CN110180492A - A kind of active filter and its preparation method and application for removing magnesium ion - Google Patents

Abstract

The invention belongs to the technical field of active filter materials, and in particular relates to a method for preparing an active filter material for removing magnesium ions. 1-2): 1 is uniformly mixed, stirred for 40-50h, filtered, and the filter cake is taken out and dried to obtain product A; S2, product A and mass concentration are 10%-15% alkaline solution—according to mass ratio, 1: (1-1.5) uniform mixing, stirring for 40-50h, to obtain product B; S3, be that the magnesium ion solution of 10%-12% with product B and mass concentration is 1: (1-1.8) uniform according to mass ratio Mixing, stirring and soaking for 2-4h, adding alkali solution II with a mass concentration of 12%-16% to obtain product C; S4, washing off residual magnesium sulfate solution and alkali solution II on the surface of product C, and drying to obtain an active filter material. The beneficial effects of the present invention are: the particle size of the active filter material obtained by the present invention is relatively fine, showing a colorless crystal state, and the removal of magnesium ions is rapid and efficient.

Description

A kind of active filter material for removing magnesium ion and its preparation method and application

technical field

The invention belongs to the technical field of active filter materials, and in particular relates to an active filter material for removing magnesium ions and a preparation method and application thereof.

Background technique

At present, the monitoring of various sewage treatment plants shows that the content of magnesium ions in the leachate of waste incineration power generation is relatively high. Although magnesium is an essential element for human growth, high concentrations of magnesium ions will bring some disadvantages to production and life. For example, when the effluent containing high magnesium ions is reused, it will cause scaling in the pipeline and block the pipeline. In addition, the leachate of waste incineration power generation with high magnesium ions will inhibit the microorganisms in the activated sludge and affect the quality of the effluent.

At present, there are many methods for removing magnesium ions from leachate of waste incineration power generation, such as biological adsorbent method and activated sludge method. The biosorbent method has a better removal effect of magnesium ions, but the removal effect is unstable and will be affected by some external environmental factors (initial magnesium ion concentration, stirring speed); the activated sludge method can remove magnesium ions quickly and efficiently, but Susceptible to solution pH.

SUMMARY OF THE INVENTION

In order to solve the above problems, the present invention provides a method for preparing an active filter material for removing magnesium ions, and the active filter material prepared by the method is stable and efficient in removing magnesium ions.

The present invention provides the following technical solutions:

A preparation method for an active filter material for removing magnesium ions, comprising the steps,

S1, the quartz sand and the acid solution with mass concentration of 10%-15% are uniformly mixed according to the mass ratio of (1-2): 1, stirred for 40-50h, filtered, and the filter cake is taken out and dried to obtain product A;

S2, product A is uniformly mixed with the alkali solution whose mass concentration is 10%-15% according to the mass ratio of 1:(1-1.5), stirred for 40-50h, filtered, and the filter cake is taken out and dried, then at 300 Calcined at -500°C for 3-5h, cooled to 20-30°C to obtain product B;

S3, the product B and the magnesium ion solution with a mass concentration of 10%-12% are uniformly mixed according to the mass ratio of 1: (1-1.8), and the alkali solution with a mass concentration of 12%-16% is added after stirring and soaking for 2-4h 2. Control the pH to be 9-10, stir and react at 20-30 ° C for 1-2 h, filter, and take out the filter cake to obtain product C;

S4, washing off the residual magnesium ion solution and alkali solution 2 on the surface of the product C, and drying to obtain an active filter material.

Preferably, in the S2, before uniformly mixing the product A with the alkali solution with a mass concentration of 10%-15% according to a mass ratio of 1:(1-1.5), first use a mass concentration of 1%-3% The alkaline solution of the product A was washed 2-4 times for 3-5 min each time.

Preferably, in the S1, the acid solution is selected from any one or a mixture of any of a hydrochloric acid solution, a sulfuric acid solution, an oxalic acid solution, and a hydrofluoric acid solution;

In described S2, alkali solution—is selected from any one or any mixture of several in sodium hydroxide solution, potassium hydroxide solution, lithium hydroxide solution;

In the S3, the alkali solution II is selected from any one or a mixture of any of the sodium hydroxide solution, potassium hydroxide solution, and lithium hydroxide solution.

Preferably, in the S3, the magnesium ion solution is a magnesium sulfate solution or a magnesium chloride solution.

Preferably, the method of washing off the residual magnesium ion solution and alkali solution 2 on the surface of product C in S4 is to first wash 1-3 times with sodium hydroxide solution with a mass concentration of 1%-3%, each time 3-5min , and then washed with distilled water 2-4 times, each 3-5min.

Preferably, the particle size of the quartz sand is 1.2-1.5 mm.

The present invention also provides an active filler, which is prepared by any of the methods described above.

The active filler of the present invention is used for removing magnesium ions in the leachate of waste incineration power generation.

The beneficial effects of the present invention are:

1. In the present invention, the quartz sand is successively etched under acidic and alkaline conditions, and under alkaline conditions, magnesium ions are converted into Mg(OH) ₂ to precipitate and adsorb on the surface of the quartz sand to obtain an active filter material. The particle size of the active filter material is fine, showing a colorless crystal state, and the removal of magnesium ions is rapid and efficient.

2. The preparation method can be performed at room temperature without heating, and the whole operation is simple.

3. The active filter material prepared by the present invention can effectively reduce the concentration of magnesium ions in the leachate of waste incineration power generation, and the removal rate of magnesium ions is above 80%. up 90.2%.

Detailed ways

The present invention will be specifically described below with reference to specific embodiments.

Example 1

A preparation method for an active filter material for removing magnesium ions, comprising the steps,

S1, uniformly mix quartz sand with a particle size of 1.2mm and a hydrochloric acid solution with a mass concentration of 10% according to a mass ratio of 1:1, stir for 40h, filter, take out the filter cake and dry to obtain product A;

S2. Use the sodium hydroxide solution with a mass concentration of 1% to wash the product A twice, 5 minutes each time, and mix the washed product A with a sodium hydroxide solution with a mass concentration of 10% according to a mass ratio of 1:1. , stirred for 40h, filtered, the filter cake was taken out and dried, then calcined at 300°C for 5h, cooled to 20°C to obtain product B;

S3. Mix the product B and the magnesium sulfate solution with a mass concentration of 10% uniformly according to a mass ratio of 1:1, stir and soak for 2 hours, add a sodium hydroxide solution with a mass concentration of 12%, control the pH to be 9, and stir at 20 °C The reaction was carried out for 1 h, filtered, and the filter cake was taken out to obtain product C;

S4, first wash once with 1% sodium hydroxide solution, each time for 3 minutes, then wash with distilled water twice, each time for 3 minutes, wash away the residual magnesium sulfate solution and sodium hydroxide solution on the surface of product C, and dry Then the active filter material is obtained.

Example 2

A preparation method for an active filter material for removing magnesium ions, comprising the steps,

S1, uniformly mix the quartz sand with a particle size of 1.4mm and a hydrochloric acid solution with a mass concentration of 12% according to a mass ratio of 1.5:1, stir for 48h, filter, take out the filter cake and dry to obtain product A;

S2. Use a sodium hydroxide solution with a mass concentration of 2% to wash the product A for 3 times, 4 minutes each time, and mix the washed product A with a sodium hydroxide solution with a mass concentration of 12% according to a mass ratio of 1:1.2. , stirred for 48h, filtered, the filter cake was taken out and dried, then calcined at 400°C for 4h, cooled to 25°C to obtain product B;

S3. Mix the product B and the magnesium sulfate solution with a mass concentration of 11% uniformly according to a mass ratio of 1:1.4, stir and soak for 3 hours, add a sodium hydroxide solution with a mass concentration of 14%, control the pH to 9, and stir at 25 ° C The reaction was carried out for 1 h, filtered, and the filter cake was taken out to obtain product C;

S4, first wash 2 times with a sodium hydroxide solution with a mass concentration of 1%-3%, each 4min, and then wash with distilled water 3 times, each 4min, wash away the residual magnesium sulfate solution and sodium hydroxide on the surface of product C The solution is dried to obtain an active filter material.

Example 3

A preparation method for an active filter material for removing magnesium ions, comprising the steps,

S1, uniformly mix quartz sand with a particle size of 1.2 mm and a hydrochloric acid solution with a mass concentration of 10% according to a mass ratio of 1.5:1, stir for 50h, filter, take out the filter cake and dry to obtain product A;

S2, using the sodium hydroxide solution with a mass concentration of 3% to wash the product A twice, 3min each time, the washed product A and the sodium hydroxide solution with a mass concentration of 10 are uniformly mixed according to a mass ratio of 1:1.3, Stir for 40h, filter, take out the filter cake and dry, then calcinate at 500°C for 5h, and cool to 20°C to obtain product B;

S3. Mix the product B and the magnesium sulfate solution with a mass concentration of 12% uniformly according to the mass ratio of 1:1.6. After stirring and soaking for 4 hours, add a sodium hydroxide solution with a mass concentration of 14%, control the pH to 9, and stir at 30 ° C. The reaction was carried out for 1 h, filtered, and the filter cake was taken out to obtain product C;

S4, first wash once with 1% sodium hydroxide solution for 3 minutes each time, then wash with distilled water twice for 5 minutes each time, wash away the residual magnesium sulfate solution and sodium hydroxide solution on the surface of product C, and dry Then the active filter material is obtained.

Example 4

A preparation method for an active filter material for removing magnesium ions, comprising the steps,

S1, uniformly mix the quartz sand with a particle size of 1.2mm and a hydrochloric acid solution with a mass concentration of 15% according to a mass ratio of 1.2:1, stir for 40h, filter, take out the filter cake and dry to obtain product A;

S2. Use the sodium hydroxide solution with a mass concentration of 1% to wash the product A for 4 times, 5 minutes each time, and the washed product A and the sodium hydroxide solution with a mass concentration of 15% are uniformly 1:1.5 in mass ratio Mixed, stirred for 50 hours, filtered, the filter cake was taken out and dried, then calcined at 500 °C for 5 hours, cooled to 30 °C to obtain product B;

S3. The product B is uniformly mixed with the magnesium sulfate solution with a mass concentration of 10% according to the mass ratio of 1:1.5. After stirring and soaking for 4 hours, a sodium hydroxide solution with a mass concentration of 14% is added, and the pH is controlled to be 10. Stir at 30 °C The reaction was carried out for 1-2h, filtered, and the filter cake was taken out to obtain product C;

S4, first wash once with 3% sodium hydroxide solution, each time for 5 minutes, then wash with distilled water twice, each time for 5 minutes, wash away the residual magnesium sulfate solution and sodium hydroxide solution on the surface of product C, and dry Then the active filter material is obtained.

Example 5

A preparation method for an active filter material for removing magnesium ions, comprising the steps,

S1, uniformly mix quartz sand with a particle size of 1.5mm and a hydrochloric acid solution with a mass concentration of 15% according to a mass ratio of 2:1, stir for 50h, filter, take out the filter cake and dry to obtain product A;

S2. Use the sodium hydroxide solution with a mass concentration of 3% to wash the product A for 4 times, 5 minutes each time, and uniformly mix the washed product A and the sodium hydroxide solution with a mass concentration of 15% according to a mass ratio of 1:1.5 , stirred for 50h, filtered, the filter cake was taken out and dried, then calcined at 500°C for 5h, cooled to 30°C to obtain product B;

S3. Mix the product B and the magnesium sulfate solution with a mass concentration of 12% uniformly according to a mass ratio of 1:1.8, stir and soak for 4 hours, add a sodium hydroxide solution with a mass concentration of 16%, control the pH to be 10, and stir at 30 °C The reaction was carried out for 2h, filtered, and the filter cake was taken out to obtain product C;

S4, first wash 3 times with 3% sodium hydroxide solution, each 5min, then wash 4 times with distilled water, 5min each time, wash away the residual magnesium sulfate solution and sodium hydroxide solution on the surface of product C, and dry Then the active filter material is obtained.

In the embodiment of the present invention 1-5, magnesium sulfate solution can be replaced with magnesium chloride solution;

The hydrochloric acid solution can be replaced with any one or any mixture of hydrochloric acid solution, sulfuric acid solution, oxalic acid solution and hydrofluoric acid solution;

The sodium hydroxide solution can be replaced by any one of sodium hydroxide solution, potassium hydroxide solution, and lithium hydroxide solution or a mixture of any of them.

Magnesium removal performance test

The leachate of waste incineration power generation is successively treated by aeration, coagulation, precipitation, and quartz sand filtration, and the supernatant is introduced into 5 parallel reactors with a diameter of 45mm and a height of 1.2m. The 5 reactors correspond to The active filter materials prepared in Examples 1-5 were filled, and the filling height was 0.8 m. The flow rate of the leachate was controlled at 18L/h, and it was operated continuously for 30 days. The active filter material was rinsed with distilled water every 3 days. The magnesium ion concentration at the inlet and outlet of the 5 reactors was detected every day. The results are shown in the following table. .

As can be seen from the above table, the use of the active filter material prepared by the present invention can effectively reduce the concentration of magnesium ions in the leachate of waste incineration power generation, and the removal rate of magnesium ions is all above 80%, and the best effect is prepared in Example 2. As the active filler, the removal rate of magnesium ions reached 90.2%, because after the quartz sand was pickled to remove the metal impurities on the surface, the particle size of the quartz sand became smaller, the porosity became higher, and the specific surface area of the matrix increased. After immersion and calcination in alkaline solution of corresponding concentration, the content of Mg(OH) ₂ is also more abundant and fuller due to the diversity of non-zeolite pore structure of silicate itself. In the actual reaction process, the concentration of OH ^- is too high or too low, which will lead to loss of magnesium ions or incomplete reaction, thereby reducing the removal rate. However, the active filter material prepared in Example 2 fully exerts the adsorption effect of magnesium ions in the landfill leachate with the assistance of the pore channel effect of quartz sand, thereby improving the removal rate of magnesium ions by the filter material, so that the garbage in this example is The magnesium ion removal rate in the leachate is better than other examples.

The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still understand the foregoing embodiments. The technical solutions described are modified, or some technical features thereof are equivalently replaced. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims (8)

1. a kind of for removing the preparation method of the active filter of magnesium ion, which is characterized in that include the following steps,

S1, by the acid solution that quartz sand and mass concentration are 10%-15% according to mass ratio be (1-2): 1 uniformly mixes, and stirs 40-50h is handled, filter cake is taken out and dried, obtains product A by filtering；

S2, by the aqueous slkali one that product A and mass concentration are 10%-15% according to mass ratio it is 1:(1-1.5) uniformly mix, it stirs Processing 40-50h is mixed, filter cake is taken out and dried, then calcined 3-5h at 300-500 DEG C, be cooled to 20-30 DEG C, obtain by filtering To product B；

S3, by the magnesium ion solution that product B and mass concentration are 10%-12% according to mass ratio it is 1:(1-1.8) uniformly mix, Addition mass concentration is the aqueous slkali two of 12%-16% after 2-4h is impregnated in stirring, and control pH is 9-10, anti-in 20-30 DEG C of stirring 1-2h is answered, filters, filter cake is taken out, product C is obtained；

S4, the remaining magnesium ion solution of product C Surface, aqueous slkali two are washed away, obtains active filter after dry.

2. according to claim 1 a kind of for removing the preparation method of the active filter of magnesium ion, which is characterized in that institute State in S2, according to mass ratio be 1:(1-1.5 in the aqueous slkali one for being 10%-15% by product A and mass concentration) uniformly mix Before, it is washed 2-4 times using aqueous slkali a pair of product A that mass concentration is 1%-3% first, each 3-5min.

3. according to claim 2 a kind of for removing the preparation method of the active filter of magnesium ion, which is characterized in that institute State in S1, acid solution in hydrochloric acid solution, sulfuric acid solution, oxalic acid solution, hydrofluoric acid solution any one or it is any several Mixture；

In the S2, aqueous slkali one in sodium hydroxide solution, potassium hydroxide solution, lithium hydroxide solution any one or Any several mixture；

In the S3, aqueous slkali two in sodium hydroxide solution, potassium hydroxide solution, lithium hydroxide solution any one or Any several mixture.

4. according to claim 1 a kind of for removing the preparation method of the active filter of magnesium ion, which is characterized in that institute It states in S3, magnesium ion solution is Adlerika or magnesium chloride solution.

5. according to claim 1 a kind of for removing the preparation method of the active filter of magnesium ion, which is characterized in that institute It states and washes away the remaining magnesium ion solution of product C Surface in S4, the method for aqueous slkali two is the hydrogen for being first 1%-3% with mass concentration Sodium hydroxide solution is washed 1-3 times, each 3-5min, then is washed with distilled water 2-4 times, each 3-5min.

6. according to claim 1 a kind of for removing the preparation method of the active filter of magnesium ion, which is characterized in that institute The partial size for stating quartz sand is 1.2-1.5mm.

7. a kind of active filler, which is characterized in that prepared by method described in any one of claims 1-6.

8. a kind of active filler as claimed in claim 7 is used to remove the magnesium ion in waste incineration and generating electricity percolate.