CN110180492B - Active filter material for removing magnesium ions, and preparation method and application thereof - Google Patents
Active filter material for removing magnesium ions, and preparation method and application thereof Download PDFInfo
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- CN110180492B CN110180492B CN201910309803.8A CN201910309803A CN110180492B CN 110180492 B CN110180492 B CN 110180492B CN 201910309803 A CN201910309803 A CN 201910309803A CN 110180492 B CN110180492 B CN 110180492B
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/06—Contaminated groundwater or leachate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
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Abstract
The invention belongs to the technical field of active filter materials, and particularly relates to a preparation method of an active filter material for removing magnesium ions, which comprises the following steps of S1, uniformly mixing quartz sand and an acid solution with the mass concentration of 10-15% according to the mass ratio of (1-2) to 1, stirring for 40-50h, filtering, taking out a filter cake, and drying to obtain a product A; s2, uniformly mixing the product A with an alkali solution I with the mass concentration of 10-15% according to the mass ratio of 1 (1-1.5), and stirring for 40-50h to obtain a product B; s3, uniformly mixing the product B with a magnesium ion solution with the mass concentration of 10% -12% according to the mass ratio of 1 (1-1.8), stirring and soaking for 2-4h, and adding an alkali solution II with the mass concentration of 12% -16% to obtain a product C; s4, washing off the magnesium sulfate solution and the second alkali solution remained on the surface of the product C, and drying to obtain the active filter material. The invention has the beneficial effects that: the active filter material obtained by the method has fine granularity, is in a colorless crystal state, and can quickly and efficiently remove magnesium ions.
Description
Technical Field
The invention belongs to the technical field of active filter materials, and particularly relates to an active filter material for removing magnesium ions, and a preparation method and application thereof.
Background
At present, the monitoring of various sewage treatment plants shows that the content of magnesium ions in the leachate generated by the waste incineration power generation is high, although magnesium is an essential element for the growth of human bodies, the high-concentration magnesium ions bring some disadvantages to production and life. For example, when the effluent containing high magnesium ions is recycled, the pipeline can be blocked due to scaling in the pipeline, and in addition, the leachate of the waste incineration power generation with high magnesium ions can inhibit microorganisms in the activated sludge so as to influence the quality of the effluent.
At present, there are many methods for removing magnesium ions from leachate generated by garbage incineration power generation, such as a biological adsorbent method and an activated sludge method. The biological adsorbent method has good effect of removing magnesium ions, but the removal effect is unstable and can be influenced by some external environmental factors (initial magnesium ion concentration and stirring speed); the activated sludge process is fast and efficient in removing magnesium ions, but is susceptible to the pH of the solution.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for preparing an active filter material for removing magnesium ions, which is stable and efficient in removing magnesium ions.
The invention provides the following technical scheme:
a preparation method of an active filter material for removing magnesium ions comprises the following steps,
s1, uniformly mixing quartz sand and an acid solution with the mass concentration of 10-15% according to the mass ratio of (1-2) to 1, stirring for 40-50h, filtering, taking out a filter cake, and drying to obtain a product A;
s2, uniformly mixing the product A with an alkali solution I with the mass concentration of 10-15% according to the mass ratio of 1 (1-1.5), stirring for 40-50h, filtering, taking out and drying a filter cake, calcining for 3-5h at the temperature of 300-500 ℃, and cooling to 20-30 ℃ to obtain a product B;
s3, uniformly mixing the product B with a magnesium ion solution with the mass concentration of 10% -12% according to the mass ratio of 1 (1-1.8), stirring and soaking for 2-4h, adding a second alkali solution with the mass concentration of 12% -16%, controlling the pH to be 9-10, stirring and reacting for 1-2h at 20-30 ℃, filtering, and taking out a filter cake to obtain a product C;
and S4, washing away the magnesium ion solution and the alkali solution II remained on the surface of the product C, and drying to obtain the active filter material.
Preferably, in the S2, before the product A and the alkaline solution I with the mass concentration of 10% -15% are uniformly mixed according to the mass ratio of 1 (1-1.5), the product A is washed for 2-4 times by using the alkaline solution with the mass concentration of 1% -3% for 3-5min each time.
Preferably, in S1, the acid solution is selected from any one of a hydrochloric acid solution, a sulfuric acid solution, an oxalic acid solution, and a hydrofluoric acid solution, or a mixture of any several of them;
in the S2, the alkali solution I is any one or a mixture of any more of a sodium hydroxide solution, a potassium hydroxide solution and a lithium hydroxide solution;
in the S3, the second alkali solution is any one or a mixture of any more of a sodium hydroxide solution, a potassium hydroxide solution and a lithium hydroxide solution.
Preferably, in S3, the magnesium ion solution is a magnesium sulfate solution or a magnesium chloride solution.
Preferably, the method for washing away the magnesium ion solution and the second alkali solution remaining on the surface of the product C in S4 is to wash the product C for 1 to 3 times and 3 to 5min each time by using a sodium hydroxide solution with a mass concentration of 1 to 3 percent, and wash the product C for 2 to 4 times and 3 to 5min each time by using distilled water.
Preferably, the particle size of the quartz sand is 1.2-1.5 mm.
The invention also provides an active filler prepared by the method of any one of the above.
The active filler is used for removing magnesium ions in the leachate generated by the waste incineration power generation.
The invention has the beneficial effects that:
1. the invention carries out etching treatment on the quartz sand under acidic and alkaline conditions in turn,converting magnesium ions to Mg (OH) under basic conditions 2 Precipitating and adsorbing on the surface of quartz sand to obtain an active filter material, wherein the obtained active filter material has fine granularity, is in a colorless crystal state, and can rapidly and efficiently remove magnesium ions.
2. The preparation method is carried out at normal temperature, heating is not needed, and the whole operation is simple.
3. The active filter material prepared by the invention can effectively reduce the concentration of magnesium ions in the garbage incineration power generation leachate, the removal rate of the magnesium ions is over 80 percent, the active filler with the best effect can achieve the removal rate of the magnesium ions by 90.2 percent.
Detailed Description
The present invention will be described in detail with reference to the following examples.
Example 1
A preparation method of an active filter material for removing magnesium ions comprises the following steps,
s1, uniformly mixing quartz sand with the particle size of 1.2mm and a hydrochloric acid solution with the mass concentration of 10% according to the mass ratio of 1:1, stirring for 40 hours, filtering, taking out a filter cake, and drying to obtain a product A;
s2, washing the product A for 2 times by using a sodium hydroxide solution with the mass concentration of 1%, each time for 5min, uniformly mixing the washed product A with a sodium hydroxide solution with the mass concentration of 10% according to the mass ratio of 1:1, stirring for 40h, filtering, taking out and drying a filter cake, calcining for 5h at 300 ℃, and cooling to 20 ℃ to obtain a product B;
s3, uniformly mixing the product B with a magnesium sulfate solution with the mass concentration of 10% according to the mass ratio of 1:1, stirring and soaking for 2 hours, adding a sodium hydroxide solution with the mass concentration of 12%, controlling the pH to be 9, stirring and reacting for 1 hour at 20 ℃, filtering, and taking out a filter cake to obtain a product C;
and S4, washing the filter material for 1 time and 3min each time by using a sodium hydroxide solution with the mass concentration of 1%, washing the filter material for 2 times and 3min each time by using distilled water, washing the residual magnesium sulfate solution and the residual sodium hydroxide solution on the surface of the product C, and drying to obtain the active filter material.
Example 2
A preparation method of an active filter material for removing magnesium ions comprises the following steps,
s1, uniformly mixing quartz sand with the particle size of 1.4mm and a hydrochloric acid solution with the mass concentration of 12% according to the mass ratio of 1.5:1, stirring for 48 hours, filtering, taking out a filter cake, and drying to obtain a product A;
s2, washing the product A for 3 times by using a sodium hydroxide solution with the mass concentration of 2%, wherein each time is 4min, uniformly mixing the washed product A with a sodium hydroxide solution with the mass concentration of 12% according to the mass ratio of 1:1.2, stirring for 48h, filtering, taking out and drying a filter cake, calcining for 4h at 400 ℃, and cooling to 25 ℃ to obtain a product B;
s3, uniformly mixing the product B with a magnesium sulfate solution with the mass concentration of 11% according to the mass ratio of 1:1.4, stirring and soaking for 3 hours, adding a sodium hydroxide solution with the mass concentration of 14%, controlling the pH to be 9, stirring and reacting for 1 hour at 25 ℃, filtering, and taking out a filter cake to obtain a product C;
and S4, washing the filter material for 2 times and 4min each time by using a sodium hydroxide solution with the mass concentration of 1-3%, washing the filter material for 3 times and 4min each time by using distilled water, washing the residual magnesium sulfate solution and the residual sodium hydroxide solution on the surface of the product C, and drying to obtain the active filter material.
Example 3
A preparation method of an active filter material for removing magnesium ions comprises the following steps,
s1, uniformly mixing quartz sand with the particle size of 1.2mm and a hydrochloric acid solution with the mass concentration of 10% according to the mass ratio of 1.5:1, stirring for 50 hours, filtering, taking out a filter cake, and drying to obtain a product A;
s2, washing the product A for 2 times and 3min each time by using a sodium hydroxide solution with the mass concentration of 3%, uniformly mixing the washed product A with a sodium hydroxide solution with the mass concentration of 10 according to the mass ratio of 1:1.3, stirring for 40h, filtering, taking out and drying a filter cake, calcining for 5h at 500 ℃, and cooling to 20 ℃ to obtain a product B;
s3, uniformly mixing the product B with a magnesium sulfate solution with the mass concentration of 12% according to the mass ratio of 1:1.6, stirring and soaking for 4 hours, adding a sodium hydroxide solution with the mass concentration of 14%, controlling the pH to be 9, stirring and reacting for 1 hour at 30 ℃, filtering, and taking out a filter cake to obtain a product C;
and S4, washing for 1 time and 3min each time by using a sodium hydroxide solution with the mass concentration of 1%, washing for 2 times and 5min each time by using distilled water, washing out the magnesium sulfate solution and the sodium hydroxide solution which are remained on the surface of the product C, and drying to obtain the active filter material.
Example 4
A preparation method of an active filter material for removing magnesium ions comprises the following steps,
s1, uniformly mixing quartz sand with the particle size of 1.2mm and a hydrochloric acid solution with the mass concentration of 15% according to the mass ratio of 1.2:1, stirring for 40 hours, filtering, taking out a filter cake, and drying to obtain a product A;
s2, washing the product A for 4 times, each time for 5min, by using a sodium hydroxide solution with the mass concentration of 1%% to uniformly mix the washed product A with a sodium hydroxide solution with the mass concentration of 15% according to the mass ratio of 1:1.5, stirring for 50h, filtering, taking out and drying a filter cake, calcining for 5h at 500 ℃, and cooling to 30 ℃ to obtain a product B;
s3, uniformly mixing the product B with a magnesium sulfate solution with the mass concentration of 10% according to the mass ratio of 1:1.5, stirring and soaking for 4 hours, adding a sodium hydroxide solution with the mass concentration of 14%, controlling the pH to be 10, stirring and reacting for 1-2 hours at 30 ℃, filtering, and taking out a filter cake to obtain a product C;
and S4, washing the filter material for 1 time and 5min each time by using a sodium hydroxide solution with the mass concentration of 3%, washing the filter material for 2 times and 5min each time by using distilled water, washing the residual magnesium sulfate solution and the residual sodium hydroxide solution on the surface of the product C, and drying to obtain the active filter material.
Example 5
A preparation method of an active filter material for removing magnesium ions comprises the following steps,
s1, uniformly mixing quartz sand with the particle size of 1.5mm and a hydrochloric acid solution with the mass concentration of 15% according to the mass ratio of 2:1, stirring for 50 hours, filtering, taking out a filter cake, and drying to obtain a product A;
s2, washing the product A for 4 times by using a sodium hydroxide solution with the mass concentration of 3%, each time for 5min, uniformly mixing the washed product A with a sodium hydroxide solution with the mass concentration of 15% according to the mass ratio of 1:1.5, stirring for 50h, filtering, taking out and drying a filter cake, calcining for 5h at 500 ℃, and cooling to 30 ℃ to obtain a product B;
s3, uniformly mixing the product B with a magnesium sulfate solution with the mass concentration of 12% according to the mass ratio of 1:1.8, stirring and soaking for 4 hours, adding a sodium hydroxide solution with the mass concentration of 16%, controlling the pH to be 10, stirring and reacting for 2 hours at 30 ℃, filtering, and taking out a filter cake to obtain a product C;
and S4, washing for 3 times and 5min each time by using a sodium hydroxide solution with the mass concentration of 3%, washing for 4 times and 5min each time by using distilled water, washing away the magnesium sulfate solution and the sodium hydroxide solution which are remained on the surface of the product C, and drying to obtain the active filter material.
In embodiments 1 to 5 of the present invention, the magnesium sulfate solution may be replaced with a magnesium chloride solution;
the hydrochloric acid solution can be replaced by any one or a mixture of any more of hydrochloric acid solution, sulfuric acid solution, oxalic acid solution and hydrofluoric acid solution;
the sodium hydroxide solution can be replaced by any one or a mixture of any more of sodium hydroxide solution, potassium hydroxide solution and lithium hydroxide solution.
Detection of magnesium ion removal performance
After sequentially carrying out aeration, coagulation, precipitation and quartz sand filtration treatment on the refuse incineration power generation leachate, introducing supernate into 5 parallel reactors with the diameter of 45mm and the height of 1.2m, and correspondingly filling the 5 reactors with the active filter materials prepared in the embodiments 1-5, wherein the filling heights are all 0.8 m. The flow rate of the percolate is controlled at 18L/h, the operation is continuously carried out for 30 days, the active filter material is washed once every 3 days by using distilled water, the magnesium ion concentration of the water inlet and the water outlet of 5 reactors is respectively detected every day, and the results are shown in the following table.
As can be seen from the above table, the active filter material prepared by the invention can effectively reduce the concentration of magnesium ions in the leachate generated by garbage incineration and power generation, and the removal rate of the magnesium ions is more than 80%, wherein the best effect is the active filler prepared in example 2, and the removal rate of the magnesium ions reaches 90.2%, because the quartz sand is pickled to remove metal impurities on the surface, the granularity of the quartz sand is reduced, the porosity is increased, the specific surface area of the substrate is increased, and after the quartz sand is soaked and calcined in the alkaline solution with the concentration corresponding to that of example 2, the quartz sand is Mg (OH) 2 The content of the silicate is more abundant and full due to the diversity of the non-zeolite pore canal structure of the silicate. OH during the actual reaction - Too high or too low a concentration of (b) may result in loss of magnesium ions or incomplete reaction, thereby reducing the removal rate. However, the active filter material prepared in example 2 sufficiently exerts the adsorption effect of magnesium ions in the landfill leachate with the aid of the pore effect of quartz sand, so as to improve the removal rate of the filter material on the magnesium ions, and the removal rate of the magnesium ions in the landfill leachate in this example is better than that in other examples.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention as defined in the following claims. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of an active filter material for removing magnesium ions is characterized by comprising the following steps,
s1, uniformly mixing quartz sand and an acid solution with the mass concentration of 10-15% according to the mass ratio of (1-2) to 1, stirring for 40-50h, filtering, taking out a filter cake, and drying to obtain a product A;
s2, uniformly mixing the product A with an alkali solution I with the mass concentration of 10-15% according to the mass ratio of 1 (1-1.5), stirring for 40-50h, filtering, taking out and drying a filter cake, calcining for 3-5h at the temperature of 300-500 ℃, and cooling to 20-30 ℃ to obtain a product B;
s3, uniformly mixing the product B with a magnesium ion solution with the mass concentration of 10% -12% according to the mass ratio of 1 (1-1.8), stirring and soaking for 2-4h, adding a second alkali solution with the mass concentration of 12% -16%, controlling the pH to be 9-10, stirring and reacting for 1-2h at 20-30 ℃, filtering, and taking out a filter cake to obtain a product C;
and S4, washing away the magnesium ion solution and the alkali solution II remained on the surface of the product C, and drying to obtain the active filter material.
2. The method for preparing an active filter material for removing magnesium ions according to claim 1, wherein in S2, before uniformly mixing the product A with an alkali solution with a mass concentration of 10% -15% according to a mass ratio of 1 (1-1.5), the product A is washed for 2-4 times for 3-5min by using the alkali solution with a mass concentration of 1% -3%.
3. The method for preparing the active filter material for removing magnesium ions according to claim 2, wherein in the step S1, the acid solution is selected from any one or a mixture of any several of hydrochloric acid solution, sulfuric acid solution, oxalic acid solution and hydrofluoric acid solution;
in the S2, the alkali solution I is any one or a mixture of any more of a sodium hydroxide solution, a potassium hydroxide solution and a lithium hydroxide solution;
in the S3, the alkali solution II is selected from any one or a mixture of any more of a sodium hydroxide solution, a potassium hydroxide solution and a lithium hydroxide solution.
4. The method of claim 1, wherein in the step S3, the magnesium ion solution is magnesium sulfate solution or magnesium chloride solution.
5. The method for preparing the active filter material for removing magnesium ions according to claim 1, wherein the method for washing away the magnesium ion solution and the second alkali solution remaining on the surface of the product C in S4 comprises the steps of washing 1-3 times with a sodium hydroxide solution with a mass concentration of 1% -3% for 3-5min each time, and then washing 2-4 times with distilled water for 3-5min each time.
6. The method for preparing an active filter material for removing magnesium ions according to claim 1, wherein the particle size of the quartz sand is 1.2-1.5 mm.
7. An activated filler, characterized by being prepared by the process of any one of claims 1-6.
8. An active filler as claimed in claim 7 for use in the removal of magnesium ions from landfill leachate.
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| WO2018168558A1 (en) * | 2017-03-14 | 2018-09-20 | オルガノ株式会社 | Water treatment method, magnesium agent for water treatment, and method for producing magnesium agent for water treatment |
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| JP5905669B2 (en) * | 2011-05-23 | 2016-04-20 | 日鉄住金環境株式会社 | Hazardous material treatment material and method |
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