CN103693758A - Method for treating methylene blue dye wastewater - Google Patents
Method for treating methylene blue dye wastewater Download PDFInfo
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- CN103693758A CN103693758A CN201310733073.7A CN201310733073A CN103693758A CN 103693758 A CN103693758 A CN 103693758A CN 201310733073 A CN201310733073 A CN 201310733073A CN 103693758 A CN103693758 A CN 103693758A
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Abstract
The invention relates to a method for treating methylene blue dye wastewater. Firstly, diatomite is evenly mixed with calcium raw materials, alkali activator and water, and is put in a high-pressure hydrothermal reaction kettle after the compression molding to react for 1-48 hours at the temperature of 100-200 DEG C to obtain a diatomite-based porous adsorbent containing C-S-H, tobermorite and analcite; then, the diatomite-based porous adsorbent is put in a conical bottle accommodated with a liquid culture medium; 5-20% of yeast powder by mass is added to regulate the pH to be 5-8 and to cultivate for 2-48 h under the constant-temperature condition of 15-35 DEG C on a reciprocal shaking table with the speed of 60-120 rpm so as to obtain a yeast-loaded diatomite-based porous adsorbent; finally, 1-10 g of the yeast-loaded porous adsorbent is added in the methylene blue dye wastewater with per liter concentration of 100-1000 mg/L to treat for 1-48 h at the temperature of 25-45 DEG C on the reciprocal shaking table with the pH of 4 to 10 and the speed of 60-120 rpm; the concentration of the treated methylene blue wastewater is measured through a spectrophotometer method; the result shows that the removal rate of the methylene blue dye exceeds 90%. The method has the advantages of simple process, low cost and no secondary pollution, and is suitable for the industrial treatment of the methylene blue dye wastewater.
Description
Technical field
The present invention relates to a kind of method of processing methylene blue dye waste water, specifically on the curing Diatomite-based Porous sorbent material of hydro-thermal, load yeast is processed methylene blue dye waste water, belongs to dye wastewater treatment technology field.
Background technology
Along with the development of dyestuff and printing and dyeing industry, organic dye waste water has become one of main pollution source of water body.Waste water from dyestuff complicated component, organic content is large, and great majority are to take the form that the aromatic groups such as benzene, naphthalene, anthracene, quinone are parent to exist, and has the features such as colourity is dark, strong toxicity, difficult degradation, and water surrounding has been formed to day by day serious threat.Simultaneously, when the waste water that contains dyestuff enters in nature waters because the colourity of dyestuff is dark, so content seldom also can produce the color of highly significant, cause water body color and luster to pollute, not only can impact the vision system of the mankind or animal, and can reduce in sunlight arrival water or water-bed intensity, affect the photosynthesis of water body Green plant, finally cause water ecosystem to worsen, cause biological mortality.Therefore the comprehensive regulation of waste water from dyestuff has become one of current problem demanding prompt solution.
Methylene blue (MB) is a kind of thiazine dyestuff, is widely used in cotton, and wood and silk are painted, is the most common dyestuff, but it is difficult to be degraded by some conventional methods, easily causes serious problem of environmental pollution.Organic dye waste water comprises that the processing of methylene blue dye waste water mainly contains oxidation style, photocatalytic method, Coagulation Method, membrane separation process and absorption method etc. at present.In above treatment process, oxidation technology cost is high, conventional oxygenant exist oxidation capacity poor, there is the features such as selective oxidation; The deficiency of photocatalytic method maximum is to need light source to irradiate system, in application, be subject to light source and weather effect.The working cost of Coagulation Method is higher, processes body refuse amount greatly and difficult treatment.Membrane separation process clearance in dyestuff is processed is high, and technique is simple, but the production cost of film is very high at present, and working pressure is large, is difficult to carry out large-scale industrialization application.The required sorbent material consumption of absorption method is large, and part sorbent material, as the cost of gac is very high, is difficult to carry out large-scale sewage disposal.Therefore, developing method simply a kind of and that efficiently process methylene blue dye waste water has great importance.
Summary of the invention
The object of the present invention is to provide a kind of method without reaching absorption under illumination, non-secondary pollution, normal temperature, degrade, remove methylene blue contaminated wastewater, specifically utilize hydrothermal technique to solidify the method for diatom soil matrix sorbing material load yeast processing dye wastewater.
For achieving the above object, the present invention observes discovery, in nature paddy field, in the vesicular structure of soil, there is soil microorganisms and the soil enzyme of One's name is legion, they contribute to absorption and the degraded of pollutent, for the field water in paddy field, there is superior purification function, this paddy field soil is actually a kind of mineral and microbial interaction to the self-purification function of water, is that the inorganic world and bios are intersected the result of infiltration mutually.But this soil still exists significant limitation in actual applications as water scavengine agent, and the self-purification ability of soil also can not show a candle to some inorganic mineral material, such as diatomite, zeolite, sepiolite etc.But in environmental engineering, after their absorb polluted matters, be difficult to and purify waste water separatedly, making the sorbent material of system be converted into mud together with sewage, sludge creation amount is increased greatly.Clearly, these mineral material granulations being become to the material with certain character is one of method solving argillization problem.Therefore, the mineral material that our use has self-purification performance is raw material, be prepared into the porous adsorbing material particulate vector with superior self-purification performance, and in the vesicular structure of this sorbent material, introduce the enzyme etc. with specific function, the environmentally conscious materials of this biocompatible is played a significant role aspect sewage disposal as porous microbial carrier.
Hydro-thermal solidifies/and synthetic technology is a kind of low temperature synthetic technology, in building-up process, can retain as much as possible the original structure of raw material inorganic mineral, simultaneously synthetic as new mineral phases such as C-S-H gel, tobermorite, euthalites, these mineral facies not only can improve the intensity of absorption carrier, also can improve the porous performance of carrier, be conducive to introduce fixation of microbe, improve sewage treating efficiency.
Technical scheme of the present invention is: first utilize hydrothermal technique diatomite material to be cured as to the high intensity, porous absorption carrier that can process methylene blue dye waste water, then through cultivation and immobilization technology, yeast is loaded on absorption carrier, thereby improve the efficiency of processing methylene blue dye waste water.Concrete technology is as follows:
The first step, the preparation of high strength Diatomite-based Porous sorbent material
First commercially available diatomite original soil is ground, cross 80 mesh sieves and dry; Then, calcareous raw material, alkali-activator, water are added in the diatomite of oven dry, mix, compression moulding under the pressure of 5～40MPa, obtains the sample after moulding; Finally, the sample after moulding is put into high-pressure hydrothermal reaction kettle, controlling temperature of reaction is 100～200 ℃, and reaction times 1～48h obtains having higher force and learns intensity (abbreviation high strength) Diatomite-based Porous sorbent material; After testing, the high strength Diatomite-based Porous sorbent material making has good water resistant power shear effect, the diatomite that its composition retains after for reaction, and a kind of in the synthetic hydrated calcium silicate gel (C-S-H) of hydro-thermal reaction, tobermorite (Tobermorite), euthalite (ANA) or 2 kinds or 3 kinds of forming in any proportion.
The quality that adds of above-mentioned calcareous raw material, alkali-activator, water is respectively 10～50%, 5～20% of diatomite quality, 5～50% mass percents;
Above-mentioned calcareous raw material is selected from the 2-5 kind a kind of or that form in any proportion in slaked lime, Wingdale, unslaked lime, rhombspar, lime feldspar:
Above-mentioned alkali-activator is selected from the 2-5 kind a kind of or that form in any proportion in sodium hydroxide, sodium metaaluminate, water glass, Starso, flyash:
Second step, the preparation of Diatomite-based Porous sorbent-loaded yeast
The high strength Diatomite-based Porous sorbent material that the first step is obtained is put into the Erlenmeyer flask that fills liquid nutrient medium, add yeast powder, the add-on of yeast powder is 5%～20% mass percent of high strength Diatomite-based Porous adsorbent mass, regulating pH value is 5～8, on the reciprocal shaking table of speed 60rpm～120rpm, the constant temperature of 15～35 ℃ is cultivated 2h～48h, obtains the Diatomite-based Porous sorbent material of load yeast;
Yeast powder used is commercially available bread beer yeast powder, or the commercially available yeast powder for the treatment of waste water from dyestuff;
The 3rd step, methylene blue dye wastewater treatment
The Diatomite-based Porous sorbent material 1～10g that adds the load yeast of second step in the methylene blue dye waste water that is 100～1000mg/L every liter of concentration, by pH regulator to 4～10, and on the reciprocal shaking table that is 60rpm～120rpm in speed, at 25～45 ℃, process 1h～48h, by spectrophotometer method, measure the concentration of processing rear methylene blue waste water, result shows, the clearance of methylene blue dye surpasses 90%, and unit adsorptive capacity surpasses 80mg/g.
Compared with prior art, the present invention has following significant advantage and effect:
1. the high strength Diatomite-based Porous sorbent material making by hydro-thermal reaction due to the present invention, compare with conventional sintering moulding process, can retain the intrinsic microvoid structure of diatomite material itself, can control porosity, pore size, pore size distribution and specific surface area again, the high strength Diatomite-based Porous sorbent material therefore obtaining is better to the absorption of methylene blue dye, decomposition and degraded texts than raw material diatomite.
2. the high strength Diatomite-based Porous sorbent material of Hydrothermal Synthesis of the present invention is retaining on the basis of diatomite favourable absorption, generate again specific surface area and obtained the hydrated calcium silicate gel (C-S-H) promoting to a certain extent, tobermorite (Tobermorite), euthalite (ANA), when sorbent material strength increase is described, absorption property is also improved, and cation exchange capacity has also obtained obvious lifting, methylene blue dye molecules is cationic dyes, therefore, high strength Diatomite-based Porous sorbent material has the adsorption treatment that is not only conducive to dye molecule to methylene blue adsorption number, also the inherent advantage that is conducive to the load of microorganism (yeast).
3. simple, the save energy of high strength Diatomite-based Porous absorbent preparation method of the present invention, has good mechanical strength, can not generate mud and cause secondary pollution after disposing of sewage, repeatedly reusable.
High strength Diatomite-based Porous sorbent material of the present invention by load yeast after, the absorption of combining yeast cell and Degradation, greatly improved the treatment effect to dye wastewater, that the preparation method of the diatom soil matrix solid adsorbent of this load yeast has is simple to operate, without complex steps, produce easily in a large number, feature with low cost, thereby be suitable for methylene blue dye wastewater treatment to carry out heavy industrialization application.
5. the removal of methylene blue dye of the present invention is simple to operate, can be at normal temperatures and pressures, without complex steps, non-secondary pollution produce, working cost is low, methylene blue dye clearance surpasses 90%, has very high actual application value.
Accompanying drawing explanation
Fig. 1 is the diatomaceous stereoscan photograph of raw material of the present invention
Fig. 2 is the C-S-H Diatomite-based Porous sorbent material and the diatomaceous XRD figure of reacting rear reservation of Hydrothermal Synthesis of the present invention
Fig. 3 is the tobermorite Diatomite-based Porous sorbent material and the diatomaceous XRD figure of reacting rear reservation of Hydrothermal Synthesis of the present invention
Fig. 4 is the euthalite Diatomite-based Porous sorbent material and the diatomaceous XRD figure of reacting rear reservation of Hydrothermal Synthesis of the present invention
Fig. 5 is that the C-S-H of the Hydrothermal Synthesis of embodiment 1 is the scanning electron microscope (SEM) photograph of thin plate platy structure
Fig. 6 is that the Tuo Bomo of the Hydrothermal Synthesis of embodiment 2 carrys out the scanning electron microscope (SEM) photograph for stone acicular structure
Fig. 7 is that the euthalite of the Hydrothermal Synthesis of embodiment 3 is the scanning electron microscope (SEM) photograph of spherical shape structure
Fig. 8 is the graph of pore diameter distribution of the different diatom soil matrix porous adsorbents of raw material diatomite and Hydrothermal Synthesis
Fig. 9 is the C-S-H load yeast of Hydrothermal Synthesis with load yeast not to the comparison of methylene blue adsorption number effect
Figure 10 is the tobermorite load yeast of Hydrothermal Synthesis with load yeast not to the comparison of methylene blue adsorption number effect
Figure 11 is the euthalite load yeast of Hydrothermal Synthesis and the not adsorption effect comparison of load yeast to methylene blue
Embodiment
The first step, the commercially available technical grade calcium hydroxide of diatomite, 1g, the 1ml deionized water of 3g being dried, crossed to 80 mesh sieves mix, tabletting machine by mixture by the Tianjin Si Chuanjingshi development in science and technology W270 * D200 of company limited * H450 specification, with 20MPa compression moulding, the demoulding, obtains the sample after moulding.Sample is put into high pressure water heating kettle, controlling temperature of reaction is 200 ℃, reaction times is 24h, the sample obtaining after hydro-thermal reaction detects as shown in Figure 2 by X-ray diffraction analysis method: in Fig. 2, (1) is the XRD figure of diatomite material, (2) be the XRD figure of the C-S-H after Hydrothermal Synthesis, as can be seen from the figure, the main component of diatomite material is quartzy (Quartz) and montmorillonite (Montomorillonite), after Hydrothermal Synthesis, the composition of the Diatomite-based Porous sorbent material obtaining is retaining on the basis of former diatomite (quartz), generated again optimization mineral C-S-H.As shown in Figure 5, C-S-H is thin plate platy structure to the structure of the C-S-H that scanning electron microscope is seen.The folding strength that detects this Diatomite-based Porous sorbent material C-S-H is 18.5Mpa, and specific surface area is 43.08m
2/ g, please see listed table 1 and table 2 below.Table 1 is the specific surface area of the different Diatomite-based Porous sorbent material of diatomite and Hydrothermal Synthesis, and table 2 is the cation exchange capacity of the different Diatomite-based Porous sorbent material of diatomite and Hydrothermal Synthesis.
Table 1
Table 2
Second step, get the C-S-H Diatomite-based Porous sorbent material that 1g aforesaid method prepares, put into the 150ml Erlenmeyer flask that fills liquid nutrient medium, the high reactivity bread beer yeast powder that adds 0.3g Shanghai Angel Yeast Co.,Ltd to produce, regulating pH value is 7, and on the reciprocal shaking table that is 120rpm in speed, with the constant temperatures of 25 ℃, cultivates 24h, with deionized water rinsing, remove meta-bolites, the residual media of yeast, finally obtain the C-S-H Diatomite-based Porous sorbent material of load yeast.
The 3rd step, the C-S-H Diatomite-based Porous sorbent material of load yeast is put into and filled the Erlenmeyer flask that 100ml concentration is the aqueous solution of methylene blue of 1000mg/L, on the reciprocal shaking table that is 120rpm in speed, with the room temperature conditions of 25 ℃, process, the sampling of 60 minute set time of interval, is placed in whizzer, within centrifugal 10 minutes under 15000r/min, gets supernatant liquor, adopt spectrophotometer, in methylene blue maximum absorption wave strong point (665nm), measure absorbancy.By absorbancy-concentration working curve, be converted into aqueous solution of methylene blue concentration.When adsorption time is 48h, methylene blue clearance is 90%, and unit adsorptive capacity is 89.75mg/g.With the not adsorption experiment comparison of the C-S-H Diatomite-based Porous sorbent material of load yeast, after load yeast, adsorptive capacity has improved 62%, please see Figure 9.
The first step, mixes the diatomite of embodiment 1,2.15g calcium hydroxide, 0.5g sodium hydroxide, 1.5ml deionized water, by mixture under tabletting machine with 15MPa compression moulding; Sample after the demoulding is put into high pressure water heating kettle to react.Controlling temperature of reaction is 175 ℃, reaction times is 12h, the sample obtaining after hydro-thermal reaction is after testing as Fig. 3, the XRD figure that wherein (1) is diatomite material, and (2) are the XRD figure of the Diatomite-based Porous sorbent material after Hydrothermal Synthesis, as can be seen from Figure 3, the main component of diatomite material is quartz and montmorillonite, after Hydrothermal Synthesis, and the diatomite base adsorbent obtaining, its composition is retaining on the basis of former diatomite (quartz), has generated optimization mineral tobermorite.As shown in Figure 6, tobermorite is acicular structure to the structure that scanning electron microscope is seen, its folding strength is 26.4Mpa, and specific surface area is 52.78m
2/ g, please see table 1 and table 2.
Second step, except getting the tobermorite Diatomite-based Porous sorbent material that 3g aforesaid method prepares, all the other processing condition are identical with embodiment 1, finally obtain the tobermorite Diatomite-based Porous sorbent material of load yeast.
The 3rd step, except being put into, the tobermorite Diatomite-based Porous sorbent material of load yeast fills the Erlenmeyer flask of aqueous solution of methylene blue that 100ml concentration is 1000mg/L, all the other processing condition are identical with embodiment 1, when adsorption time is 48h, methylene blue clearance is 85%, and unit adsorptive capacity is 73.17mg/g.With the not adsorption experiment comparison of the tobermorite Diatomite-based Porous sorbent material of load yeast, after load yeast, adsorptive capacity has improved 65.4%, please see Figure 10.
Embodiment 3
The first step, mistake 80 mesh sieve diatomite, 0.9g calcium hydroxide, 0.4g sodium hydroxide 1.3ml deionized water that 3g is dried evenly mix, by mixture under tabletting machine with 30MPa compression moulding; Sample after the demoulding is put into high pressure water heating kettle, add the deionized water of volume 1/7 in reactor, sample does not directly contact with water.Controlling temperature of reaction is 200 ℃, reaction times is 24h, the sample obtaining after hydro-thermal reaction is for after testing for euthalite Diatomite-based Porous sorbent material, please see Figure 4, Fig. 4 is that Hydrothermal Synthesis euthalite is optimized diatomite base adsorbent and diatomaceous XRD figure, the XRD figure that wherein (1) is diatomite material, (2) be the XRD figure of the diatomite base adsorbent after Hydrothermal Synthesis, as can be seen from the figure, the main component of diatomite material is quartz and montmorillonite, after Hydrothermal Synthesis, the Diatomite-based Porous sorbent material obtaining, the structure that scanning electron microscope is seen is illustrated in figure 7 spherical shape structure.Its composition is retaining on the basis of former diatomite (quartz), has generated optimization mineral euthalite.Its folding strength is 23.2Mpa, and specific surface area is 74.42m
2/ g.
Second step, gets the euthalite Diatomite-based Porous sorbent material that 3g aforesaid method prepares, and puts into the 150ml Erlenmeyer flask that fills liquid nutrient medium.Add the commercially available yeast powder for the treatment of waste water from dyestuff of 0.5g, regulating pH value is 7, and on the reciprocal shaking table that is 120rpm in speed, with the constant temperatures of 25 ℃, cultivate 24h, with deionized water rinsing, remove meta-bolites, the residual media of yeast, finally obtain the euthalite Diatomite-based Porous sorbent material of load yeast.
The 3rd step, the euthalite Diatomite-based Porous sorbent material of load yeast is put into and filled the Erlenmeyer flask that 100ml concentration is the aqueous solution of methylene blue of 1000mg/L, on the reciprocal shaking table that is 120rpm in speed, with the room temperature conditions of 25 ℃, process, the sampling of interval set time, at whizzer, with under 15000r/min centrifugal 10 minutes, get supernatant liquor, adopt spectrophotometer, in methylene blue maximum absorption wave strong point (665nm), measure absorbancy.By absorbancy-concentration working curve, be converted into aqueous solution of methylene blue concentration.When adsorption time is 48h, methylene blue clearance is 94%, and unit adsorptive capacity is 93.28mg/g.With the not adsorption experiment comparison of the euthalite optimization sorbent material of load yeast, after load yeast, adsorptive capacity has improved 34.0%, please see Figure 11.
The embodiment of the present invention related raw material diatomite original soil place of production used is Shengzhou, Zhejiang Province, its scanning electron microscope (SEM) photograph please see Figure 1, as can be seen from Figure 1, have micropore multistage, a large amount of, ordered arrangement in the diatom wall shell of diatomite original soil, this is the reason that diatomite has favourable absorption.Diatomite is a kind of inorganic mineral material with good self-purification ability, but the main problem existing in engineering application is after absorb polluted matter, to be difficult to and the secondary pollutions such as separated, generation mud of purifying waste water.
Liquid nutrient medium main component of the present invention is not contain the czapek's solution of agar, comprising: 1000ml deionized water, 30g sucrose, 3g SODIUMNITRATE, 1g potassium primary phosphate, 0.5g Repone K, 0.5 magnesium sulfate heptahydrate, 0.01g ferric sulfate.
Hydrothermal Synthesis technology of the present invention can retain on former diatomaceous basis, synthetic obtaining as hydrated calcium silicate gel (C-S-H), tobermorite, euthalite, these mineral have not only improved the intensity of sorbent material after testing, guaranteed not generate mud, also improved porous performance simultaneously, please see table 1 and Fig. 8, as can be seen from Figure 8, after Hydrothermal Synthesis, pore size distribution in sample becomes more extensive in mesoporous scope, be conducive to introduce a large amount of microorganism of load, be conducive to the absorption of dye wastewater, improve sewage treating efficiency.In addition, through detecting after Hydrothermal Synthesis, C-S-H, tobermorite and euthalite Diatomite-based Porous sorbent material, cation exchange capacity has all obtained obvious lifting (please see table 2), and methylene blue dye molecules is cationic dyes, therefore, the sorbent material of Hydrothermal Synthesis has natural advantage to methylene blue adsorption number.
From Fig. 9, Figure 10, Figure 11 adsorption curve, can find out, C-S-H, tobermorite and euthalite Diatomite-based Porous sorbent-loaded and the not adsorption effect contrast of load yeast to methylene blue, all Diatomite-based Porous sorbent materials have good adsorptivity to methylene blue solution itself, and load the Diatomite-based Porous sorbent material of yeast, its absorption methylene blue efficiency be all greatly improved.
Claims (1)
1. a method of processing methylene blue dye waste water, is characterized in that:
The first step, the preparation of high strength Diatomite-based Porous sorbent material
First commercially available diatomite is ground, cross 80 mesh sieves and dry; Then, calcareous raw material, alkali-activator, water are added in the diatomite of oven dry, mix, compression moulding under the pressure of 5～40MPa, obtains the sample after moulding; Finally, the sample after moulding is put into high-pressure hydrothermal reaction kettle, controlling temperature is 100～200 ℃, and reaction times 1～48h, obtains high strength Diatomite-based Porous sorbent material; After testing, the high strength Diatomite-based Porous sorbent material making has good water resistant power shear effect, the diatomite that its composition retains after for reaction, and a kind of in the synthetic hydrated calcium silicate gel of hydro-thermal reaction, tobermorite, euthalite or 2 kinds or 3 kinds of forming in any proportion;
The quality that adds of above-mentioned calcareous raw material, alkali-activator, water is respectively 10～50%, 5～20% of diatomite quality, 5～50% mass percents;
Above-mentioned calcareous raw material is selected from the 2-5 kind a kind of or that form in any proportion in slaked lime, Wingdale, unslaked lime, rhombspar, lime feldspar;
Above-mentioned alkali-activator is selected from the 2-5 kind a kind of or that form in any proportion in sodium hydroxide, sodium metaaluminate, water glass, Starso, flyash;
Second step, the preparation of Diatomite-based Porous sorbent-loaded yeast
The high strength Diatomite-based Porous sorbent material that the first step is obtained is put into the Erlenmeyer flask that fills liquid nutrient medium, add yeast powder, the add-on of yeast powder is 5%～20% mass percent of high strength Diatomite-based Porous adsorbent mass, regulating pH value is 5～8, on the reciprocal shaking table of speed 60rpm～120rpm, the constant temperature of 15～35 ℃ is cultivated 2h～48h, obtains the Diatomite-based Porous sorbent material of load yeast;
Yeast powder used is commercially available bread beer yeast powder, or the commercially available yeast powder for the treatment of waste water from dyestuff;
The 3rd step, methylene blue dye wastewater treatment
The Diatomite-based Porous sorbent material 1～10g that adds the load yeast of second step in the methylene blue dye waste water that is 100～1000mg/L every liter of concentration, by pH regulator to 4～10, and on the reciprocal shaking table that is 60rpm～120rpm in speed, at 25～45 ℃, process 1h～48h, by spectrophotometer method, measure the concentration of processing rear methylene blue waste water, result shows, the clearance of methylene blue dye surpasses 90%, and unit adsorptive capacity surpasses 80mg/g.
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| CN110449114A (en) * | 2019-07-23 | 2019-11-15 | 衡阳师范学院 | A kind of preparation method and application for mixing aluminium eakleite material |
| CN113231010A (en) * | 2021-06-03 | 2021-08-10 | 中南大学 | Polytype zeolite/C-S-H composite adsorption material and preparation method and application thereof |
| CN114887585A (en) * | 2022-05-13 | 2022-08-12 | 华南理工大学 | Calcium-based zeolite prepared from Ca-induced halloysite and preparation method and application thereof |
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