CN110548476A - Preparation method and application of modified volcanic cinders filter material - Google Patents
Preparation method and application of modified volcanic cinders filter material Download PDFInfo
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- CN110548476A CN110548476A CN201910939683.XA CN201910939683A CN110548476A CN 110548476 A CN110548476 A CN 110548476A CN 201910939683 A CN201910939683 A CN 201910939683A CN 110548476 A CN110548476 A CN 110548476A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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Abstract
The invention discloses a preparation method and application of a modified volcanic cinders filter material, and belongs to the technical field of water treatment. The preparation method comprises the steps of screening the volcanic cinders, then pretreating, taking ferric chloride as a modifier, soaking the pretreated volcanic cinders in a modification solution, drying after a certain time, placing in a muffle furnace for calcining, and finishing modification through multiple operations. The modified volcanic cinders filter material prepared by the method has a large specific surface area and a developed pore structure, the method disclosed by the invention cannot cause the problem of secondary pollution, volcanic cinders are cheap and easy to obtain, the modification method and the adsorption process are simple to operate, the treatment effect is good, the treatment cost is greatly saved, and the modified volcanic cinders filter material can be widely applied to the field of water treatment industry.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a preparation method and application of a modified volcanic cinders filter material.
Background
The phenol wastewater mainly refers to highly toxic organic pollutant wastewater generated in the production of petrochemical industry, pharmaceutical industry and the like. The development of an effective harmless treatment is urgently required because of the problems of respiratory irritation, liver damage, irregular heartbeat, and nervous system disorder caused by long-term exposure to Phenol wastewater (Diana P. Vargas, Liliana Giraldo, Juan Carlos Moreo. No. -Pirajan. Effect of therapeutic and Chemical Characteristics of active carbon on Phenol Adsorption in Aqueous Solutions [ J ]. Polish Journal of Chemical Technology,2017,19(4): 87-93.).
The adsorption method is widely applied to the aspect of wastewater treatment at present, and the harmful substances in the wastewater are adsorbed into pore channels by utilizing the porosity of a solid adsorbent (a small group, Shen, talking about the national monarch and the like. experimental research on phenol removal by an ozone/biological activated carbon process [ J ]. Chinese water supply and drainage 2015,31(01): 69-71.). The adsorbents commonly available on the market are activated carbon, adsorbent resins, modified chitosan adsorbents, etc., which are widely used but are expensive (Jordan Georgin, Dison S.P. Franco, Patricia Gransi, et al. patent of center fire bark ash adsorbent for the removal of 97dye from resource effluences [ J ]. Environmental Science and Pollution Research,2019,26(19): 19207-.
The volcanic cinders are low-cost porous materials which are rich in mineral resources and convenient to mine, have the advantages of acid and alkali resistance, corrosion resistance, good permeability and the like, and can be used as adsorbing materials (Wangwu, research progress on preparing green building materials by using regional natural raw materials volcanic cinders [ J ]. Chinese building materials, 2018, (07): 121-124.). However, the specific surface area of the original volcanic cinders is not high, and the aperture is too large, so that the effect of directly adsorbing the volcanic cinders is not ideal.
Disclosure of Invention
The invention aims to solve the problems of high cost, difficult operation of modifying a filter material and complex process of treating phenol wastewater of the existing adsorbent, and provides a preparation method and application of a modified volcanic cinders filter material.
In order to achieve the purpose, the invention provides the following scheme:
The invention provides a preparation method of a modified volcanic cinders filter material, which comprises the following steps:
(1) Sieving the scoria, cleaning, drying and then carrying out pretreatment;
(2) And (2) coating modification, namely soaking the volcanic cinders pretreated in the step (1) in FeCl 3 solution, drying, then placing the volcanic cinders in a muffle furnace for ignition, and repeating the steps of soaking, drying and ignition until the surface of the volcanic cinders is not wet any more, thus obtaining the modified volcanic cinders filter material.
As a further improvement of the invention, the sieving in the step (1) is to sieve the scoria through 1.5mm and 1.0mm of apertures respectively.
As a further improvement of the invention, the pretreatment in the step (1) is to soak the dried volcanic cinders in dilute hydrochloric acid for 24-36h, wash the volcanic cinders to be neutral by distilled water, dry the volcanic cinders and cool the volcanic cinders. The pretreatment process comprises the steps of cleaning dust on the surface of volcanic cinders, removing impurities blocking gaps and providing a larger space for coating modification.
As a further improvement of the invention, the drying temperature in the step (1) is 100-120 ℃.
As a further improvement of the invention, the feed-liquid ratio of the scoria to the FeCl 3 solution in the step (2) is 5 g: 8 mL.
As a further improvement of the invention, the soaking time of the step (2) is 10-25 min.
As a further improvement of the invention, the drying temperature in the step (2) is 100-120 ℃.
As a further improvement of the invention, the burning temperature of the step (2) is 400-.
as a further improvement of the invention, the coating times are more than or equal to 4. The coating times are more than or equal to 4, so that the modified coating is more uniform, and the adhesion of the surface modifier on the surface of the volcanic cinders is enhanced.
the invention also provides a modified volcanic cinders filter material prepared by the preparation method.
The invention also provides application of the modified volcanic cinders filter material, and the modified volcanic cinders filter material is applied to adsorption treatment of wastewater.
As a further improvement of the invention, the modified volcanic cinders filter material is applied to the adsorption treatment of phenol-containing wastewater.
As a further improvement of the invention, the modified volcanic cinders filter material is applied to the adsorption treatment of the phenol-containing wastewater, and comprises the following steps:
The modified volcanic cinders filter material is placed in waste water containing phenol, the addition amount is 1% -5%, the pH value of the phenol waste water is adjusted to 6.5-7.5, vibration adsorption is carried out at the temperature of 25-35 ℃, the modified volcanic cinders filter material is taken out after 2.5-3.5h, the vibration speed is 80 r.min -1, and the modified volcanic cinders filter material is filtered after standing for 10 min.
The invention discloses the following technical effects:
3The method comprises the steps of firstly, pretreating the volcanic cinders, namely cleaning dust on the surface of the volcanic cinders, soaking the volcanic cinders in dilute hydrochloric acid, removing impurities blocking gaps, cleaning the surface of the volcanic cinders, and providing a larger space for coating modification.
The modified volcanic cinders filter material prepared by the invention has the advantages of low cost, low metal leaching toxicity, no secondary pollution problem such as sludge and the like, high adsorption efficiency and convenient recovery.
the modified volcanic cinders filter material provided by the invention has the effects of high efficiency and low cost, and solves the problems of high cost, difficult operation of filter material modification and complex process of treating phenol wastewater of the existing adsorbent. The modified volcanic cinders filter material is used for treating phenol wastewater, so that water treatment cost is saved, and reference is provided for phenol wastewater adsorption tests.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a scanning electron micrograph of the modified volcanic cinders filter material prepared in example 1;
FIG. 2 is a graph showing the effect of the modified volcanic cinders filter material prepared in example 1 on the adsorption treatment effect of phenol-simulated wastewater;
FIG. 3 is a graph showing the effect of the modified volcanic cinders prepared in example 1 on the adsorption treatment effect due to the time for adsorbing phenol simulation wastewater;
FIG. 4 is a graph showing the effect of pH value of simulated phenol wastewater adsorbed by the modified volcanic slag filter material prepared in example 1 on the adsorption treatment;
FIG. 5 is a graph showing the effect of simulated phenol wastewater temperature adsorption on the adsorption treatment effect of the modified volcanic slag filter material prepared in example 1;
FIG. 6 is a graph showing the effect of simulated wastewater concentration of phenol adsorption on the adsorption treatment in the modified volcanic cinders prepared in example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
in order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
Firstly, sieving the volcanic cinders by using sieves with the apertures of 1.5mm and 1.0mm respectively, repeatedly washing the volcanic cinders by using tap water, drying the volcanic cinders in a 110 ℃ drying oven, taking out the volcanic cinders after drying, pretreating the volcanic cinders in a 0.lmol.L -1 diluted hydrochloric acid solution, soaking the volcanic cinders for 24 hours, washing the volcanic cinders to be neutral by using distilled water, drying the volcanic cinders in the 110 ℃ drying oven, taking out the volcanic cinders after the pretreatment is finished by cooling, soaking 50g of the pretreated volcanic cinders in 80mL of 2.5 mol.L -1 FeCl 3 solution for 20 minutes, drying the volcanic cinders in the 110 ℃ drying oven, finally, burning the volcanic cinders in a muffle furnace at 400 ℃ for 4 hours, taking out the volcanic cinders and cooling the volcanic cinders at room temperature, and repeating the steps for multiple times until the surface of the modified volcanic.
FIG. 1 is a scanning electron microscope image of the modified volcanic cinders filter material prepared in this example. As shown in figure 1, the modified volcanic cinders filter material has a large number of pores on the surface, and the specific surface area is greatly increased, so that the adsorption effect can be improved. The surface of the modified volcanic cinders is free from cracking and crazing, which shows that the modified iron oxide coating is firmly combined with the volcanic cinders.
example 2
The modified volcanic cinders filter material prepared in example 1 is used as an adsorbent, 100mL of phenol simulated wastewater with the concentration of 30mg & L -1 is placed in 6 conical flasks with the concentration of 250mL, the pH value is adjusted to 7, 2.0g, 2.5g, 3.0g, 3.5g, 4.0g and 4.5g of iron-coated modified volcanic cinders with different amounts are respectively added, the mixture is taken out after being uniformly oscillated for 2.5 hours at 30 ℃ by an oscillator, the mixture is placed for 10min and then filtered, and the absorbance of the filtered solution is measured by a TU-1901 double-beam ultraviolet-visible spectrophotometer.
FIG. 2 is a graph showing the effect of the modified volcanic cinders filter material prepared in example 1 on the adsorption treatment effect of phenol-simulated wastewater; as shown in FIG. 2, when the amount of the iron-coated modified volcanic cinders used as a filter material is 2.0g, the removal rate and the adsorption amount of phenol are high, so that the optimal amount of the adsorbent is 2.0 g.
Example 3
The modified volcanic cinders filter material prepared in the example 1 is used as an adsorbent, 100mL of phenol simulated wastewater with the concentration of 30mg & L -1 is put into 6 conical flasks with the concentration of 250mL, the pH value is adjusted to be 7, 2.0g of iron-coated modified volcanic cinders are added respectively, the mixture is taken out after being uniformly oscillated for 1.0h, 1.5h, 2.0h, 2.5h, 3.0h and 3.5h at 30 ℃ by an oscillator respectively, the mixture is kept stand for 10min and then filtered, and the absorbance of the filtered solution is measured by a TU-1901 double-beam ultraviolet-visible spectrophotometer.
FIG. 3 is a graph showing the effect of the modified volcanic cinders prepared in example 1 on the adsorption treatment effect due to the time for adsorbing phenol simulation wastewater; as shown in FIG. 3, the phenol removal rate and the amount of adsorption of the adsorbent gradually increased with the increase of the adsorption time, and the removal rate and the amount of adsorption of the adsorbent tended to decrease after 3.0 hours. When the adsorption time is 3.0h, the adsorption is balanced, and the phenol removal amount and the adsorption amount are both high; the adsorption equilibrium is destroyed by continuously prolonging the adsorption time, so the optimal adsorption time is 3.0 h.
Example 4
The modified volcanic cinders filter material prepared in example 1 was used as an adsorbent, 100mL of phenol-simulated wastewater of 30mg · L -1 was put in 6 250mL conical flasks, 2.0g of iron-coated modified volcanic cinders were added, pH values were adjusted to 1.5, 3.0, 4.5, 6.0, 7.5, and 9.0, and the mixture was shaken at 30 ℃ for 3.0 hours at constant speed by a shaker, and then taken out, and after standing for 10min, the solution was filtered, and absorbance thereof was measured by TU-1901 dual-beam uv-vis spectrophotometry.
FIG. 4 is a graph showing the effect of pH value of simulated phenol wastewater adsorbed by the modified volcanic slag filter material prepared in example 1 on the adsorption treatment; as shown in fig. 4, the phenol removal rate and the adsorption amount of the adsorbent increase with the increase of the pH, and decrease with the pH of 7.5, and when the pH is 7.5, the phenol removal rate and the adsorption amount are both high, and the adsorption reaches equilibrium; when the pH value is too low, the solution is in a strong acid state, so that the adsorption balance is damaged; when the pH value is too high, the solution is in a strong alkaline state, phenol is in weak acidity, neutralization reaction occurs, adsorption is influenced, and the optimal pH value is 7.5.
Example 5
The modified volcanic cinders filter material prepared in example 1 was used as an adsorbent, 100mL of phenol-simulated wastewater 30mg · L -1 was placed in 6 250mL conical flasks, pH was adjusted to 7.5, 2.0g of iron-coated modified volcanic cinders were added, the mixture was shaken at constant speed by an oscillator at 15 ℃,20 ℃, 25 ℃, 30 ℃, 35 ℃ and 40 ℃ for 3.0h, then taken out, left to stand for 10min and filtered, and the absorbance of the filtered solution was measured by TU-1901 dual-beam uv-vis spectrophotometry.
FIG. 5 is a graph showing the effect of simulated phenol wastewater temperature adsorption on the adsorption treatment effect of the modified volcanic slag filter material prepared in example 1; as shown in fig. 5, the phenol removal rate and the adsorption amount of the adsorbent increase with the increase of the adsorption temperature, and decrease with the temperature of 30 ℃, and when the temperature reaches 30 ℃, the system reaches the adsorption equilibrium, and desorption occurs at the increased temperature, so the optimum adsorption temperature is 30 ℃.
Example 6
Using the iron-coated modified volcanic cinders obtained in example 1 as an adsorbent, 100mL of phenol-simulated wastewater having a concentration of 30 mg. L -1, 60 mg. L -1, 100 mg. L -1, 150 mg. L -1, 180 mg. L -1, and 200 mg. L -1 was placed in 6 250mL conical flasks, respectively, adjusted to pH 7.5, added with 2.0g, 4.0g, 6.7g, 10.0g, 12.0g, and 13.4g of iron-coated modified volcanic cinders, respectively, and shaken at 30 ℃ for 3.0 hours at a constant speed by a shaker, and then taken out, left to stand for 10 minutes, filtered, and the absorbance of the filtered solution was measured by a TU-1901 dual-beam UV-visible spectrophotometer.
FIG. 6 is a graph showing the effect of the modified volcanic cinders prepared in example 1 on the adsorption treatment effect due to the concentration of the simulated phenol wastewater, wherein as shown in FIG. 6, the removal rate and the adsorption amount of phenol by the adsorbent are almost the same as the concentration of the simulated phenol wastewater increases when the concentration of the simulated phenol wastewater is within 150 mg.L -1, and wherein as the concentration of the simulated phenol wastewater exceeds 150 mg.L -1, the removal rate and the adsorption amount of phenol by the adsorbent gradually decrease as the concentration of the simulated phenol wastewater increases due to the lack of adsorption time and insufficient adsorption space in the same proportion, so that the iron-coated modified volcanic cinders are suitable for treating the phenol waste liquid with the concentration of 30-150 mg.L -1.
Example 7
The iron-coated modified volcanic cinders prepared in example 1 were used as an adsorbent, 100mL of simulated phenol wastewater with a concentration of 30mg · L -1 was placed in a 250mL conical flask, 2g of modified volcanic cinders were added, the pH value was adjusted to 7.5, the wastewater was taken out after shaking at 30 ℃ for 3.0h with an oscillator at a constant speed, the filtrate was allowed to stand for 10min and the absorbance of the filtrate was measured by TU-1901 dual-beam uv-vis spectrophotometer.
Comparative example 1
Firstly, sieving the volcanic cinders by using sieves with the apertures of 1.5mm and 1.0mm respectively, repeatedly washing the volcanic cinders by using tap water, placing the volcanic cinders in an oven at the temperature of 110 ℃ for drying, then taking the volcanic cinders as an adsorbent, placing 100mL of simulated phenol wastewater with the concentration of 30 mg.L -1 in a 250mL conical flask, adding 2g of unmodified volcanic cinders, adjusting the pH value to 7.5, oscillating the volcanic cinders at the temperature of 30 ℃ for 3.0 hours at a constant speed by using an oscillator, taking the volcanic cinders out, standing the volcanic cinders for 10 minutes, filtering the volcanic cinders, and measuring the absorbance of the filtered solution by using a TU.
As a result, it was found that the phenol waste water was directly adsorbed by the unmodified scoria, and that the phenol removal rate was 39.7% and the adsorption amount was 0.506mg g -1.
According to the above contents, the consumption of the modified volcanic cinders filter material is 2.0-2.5g, preferably 2.0g, and the adsorption effect is better, researches show that when the initial concentration of the phenol simulation wastewater is 30 mg.L -1, and the consumption of the adsorbent is 2.0g, the adsorption rate and the adsorption capacity of the iron-coated modified volcanic cinders to the phenol reach a saturated state.
From the above, the adsorption time of the modified volcanic cinders filter material is 2.5-3.5h, preferably 3.0h, and the adsorption effect is better. Researches find that when the adsorption time is 3.0h, the adsorption rate and the adsorption capacity of the iron-coated modified volcanic cinders to phenol reach a saturated state.
From the above, the modified volcanic cinders filter material has a pH value of 6.5-7.5, preferably 7.5, and has a better adsorption effect. Research shows that when the adsorption pH value is 7.5, the adsorption rate and the adsorption quantity of the iron-coated modified volcanic cinders to the phenol reach a saturated state.
From the above, the adsorption temperature of the modified volcanic cinders filter material is 25-35 ℃, preferably 30 ℃, and the adsorption effect is better. Researches show that when the adsorption temperature is 30 ℃, the adsorption rate and the adsorption quantity of the iron-coated modified volcanic cinders to phenol reach a saturated state.
From the above, it is known that the initial concentration of the phenol wastewater is 30-200 mg.L -1, more preferably 30-150 mg.L -1, and the adsorption effect is better, and studies show that when the initial concentration is 30-150 mg.L -1, the adsorption rate is not greatly different and the adsorption amount is almost the same with the increase of the initial concentration of the phenol simulated wastewater, and when the initial concentration exceeds 150 mg.L -1, the adsorption rate and the adsorption amount are sharply reduced due to insufficient adsorption time and insufficient adsorption space in the same proportion.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. the preparation method of the modified volcanic cinders filter material is characterized by comprising the following steps of:
(1) Sieving the scoria, cleaning, drying and then carrying out pretreatment;
(2) And (2) coating modification, namely soaking the volcanic cinders pretreated in the step (1) in FeCl 3 solution, drying, then placing the volcanic cinders in a muffle furnace for ignition, and repeating the steps of soaking, drying and ignition until the surface of the volcanic cinders is not wet any more, thus obtaining the modified volcanic cinders filter material.
2. The method for preparing the modified volcanic cinders filter material as claimed in claim 1, wherein the sieving in step (1) is performed by sieving the volcanic cinders with sieves with 1.5mm and 1.0mm apertures respectively.
3. The preparation method of the modified volcanic cinders filter material as claimed in claim 1, wherein the pretreatment in step (1) comprises soaking the dried volcanic cinders in dilute hydrochloric acid for 24-36h, washing with distilled water to neutrality, drying, and cooling.
4. The method for preparing the modified volcanic cinders filter material as claimed in claim 1, wherein the drying temperature in step (1) is 100-120 ℃.
5. The preparation method of the modified volcanic cinders filter material as claimed in claim 1, wherein the feed-liquid ratio of volcanic cinders to the FeCl 3 solution in the step (2) is 5 g: 8 mL.
6. the method for preparing the modified volcanic cinders filter material as claimed in claim 1, wherein the soaking time in the step (2) is 10-25 min.
7. The method for preparing the modified volcanic cinders filter material as claimed in claim 1, wherein the drying temperature in the step (2) is 100-120 ℃.
8. the method for preparing the modified volcanic cinders filter material as claimed in claim 1, wherein the burning temperature in the step (2) is 400-.
9. A modified volcanic cinders filter material, characterized in that, it is prepared by the preparation method of any one of claims 1-8.
10. The use of the modified volcanic cinders filter material of claim 9, wherein the modified volcanic cinders filter material is used for the adsorption treatment of wastewater.
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| CN114602423A (en) * | 2022-03-30 | 2022-06-10 | 张更宇 | Preparation method of modified volcanic cinders filler |
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Application publication date: 20191210 |