CN102126758A - Method for preparing efficient nano ferric oxide drinking water type flocculants - Google Patents
Method for preparing efficient nano ferric oxide drinking water type flocculants Download PDFInfo
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- CN102126758A CN102126758A CN 201110102102 CN201110102102A CN102126758A CN 102126758 A CN102126758 A CN 102126758A CN 201110102102 CN201110102102 CN 201110102102 CN 201110102102 A CN201110102102 A CN 201110102102A CN 102126758 A CN102126758 A CN 102126758A
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Abstract
The invention relates to a method for preparing efficient nano ferric oxide drinking water type flocculants, belonging to the technical field of preparation of inorganic nonmetal nano materials. In the invention, the nano alpha-FeOOH flocculant is prepared by a coprecipitation method and the aluminium and silicon doped nano alpha-FeOOH flocculant is prepared through doping and surface modification. Compared with the traditional preparation methods, the method has the following advantages: the method is simple and practical; the nano particle size distribution is uniform; the preparation process flow is short; the method is environment-friendly; the manufacturing cost is low; and the prepared flocculants have higher treatment effects on toxic and harmful pollutants (such as heavy metals, toxic and harmful organic matters and the like), humic acid, chroma and the like.
Description
Technical field
The present invention relates to a kind of preparation method of efficient nano ferric oxide flocculation agent and the preparation method of modified Nano ferric oxide flocculation agent, belong to the preparing technical field of inorganic nonmetallic nanometer material.
Background technology
In recent years, water environment pollution increases the weight of day by day, has not only caused shortage of water resources, and is seriously threatening the public's drinking water safety, has increased the water treatment difficulty, and is also more and more to the research of water treatment flocculant.Conventional at present flocculation agent can be divided into: inorganic flocculating agent and organic floculant, inorganic flocculating agent is widely used because its source is wide.Wherein, inorganic macromolecule flocculant poly aluminum chloride (PAC) accounts for more than 80% of China's flocculation agent actual amount, but exists aluminium composition higher, easily causes secondary pollution of water.There is following shortcoming in iron-based flocculating agent when its high efficiency receives an acclaim: 1, pH is relied on high; 2, iron ion is easily residual; 3, effluent color dilution is residual, so its application also is restricted, and nano material is because its unique nano effect also receives increasing concern in water treatment applications.
The nanometer alpha-feooh claims the nanometer iron oxide yellow again, be widely used in fields such as pigment, printing ink, plastics, food, medicine and makeup, the preparation method of alpha-feooh has a lot, industrial air oxidation process, oxymuriate oxidation method, hydroxyl oxidize method and the peptisation of mainly containing.As patent CN200510017551.X, ferric ion Fe
3+Solution join and contain hydroxide radical OH
-Solution in, fully reaction under the alkaline condition that heating is constantly stirred simultaneously, in the reaction process, heating makes reaction solution remain on slight boiling condition and constantly stirs, stirring velocity is 800-10000r/min, after the precipitation that generates is stable, filters, wash, vacuumize heat drying and be prepared into nano level ferric oxide yellow pigment.Patent CN1056668 directly prepares alpha-feooh by spent acid solution.CN1143611 has invented a kind of with the production method of producing vitriolic waste residue manufacturing ferric oxide yellow pigment.Alpha-feooh difficult quality control by the traditional method preparation, size range is wide, it is closely related that its performance and morphological structure comprise that size, distribution, product type structure and form and aspect etc. have, and therefore launched research for the controlled alpha-feooh of preparation pattern, as Fe among the patent CN200810042869
3+And Fe
2+Add ethanol and polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO) triblock copolymer in the mixed aqueous solution, add NaOH solution then, preparation alpha-feooh nanometer rod.Patent CN02137552.6 under certain temperature and stirring velocity, joins refining green vitriol FeSO with a certain amount of mixed additive Sodium hexametaphosphate 99 and alkylphenol polyoxyethylene (OP-10)
4In the solution, react under the logical oxygen.
The present invention is by the improvement to alpha-feooh traditional preparation process method, obtain the controlled nanometer α of particle diameter and form-F eOOH, and made nano-sized iron oxide tap water type flocculation agent by mode such as surface modification, impurity and the shortcoming that exists in conjunction with iron-based flocculating agent.
Summary of the invention
The objective of the invention is by prefabricated advantage form nanometer alpha-feooh, prepare a kind of efficient nano alpha-feooh tap water type flocculation agent, this flocculation agent has overcome the above-mentioned shortcoming of iron-based flocculating agent, obtained a kind of efficient, noresidue, pollution-free, be used for the nano flocculant of tap water cheaply.The nanometer alpha-feooh is the preparation method improve traditional method, by simple technical process, obtained even particle size distribution, can control nanometer alpha-feooh pattern, the preparation method of the efficient nano alpha-feooh flocculation agent that production cost is low, for the nanometer alpha-feooh particle that makes preparation obtains better application, to its research of having carried out mixing silicon and having mixed the impurity of aluminium, up to the present, most of documents adopt physical doping to alpha-feooh, have only only a few to adopt impurity, this is because impurity is subjected to the restriction of ion factor, have only the approaching ion of size and character just to mix easily. but impurity can change crystalline growth microenvironment effectively, and the particle that influences product is too little, shape and physicochemical property.By the nanometer alpha-feooh is carried out modification, mix silicon and mix aluminium its surface property is changed, and then the dispersiveness of its aqueous solution is improved.Purpose of the present invention is achieved through the following technical solutions, and is described in detail as follows:
1, a kind of preparation method of efficient nano ferric oxide tap water type flocculation agent, it is by ferrous sulfate FeSO
4With yellow soda ash Na
2CO
3The reaction, generates stable post precipitation, through the washing, the drying and make, it is characterized in that: ferrous sulfate FeSO
4Concentration 0.05-0.5mol/L is at initial reaction stage N
2Protection feeds Na down
2CO
3The aqueous solution drips yellow soda ash Na
2CO
3Aqueous solution speed 10-60mL/min, the water-bath temperature constantly stirs in the reaction process at 25-75 ℃, bubbling air in the oxidising process, in nucleation and crystal growth phase, system pH remains on certain limit, reaction 3-4h promptly gets nano level alpha-feooh particle to washing of precipitate, drying, grinding.
The preparation method of described efficient nano ferric oxide tap water type flocculation agent, the FeSO that nucleation stage is used
4And Na
2CO
3Mol ratio is designated as R, at this R 0.5-1.5; Initial reaction stage is at N
2Protection feeds Na down
2CO
3Solution.
The preparation method of described efficient nano ferric oxide tap water type flocculation agent, in reaction process, stirring velocity is 500-4000r/min, bubbling air speed is 0.5-3L/min in the oxidising process.
The preparation method of described efficient nano ferric oxide tap water type flocculation agent, system pH maintains 6-7 automatically in the nucleation process; System pH should remain on 4-5 in crystal growing process, by dripping Na
2CO
3Solution is controlled.
The particle diameter of described efficient nano ferric oxide tap water type flocculation agent is strict controlled in nano level, and production cost is reduced near poly-ferric chloride, and clearance improves more than 30%.
2, a kind of preparation method who efficiently mixes the nano-sized iron oxide tap water type flocculation agent of Al: press the certain mol proportion reaction by finite concentration copperas solution and alum liquor, the mol ratio of Al/Fe: 0.01-0.5, in the different step of reaction 0-240min reaction of mixing, other reaction conditions is identical with above-mentioned claim 1.
3, a kind of preparation method who efficiently mixes the nano-sized iron oxide tap water type flocculation agent of Si: press the certain mol proportion reaction by finite concentration copperas solution and sodium silicate solution, the mol ratio of Si/Fe: 0.01-0.08, in the different step of reaction 0-240min reaction of mixing, other reaction conditions is identical with above-mentioned claim 1.
The characteristics that the present invention prepares efficient nano alpha-feooh flocculation agent method are:
1. the starting material of Cai Yonging conveniently are easy to get, and do not have any organic compound, are prepared at normal temperatures and pressures, can reduce production costs and environmental protection.
2. by controlling reactant concn, temperature of reaction, adding alkali speed and air flow quantity, can control nanometer alpha-feooh granule-morphology and size, the nanometer alpha-feooh particle lattice perfection, the purity that obtain are higher, and particles dispersed is good, big or small homogeneous.
3. mix in the different steps of reaction, can reduce the viscosity of synthetic system, accelerate speed of reaction, improve the dispersiveness of the adulterated nanometer alpha-feooh aqueous solution.
4. Zhi Bei efficient nano alpha-feooh flocculation agent and adulterated nanometer alpha-feooh flocculation agent have good removal effect to organism, heavy metal and toxic substance.
5. technological operation simply can be carried out industrialized expansion production.
Description of drawings
Fig. 1 is the TEM photo of embodiment 1 products obtained therefrom.
Fig. 2 is the TEM photo of embodiment 2 products obtained therefroms.
Fig. 3 is the TEM photo of embodiment 3 products obtained therefroms.
Fig. 4 is the TEM photo of embodiment 4 products obtained therefroms.
Fig. 5 is the TEM photo of embodiment 5 products obtained therefroms.
Fig. 6 is the XRD photo of embodiment 5 products obtained therefroms.
Embodiment
Provide several specific embodiment of the present invention below, so that the present invention is described in more details, all products all pass through the identification of phases of XRD thing and tem observation microscopic appearance
Embodiment 1
Get the FeSO that 200ml concentration is 0.05mol/L
4Solution is water bath with thermostatic control in four-hole boiling flask, and temperature feeds N at 25 ℃
2Drive in the bottle behind the air, adding 200mL concentration is the Na of 0.05mol/L
2CO
3Solution, adding speed are 10mL/min, stir and make its abundant mixing, and stirring velocity 3600r/min is with N
2Switch to air, air flow quantity is 2L/min, preparation nanometer alpha-feooh.Initial reaction stage is a nucleation process, and in this process, pH value of solution is kept definite value 6-7 automatically, and when system pH began to descend, nucleation process finished, and the mixing solutions color is yellow.Proceed to carry out the crystalline growth after will containing the ageing of solution 2h of alpha-feooh crystal seed.By dripping Na
2CO
3Solution hierarchy of control pH is 4-5, the precipitation repeated washing to generating after reaction is finished, and grinding powder promptly gets the alpha-feooh particle that particle diameter is 20nm behind the heat drying, the particle lattice perfection, the purity height, particles dispersed is good, big or small homogeneous.Its TEM microscopic appearance as shown in Figure 1.
Get the FeSO that 200ml concentration is 0.05mol/L
4Solution is water bath with thermostatic control in four-hole boiling flask, and temperature feeds N at 35 ℃
2Drive in the bottle behind the air, adding 200mL concentration is the Na of 0.05mol/L
2CO
3Solution, adding speed are 10mL/min, stir and make its abundant mixing, and stirring velocity 3600r/min is with N
2Switch to air, air flow quantity is 2L/min, preparation nanometer alpha-feooh.Initial reaction stage is a nucleation process, and in this process, pH value of solution is kept definite value 6-7 automatically, and when system pH began to descend, nucleation process finished, and the mixing solutions color is yellow.Proceed to carry out the crystalline growth after will containing the ageing of solution 2h of alpha-feooh kind.By dripping Na
2CO
3Solution hierarchy of control pH is 4-5, the precipitation repeated washing to generating after reaction is finished, and grinding powder promptly gets the alpha-feooh particle that particle diameter is 20nm behind the heat drying, the particle lattice perfection, the purity height, particles dispersed is good, big or small homogeneous.Its TEM microscopic appearance as shown in Figure 2.
Embodiment 3
Getting 200ml concentration is 0.05mol/L FeSO
4Solution and Al
2(SO
4)
318H
2O solution, the water bath with thermostatic control in four-hole boiling flask of the mixing solutions of Al/Fe-0.15, temperature feeds N at 35 ℃
2Drive in the bottle behind the air, adding 200mL concentration is the Na of 0.05mol/L
2CO
3The aqueous solution, adding speed are 10mL/min, stir and make its abundant mixing, and stirring velocity 3600r/min is with N
2Switch to air, air flow quantity is 2L/min, preparation nanometer alpha-feooh.Initial reaction stage is a nucleation process, and in this process, pH value of solution is kept definite value 6-7 automatically, and when system pH began to descend, nucleation process finished, and the mixing solutions color is yellow.Proceed to carry out the crystalline growth after will containing the ageing of solution 2h of alpha-feooh crystal seed.By dripping Na
2CO
3Solution hierarchy of control pH is 4-5, the precipitation repeated washing to generating after reaction is finished, and grinding powder promptly gets the alpha-feooh particle that particle diameter is 18nm behind the heat drying, the particle lattice perfection, the purity height, particles dispersed is good, big or small homogeneous.Its TEM microscopic appearance as shown in Figure 3.
Embodiment 4
Getting 200ml concentration is 0.25mol/LFeSO
4Solution and Na
2SiO
39H
2O solution, the water bath with thermostatic control in four-hole boiling flask of the mixing solutions of Al/Fe-0.01, temperature feeds N at 35 ℃
2Drive in the bottle behind the air, adding 200mL concentration is the Na of 0.05mol/L
2CO
3The aqueous solution, adding speed are 10mL/min, stir and make its abundant mixing, and stirring velocity 3600r/min is with N
2Switch to air, air flow quantity is 2L/min, preparation nanometer alpha-feooh.Initial reaction stage is a nucleation process, and in this process, pH value of solution is kept definite value 6-7 automatically, and when system pH began to descend, nucleation process finished, and the mixing solutions color is yellow.Proceed to carry out the crystalline growth after will containing the ageing of solution 2h of alpha-feooh crystal seed.By dripping Na
2CO
3Solution hierarchy of control pH is 4-5, the precipitation repeated washing to generating after reaction is finished, and grinding powder behind the heat drying, as shown in Figure 4.Fig. 5 and Fig. 6 carry out the Na that adds behind the 60min for reaction
2SiO
39H
2The TEM figure and the XRD figure of the nanometer alpha-feooh of mixing silicon of O formulations prepared from solutions.
Embodiment 5
Taking by weighing difference mixes than mixing silicon nanometer alpha-feooh sample and is respectively 5.0,10.0,15.0,20.0,30.0 and 50mg/L, the PFOS starting point concentration is 2mg/L, the pH value is 3.0, under 25 ℃ constant temperature, vibrate, get supernatant liquor, the concentration results of measuring PFOS shows: clearance is up to 90.49%.
Embodiment 6
Get the 40mL water sample and join in a series of 500mL beakers, add mass concentration respectively and be 50,100,200,300,400 and the alpha-feooh of 600mg/L mix Si (0,0.01,0.02) and carry out coagulation and stir.Coagulation condition is for stirring soon: 300r/min, 2min, stir slowly: 40r/min, 10min, the coagulation temperature is 25 ℃.Get the solution supernatant liquor behind the sedimentation 30min.Measure Mn2+ variation in the water, the result shows: alpha-feooh is mixed Si (0.02) removal effect can reach 83%.
Claims (9)
1. the preparation method of an efficient nano tap water type flocculation agent, it is by ferrous sulfate FeSO
4With yellow soda ash Na
2CO
3The reaction, generates stable post precipitation, through the washing, the drying and make, it is characterized in that: ferrous sulfate FeSO
4Concentration 0.05-0.5mol/L, initial reaction stage is at N
2Protection feeds Na down
2CO
3Solution flow: 10-60mL/min, the water-bath temperature is at 25-75 ℃, constantly stir in the reaction process, bubbling air in the oxidising process, in nucleation and crystal growth phase, system pH remains on certain limit, and reaction 3-4h promptly gets the nanometer alpha-feooh particle of different-shape (needle-like, spindle shape, lengthy motion picture shape, hollow form, bar-shaped etc.) and size to washing of precipitate, drying, grinding.
2. the preparation method of a kind of efficient nano tap water type flocculation agent according to claim 1 is characterized in that: efficient nano ferric oxide flocculation agent is mainly the nanometer alpha-feooh and mixes aluminium and the modified Nano alpha-feooh of mixing silicon.This flocculation agent very easily makes water-borne glue body particle take off surely, forms flco, and flco is big and closely knit, is easy to sedimentation; Simultaneously nano-sized iron oxide has great specific surface area and surface hydroxyl, the organic matter in can planar water, heavy metal ion etc.
3. the preparation method of a kind of efficient nano tap water type flocculation agent according to claim 1 is characterized in that: FeSO4 that nucleation stage is used and Na2CO3 mol ratio are designated as R, at this R-0.5-1.5; Initial reaction stage feeds Na2CO3 solution under the N2 protection.
4. the preparation method of a kind of efficient nano tap water type flocculation agent according to claim 1 is characterized in that: in reaction process, stirring velocity is 500-4000r/min, and bubbling air speed is 0.5-3L/min in the oxidising process.
5. the preparation method of a kind of efficient nano tap water type flocculation agent according to claim 1, it is characterized in that: system pH maintains 6-7 automatically in the nucleation process; System pH should remain on 4-5 in crystal growing process, by dripping Na
2CO
3The aqueous solution is regulated.
6. the particle diameter of a kind of efficient nano ferric oxide tap water type flocculation agent according to claim 1 is strict controlled in nano level, and production cost is reduced near poly-ferric chloride, and clearance improves more than 30%.
7. the preparation method of a kind of efficient nano tap water type flocculation agent according to claim 1, it is characterized in that: the impurity that can carry out Al, press the mol ratio of certain mol proportion reaction Al/Fe: 0.01-0.5 by finite concentration copperas solution and alum liquor, in the different step of reaction 0-240min reaction of mixing, other reaction conditions is identical with above-mentioned claim 1.
8. the preparation method of a kind of efficient nano tap water type flocculation agent according to claim 1, it is characterized in that: the impurity that can carry out Si, press the certain mol proportion reaction by finite concentration copperas solution and sodium silicate solution, the mol ratio of Si/Fe: 0.01-0.08, in the different step of reaction 0-240min reaction of mixing, other reaction conditions is identical with above-mentioned claim 1.
9. the preparation method of a kind of efficient nano tap water type flocculation agent according to claim 1 is characterized in that: this flocculation agent to the clearance of humic acid more than 55%; Turbidity removal rate is more than 80%; Chroma removal rate is more than 85%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110026195A (en) * | 2019-05-05 | 2019-07-19 | 河北师范大学 | A kind of high activity α-Fe2O3Nanometer sheet and its preparation method and application |
| CN111661878A (en) * | 2019-03-05 | 2020-09-15 | 中国石油天然气股份有限公司 | Preparation method of nano alpha-iron oxide hydroxide |
| CN113457694A (en) * | 2021-06-04 | 2021-10-01 | 华南师范大学 | Composite catalyst and preparation method and application thereof |
| CN115818723A (en) * | 2022-09-30 | 2023-03-21 | 江苏福友化肥催化净化环保材料有限公司 | Synthesis process for synthesizing alpha-iron oxyhydroxide by liquid-liquid method |
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| CN1079945A (en) * | 1993-06-25 | 1993-12-29 | 四川省物资贸易中心应用技术研究所 | Inorganic compounded flocculante for water treatment and preparation method thereof |
| CN1515508A (en) * | 2003-06-02 | 2004-07-28 | 北京天润百萌国际环境技术有限公司 | Inorganic argillaceos conversion agglutination purification treatment agent |
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2011
- 2011-04-22 CN CN 201110102102 patent/CN102126758A/en active Pending
Patent Citations (2)
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|---|---|---|---|---|
| CN1079945A (en) * | 1993-06-25 | 1993-12-29 | 四川省物资贸易中心应用技术研究所 | Inorganic compounded flocculante for water treatment and preparation method thereof |
| CN1515508A (en) * | 2003-06-02 | 2004-07-28 | 北京天润百萌国际环境技术有限公司 | Inorganic argillaceos conversion agglutination purification treatment agent |
Non-Patent Citations (1)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》 20101015 苏敏 掺杂纳米alpha-FeOOH的制备及应用研究 第10页第1.9节，第12页第2.1.2.1-2.1.2.2节，第13页第2.1.2.3节，第14-15页第2.2.1.1节，第16页第2.2.1.2节，第21-22页第2.2.2.1节，图2.1，2.2，2.4 1-9 , 第10期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111661878A (en) * | 2019-03-05 | 2020-09-15 | 中国石油天然气股份有限公司 | Preparation method of nano alpha-iron oxide hydroxide |
| CN110026195A (en) * | 2019-05-05 | 2019-07-19 | 河北师范大学 | A kind of high activity α-Fe2O3Nanometer sheet and its preparation method and application |
| CN110026195B (en) * | 2019-05-05 | 2021-09-03 | 河北师范大学 | High-activity alpha-Fe2O3Nanosheet and preparation method and application thereof |
| CN113457694A (en) * | 2021-06-04 | 2021-10-01 | 华南师范大学 | Composite catalyst and preparation method and application thereof |
| CN113457694B (en) * | 2021-06-04 | 2023-04-28 | 华南师范大学 | Composite catalyst and preparation method and application thereof |
| CN115818723A (en) * | 2022-09-30 | 2023-03-21 | 江苏福友化肥催化净化环保材料有限公司 | Synthesis process for synthesizing alpha-iron oxyhydroxide by liquid-liquid method |
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Application publication date: 20110720 |