CN101602517A - A kind for the treatment of agent for molten polyaluminium ferric chloride and preparation method thereof - Google Patents

A kind for the treatment of agent for molten polyaluminium ferric chloride and preparation method thereof Download PDF

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CN101602517A
CN101602517A CNA2009101086390A CN200910108639A CN101602517A CN 101602517 A CN101602517 A CN 101602517A CN A2009101086390 A CNA2009101086390 A CN A2009101086390A CN 200910108639 A CN200910108639 A CN 200910108639A CN 101602517 A CN101602517 A CN 101602517A
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molten
ferric chloride
iron
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chloride
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CN101602517B (en
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王龙庆
李凯
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Shenzhen Zhongrun Industry Technology Development Co Ltd
Dongguan Huaqing Water Purification Technology Co Ltd
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Shenzhen Zhongrun Industry Technology Development Co Ltd
Dongguan Huaqing Water Purification Technology Co Ltd
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Abstract

The invention discloses a kind for the treatment of agent for molten polyaluminium ferric chloride and production method thereof with stable high Fe content, utilize the heat release of hydrochloric acid and calcium aluminate to carry out autothermal reaction, add ferric chloride Solution then and be respectively applied for additional source of iron and make high Fe content poly aluminium chloride iron stablize, be easy to separate with the hydration magnesium basic carbonate, reactant obtains stablizing high Fe content poly aluminium chloride iron after filtration.This method cost is low, consumption of natural resource and the energy is few, pollution-free, can obtain good purifying water effect with less consumption.

Description

A kind for the treatment of agent for molten polyaluminium ferric chloride and preparation method thereof
Technical field
The invention belongs to domain of inorganic chemistry, specifically, relate to a kind for the treatment of agent for molten polyaluminium ferric chloride that is used for water treatment, the invention still further relates to its preparation method.
Background technology
The coagulating sedimentation processing that water is carried out in dosing is one of topmost method of water treatment.Water treatment agent mainly contains aluminium salt and molysite two classes.With the poly aluminium chloride be the aluminium brine treatment agent of representative have purify water, low-consuming, advantage such as cohesion is fast, but also have shortcoming such as the light and moisture percentage in sewage sludge height of flco.The molysite water conditioner that with iron(ic) chloride is representative has advantages such as flco is heavy, moisture percentage in sewage sludge is low, but also has shortcomings such as product corrodibility is strong, the jaundice of purifying waste water.Ferruginous poly aluminium chloride water conditioner---poly aluminium chloride iron (PAFC) then has the advantage of two class water conditioners concurrently, have purify water, low-consuming, characteristics such as moisture percentage in sewage sludge is low, raw material sources are wide, be particularly suitable for various wastewater treatments and water supply purification.
Yet because very easily hydrolysis of molysite, PAFC is extremely unstable in production and storage process, brings very big difficulty for production and use, and is more obvious when iron level is higher especially.And if iron level is lower, then can not give full play to the performance of molysite water conditioner, the advantage of PAFC product is also not obvious.
In addition, also there are problems in existing P AFC production technology, mainly comprises:
1, product aluminium, iron effective component content are low (following all by Al 2O 310% liquid PAFC comes comparison).For example, the product index for preparing of the production method of the disclosed aluminium iron polychloride of Chinese patent CN101215032A is Al 2O 3〉=3.22%, well below the Al of GB GB15892-2003 requirement 2O 3〉=10% standard, Fe 2O 3Be for 〉=1.10% (being equivalent to Fe 〉=0.77%); In the feed liquid according to the preparation of Chinese patent CN101172684A disclosed method, Fe 2O 3〉=1.0% (being equivalent to Fe 〉=0.70%).And among the Chinese patent CN101058452A: Fe only is 0.33%.
2, the production cycle is long, efficient is low.For example, in the method for the disclosed synthesized polymer aluminium chloride ferrum of Chinese patent CN101058452A, only the reaction times is just more than 20 hours; The reaction times is more than 4-5 hour in the production method of the disclosed aluminium iron polychloride of CN101215032A; Among the preparation method of the polymorphic aluminium iron polychloride of the disclosed coagulating agent of CN1539753A, about 4-6 of reaction times hour; Among the preparation method of the disclosed aluminum chlorate of polymerized silicic acid of CN1519852A, the reaction times is more than 3 hours.
Add a large amount of basic cpds when 3, adjusting basicity, cause that cost significantly rises, harmful salt increases, consumes a large amount of raw material hydrochloric acid, and do not increase many-sided disadvantageous effect such as effective ingredient.For example, add NaoH, KoH, CaO, Na in the production method of the disclosed aluminium iron polychloride of CN101215032A 2CO 3Or NaHCO 3Deng; Add NaoH, Ca (OH) in the production method of the disclosed aluminum chlorate of polymerized silicic acid of CN101172684A 2, Na 2CO 3Or NH 4OH etc.; CN1544349A is disclosed to be prepared with wastewater from phthalocyanine green production in the method for aluminium iron polychloride floculant with NaOH or Ca (OH) 2As basifier.
4, energy expenditure height.The production method of prior art all need be used steam heating and a large amount of power power consumptions usually.
5, insoluble object height increases the labour intensity that uses.
Therefore, develop that a kind of cost is low, efficient is high, power consumption less and the more excellent PAFC water conditioner of product performance significant.
Summary of the invention
An object of the present invention is deficiency, a kind for the treatment of agent for molten polyaluminium ferric chloride with stable high Fe content is provided at existing PAFC production technology.
Another object of the present invention is to provide the method for producing this stable high Fe content treating agent for molten polyaluminium ferric chloride.This method technology is simple, with short production cycle, efficient is high, consume resource and the energy few, the PAFC product effective ingredient aluminium of acquisition, iron level are all higher, and shelf-stable, product purifies water more excellent.
According to an aspect of the present invention, treating agent for molten polyaluminium ferric chloride, it contains Al 2O 3Massfraction be 10-14%; With Al 2O 310% content meter, Fe 2O 3Massfraction is 1.7-3.6% (massfraction that is equivalent to Fe is 1.2-2.5%), insolubles≤0.05% weight.Contain the hydration magnesium basic carbonate in the treating agent for molten polyaluminium ferric chloride of the present invention, can stablize to place and never degenerate more than 1 year.
Treating agent for molten polyaluminium ferric chloride of the present invention mainly is with technical hydrochloric acid and calcium aluminate (CaOAl 2O 3) be raw material, replenish source of iron with iron(ic) chloride, be stablizer with the hydration magnesium basic carbonate, generate fast and stablize high Fe content poly aluminium chloride iron (PAFC).Specifically, may further comprise the steps:
1) with 10 weight part massfractions be the calcium aluminate reaction of 20% hydrochloric acid and 4 weight parts, temperature of reaction 80-110 ℃, reaction times 0.3-1 hour;
2) adding 1.5-4 weight part massfraction in the reaction solution of step 1) is 40% iron(ic) chloride, the hydration magnesium basic carbonate of 0.08-0.16 weight part and the water of 3.5-4.5 weight part, continues reaction 0.3-1 hour;
3) collection step 2) reaction product that obtains obtains described treating agent for molten polyaluminium ferric chloride.
Wherein, step 1 is a step of reaction, utilizes reaction to generate heat and impels reaction to continue to carry out, and temperature of reaction is maintained at about 80-110 ℃; What specify is that calcium aluminate is also adjusted agent as basicity except that as the reaction raw materials, can play basification and effective ingredient Al simultaneously 2O 3Dual-use function, and do not produce deleterious sodium salt and ammonia salt, only contain a spot of calcium chloride;
Step 2 is the adjusting stage, wherein ferric chloride Solution is used for replenishing the iron components contents, the hydration magnesium basic carbonate is as stablizer, be used for making the iron component to be present in poly aluminium chloride solution in a large number and stably, the basicity of calcium aluminate performance is simultaneously adjusted the effect of agent, generates the poly aluminium chloride iron of high Fe content;
The treatment stage that step 3 being, reacting liquid filtering is obtained the transparent filtrate of brown, the treating agent for molten polyaluminium ferric chloride with stable high Fe content promptly of the present invention.
The treating agent for molten polyaluminium ferric chloride that aforesaid method makes according to the present invention has following character: Al 2O 3Massfraction be 10-14%; With Al 2O 310% content meter, Fe 2O 3Massfraction is 1.7-3.6% (massfraction that is equivalent to Fe is 1.2-2.5%), and insolubles≤0.05% can be stablized to place and never degenerate more than 1 year.
The advantage that the present invention compared with prior art has is:
1) technology is simple, and is with short production cycle, efficient is high.Whole process of production only needs about 1-2 hour, and reaction do not have waste gas and waste water generation substantially, and solid slag is few, can realize that product produces fast, raising equipment service efficiency, and help protecting environment.
2) save the energy and equipment, production cost is low.Production process of the present invention effectively utilizes the reaction liberated heat, does not need to provide in addition heat energy, and save energy has been saved steam and boiler plant that traditional processing technology is used to heat; Avoid using the various basic cpds that add in the traditional technology in addition, further reduced production cost.
3) product effective ingredient aluminium, iron level height, impurity is few.Each effective constituent of product of the present invention all reaches or is higher than the content of standard index or prior art products, iron level especially, even be higher than the PAFC product iron content (Fe of prior art 2O 3≤ 1.5%) more than one times; And product does not contain sodium salt and ammonium salt impurity, insolubles can reach≤and 0.05% high level, CaCl 2Content is lower than general commercially available prod.
4) product stability is good, and purifying water effect is good.Product of the present invention can be placed more than 1 year and to keep stable and never degenerate, 6 months the standard that requires considerably beyond GB GB15892-2003, and the equivalent dosage during water treatment is lower than existing commercially available prod, and purifying water effect is better.
Brief Description Of Drawings
Fig. 1 has the process flow sheet of the treating agent for molten polyaluminium ferric chloride of stable high Fe content for the embodiment of the invention 1 preparation.
Embodiment
The invention will be further described by following examples, but do not limit the present invention.
Embodiment 1 stablizes the preparation of high Fe content poly aluminium chloride iron
In the 3000L glassed steel reaction vessels, add 20% industrial synthesis hydrochloric acid 1860kg, add calcium aluminate powder (CaOAl successively 2O 3, Al 2O 3Content: 53%, Fe content: 750kg 1.75%), temperature of reaction is remained between 80-110 ℃ by exothermic heat of reaction, stirring reaction 30min, ferric chloride in aqueous solution 460kg, hydration magnesium basic carbonate (MgO:41%) 22kg of adding 40% in reactant, continue reaction 30min, in this reactant, add water to cumulative volume then and be about 3000L.Reaction solution filters with chamber-type press filter, and about 30min filters and finishes, and adds suitable quantity of water washing filter residue, obtains transparent PAFC solution product 3850kg, and its composition is as shown in table 1.This liquid product can be stored in the acid-resistant container.
Embodiment 2 stablizes the preparation of high Fe content poly aluminium chloride iron
In the 3000L glassed steel reaction vessels, add 20% industrial synthesis hydrochloric acid 1860kg, add calcium aluminate powder 750kg successively, temperature of reaction is remained between 80-110 ℃ by exothermic heat of reaction, stirring reaction 25min, ferric chloride in aqueous solution 280kg, the hydration magnesium basic carbonate 22kg of adding 40% in reactant, continue reaction 20min, in this reactant, add water to cumulative volume then and be about 2900L.Reaction solution filters with chamber-type press filter, and about 30min filters and finishes, and adds suitable quantity of water washing filter residue, obtains transparent PAFC solution product 3630kg, and its composition is as shown in table 1.
Embodiment 3 stablizes the preparation of high Fe content poly aluminium chloride iron
In the 3000L glassed steel reaction vessels, add 20% industrial synthesis hydrochloric acid 1860kg, add calcium aluminate powder 750kg successively, temperature of reaction is remained between 80-110 ℃ by exothermic heat of reaction, stirring reaction 40min, ferric chloride in aqueous solution 750kg, hydration magnesium basic carbonate (MgO:41%) 30kg of adding 40% in reactant, continue reaction 40min, in this reactant, add water to cumulative volume then and be about 3300L.Reaction solution filters with chamber-type press filter, and about 70min filters and finishes, and adds suitable quantity of water washing filter residue, obtains transparent PAFC solution product 4180kg, and its composition is as shown in table 1.
The preparation of embodiment 4 poly aluminium chloride iron in contrast
The preparation method is identical with embodiment 1, and difference is: the ferric chloride Solution dosage is 160kg, does not add the hydration magnesium basic carbonate.Add water to about 3100L before the filtration, the about 65min of reaction solution filters and finishes, and obtains little muddy PAFC solution product 3850kg, and its composition is as shown in table 1.
Table 1: the quality index of PAFC product of the present invention and commercially available PAFC product relatively
Figure G2009101086390D00051
Annotate: commercially available PAFC: Gongyi City's star reaches the chemical plant and produces trade(brand)name liquid poly aluminium chloride iron, lot number 20090425;
As can be seen from Table 1, the PAFC product of embodiment 1 is the brown transparent liquid, and its effective constituent aluminium content meets and exceeds national standard, and especially iron level more reaches 1.81% high level, far above similar commercially available prod.In addition, compare with embodiment 4, the product of embodiment 1 can be placed preservation, and it is stable that quality keeps, show that the hydration magnesium basic carbonate brought into play the effect of stable ferrous components, further identity basis method of the present invention can be produced and be obtained stablizing high Fe content poly aluminium chloride iron product.
Table 2: the coagulation effect of PAFC product of the present invention and commercially available PAFC product relatively
Figure G2009101086390D00052
Figure G2009101086390D00061
Table 3: that uses PAFC product of the present invention and commercially available PAFC product purifies water index relatively
Annotate: cleaning test water: the former water of Dongguan polluted river channel, 12 ℃ of water temperatures, basicity 130.9mg/L, pH7.68, turbidity 58.6NTU.
As can be seen from Table 2, adding under the identical situation of dose, using the turbidity of purifying waste water of embodiment 1PAFC product significantly to be lower than the reference product and similar commercially available prod of using embodiment 4, and putting down when identical when surplus muddy water, embodiment 1 product usage quantity is minimum.In addition, as shown in table 3, the water quality after the PAFC of embodiment 1 product purifies, each index all obviously is better than reference product and commercially available prod.This shows that the PAFC product that makes according to the inventive method has very strong water purification function, and can reach the purifying water effect identical with other like product with consumption still less.

Claims (6)

1, a kind for the treatment of agent for molten polyaluminium ferric chloride wherein contains Al 2O 3Massfraction be 10-14%; With Al 2O 3X10% content meter, Fe 2O 3Massfraction is 1.7-3.6%, and the massfraction of Fe is 1.2-2.5%, insolubles≤0.05% weight.
2, the described treating agent for molten polyaluminium ferric chloride of claim 1 is characterized in that wherein further containing the hydration magnesium basic carbonate, and with Al 2O 310% content meter, content of magnesia is between 0.1-1.0%.
3, claim 1 or 2 described treating agent for molten polyaluminium ferric chloride is characterized in that described treating agent for molten polyaluminium ferric chloride prepares with following preparation method:
After hydrochloric acid and calcium aluminate reaction, adding iron(ic) chloride is stablizer with the hydration magnesium basic carbonate, adds an amount of water, prepares to have stable high Fe content poly aluminium chloride iron;
Wherein said each composition weight proportion is: 20% hydrochloric acid: calcium aluminate: iron(ic) chloride: hydration magnesium basic carbonate: water=10: 4: 1.5-4: 0.08-0.16: 3.5-4.5.
4, the described treating agent for molten polyaluminium ferric chloride of claim 3 is characterized in that described preparation method comprises the steps:
1) with 10 weight part massfractions be the calcium aluminate reaction of 20% hydrochloric acid and 4 weight parts, temperature of reaction 80-110 ℃, reaction times 0.3-1 hour;
2) adding 1.5-4 weight part massfraction in the reaction solution of step 1) is 40% iron(ic) chloride, the hydration magnesium basic carbonate of 0.08-0.16 weight part and the water of 3.5-4 weight part, continues reaction 0.3-1 hour;
3) collection step 2) reaction product that obtains obtains described treating agent for molten polyaluminium ferric chloride.
5, a kind of preparation has the method for stable high Fe content treating agent for molten polyaluminium ferric chloride, it is characterized in that, utilize the heat release of hydrochloric acid and calcium aluminate to carry out autothermal reaction, replenish source of iron with iron(ic) chloride, with the hydration magnesium basic carbonate is stablizer, add suitable quantity of water, preparation has the treating agent for molten polyaluminium ferric chloride of stable high Fe content;
Wherein said each composition weight proportion is: 20% hydrochloric acid: calcium aluminate: iron(ic) chloride: hydration magnesium basic carbonate: water=10: 4: 1.5-4: 0.08-0.16: 3.5-4.5.
6, method according to claim 5 may further comprise the steps:
1) be the calcium aluminate reaction of 20% technical hydrochloric acid and 4 weight parts with 10 weight part massfractions, keeping temperature is 80-110 ℃, reacts about 0.5 hour;
2) ferric chloride in aqueous solution of the massfraction 40% of adding 1.5-4 weight part and the hydration magnesium basic carbonate of 0.08-0.16 weight part in the reaction solution of step 1 reacted about 0.5 hour;
3) in the reaction solution of step 2, add the water of 3.5-4.5 weight part, mix, filter, obtain the treating agent for molten polyaluminium ferric chloride product.
CN2009101086390A 2009-07-08 2009-07-08 Treating agent for molten polyaluminium ferric chloride and preparation method thereof Active CN101602517B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103351045A (en) * 2013-07-18 2013-10-16 山东中科天泽净水材料有限公司 Nano composite polyaluminum ferric chloride flocculant and preparation method thereof
CN103896381A (en) * 2014-04-10 2014-07-02 百色学院 Method for preparing polyaluminum ferric chloride from waste liquid in activated clay production
CN104211148A (en) * 2014-08-18 2014-12-17 张少强 Compounded flocculating agent for processing heavy metals in electroplating wastewater and preparation method thereof
CN113955806A (en) * 2021-03-12 2022-01-21 衡阳市建衡实业有限公司 Production method of polyaluminum ferric chloride

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103351045A (en) * 2013-07-18 2013-10-16 山东中科天泽净水材料有限公司 Nano composite polyaluminum ferric chloride flocculant and preparation method thereof
CN103896381A (en) * 2014-04-10 2014-07-02 百色学院 Method for preparing polyaluminum ferric chloride from waste liquid in activated clay production
CN103896381B (en) * 2014-04-10 2016-06-29 百色学院 A kind of method that waste liquid utilized in activated clay production prepares PAFC
CN104211148A (en) * 2014-08-18 2014-12-17 张少强 Compounded flocculating agent for processing heavy metals in electroplating wastewater and preparation method thereof
CN113955806A (en) * 2021-03-12 2022-01-21 衡阳市建衡实业有限公司 Production method of polyaluminum ferric chloride
CN113955806B (en) * 2021-03-12 2023-08-01 衡阳市建衡实业有限公司 Production method of polyaluminum ferric chloride

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