CN103191684A - Preparation method and application of polymeric phosphato aluminum iron chloride coagulant - Google Patents

Preparation method and application of polymeric phosphato aluminum iron chloride coagulant Download PDF

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Publication number
CN103191684A
CN103191684A CN2013101542934A CN201310154293A CN103191684A CN 103191684 A CN103191684 A CN 103191684A CN 2013101542934 A CN2013101542934 A CN 2013101542934A CN 201310154293 A CN201310154293 A CN 201310154293A CN 103191684 A CN103191684 A CN 103191684A
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aluminum
phosphato
polymeric
preparation
reaction
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CN103191684B (en
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张鹏
任伯帜
郑谐
刘科家
杨旭明
安越
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Hunan University of Science and Technology
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Hunan University of Science and Technology
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Abstract

The invention discloses a preparation method and application of a polymeric phosphato aluminum iron chloride coagulant under a micro-wave irradiation condition. The method comprises the steps of: based on aluminum polychloride and FeCl3.6H2O as main materials, adding water to dissolve and evenly mixing; then adding disodium hydrogen phosphate solution to adjust the molar ratio of phosphorus to ferro-aluminum; putting into a microwave reactor to radiate and heat, so as to polymerize under a microwave condition; taking out from the microwave reactor; adding NaOH solution to adjust the alkalization degree and continuing to react for a period of time under the condition of a water bath; and finally curing at normal temperature to obtain polymeric phosphato aluminum iron chloride. The prepared polymeric phosphato aluminum iron chloride coagulant can be widely applied to treatment of source water, and treatment of industrial wastewater and domestic wastewater; and the function is superior to that of common aluminum polychloride and ferric polychloride. The polymeric phosphato aluminum iron chloride disclosed by the invention can effectively reduce the turbidity and UV254 of a water body in feedwater treatment; and the polymeric phosphato aluminum chloride iron disclosed by the invention has good removal effect on the turbidity, chemical oxygen demand (COD) and total phosphorus in domestic wastewater and industrial wastewater.

Description

A kind of preparation method of poly-phosphorus aluminum ferric chloride flocculant and application
Technical field
The invention belongs to chemical and environment-friendly engineering technical field, be specifically related to preparation and the application of poly-phosphorus aluminum ferric chloride flocculant under a kind of microwave radiation condition.
Background technology
In water-treatment technology field, flocculation is one of most important treatment step, and it has, and technology is simple, processing cost is low, high treating effect, is widely used in the water treatment.
Poly-phosphorus aluminium chloride ferrum is a kind of efficient inorganic high polymer coagulant that grew up in the last few years, because it has possessed the advantage of aluminium polychloride and poly-ferric chloride simultaneously, and after using it for water treatment, effluent color dilution is significantly less than the colourity after poly-ferric chloride and bodied ferric sulfate are handled, and the residual quantity of aluminium residual after will being lower than aluminium polychloride and handling.Should have the very high degree of polymerization by poly-phosphorus aluminium chloride ferrum simultaneously, and catch volume and sweep ability so can well bring into play adsorption bridging and net.Can be widely used in the middle of the processing for source water of Industrial Wastewater Treatment, sanitary sewage disposal and water supply plant.
The preparation technology of poly-phosphorus aluminium chloride ferrum is ripe gradually for many years, but synthetic route is various, traditional synthesis technique still has can improved place, as: generated time is longer, energy consumption is higher, advocating energetically in current country under the situation of energy-saving and emission-reduction, select the method for the poly-phosphorus aluminium chloride ferrum of low-energy consumption preparing, is researcher's urgent problem in this area.And microwave has advantages such as simple to operate, heating is fast, initiation time weak point as a kind of novel new and high technology, and is energy-efficient, meets the requirement of national environmental protection strategy, has potential wide application prospect
Summary of the invention
One of purpose of the present invention is at poly-long, the high deficiency of application cost of phosphorus aluminum ferric chloride flocculant reaction time of preparation in the existing water technology, and the preparation method of the effective poly-phosphorus aluminum ferric chloride flocculant of a kind of generated time weak point, stable performance, water treatment is provided.
The preparation method of the poly-phosphorus aluminum ferric chloride flocculant of the present invention comprises the steps:
(1) under the room temperature, with certain amount of fluid aluminium polychloride or the solid polyaluminium chloride aqueous solution and FeCl 3The aqueous solution places container, and stirs 3～15min, adds Na again 2HPO 42H 2The aqueous solution of O continues to stir 3～15min it is mixed;
(2) container that step (1) is equipped with mixed solution places in the middle of the microwave reactor, open microwave, under 20～100W microwave radiation condition, make temperature rise to 40～120 ℃ of reaction temperatures rapidly, make microwave power control at 20～60W then, keep reaction temperature certain, reaction 3～15min;
(3) after reaction finishes in microwave reactor container is taken out, place again under 30～60 ℃ of water bath condition, add a certain amount of NaOH solution and regulate basicity, continue reaction 2～24h;
(4) after reaction is finished, with product slaking 2～24h at normal temperatures, obtain the poly-phosphorus aluminum ferric chloride flocculant of rufous.
Specifically, in the step (1), the Al/Fe mol ratio is controlled between 0.1～8.0; The control of P/ (Al+Fe) mol ratio is between 0.1～0.6.
In the step (3), basicity is controlled between 0.1～0.6.
Two of purpose of the present invention is to provide the application of the poly-phosphorus aluminum ferric chloride flocculant of method for preparing, namely is used for to water treatment turbidity and UV 254Removal, be used for turbidity, COD and total phosphorus in sanitary sewage and the factory effluent reduction water body.
Than prior art, beneficial effect of the present invention be embodied in following some:
(1) preparation method of the present invention adopts microwave radiation polymerization technology, and microwave can promote polymerisation, and the reaction system quick heating, can significantly shorten generated time.
(2) under the microwave radiation condition, can overcome the uneven shortcoming of being heated in the aqueous solution heating process, and reactant character is more stable, not perishable.
(3) flocculant of the inventive method preparation is of many uses, can be widely used in in the middle of water treatment and the wastewater treatment, and it is good to have a treatment effect, the fireballing characteristics of settling of floccus.
The specific embodiment
The present invention is described in further detail below in conjunction with concrete experiment embodiment.
Embodiment 1:
(1) under the room temperature, get the PAC(aluminium polychloride of 6 parts by volume 2mol/L) FeCl of the aqueous solution and 4 parts by volume 2mol/L 3The aqueous solution places container, stirs 3min, adds the Na of 2mol/L again 2HPO 42H 2The O aqueous solution, the mol ratio P/ (Al+Fe) that regulates phosphorus and ferro-aluminum is 0.2, continues to stir 10min it is mixed;
(2) container is placed microwave reactor, open microwave, under 100W microwave radiation condition, make temperature rise to 60 ℃ of reaction temperatures rapidly, reduce microwave power then to 40W, make reaction temperature control at 60 ℃ of polymerisation 8min;
(3) container is taken out from microwave reactor after, the NaOH solution that adds 4mL2mol/L under 50 ℃ of water bath condition is regulated basicity, continues reaction 4h;
(4) after reaction is finished, with product slaking 8h at normal temperatures;
(5) making outward appearance is that rufous liquid, basicity are 0.42 poly-phosphorus aluminium chloride ferrum.
Embodiment 2:
(1) under the room temperature, get the PAC(aluminium polychloride of 5 parts by volume 2mol/L) FeCl of the aqueous solution and 4 parts by volume 3mol/L 3The aqueous solution places container, stirs 3min, adds the Na of 2mol/L again 2HPO 42H 2The O aqueous solution, the mol ratio P/ (Al+Fe) that regulates phosphorus and ferro-aluminum is 0.3, continues to stir 10min it is mixed;
(2) container is placed microwave reactor, open microwave, under 100W microwave radiation condition, make temperature rise to 60 ℃ of reaction temperatures rapidly, reduce microwave power then to 40W, make reaction temperature control at 50 ℃ of polymerisation 10min;
(3) container is taken out from microwave reactor after, the NaOH solution that adds 4mL2mol/L under 60 ℃ of water bath condition is regulated basicity, continues reaction 4h;
(4) after reaction is finished, with product slaking 10h at normal temperatures;
(5) making outward appearance is that rufous liquid, basicity are 0.51 poly-phosphorus aluminium chloride ferrum.
Product of the present invention is applied to the embodiment of water treatment:
With the poly-phosphorus aluminum ferric chloride flocculant of the product P PFAC(of the embodiment of the invention 1 and embodiment 2), industrial PFC, industrial PAC be used for the removal of sanitary sewage turbidity, COD, coagulation effect is as shown in table 1:
Table 1
? COD clearance (%) Turbidity removal rate (%)
Embodiment 1 product 83.4 97.6
Embodiment 2 products 89.2 93.9
Industry PFC 68.6 74.3
Industry PAC 73.1 82.6
From table 1 as seen, the poly-phosphorus aluminum ferric chloride flocculant of the inventive method preparation to the clearance of sanitary sewage turbidity, COD apparently higher than industrial PFC and industrial PAC.

Claims (4)

1. the preparation method of a poly-phosphorus aluminum ferric chloride flocculant is characterized in that comprising the steps:
(1) under the room temperature, with certain amount of fluid aluminium polychloride or the solid polyaluminium chloride aqueous solution and FeCl 3The aqueous solution places container, and stirs 3～15min, adds Na again 2HPO 42H 2The aqueous solution of O continues to stir 3～15min it is mixed;
(2) container that step (1) is equipped with mixed solution places in the middle of the microwave reactor, open microwave, under 20～100W microwave radiation condition, make temperature rise to 40～120 ℃ of reaction temperatures rapidly, make microwave power control at 20～60W then, keep reaction temperature certain, reaction 3～15min;
(3) after reaction finishes in microwave reactor container is taken out, place again under 30～60 ℃ of water bath condition, add a certain amount of NaOH solution and regulate basicity, continue reaction 2～24h;
(4) after reaction is finished, with product slaking 2～24h at normal temperatures, obtain the poly-phosphorus aluminum ferric chloride flocculant of rufous.
2. according to the preparation method of the described poly-phosphorus aluminum ferric chloride flocculant of claim 1, it is characterized in that: in the step (1), the Al/Fe mol ratio is controlled between 0.1～8.0; The control of P/ (Al+Fe) mol ratio is between 0.1～0.6.
3. according to the preparation method of the described poly-phosphorus aluminum ferric chloride flocculant of claim 1, it is characterized in that: in the step (3), basicity is controlled between 0.1～0.6.
4. the application of the poly-phosphorus aluminum ferric chloride flocculant of method preparation according to claim 1 is characterized in that: be used for to water treatment turbidity and UV 254Removal, be used for turbidity, COD and total phosphorus in sanitary sewage and the factory effluent reduction water body.
CN201310154293.4A 2013-04-28 2013-04-28 Preparation method and application of polymeric phosphato aluminum iron chloride coagulant Expired - Fee Related CN103191684B (en)

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Publication number Priority date Publication date Assignee Title
CN106480314A (en) * 2015-11-25 2017-03-08 湖南恒光化工有限公司 A kind of Application way of sulfuric acid iron ore relieving haperacidity waste residue
CN109250795A (en) * 2018-09-21 2019-01-22 六盘水师范学院 The method that type micro-wave radiation method for the treatment of different things alike quickly prepares polysilicate aluminum ferric sulfate
CN110615422A (en) * 2019-09-26 2019-12-27 常熟理工学院 Preparation method of poly-phosphorus ferric chloride aluminum flocculant
CN115520946A (en) * 2022-04-11 2022-12-27 江苏世邦生物工程科技有限公司 Biological composite flocculant for heavy metal ion adsorption and preparation method thereof

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CN102807275A (en) * 2012-07-16 2012-12-05 三明学院 Modified cellulose wastewater treatment flocculating agent and preparation method thereof

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CN1515507A (en) * 2003-01-08 2004-07-28 中国科学院沈阳应用生态研究所 Ecological safety composite type iron system high-effective flocculating agent
US8147695B2 (en) * 2007-06-22 2012-04-03 I. Kruger Inc. Method of removing phosphorus from wastewater
CN101172596A (en) * 2007-10-10 2008-05-07 广西民族大学 Method for rapid synthesis of aluminum orthophosphate salt polyalcohol
CN101704568A (en) * 2009-11-06 2010-05-12 江苏科技大学 PPAC and PFPS coagulant, preparation method and application thereof
CN102807275A (en) * 2012-07-16 2012-12-05 三明学院 Modified cellulose wastewater treatment flocculating agent and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106480314A (en) * 2015-11-25 2017-03-08 湖南恒光化工有限公司 A kind of Application way of sulfuric acid iron ore relieving haperacidity waste residue
CN109250795A (en) * 2018-09-21 2019-01-22 六盘水师范学院 The method that type micro-wave radiation method for the treatment of different things alike quickly prepares polysilicate aluminum ferric sulfate
CN110615422A (en) * 2019-09-26 2019-12-27 常熟理工学院 Preparation method of poly-phosphorus ferric chloride aluminum flocculant
CN115520946A (en) * 2022-04-11 2022-12-27 江苏世邦生物工程科技有限公司 Biological composite flocculant for heavy metal ion adsorption and preparation method thereof

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