CN104826579A - Magnetic kieselguhr adsorbent, preparation method and application thereof - Google Patents
Magnetic kieselguhr adsorbent, preparation method and application thereof Download PDFInfo
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- CN104826579A CN104826579A CN201510121233.1A CN201510121233A CN104826579A CN 104826579 A CN104826579 A CN 104826579A CN 201510121233 A CN201510121233 A CN 201510121233A CN 104826579 A CN104826579 A CN 104826579A
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Abstract
The invention discloses a magnetic kieselguhr adsorbent, a preparation method and an application thereof. The magnetic kieselguhr adsorbent includes kieselguhr as a core body and a Fe3O4 shell body coating the surface of the kieselguhr. The preparation method includes the steps of preparing a mixed solution containing the kieselguhr, depositing Fe3O4 on the surface of the kieselguhr, aging the Fe3O4, and washing, vacuum-drying and crushing the semi-product to obtain the magnetic kieselguhr adsorbent. The magnetic kieselguhr adsorbent has a large specific surface area and also excellent magnetism, so that the magnetic kieselguhr adsorbent is excellent in absorption property, especially copper ion absorption property. In addition, the magnetic kieselguhr adsorbent is stable in structure so that the magnetic kieselguhr adsorbent is available in purification of copper-containing waste water or water from drinking water sources.
Description
Technical field
The invention belongs to water-treatment technology field, particularly a kind of magnetic diatomite adsorbant and preparation method thereof and application.
Background technology
Along with the fast development of economy and improving constantly of industrialization degree, the particularly development of electron trade, as the development of the technology such as what plating of printed circuit, cause producing and a large amount of be rich in copper waste water, as printed circuit board (PCB) etching waste water, electroplating wastewater etc., in its copper-containing wastewater, copper content is generally up to 0.1-35g/L, substantially exceeds sewage drainage standard (GB8978-1996), if directly discharged, can serious environment pollution.What is more, and this is rich in copper waste water or the non-compliant waste water of purified treatment directly enters rivers, causes drinking water source contaminated, causes pollution like this, cause harm to the health of people to people's domestic water.
Therefore, how treatment and purification copper ions waste water and the drinking water resource containing copper ion become the problem that must solve.Treatment and purification copper method for treating water conventional is at present generally adopt chemical deposition, as in printed circuit board copper-containing wastewater, water process Zhong You mono-road waste water is divided mainly to exist with the form containing complex state copper, generally adopting sulphide precipitation to process containing complex copper waste water, precipitating copper ion in copper-containing wastewater by adding the dissolvable sulfide that can generate stable copper sulfide precipitation with copper ion in copper-containing wastewater.But the copper sulfide precipitation particle using the method process to produce is little, and sedimentation effect is poor, is usually suspended in water body, and discharge of wastewater copper ion finally can be caused to exceed standard, and treatment effect is poor.And technique difficulty controls, cost is high.
And adopt adsorbent to carry out purifying waste water processing such as copper ions waste water not need special technique and condition comparatively speaking, wherein, conventional diatomite is used to the conventional material of adsorbent.
Diatomite be the remains of the Diatomeae grown in ocean or lake at subaqueous deposit, a kind of nonmetallic mineral formed gradually through natural environment effect, diatomite adsorbant, belongs to environmental protection brand-new material field.Diatomaceous color is divided into white, canescence, grey and terra brown etc.Containing discoid in diatomite microstructure, the micropore layer structure of the shapes such as screen casing shape and sieve plate shape, it is intensive that this special layer structure has micropore, and bulk density is little, has the feature of larger specific area, thus make diatomite have strong absorption property.But diatomite is difficult to the copper of low concentration in the waste water of Treatment of Copper and drinking water source as adsorbent, when processing, adsorption rate is low and reclaim more difficult.Therefore, how developing a kind of can absorbing copper ion and the adsorbent that effectively can realize adsorbent and water Separation of Solid and Liquid be effectively a technical barrier.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, a kind of magnetic diatomite adsorbant and preparation method thereof and application are provided, to solve the technical problem of the not enough and separation difficulty of adsorption capacity that diatomite Treatment of Copper waste water and source water exist etc.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A kind of magnetic diatomite adsorbant, comprises the diatomite as nucleome and the tri-iron tetroxide shell layer being coated on diatomite surface.
And a kind of magnetic diatomite adsorbant preparation method, comprises the steps:
Diatomite is dispersed in the mixture solution containing molysite and ferrous salt, is formed containing diatomaceous mixed solution;
The described diatomaceous mixed solution pH of containing being adjusted to 7-9 makes molysite and ferrous salt reaction generate tri-iron tetroxide;
Separation of Solid and Liquid, washing, vacuum drying, break process is carried out after having the reactant liquor of tri-iron tetroxide to carry out burin-in process generation.
And, the application in the purified treatment of copper-containing wastewater or drinking water resource of magnetic diatomite adsorbant of the present invention or the magnetic diatomite adsorbant prepared as magnetic diatomite adsorbant preparation method of the present invention.
Magnetic diatomite adsorbant of the present invention adopts tri-iron tetroxide as clad, carries out modification, magnetic diatomite adsorbant of the present invention is had on the basis of large specific area characteristic to diatomite, also has excellent magnetic.Therefore, magnetic diatomite adsorbant of the present invention, on the basis with excellent absorption property, has the ability of excellent absorbing copper ion.In addition, this magnetic diatomite adsorbant structure of the present invention is nucleocapsid clad structure, therefore, and its Stability Analysis of Structures, thus the stability that ensure that its performance such as absorption property and magnetic.
Magnetic diatomite adsorbant preparation method of the present invention adopts sedimentation directly in diatomite surface deposition growth tri-iron tetroxide shell layer, makes the magnetic diatomite adsorbant Stability Analysis of Structures prepared.Meanwhile, the tri-iron tetroxide shell layer of deposition growing carries out coating modification to diatomite, thus make the magnetic diatomite adsorbant of preparation have large specific area characteristic and excellent magnetic, thus give absorption property and the magnetic of magnetic diatomite adsorbant excellence.In addition, magnetic diatomite adsorbant preparation method process conditions of the present invention are easy to control, and raw material easily obtains, and therefore, the magnetic diatomite adsorbant stable performance of preparation, cost is low.
Because magnetic diatomite adsorbant of the present invention has absorption property as above-mentioned excellence and magnetic, therefore, magnetic diatomite adsorbant of the present invention can be effective to the purified treatment of waste water or drinking water resource especially copper-containing wastewater or the drinking water resource containing trace copper, and the effective absorption realized copper ion, realize the effective purification to waste water or drinking water resource, excellent solid-liquid separation effect can be obtained simultaneously under additional magnetic fields, thus overcome the technical problem of the Separation of Solid and Liquid difficulty after existing Process of Wastewater with Diatomite.
Detailed description of the invention
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The embodiment of the present invention provides a kind of specific area large, the magnetic diatomite adsorbant of tool.This magnetic diatomite adsorbant is nucleocapsid structure, and its nucleome is diatomite, and housing is tri-iron tetroxide (Fe
3o
4), that is to say the coated diatomite of tri-iron tetroxide.Like this, this magnetic diatomite adsorbant adopts tri-iron tetroxide as clad, carries out modification to diatomite, makes magnetic diatomite adsorbant of the present invention have large specific area and excellent magnetic.Therefore, the structure of magnetic diatomite adsorbant of the present invention has excellent absorption property especially to the absorption property of copper ion excellence.In addition, this magnetic diatomite adsorbant is nucleocapsid clad structure, its Stability Analysis of Structures, thus the stability that ensure that its performance such as absorption property and magnetic.
In order to improve the structural stability of above-mentioned magnetic diatomite adsorbant and improve its magnetic behavior, in one embodiment, in this magnetic diatomite adsorbant, diatomite is 0.48-0.68 with the Weight control ratio of tri-iron tetroxide.By to tri-iron tetroxide shell or effectively can control with diatomaceous amount and optimize specific area and the magnetic of this magnetic diatomite adsorbant, thus improve its absorption property and magnetic behavior.
In another embodiment, the grain diameter of above-described embodiment magnetic diatomite adsorbant is 200-250.Therefore, in the various embodiments described above, magnetic diatomite adsorbant specific surface is large, and magnetic is high, therefore has excellent absorption property especially to the absorption property of copper ion, and its Stability Analysis of Structures.
Correspondingly, the embodiment of the present invention also provides a kind of magnetic diatomite adsorbant preparation method, comprises the steps:
Medical metal matrix material selection range is wide, the method forming composite ceramics rete on medical metal implant material surface that biologically active is high, and it comprises the steps:
Step S01: be dispersed to by diatomite in the mixture solution containing molysite and ferrous salt, is formed containing diatomite mixed solution;
Step S02: make molysite and ferrous salt reaction generate tri-iron tetroxide by being adjusted to 7-9 containing diatomite mixed solution pH described in preparing in step S01;
Step S03: carry out Separation of Solid and Liquid, washing, vacuum drying, break process after having the reactant liquor of tri-iron tetroxide to carry out burin-in process generation in step S02.
Particularly, in above-mentioned steps S01, the addition of molysite and ferrous salt can be prepared according to the reaction mol ratio of the iron ion and ferrous ion of preparing tri-iron tetroxide.In one embodiment, the mol ratio of molysite and ferrous salt is 1:1-1.4:1, and in one embodiment, the mol ratio of molysite and ferrous salt is about 1.2:1.In another specific embodiment, this molysite is selected from FeCl
36H
2o.In another embodiment, this ferrous salt is selected from FeCl
24H
2o, FeSO
47H
2at least one in O.Therefore, in a further embodiment, this FeCl
36H
2o and FeCl
24H
2the mol ratio of O is (1 ~ 1.2): 1.
By controlling the ferrous salt in above-mentioned steps S01 and molysite kind and both ratios, realize the control to step S02 tri-iron tetroxide crystal microstructure, to make it have high magnetic behavior and large specific area, to realize the raising of product magnetic diatomite adsorbant adsorption capacity especially to the raising of copper absorption ability.
In this step S01, diatomite is dispersed to the mixture solution containing molysite and ferrous salt, diatomite is made fully to contact with ferrous salt with molysite and adsorb, so that the product tri-iron tetroxide that above-mentioned steps S02 molysite and ferrous salt react can become deposition at diatomite.In order to control the amount of the tri-iron tetroxide being deposited on diatomite surface, in one embodiment, described diatomite is 1:1-1.5:1 with the gross weight ratio of described molysite and ferrous salt.To the control of this diatomite adding proportion, indirectly realize the control to product magnetic diatomite adsorbant structural stability, adsorption capacity and magnetic behavior, to improve magnetic diatomite adsorbant and magnetic behavior.
In another embodiment, this diatomite particle diameter is 250-300.
In one embodiment, the solvent of mixture solution can be water, is preferably distilled water, deionized water etc.In another embodiment, the weight concentration of this mixture solution controls as 0.047-0.094 (g/mL).By the control to mixed solution concentration, to realize the control to above-mentioned steps S02 tri-iron tetroxide throughput rate and microstructure, to improve end product magnetic diatomite adsorbant absorption property and magnetic.
Above-mentioned steps S02, when by when being adjusted to 7-9 scope containing the pH of diatomite mixed solution, molysite and ferrous salt are survived tri-iron tetroxide precipitation under-OH effect, and this precipitation are precipitated and is adsorbed on diatomite surface.This molysite and the ferrous salt chemical equation under-OH effect is as follows:
Fe
2++2Fe
3++8OH
-→Fe
3O
4↓+4H
2O -----(1)。
In addition, pH containing diatomite mixed solution is adjusted to 7-9 except making molysite and ferrous salt reaction, also by regulating pH to realize the control of microstructure generated product tri-iron tetroxide deposition, there is higher magnetic and absorption property especially to the absorption property of copper ion to make the microstructure of the tri-iron tetroxide generated.
In a further embodiment, control and regulate pH ammoniacal liquor, the NaOH containing diatomite mixed solution, the pH of mixed liquor is adjusted to 7-9.In one embodiment, this ammoniacal liquor is the concentrated ammonia liquor dilution 4-10 ammonia spirit doubly of 25%.
In one embodiment, the molysite in this step S02 and ferrous salt reaction generate in the process of tri-iron tetroxide, and the temperature of described mixture solution is 40-60 DEG C.That is to say the control to above-mentioned chemical equation (1) temperature, to realize the control of microstructure generated product tri-iron tetroxide deposition, there is higher magnetic and absorption property especially to the absorption property of copper ion to make the microstructure of the tri-iron tetroxide generated.
In addition, it should be understood that the time that above-mentioned chemical equation (1) reacts has been sufficient.When regulating mixed solution pH, be preferably attended by stir process operation.
In above-mentioned steps S03, be grow into precipitate tri-iron tetroxide the microstructure having and have high magnetic and bigger serface under this condition to reactant liquor burin-in process, thus improve the magnetic of product magnetic diatomite adsorbant and absorption property especially to the absorption property of copper ion.In addition, in burin-in process process, also improve the adhesion between tri-iron tetroxide and diatomite, thus improve the Stability Analysis of Structures performance of product magnetic diatomite adsorbant.Therefore, in one embodiment, described ageing method is that generation is had the reactant liquor of tri-iron tetroxide at bath temperature is 40-60 DEG C aging 1 ~ 3 hour.
In this step S03, after the reactant liquor after burin-in process carries out Separation of Solid and Liquid, surface deposition has the diatomite of tri-iron tetroxide to be collected, therefore, this Separation of Solid and Liquid can adopt the solid-liquid separating method of this area routine, as centrifugal, filtration etc., is effectively collected as long as can realize precipitation.
The object of washing Separation of Solid and Liquid filter residue is to remove residual reactant or other impurity.Therefore, in one embodiment, washing adopts absolute ethyl alcohol and distilled water washing for several times.
Carrying out vacuum drying to the filter residue of washing is in order to avoid in drying, tri-iron tetroxide is further oxided, and realize the object of its drying, in one embodiment, vacuum drying time controling is 6-10 hour simultaneously.After its drying, break process is carried out in order to obtain the target product magnetic diatomite adsorbant of certain particle size range to it.In one embodiment, after break process, cross 300 orders to sieve.
Therefore, embodiment of the present invention magnetic diatomite adsorbant preparation method adopts sedimentation directly in diatomite surface deposition growth tri-iron tetroxide shell layer, makes the magnetic diatomite adsorbant Stability Analysis of Structures prepared.The tri-iron tetroxide being deposited on diatomite surface grows into tri-iron tetroxide shell layer through burin-in process, realize diatomite coating modification, thus make the magnetic diatomite adsorbant of preparation have large specific area characteristic and excellent magnetic, thus give absorption property and the magnetic of magnetic diatomite adsorbant excellence.In addition, magnetic diatomite adsorbant preparation method process conditions of the present invention are easy to control, and raw material easily obtains, and therefore, the magnetic diatomite adsorbant stable performance of preparation, cost is low.
Correspondingly, the invention described above embodiment magnetic diatomite adsorbant with and preparation method thereof basis on, the embodiment of the present invention additionally provides embodiment of the present invention magnetic diatomite adsorbant to the application in waste water or drinking water source purifying water process.In one embodiment, embodiment of the present invention magnetic diatomite adsorbant is to the application in copper-containing wastewater or drinking water source purifying water process.Because the invention described above embodiment magnetic diatomite adsorbant has absorption property excellent as described above and magnetic, and the effective absorption realized copper ion, realize the effective purification to waste water or drinking water resource, excellent solid-liquid separation effect can be obtained simultaneously under additional magnetic fields, thus overcome the technical problem of the Separation of Solid and Liquid difficulty after existing Process of Wastewater with Diatomite.
Particularly, during by being used in the copper ion process of low concentration in copper ions waste water and drinking water of embodiment of the present invention magnetic diatomite adsorbant mentioned above, this magnetic diatomite exceeds about 40% to the adsorption effect of copper ion than existing common diatomite effect after measured.And compared with common diatomite, embodiment of the present invention magnetic diatomite adsorbant mentioned above is not harsh for the conditional request of the copper ion removing low concentration in Cu in waste water ion and drinking water, as in one embodiment, the condition of its application may be controlled to: pH scope 6-9, temperature: 5-30 DEG C, equilibrium concentration is low.In addition, embodiment of the present invention magnetic diatomite adsorbant mentioned above and other ion eutectoid content also have good result, non-iron-ion discharges, and adsorption process does not affect by dissolved organic matter matter in water, and regeneration cost is low, can repeatedly recycle, if the number of times that can be recycled is up to 4 times, adsorption capacity remains on more than 80%, and reaction is very fast, clearance is higher, can not produce secondary pollution.
Above-mentioned magnetic diatomite adsorbant and preparation method thereof and application is illustrated below by way of multiple embodiment.
Embodiment 1
A kind of magnetic diatomite adsorbant and preparation method thereof.This magnetic diatomite adsorbant is preparation method comprise the steps:
The conical flask that 100mL distilled water is housed is put into the water-bath of 40 DEG C, add 7gFeCl
36H
2o and 7gFeCl
24H
2o, then add 7g diatomite to the inside, 25% concentrated ammonia liquor adding dilution 4 times under rapid stirring regulates pH value to 8, make it to produce brownish black precipitation, aging 1 hour of water-bath, adopts absolute ethyl alcohol and distilled water to replace washing 4 times, atrament is put into vacuum drying chamber and dries, temperature is 60 DEG C, dry 6 hours, pulverize after cooling and obtain magnetic diatomite, inner casing was diatomite, shell is magnetic oxide, and composition is Fe
3o
4.
Embodiment 2
A kind of magnetic diatomite adsorbant and preparation method thereof.This magnetic diatomite adsorbant is preparation method comprise the steps:
The conical flask that 100mL distilled water is housed is put into the water-bath of 40 DEG C, add 2.7gFeCl
36H
2o and 2gFeCl
24H
2o, then add 4.7g diatomite to the inside, 25% concentrated ammonia liquor adding dilution 4 times under rapid stirring regulates pH value to 8, make it to produce brownish black precipitation, aging 2 hours of water-bath, adopts absolute ethyl alcohol and distilled water to replace washing 4 times, atrament is put into vacuum drying chamber and dries, temperature is 60 DEG C, dry 6 hours, pulverize after cooling and obtain magnetic diatomite, inner casing was diatomite, shell is magnetic oxide, and composition is Fe
3o
4.
Embodiment 3
A kind of magnetic diatomite adsorbant and preparation method thereof.This magnetic diatomite adsorbant is preparation method comprise the steps:
The conical flask that 100mL distilled water is housed is put into the water-bath of 50 DEG C, add 2.7gFeCl
36H
2o and 2gFeCl
24H
2o, then add 4.7g diatomite to the inside, the concentrated ammonia liquor adding 25% of dilution 5 times under rapid stirring regulates pH value to 9, make it to produce brownish black precipitation, aging 2 hours of water-bath, adopts absolute ethyl alcohol and distilled water to replace washing 4 times, atrament is put into vacuum drying chamber and dries, temperature is 60 DEG C, dry 8 hours, pulverize after cooling and obtain magnetic diatomite, inner casing was diatomite, shell is magnetic oxide, and composition is Fe
3o
4.
Comparative example 1
Common diatomite is provided.
Correlated performance is tested
The common diatomite that the magnetic diatomite adsorbant provided by above-described embodiment 1-3 and comparative example 1 provide carries out copper absorption test, and concrete grammar is as follows:
The magnetic diatomite adsorbant that the embodiment 1-3 getting 0.3g respectively provides and the common diatomite that comparative example 1 provides respectively Treatment of Copper ion are 0.5mg/L, 1mg/L, 3mg/L, 5mg/L, 10mg/L, the aqueous solution of 20mg/L, processes content of copper ion in the aqueous solution measuring each copper ion Graded amounts after 30 minutes respectively, thus draws absorption or the removal rate of copper ion.Correlation test data are described in table 1 below after measured.
As shown in Table 1, at identical conditions, the magnetic diatomite adsorbant that the embodiment of the present invention provides has excellent copper absorption ability, and with common diatom soil phase ratio, it is significantly improved adsorption of cupper ions and copper ion removal rate.
In addition, the magnetic diatomite adsorbant provided due to the embodiment of the present invention has the Fe 3 O 4 magnetic clad of rock-steady structure, therefore, under the effect of externally-applied magnetic field, can effectively realize, embodiment of the present invention magnetic diatomite adsorbant is separated with water, improves the efficiency of its Separation of Solid and Liquid.
Table 1
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a magnetic diatomite adsorbant, comprises the diatomite as nucleome and the tri-iron tetroxide shell layer being coated on diatomite surface.
2. magnetic diatomite adsorbant as claimed in claim 1, is characterized in that: the weight ratio of described diatomite and tri-iron tetroxide is 0.48-0.84.
3. magnetic diatomite adsorbant as claimed in claim 1 or 2, is characterized in that: the grain diameter of described magnetic diatomite adsorbant is 200-300 order.
4. a magnetic diatomite adsorbant preparation method, comprises the steps:
Diatomite is dispersed in the mixture solution containing molysite and ferrous salt, is formed containing diatomite mixed solution;
The described diatomaceous mixed solution pH of containing being adjusted to 7-9 makes molysite and ferrous salt reaction generate tri-iron tetroxide;
Separation of Solid and Liquid, washing, vacuum drying, break process is carried out after having the reactant liquor of tri-iron tetroxide to carry out burin-in process generation.
5. magnetic diatomite adsorbant preparation method as claimed in claim 4, is characterized in that: described molysite and ferrous salt reaction generate in the process of tri-iron tetroxide, and the temperature of described mixture solution is 40-60 DEG C.
6. magnetic diatomite adsorbant preparation method as claimed in claim 4, is characterized in that: described containing in diatomaceous mixed solution, the mol ratio of described molysite and ferrous salt is 1:1-2:1.
7. the magnetic diatomite adsorbant preparation method as described in as arbitrary in claim 4-6, is characterized in that: described containing in diatomaceous mixed solution, and the gross weight of described diatomite and described molysite and ferrous salt is than being 1:1-1:2.
8. the magnetic diatomite adsorbant preparation method as described in as arbitrary in claim 4-6, is characterized in that: described ageing method generation is had the reactant liquor of tri-iron tetroxide at bath temperature is 40-60 DEG C aging 1 ~ 3 hour; And/or
Described vacuum drying temperature is 60-80 DEG C.
9. the magnetic diatomite adsorbant as described in as arbitrary in claim 1-3 or as arbitrary in claim 4-8 as described in the application of the magnetic diatomite adsorbant prepared of magnetic diatomite adsorbant preparation method in the purified treatment of copper-containing wastewater or drinking water resource.
10. the application of magnetic diatomite adsorbant as claimed in claim 9 in the purified treatment of copper-containing wastewater or drinking water source, it is characterized in that: described magnetic diatomite adsorbant before application, also comprises the step that after adopting diluted acid pickling processes, distilled water washing, drying process.
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Application publication date: 20150812 |