high electric charge, be considered to nanometer species minimum and the most stable in polymeric aluminum chlorides solution.But domestic and international each technical field attempts various synthesis preparation method so far, the high concentration with industrial application value all cannot be obtained, high Al 13the polymeric aluminum solution of content and rafifinal 13 solid product.
Within 2006, Sun Zhong is in Chinese J.Struct.Chem.25 (10): 1217-1227 reports and Keggin-Al 13there is same polymeric degree, composition, the P-Al that structure is different 13(Al 13(OH) 24(H 2o) 24cl 1513H 2o), its polycation is with 15 positive charges, and number of patent application 200510064782.6 discloses under 200 DEG C of autoclave conditions, with aluminium hydroxide, crystal aluminum chloride, water for raw material obtains high-purity P-Al 13method, and prove P-Al 13all show under different pH value and compared Keggin-Al 13better go turbid ability, wider effective flocculation adds the water pH value of scope and adaptation.Show thus, P-Al 13be a kind of superior performance, rising efficient flocculant, to exploitation Huanghe water, processes various waste water, saves groundwater resources significant.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method taking flyash as raw material and develop solid-state efficient flocculant aluminium polychloride, and this method take flyash as raw material, by intermediate product α-Al (OH) 3the solid-state efficient flocculant P-Al that development high-purity, the flocculating property that form is single are superior 13.
For solving the problems of the technologies described above, the present invention proposes following scheme: a kind of method taking flyash as raw material and develop solid-state efficient flocculant aluminium polychloride, it is characterized in that, take flyash as raw material, by intermediate product α-Al (OH) 3development Al 13(OH) 24(H 2o) 24cl 1513H 2(P-Al is counted in letter to O 13), comprise following five steps:
1. high-temperature fusion reaction: by flyash and sodium carbonate by 0.8 ~ 2.0: 1 quality mix than porphyrize, calcination 30 ~ 150min at 750 ~ 950 DEG C in Muffle furnace, after clinker cooling to room temperature abundant grind for subsequent use;
2. acid-leaching reaction: in above-mentioned grog, adds the hydrochloric acid of 3 ~ 12mol/L, and every gram of grog correspondence adds the hydrochloric acid of 4 ~ 20mL volume, after fully stirring, filters and obtain pickle liquor after room temperature leaves standstill 5 ~ 30min;
3. α-Al (OH) 3preparation: get above-mentioned pickle liquor, under 70 DEG C ~ 90 DEG C conditions, drip concentration be greater than the sodium hydroxide solution of 4mol/L to pH=7.5 ~ 8.5, be precipitated, filter filter cake is α-Al (OH) 3, repeatedly wash and after drying porphyrize for subsequent use;
4. P-Al 13preparation: by α-Al (OH) 3under reflux conditions with 8 ~ 12mol/L hydrochloric acid reaction, reaction temperature is at 110 ~ 120 DEG C, condition of normal pressure issues unboiled water solution-polymerisation 6 ~ 10 hours, obtain storing solution, its hydroxide aluminium ratio basicity is made to be 0.4 ~ 1.3, after filtering while hot, filtrate moves into crystallizer, evaporative crystallization at room temperature ~ 50 DEG C, waits to separate out Al 13(OH) 24(H 2o) 24cl 1513H 2be separated after O crystal or powder, solid product, through washing, dries product at room temperature ~ 50 DEG C, obtained solid-state efficient flocculant Al 13(OH) 24(H 2o) 24cl 1513H 2o, filtrate reusable edible;
5. mother liquid recycling: the mother liquor that 4. walk gained is all incorporated to and 2. walks in the pickle liquor of gained and recycle, the object of aluminium ion maximize conversion, zero-emission can be realized.
The experimental principle of this method:
1, solid phase fusion reaction:
The principal crystalline phase material of flyash is mullite, and amorphous phase material is alumina silicate glass body.Mullite is insoluble to acid at normal temperatures, is also insoluble to alkali.But under heating condition, can react with alkaline matter.This experiment take sodium carbonate as flux, and under the high temperature conditions, flyash and sodium carbonate react, and generates nepheline.
Al 6Si 2O 13+Na 2CO 3＝2NaAlSiO 4+2Al 2O 3+CO 2
Meanwhile, the Al of reaction generation 2o 3with the magma cell in flyash also can and Na 2cO 3react:
Al 2O 3+2SiO 2+Na 2CO 3＝2NaAlSiO 4+CO 2
2, acid-leaching reaction:
Nepheline is acid soluble material, can be decomposed generate silica gel and Al by acid 3+; Realize effective separation of sial.
NaAlSiO 4+4H +＝Al 3++Na ++H 2O+H 2SiO 3
3, α-Al (OH) 3preparation: sodium hydroxide solution and liquor alumini chloridi react the aluminium hydroxide that can obtain variform, but by control temperature and pH, can obtain α-Al (OH) 3single form.
4, P-Al 13preparation:
By α-Al (OH) 3determining to be hydrolyzed with hydrochloric acid at temperature-and polymerisation reach certain basicity, just obtain in solution comprising P-Al 13in interior various polymeric aluminum forms, after reaching corresponding saturation degree, P-Al 13hydrochloride can natural crystallization.
5, Recycling Mother Solution:
Due to preparation P-Al 13reaction do not introduce other ion any, so residue mother liquor can merge with pickle liquor and recycles, reach the object of zero-emission.
High-temperature fusion reaction described in this method refers to: the high temperature solid-phase sintering method adopting sodium carbonate and flyash, is intended to the dominant phase mullite in flyash, at high temperature reacts the nepheline grog generating and be soluble in acid with sodium carbonate; Acid-leaching reaction refers to: by the acid dip of above-mentioned grog salt, Silicified breccias is effectively separated, and obtaining take iron ion as the liquor alumini chloridi of major impurity ion; α-Al (OH) 3preparation refer to: by pickle liquor, under constant temperature with NaOH regulate pH with obtained α-Al (OH) 3; P-Al 13preparation refer to: with α-Al (OH) 3for raw material be hydrolyzed with hydrochloric acid under high-temperature pressure condition-polymerisation obtains storing solution, left at room temperature, P-Al 13hydrochloride, by nature crystallization, obtains product after filtration; Mother liquid recycling refers to: by P-Al 13preparation process in the mother liquor of gained be all incorporated in the pickle liquor of acid-leaching reaction gained and recycle, the object of aluminium ion maximize conversion, zero-emission can be realized.
The mass ratio of the flyash described in this method and sodium carbonate, and dominant phase mullite and sodium carbonate complete reaction in flyash are guaranteed in the determination of calcining heat and time, and not cause premised on energy waste.
The sour consumption of the hydrochloric acid leaching grog described in this method is that, loss late maximum according to the leaching rate of aluminium in flyash is minimised as according to drawing; The recyclable recycling of excessive hydrochloric acid.
α-Al (OH) described in this method 3preparation temperature be 70 ~ 90 DEG C, adjust ph is 7.5 ~ 8.5.
α-Al (OH) described in this method 3not necessarily require it is freshly prepd compound.
Described in this method with α-Al (OH) 3for raw material is in 110 ~ 120 DEG C of temperature ranges, is hydrolyzed-polymerisation 6 ~ 10 hours under condition of normal pressure with hydrochloric acid, obtains storing solution.
α-Al (OH) described in this method 3the storing solution basicity (hydroxide aluminium ratio) ensureing end reaction with the used in amounts of hydrochloric acid is 0.4 ~ 1.3.
Gained α-Al (OH) described in this method 3al species to can be implemented under condition of normal pressure with hydrochloric acid reaction and reaches preparation P-Al 13basicity.
α-Al (OH) described in this method 3with the reactant liquor of hydrochloric acid, naturally P-Al can be separated out at ambient temperature 13crystallization, directly obtains solid-state efficient flocculant after filtration, without the need to other solidification equipment any and technique.
Preparation P-Al described in this method 13required raw material is only α-Al (OH) 3and hydrochloric acid, do not need other any catalyst or reagent, namely in preparation process, do not introduce other any foreign ion except Al (III).
P-Al described in this method 13residue mother liquor reusable edible after hydrochloride crystallization, is at the bottom of a kind of aluminium ion loss late, conversion ratio is high, the preparation P-Al of zero-emission 13method.Advantage of the present invention:
The present invention has following outstanding advantage:
1, flyash is converted into solid-state efficient flocculant by this method, provides a kind of approach realizing the comprehensive utilization of flyash high added value.
2, this method is easy to operation, affecting parameters is few, product quality is secure.
3, this method has been sought a kind of passing through and has been regulated temperature, pH value, prepares α-Al (OH) fast 3method.
4, this method to can be implemented under condition of normal pressure with aluminium hydroxide is that P-Al prepared by raw material 13.
5, this method makes P-Al by adjusted saturation degree 13nature crystallization, obtains solid-state efficient flocculant, without the need to other solidification equipment any and technique.
6, this method prepares P-Al 13other any foreign ion except Al (III) is not introduced in process.
7, its composition P-Al that effectively flocculates of this method products therefrom 13content is up to more than 93%, and excellent aqueous solubility, does not have water-insoluble, and products therefrom meets national standard (GB15892-2009) high-class product specification.
8, this method is at the bottom of a kind of aluminium ion loss late, conversion ratio is high, the preparation P-Al of zero-emission 13method.
9, products obtained therefrom P-Al of the present invention 13flocculating effect is better than Keggin-Al 13([AlO 4al 12(OH) 24(H 2o) 12] 7+).Contrast experiment is as shown in table 1.From table, P-Al prepared by the present invention 13with Keggin-Al 13compare, no matter high concentrtion stablizes water sample and the astable water sample of low turbidity, all show and compare Keggin-Al 13superior flocculating effect.
Table 1, P-Al 13with Keggin-Al 13 aflocculating experiment bresult
Annotation a: Keggin-Al 13preparation adopts slowly drips alkaline process: under constant temperature oil bath 80 DEG C, strong magnetic agitation condition, to AlCl 3slowly drip NaOH solution in solution, rate of addition controls at about 0.6mL/min.Be cooled to room temperature after dropwising, slaking certain hour must contain Keggin-Al 13polymerization PAC solution, Al bcontent about 80%, 27al-NMR characterizes proves that it is mainly Keggin-Al 13.Annotation b: flocculating experiment adopts chamber test method: instrument adopts JJ-4 type six electric mixer, 500mL simulated water sample is injected beaker, start and stir, in water sample, a certain amount of flocculant is dropped under rapid stirring (rotating speed is 200r/min), change at a slow speed (rotating speed is 40r/min) into after continuing rapid stirring 1min and stir 15min, stop stirring and standing sedimentation 15min.Precipitation terminates to draw primary water sample liquid from 1cm under liquid level, adopts 2100N type transmissometer to detect its residual turbidity.)
Accompanying drawing explanation
Fig. 1 is process chart.
Fig. 2 is intermediate product α-Al (OH) 3xRD collection of illustrative plates.
Fig. 3 is for separating out P-Al for the first time 13the XRD collection of illustrative plates of product.
Fig. 4 is for separating out P-Al for the second time 13the XRD collection of illustrative plates of product.
Fig. 5 is for separating out P-Al for the third time 13the XRD collection of illustrative plates of product.
Fig. 6 separates out P-Al the 4th time 13the XRD collection of illustrative plates of product.
Detailed description of the invention
The present invention will be further described by the following examples, but the scope of protection of present invention not scope of protecting in embodiment of limitation.
1, high-temperature fusion reaction: the flyash of Huhehaote power plant and sodium carbonate are pressed the mass ratio of 1.2: 1, mixes the two porphyrize in mortar, 870 DEG C of calcination 80min in Muffle furnace.After clinker cooling to room temperature, fully grinding is for subsequent use.(flyash Al 2o 3content is 49.2%)
2, acid-leaching reaction: get above-mentioned grog 75.2g in beaker, add 380mL concentrated hydrochloric acid and 20mL distilled water, after fully stirring, room temperature leaves standstill 5min, filters and obtains pickle liquor.
3, α-Al (OH) 3preparation: get above-mentioned pickle liquor, drip under 70 DEG C of conditions concentration be the sodium hydroxide solution of 8mol/L to pH=8, be precipitated, filter filter cake is α-Al (OH) 3, repeatedly wash and after drying porphyrize for subsequent use.The XRD characterization result of product is shown in accompanying drawing 2.
4, P-Al 13preparation: (1) gets 43g α-Al (OH) 3in 500mL there-necked flask, under reflux conditions add 74mL concentrated hydrochloric acid and 15mL distilled water, after reacting 30min under room temperature condition, be warming up to 120 DEG C and continue reaction, stop reaction after coreaction 6h, filter while hot and obtain storing solution, its basicity (hydroxide aluminium ratio) is 1.2, move into crystallizer and in room temperature condition spontaneous nucleation, wait to separate out Al 13(OH) 24(H 2o) 24cl 1513H 2o (P-Al 13) be separated after crystal.Product ethanol washs, and preserves in the air-dry rear weighing of room temperature.
Sample analysis result: solid product gross mass: 13.51g, wherein P-Al 13mass content is 94.2%, aluminium ion conversion ratio: 16.28%.Residue mother liquor 140.48g.The XRD characterization result of product is shown in accompanying drawing 3.
(2) the residue mother liquor of (1) is incorporated to the pickle liquor of second step, under 70 DEG C of conditions, drips NaOH to pH=8, again obtain α-Al (OH) 3solid, gets the α-Al (OH) of 43g 3repeat (1) step experimental procedure, again obtain P-Al 13crystallization.
Sample analysis result: solid product gross mass: 13.49g, wherein P-Al 13mass content is 93.5%, is: 28.58% with the worthwhile total aluminium ion conversion ratio of first set reaction.The XRD characterization result of residue mother liquor 140.50g product is shown in accompanying drawing 4.
(3) the residue mother liquor of (2) is incorporated to the pickle liquor of second step, under 70 DEG C of conditions, drips NaOH to pH=8, again obtain α-Al (OH) 3solid, gets the α-Al (OH) of 43g 3again repeat (1) step experimental procedure, again obtain P-Al 13crystallization.
Sample analysis result: solid product gross mass: 13.52g, wherein P-Al 13mass content is 95.7%, is: 34.44% with the worthwhile total aluminium ion conversion ratio of front two secondary response.Residue mother liquor 140.48g.The XRD characterization result of product is shown in accompanying drawing 5.
(4) the residue mother liquor of (3) is incorporated to the pickle liquor of second step, under 70 DEG C of conditions, drips NaOH to pH=8, again obtain α-Al (OH) 3solid, gets the α-Al (OH) of 43g 3again repeat (1) step experimental procedure, again obtain P-Al 13crystallization.
Sample analysis result: solid product gross mass: 13.53g, wherein P-Al 13mass content is 94.1%, is: 40.12% with the worthwhile total aluminium ion conversion ratio of front third-order reaction.Residue mother liquor 140.47g.
Aluminium ion conversion ratio according to front four experiments can go out by theory calculate: after the 5th mother liquid recycling, aluminium ion conversion ratio can reach: 48.07%; The aluminium ion conversion ratio of the 6th mother liquid recycling is: 50.96%.Namely Recycling Mother Solution number of times is more, and aluminium ion conversion ratio is higher, finally can realize aluminum ions zero-emission.

Claims (1)

1. taking flyash as the method that solid-state efficient flocculant aluminium polychloride developed by raw material, it is characterized in that, take flyash as raw material, by intermediate product α-Al (OH) 3development Al 13(OH) 24(H 2o) 24cl 1513H 2(P-Al is counted in letter to O 13), comprise following five steps:
1. high-temperature fusion reaction: by flyash and sodium carbonate by 0.8 ~ 2.0: 1 quality mix than porphyrize, calcination 30 ~ 150min at 750 ~ 950 DEG C in Muffle furnace, after clinker cooling to room temperature abundant grind for subsequent use;
2. acid-leaching reaction: in above-mentioned grog, adds the hydrochloric acid of 3 ~ 12mol/L, and every gram of grog correspondence adds the hydrochloric acid of 4 ~ 20mL volume, after fully stirring, filters and obtain pickle liquor after room temperature leaves standstill 5 ~ 30min;
3. α-Al (OH) 3preparation: get above-mentioned pickle liquor, under 70 DEG C ~ 90 DEG C conditions, drip concentration be greater than the sodium hydroxide solution of 4mol/L to pH=7.5 ~ 8.5, be precipitated, filter filter cake is α-Al (OH) 3, repeatedly wash and after drying porphyrize for subsequent use;
4. P-Al 13preparation: by α-Al (OH) 3under reflux conditions with 8 ~ 12mol/L hydrochloric acid reaction, reaction temperature is at 110 ~ 120 DEG C, condition of normal pressure issues unboiled water solution-polymerisation 6 ~ 10 hours, obtain storing solution, its basicity (hydroxide aluminium ratio) is made to be 0.4 ~ 1.3, after filtering while hot, filtrate moves into crystallizer, evaporative crystallization at room temperature ~ 50 DEG C, waits to separate out Al 13(OH) 24(H 2o) 24cl 1513H 2be separated after O crystal or powder, solid product, through washing, dries product at room temperature ~ 50 DEG C, obtained solid-state efficient flocculant Al 13(OH) 24(H 2o) 24cl 1513H 2o, filtrate reusable edible;
5. mother liquid recycling: the mother liquor that 4. walk gained is all incorporated to and 2. walks in the pickle liquor of gained and recycle.
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CN109778303A (en) * 2019-02-27 2019-05-21 内蒙古大学 A method of preparing Keggin polycation chloride crystals
US10519560B2 (en) 2017-05-05 2019-12-31 Hamilton Sundstrand Corporation Process for making uniform aluminum oxide coating
CN112028099A (en) * 2020-08-20 2020-12-04 楚祯劼 Clean production process for preparing polyaluminum chloride from fly ash
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CN115504555A (en) * 2022-09-27 2022-12-23 齐鲁工业大学 Coal gasification slag-based composite ferric aluminum silicate flocculant and preparation method and application thereof

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US10519560B2 (en) 2017-05-05 2019-12-31 Hamilton Sundstrand Corporation Process for making uniform aluminum oxide coating
CN107021765A (en) * 2017-05-25 2017-08-08 中国科学院过程工程研究所 A kind of method that utilization aluminous fly-ash prepares the coproducing polymerized aluminium chloride of mullite
CN109778303A (en) * 2019-02-27 2019-05-21 内蒙古大学 A method of preparing Keggin polycation chloride crystals
CN109734167A (en) * 2019-03-08 2019-05-10 宁夏水投清水源水处理科技有限公司 A kind of preparation process of the efficient polymeric aluminum chloride for wastewater treatment
CN112028099A (en) * 2020-08-20 2020-12-04 楚祯劼 Clean production process for preparing polyaluminum chloride from fly ash
CN112174279A (en) * 2020-11-13 2021-01-05 陕西科技大学 Polymeric aluminosilicate inorganic flocculant and preparation method and application thereof
CN112174279B (en) * 2020-11-13 2022-08-02 陕西科技大学 Polymeric aluminosilicate inorganic flocculant and preparation method and application thereof
CN115504555A (en) * 2022-09-27 2022-12-23 齐鲁工业大学 Coal gasification slag-based composite ferric aluminum silicate flocculant and preparation method and application thereof
CN115504555B (en) * 2022-09-27 2023-09-26 齐鲁工业大学 Coal gas slag-based composite ferric aluminum silicate flocculant and preparation method and application thereof

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