CN108298648A - Multi-functional polysilicate flocculant and its preparation method and application - Google Patents

Multi-functional polysilicate flocculant and its preparation method and application Download PDF

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Publication number
CN108298648A
CN108298648A CN201810234237.4A CN201810234237A CN108298648A CN 108298648 A CN108298648 A CN 108298648A CN 201810234237 A CN201810234237 A CN 201810234237A CN 108298648 A CN108298648 A CN 108298648A
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polysilicate
functional
flocculant
preparation
salt
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CN201810234237.4A
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CN108298648B (en
Inventor
唐娜
肖杨杨
王小聪
张洪锋
吴夏芊
李娟�
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Tianjin University of Science and Technology
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Tianjin University of Science and Technology
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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
    • C02F1/48Treatment of water, waste water, or sewage with magnetic or electric fields
    • C02F1/488Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
    • 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
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/08Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/11Turbidity
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The present invention relates to multi-functional polysilicate flocculants and its preparation method and application, wherein multi-functional polysilicate flocculant includes the constituent of following mass percent:40~60wt% of modified polysilicate salt;5~25wt% of magnetic ferroferric oxide nano-particles;15~35wt% of mesoporous TiO 2.The flocculant of the present invention improves the stability of polysilicate, ability of the flocculant to processing waste water is improved simultaneously, except wasted energy power is up to 95% or more, and Magnetic Isolation sediment can be passed through, secondary pollution is avoided, it is very notable in sanitary sewage, spraying waste water, paper waste and dyeing waste water etc. treatment effect.

Description

Multi-functional polysilicate flocculant and its preparation method and application
Technical field
The present invention relates to inorganic polymer field, more particularly to multi-functional polysilicate flocculant and preparation method thereof and answer With.
Background technology
Modern economy industry quickly development, sanitary sewage is also growing day by day with industrial wastewater, as people are for environment The attention degree of pollution is higher and higher, and for the attention rate of industrial wastewater and sanitary sewage disposal, also when the river rises the boat goes up.In order to ensure The sustainable use of water resource, flocculent precipitation is most widely used in solving water pollution problems.Band in its structure of polysilicon acid There is a large amount of hydroxyl, hydrogen bond can be formed, enhances its adsorption capacity, and its structure can form the structures such as netted, spatial networks, It has greatly reinforced its net and has caught ability, formed larger floccule body, accelerated sedimentation is completed to be separated by solid-liquid separation.But polysilicon acid is not steady enough Calmly, performance when and the degree of polymerization is inadequate is also poor, so it is caused not come into operation extensively.
From the nineties in last century, a kind of novel polysilicon acid flocculant is found that with the continuous research of domestic scholars, The degree of polymerization etc. for not only substantially prolonging the holding time of polysilicon acid, while also improving it is used it for when handling water, Its turbidity removal performance is improved, and the dosage of flocculant is greatly reduced.
By the study found that these optimizations have benefited from a small amount of metal ion, to which polysilicate flocculation be obtained by the reaction Agent.Its performance is apparently higher than single use polysilicon acid, to receive the attention of researcher.Excellent performance be because metal from Son has charge neutrality performance, while polysilicon acid also has stronger adsorption-flocculation performance, is imitated under the two collective effect The excellent product of fruit.
Researchers characterize by multiple research, find polysilicate flocculant compared with polysilicon acid flocculant, wadding Solidifying de- stability can be more excellent.And study and also found in nearest scholars, be not only metal ion has optimization function to it, And the performance of flocculant can be also improved when there is boron ion addition.Due to inorganic coagulant polysilicate have it is incomparable excellent Gesture, this also makes it have the status that can not be ignored in inorganic polymer flocculant, but whether flocculant brings secondary pollution Still leave a question open up at present, how the pollutant to get off that flocculates detaches also from water body without effectively method.
Invention content
The purpose of the present invention is at least one, the multi-functional polysilicate flocculants of present invention offer in order to solve the above problem And its preparation method and application.
According to an aspect of the present invention, a kind of multi-functional polysilicate flocculant, including following composition are provided:It is modified poly- Silicate composite magnetic ferriferrous oxide nano-particle and mesoporous TiO 2.
Wherein, the percentage composition of each ingredient is in multi-functional polysilicate flocculant:
40~60wt% of modified polysilicate salt
5~25wt% of magnetic ferroferric oxide nano-particles
15~35wt% of mesoporous TiO 2
Wherein, the grain size of mesoporous TiO 2 is 2-10nm.
According to another aspect of the present invention, a kind of preparation method of the multi-functional polysilicate flocculant is provided, including Following steps:
Prepare modified polysilicate salt solid powder.
Magnetic carrier and mesoporous TiO 2 and modified polysilicate salt solid powder is abundant in mortar by a certain percentage Grinding, you can obtain the multi-functional polysilicate flocculant.
Wherein, magnetic carrier is at least one of ferroso-ferric oxide and γ-di-iron trioxide.
Wherein, the step of preparing modified polysilicate salt solid powder be:
Specific silicate solutions are instilled into sulfuric acid solution, until when the pH value of mixed solution is 4, stop being added dropwise.
After reacting 3h, continue that concentrated sulfuric acid solution is added dropwise in the mixed solution for instilling sodium silicate solution, until the PH of solution Value is 2, stops being added dropwise.
Mixed metal salt is added into the mixed solution after dropwise addition concentrated sulfuric acid solution.
After reacting 3h again, the mixed solution of mixed metal salt is added in heating evaporation, obtains modified polysilicate salt solid powder.
Wherein, mixed metal salt is at least two in potassium sulfate, zinc sulfate, ferric trichloride, sodium tetraborate and magnesium chloride.
Wherein, specific polysilicate is at least one of sodium metasilicate, sodium silicate, potassium silicate and potassium water glass.
According to the third aspect of the invention we, a kind of multi-functional polysilicate flocculant is provided in catalytic degradation organic matter Effect.
Magnetic carrier, mesoporous TiO 2 change the crystal of polysilicate flocculant with polysilicate flocculant by mixing Pattern forms a kind of multi-functional polysilicate flocculant of porous pattern.This porous pattern increases flocculant and colloid Grain contact area, to improve the flocculating effect of polysilicate flocculant.This porous structure also increases mesoporous TiO 2 With the time of contact of organic matter, organic matter degradation rate is also substantially increased.Magnetic carrier is covered by this porous flocculant, This is substantially increased can magnetic recovery rate.
The invention has the advantages that:
1, the present invention can magnetic recovery multi-functional polysilicate flocculant, improve the stability of polysilicate, simultaneously Flocculant is improved to handling the ability of waste water, and secondary pollution, application range can be avoided by Magnetic Isolation sediment Extensively, sanitary sewage, spraying waste water, paper waste, dyeing waste water etc. treatment effect are very notable.
2, the present invention can magnetic recovery multi-functional polysilicate flocculant preparation method, on the one hand improve poly- silicon salt Stability, on the other hand improve polysilicate processing waste water ability.
3, the present invention can magnetic recovery multi-functional polysilicate flocculant preparation method it is simple for process, it is at low cost, effect Fruit is notable.
Description of the drawings
By reading the detailed description of hereafter preferred embodiment, various other advantages and benefit are common for this field Technical staff will become clear.Attached drawing only for the purpose of illustrating preferred embodiments, and is not considered as to the present invention Limitation.And throughout the drawings, the same reference numbers will be used to refer to the same parts.In the accompanying drawings:
Fig. 1 shows the fourier infrared spectrogram of the multi-functional polysilicate flocculant according to embodiment of the present invention;
Fig. 2 shows the X-ray diffraction spectrograms according to the multi-functional polysilicate flocculant of embodiment of the present invention;
Fig. 3 shows the scanning electron microscope diagram of the multi-functional polysilicate flocculant according to embodiment of the present invention;
Fig. 4 shows the magnetic recovery schematic diagram of the multi-functional polysilicate flocculant according to embodiment of the present invention;
Fig. 5 shows the treatment effect for ink of the multi-functional polysilicate flocculant according to embodiment of the present invention Schematic diagram.
Specific implementation mode
The illustrative embodiments of the disclosure are more fully described below with reference to accompanying drawings.Although showing this public affairs in attached drawing The illustrative embodiments opened, it being understood, however, that may be realized in various forms the disclosure without the reality that should be illustrated here The mode of applying is limited.It is to be able to be best understood from the disclosure on the contrary, providing these embodiments, and can be by this public affairs The range opened completely is communicated to those skilled in the art.
Embodiment 1
Polysilicate composite flocculation agent X1 includes following composition:Modified polysilicate salt 50wt%;Magnetic ferroferric oxide is received Rice corpuscles 25wt%;Mesoporous TiO 2 25wt%.
Wherein, the fourier infrared spectrogram of polysilicate composite flocculation agent X1 is as shown in Figure 1, polysilicate composite flocculation agent The X-ray diffraction spectrogram of X1 as shown in Fig. 2, the scanning electron microscope diagram of polysilicate composite flocculation agent X1 as shown in figure 3, more The magnetic recovery schematic diagram of function polysilicate flocculant X1 as shown in figure 4, multi-functional polysilicate flocculant X1 for ink Treatment effect schematic diagram it is as shown in Figure 5.
The sewage of 200ml is handled using 200ppm polysilicate composite flocculation agent X1, obvious processing effect is removed Turbid effect reaches 95% or more, specific as shown in table 1.Degradation of organic substances COD of the polysilicate composite flocculation agent to surface waste water Effect is more notable, and specific data embody in table 2.
Table 1:The turbidity removal ability of polysilicate composite flocculation agent X1 detects table
Table 2:The COD degradation ability of polysilicate composite flocculation agent X1 detects table
Wherein, the data of table 2 are obtained by permanganimetric method measurement.
Comparative example 1
It is right using its using magnetic ferroferric oxide nano-particles identical with content in polysilicate composite flocculation agent X1 Sewage is handled, and treatment effect is not notable, and specific data are as shown in table 3.
Table 3:The turbidity removal ability of magnetic ferroferric oxide ion detects table
Comparative example 2
Using mesoporous TiO 2 identical with content in polysilicate composite flocculation agent X1, using its to sewage at Reason, treatment effect is not notable, and specific data are as shown in table 4.
Table 4:The turbidity removal ability of mesoporous TiO 2 detects table
Comparative example 3
Using modified polysilicate salt identical with content in polysilicate composite flocculation agent X1, using its to sewage at Reason, treatment effect is general, and specific data are as shown in table 5.
Table 5:The turbidity removal ability of modified polysilicate salt detects table
Comparative example 4
Flocculant Y1 is made of the modified polysilicate salt equal with polysilicate composite flocculation agent X1 contents and magnetic carrier, Sewage of 200ml is handled using it, treatment effect is preferable, and turbidity removal effect reaches 90% or so, specifically such as 6 institute of table Show.
Table 6
Comparative example 5
Flocculant Y3 is by the modified polysilicate salt equal with polysilicate composite flocculation agent X1 contents and mesoporous TiO 2 Composition, is handled the sewage of 200ml using it, treatment effect is preferable, and turbidity removal effect is specifically as shown in table 7.
Table 7
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Any one skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in, It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of the claim Subject to enclosing.

Claims (9)

1. multi-functional polysilicate flocculant, which is characterized in that including following composition:Modified polysilicate salt composite magnetic four aoxidizes Three Fe nanometer particles and mesoporous TiO 2.
2. multi-functional polysilicate flocculant as described in claim 1, which is characterized in that the multi-functional polysilicate flocculant In the percentage composition of each ingredient be:
40~60wt% of modified polysilicate salt
5~25wt% of magnetic ferroferric oxide nano-particles
15~35wt% of mesoporous TiO 2
3. multi-functional polysilicate flocculant as described in claim 1, which is characterized in that
The grain size of the mesoporous TiO 2 is 2-10nm.
4. the preparation method of the multi-functional polysilicate flocculant as described in claims 1 to 3 is any, which is characterized in that including Following steps:
Prepare modified polysilicate salt solid powder;
Magnetic carrier and mesoporous TiO 2 are fully ground in mortar by a certain percentage with modified polysilicate salt solid powder, It can be obtained the multi-functional polysilicate flocculant.
5. preparation method as claimed in claim 4, which is characterized in that
The magnetic carrier is at least one of ferroso-ferric oxide and γ-di-iron trioxide.
6. preparation method as claimed in claim 4, which is characterized in that the step of preparing modified polysilicate salt solid powder be:
Specific silicate solutions are instilled into sulfuric acid solution, until when the pH value of mixed solution is 4, stop being added dropwise;
After reacting 3h, continue that concentrated sulfuric acid solution is added dropwise in the mixed solution for instilling sodium silicate solution, until the pH value of solution is 2, stop being added dropwise;
Mixed metal salt is added into the mixed solution after dropwise addition concentrated sulfuric acid solution;
After reacting 3h again, the mixed solution of mixed metal salt is added in heating evaporation, obtains modified polysilicate salt solid powder.
7. preparation method as claimed in claim 6, which is characterized in that
The mixed metal salt is at least two in potassium sulfate, zinc sulfate, ferric trichloride, sodium tetraborate and magnesium chloride.
8. preparation method as claimed in claim 6, which is characterized in that
The specific polysilicate is at least one of sodium metasilicate, sodium silicate, potassium silicate and potassium water glass.
9. application of the multi-functional polysilicate flocculant in catalytic degradation organic matter as described in claims 1 to 3.
CN201810234237.4A 2018-03-21 2018-03-21 Multifunctional polysilicate flocculant and preparation method and application thereof Active CN108298648B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113087098A (en) * 2021-04-02 2021-07-09 吉林化工学院 Preparation method of magnetic poly-aluminum titanium silicate-sodium alginate composite flocculant

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101712505A (en) * 2009-10-27 2010-05-26 南通立源水业科技发展有限公司 Preparation method of silicate polymer flocculant rich in active catalyst
CN103588272A (en) * 2013-11-29 2014-02-19 陈忠林 Preparation method for inorganic flocculating agent and enhanced coagulation method for treating low-temperature low-turbidity high-organic matter water body by using inorganic flocculating agent
CN105858911A (en) * 2016-04-19 2016-08-17 肥东县柯文斌家庭农场 Nanometer type water clarification agent

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101712505A (en) * 2009-10-27 2010-05-26 南通立源水业科技发展有限公司 Preparation method of silicate polymer flocculant rich in active catalyst
CN103588272A (en) * 2013-11-29 2014-02-19 陈忠林 Preparation method for inorganic flocculating agent and enhanced coagulation method for treating low-temperature low-turbidity high-organic matter water body by using inorganic flocculating agent
CN105858911A (en) * 2016-04-19 2016-08-17 肥东县柯文斌家庭农场 Nanometer type water clarification agent

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DAN CAI等: "《Journal of Applied Polymer Science》", 15 January 2018 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113087098A (en) * 2021-04-02 2021-07-09 吉林化工学院 Preparation method of magnetic poly-aluminum titanium silicate-sodium alginate composite flocculant

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