Preparation process of coal gangue modified environment-friendly adsorption material

Abstract

The invention discloses a preparation process of a coal gangue modified environment-friendly adsorption material, and relates to the technical field of adsorption material processing. Comprising the following steps: step 1, sieving crushed coal gangue with a 110-mesh sieve to obtain coal gangue particles, and carrying out magnetic separation on the coal gangue particles to remove iron; and 2, the coal gangue particles subjected to magnetic separation iron removal are sequentially subjected to acid pickling, deionized water cleaning and high-speed centrifugation, precipitates obtained through centrifugation are dried, pretreated coal gangue is obtained, a solution used for acid pickling is hydrochloric acid, the concentration of the hydrochloric acid is 3.5 mo l / L, and stirring is conducted for 2 h at the temperature of 65 DEG C. According to the preparation method, the coal gangue is subjected to acid pickling, impurity removal and calcination, impregnation modification is performed in the composite modifier, and the preliminarily modified coal gangue obtained after impregnation modification is subjected to physical activation, so that the obtained coal gangue modified environment-friendly adsorption material has a relatively high specific surface area and a relatively good adsorption effect on pollutants in sewage.

Description

Technical Field

[0001] The invention relates to the technical field of adsorption material processing, in particular to a preparation process of coal gangue modified environmentally friendly adsorption material. Background Art

[0002] The coal production process generates a large amount of solid waste—coal gangue. This large amount of coal gangue not only occupies valuable land resources, but also pollutes the surrounding air, water, and soil after long-term storage, and in serious cases, can even cause geological disasters.

[0003] A Chinese invention patent, application publication number CN115430404A, discloses a modified adsorbent material based on coal gangue, its preparation method, and application. The preparation method of the modified adsorbent material based on coal gangue comprises the following steps: (1) roasting the coal gangue, crushing it, and then mixing it with water to obtain a sample A; (2) mixing carboxymethyl starch with a nitrilotriacetic acid solution to obtain a sample B; (3) mixing the sample A and the sample B and reacting them to obtain the modified adsorbent material based on coal gangue; there is no order between the steps (1) and (2). The modified adsorbent material based on coal gangue prepared by the present invention has great advantages in the treatment of heavy metal ions in mineral processing wastewater. Compared with traditional processes, it is not only simple in process and can achieve the treatment of solid waste, but also ensures the high efficiency and environmental protection of mineral processing plant production, saves water resources, and achieves zero discharge of wastewater in production.

[0004] The above-mentioned gangue modified adsorption material can treat heavy metal ions in mineral processing wastewater, but its efficiency in treating heavy metal ions is still low. Therefore, a preparation process of a gangue modified environmentally friendly adsorption material is proposed to solve the above problem. Summary of the Invention

[0005] The purpose of the present invention is to provide a preparation process of a gangue-modified environmentally friendly adsorption material to solve the problems raised in the above background technology.

[0006] To achieve the above object, the present invention provides the following technical solution: a preparation process of a gangue-modified environmentally friendly adsorption material, comprising the following steps:

[0007] The first step: the crushed gangue is passed through a 100-200 mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0008] Step 2: The gangue particles after magnetic separation are acid-washed, washed with deionized water and centrifuged at high speed, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue;

[0009] Step 3: calcining the pretreated gangue in a calcining furnace for 1-3 hours under nitrogen protection at a calcination temperature of 600-800°C to obtain calcined gangue;

[0010] Step 4: Immersing the calcined gangue in a composite modifier, ultrasonically treating for 20-40 minutes to obtain a gangue mixture, then drying the obtained gangue mixture, washing with deionized water, and high-speed centrifuging, and drying the precipitate obtained by centrifugation to obtain preliminary modified gangue;

[0011] Step 5: Physically activate the preliminarily modified gangue obtained in the fourth step to obtain a second modified gangue, crush it again, and pass it through a 100-200 mesh sieve to obtain a gangue modified environmentally friendly adsorption material.

[0012] Furthermore, the pickling solution in the second step is hydrochloric acid with a concentration of 3-6 mol / L, and is stirred at 60-80° C. for 2 h.

[0013] Furthermore, the preparation method of the composite modifier is:

[0014] Step 1: Take cetyltrimethylammonium bromide and sodium dodecylsulfonate in a mass ratio of 1:1-2;

[0015] Step 2: dissolving it in a mixed solvent of deionized water and ethanol in a volume ratio of 7:2-5, and mixing evenly to obtain a modified material mixture;

[0016] Step 3: Add a sodium hydroxide solution with a concentration of 0.5-1 mol / L to the modified material mixture, adjust the mixture to pH = 8-9, and mix evenly to obtain a composite modifier with a mass concentration of hexadecyltrimethylammonium bromide and sodium dodecylsulfonate of 1-2 mol / L.

[0017] Furthermore, the impregnation process in the fourth step is:

[0018] The calcined gangue is mixed with the composite modifier in a solid-liquid ratio of 1:5-10, and the mixture is placed in a water bath at 55-65° C., centrifuged after 30-60 minutes, and vacuum dried at 50-70° C. for 10-12 hours.

[0019] Furthermore, the step of physically activating the preliminarily modified gangue in the fifth step is:

[0020] S1. Laying the preliminarily modified coal gangue in a corundum crucible according to a set layer thickness;

[0021] S2. Under nitrogen protection, heat the corundum crucible at a set heating rate. When the set temperature is reached, switch the nitrogen to carbon dioxide, and continue to introduce carbon dioxide at a constant temperature for 30-60 minutes.

[0022] S3. Re-introduce nitrogen into the corundum crucible until it cools to room temperature.

[0023] Furthermore, the set ply thickness is 2-5 mm.

[0024] Furthermore, the set heating rate is 3-5°C / min.

[0025] Furthermore, the set temperature value is 700-850°C.

[0026] Furthermore, in the step S2, the flow rate of carbon dioxide into the corundum crucible is 100-200 mL / min.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] The preparation process of the coal gangue modified environmentally friendly adsorption material comprises the following steps: acid washing and impurity removal of the coal gangue, calcination, impregnation modification in a composite modifier, and physical activation of the preliminarily modified coal gangue obtained after the impregnation modification; and then pore control of the obtained coal gangue modified environmentally friendly adsorption material, so that the material has a higher specific surface area and better adsorption effect on heavy metal cations and anions in sewage. DETAILED DESCRIPTION

[0029] Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative work shall fall within the scope of protection of the present invention.

[0030] The present invention provides a technical solution: a preparation process of a gangue-modified environmentally friendly adsorption material.

[0031] Example 1: The preparation process of the gangue-modified environmentally friendly adsorption material comprises the following steps:

[0032] The first step: the crushed gangue is passed through a 110-mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0033] Step 2: The gangue particles after magnetic separation are sequentially subjected to acid washing, deionized water washing and high-speed centrifugation, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue, wherein the solution used for acid washing is hydrochloric acid with a concentration of 3.5 mol / L, and stirred at 65°C for 2 hours;

[0034] Step 3: calcining the pretreated gangue in a calcining furnace for 1 hour under nitrogen protection at a calcination temperature of 620°C to obtain calcined gangue;

[0035] Step 4: Immersing the calcined gangue in a composite modifier, ultrasonically treating for 25 minutes to obtain a gangue mixture, then drying the obtained gangue mixture, washing with deionized water, and high-speed centrifuging, and drying the precipitate obtained by centrifugation to obtain preliminary modified gangue;

[0036] Wherein, the preparation method of the composite modifier is:

[0037] Step 1: Take cetyltrimethylammonium bromide and sodium dodecylsulfonate in a mass ratio of 1:1.1;

[0038] Step 2: dissolving it in a mixed solvent of deionized water and ethanol in a volume ratio of 7:3, and mixing evenly to obtain a modified material mixture;

[0039] Step 3: Add a sodium hydroxide solution with a concentration of 0.6 mol / L to the modified material mixture, adjust the mixture to pH = 8, and mix evenly to obtain a composite modifier with a mass concentration of hexadecyltrimethylammonium bromide and sodium dodecylsulfonate of 1.3 mol / L.

[0040] The specific impregnation process is:

[0041] The calcined gangue was mixed with the composite modifier at a solid-liquid ratio of 1:6, placed in a water bath at 55°C, centrifuged after 35 minutes, and vacuum dried at 55°C for 10 hours.

[0042] Step 5: Physically activate the preliminarily modified gangue obtained in the fourth step to obtain a second modified gangue, crush it again, and pass it through a 110 mesh sieve to obtain a gangue modified environmentally friendly adsorption material.

[0043] The steps of physically activating the preliminarily modified coal gangue are as follows:

[0044] S1. Laying the preliminarily modified coal gangue in a corundum crucible according to a set layer thickness, wherein the set layer thickness is 2.5 mm;

[0045] S2. Under nitrogen protection, the corundum crucible is heated at a set heating rate. When the set temperature is reached, the nitrogen is switched to carbon dioxide, and carbon dioxide is continuously introduced at a constant temperature for 35 minutes. The heating rate is set to 3°C / min, the set temperature is 750°C, and the flow rate of carbon dioxide into the corundum crucible is 100 mL / min.

[0046] S3. Re-introduce nitrogen into the corundum crucible until it cools to room temperature.

[0047] Example 2: The preparation process of the gangue-modified environmentally friendly adsorption material comprises the following steps:

[0048] Step 1: The crushed gangue is passed through a 190-mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0049] Step 2: The gangue particles after magnetic separation are sequentially subjected to acid washing, deionized water washing and high-speed centrifugation, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue, wherein the solution used for acid washing is hydrochloric acid with a concentration of 6 mol / L, and stirred at 80°C for 2 hours;

[0050] Step 3: calcining the pretreated gangue in a calcining furnace for 3 hours under nitrogen protection at a calcination temperature of 780°C to obtain calcined gangue;

[0051] Step 4: Immersing the calcined gangue in a composite modifier, ultrasonically treating for 40 minutes to obtain a gangue mixture, then drying the obtained gangue mixture, washing with deionized water, and centrifuging at high speed, and drying the precipitate obtained by centrifugation to obtain preliminary modified gangue;

[0052] Wherein, the preparation method of the composite modifier is:

[0053] Step 1: Take cetyltrimethylammonium bromide and sodium dodecylsulfonate in a mass ratio of 1:1.8;

[0054] Step 2: dissolving it in a mixed solvent of deionized water and ethanol in a volume ratio of 7:5, and mixing evenly to obtain a modified material mixed solution;

[0055] Step 3: Add a sodium hydroxide solution with a concentration of 0.9 mol / L to the modified material mixture, adjust the mixture to pH = 9, and mix evenly to obtain a composite modifier with a mass concentration of hexadecyltrimethylammonium bromide and sodium dodecylsulfonate of 2 mol / L.

[0056] The specific impregnation process is:

[0057] The calcined gangue was mixed with the composite modifier at a solid-liquid ratio of 1:9, placed in a water bath at 65°C, centrifuged after 55 minutes, and vacuum dried at 70°C for 12 hours.

[0058] Step 5: Physically activate the preliminarily modified gangue obtained in the fourth step to obtain a second modified gangue, crush it again, and pass it through a 110 mesh sieve to obtain a gangue modified environmentally friendly adsorption material.

[0059] The steps of physically activating the preliminarily modified coal gangue are as follows:

[0060] S1. Laying the preliminarily modified coal gangue in a corundum crucible according to a set layer thickness, wherein the set layer thickness is 4.5 mm;

[0061] S2. Under nitrogen protection, the corundum crucible is heated at a set heating rate. When the set temperature is reached, the nitrogen is switched to carbon dioxide, and carbon dioxide is continuously introduced at a constant temperature for 58 minutes. The heating rate is set to 5°C / min, the set temperature is 850°C, and the flow rate of carbon dioxide into the corundum crucible is 200 mL / min.

[0062] S3. Re-introduce nitrogen into the corundum crucible until it cools to room temperature.

[0063] Example 3: The preparation process of the gangue-modified environmentally friendly adsorption material comprises the following steps:

[0064] Step 1: The crushed gangue is passed through a 190-mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0065] Step 2: The gangue particles after magnetic separation are sequentially subjected to acid washing, deionized water washing and high-speed centrifugation, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue, wherein the solution used for acid washing is hydrochloric acid with a concentration of 6 mol / L, and stirred at 80°C for 2 hours;

[0066] Step 3: calcining the pretreated gangue in a calcining furnace for 3 hours under nitrogen protection at a calcination temperature of 780°C to obtain calcined gangue;

[0067] Step 4: The calcined gangue obtained in the third step is crushed again and passed through a 110-mesh sieve to obtain a gangue-modified environmentally friendly adsorption material.

[0068] Example 4: The preparation process of the gangue-modified environmentally friendly adsorption material comprises the following steps:

[0069] Step 1: The crushed gangue is passed through a 190-mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0070] Step 2: The gangue particles after magnetic separation are sequentially subjected to acid washing, deionized water washing and high-speed centrifugation, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue, wherein the solution used for acid washing is hydrochloric acid with a concentration of 6 mol / L, and stirred at 80°C for 2 hours;

[0071] Step 3: Immersing the obtained pretreated gangue in a composite modifier, ultrasonically treating for 40 minutes to obtain a gangue mixture, then drying the obtained gangue mixture, washing with deionized water, and high-speed centrifuging, and drying the precipitate obtained by centrifugation to obtain preliminary modified gangue;

[0072] Wherein, the preparation method of the composite modifier is:

[0073] Step 1: Take cetyltrimethylammonium bromide and sodium dodecylsulfonate in a mass ratio of 1:1.8;

[0074] Step 2: dissolving it in a mixed solvent of deionized water and ethanol in a volume ratio of 7:5, and mixing evenly to obtain a modified material mixed solution;

[0075] Step 3: Add a sodium hydroxide solution with a concentration of 0.9 mol / L to the modified material mixture, adjust the mixture to pH = 9, and mix evenly to obtain a composite modifier with a mass concentration of hexadecyltrimethylammonium bromide and sodium dodecylsulfonate of 2 mol / L.

[0076] The specific impregnation process is:

[0077] The pretreated gangue was mixed with the composite modifier at a solid-liquid ratio of 1:9, placed in a water bath at 65°C, centrifuged after 55 minutes, and vacuum dried at 70°C for 12 hours.

[0078] Step 4: The preliminarily modified gangue obtained in the third step is crushed again and passed through a 110-mesh sieve to obtain a gangue-modified environmentally friendly adsorption material.

[0079] Example 5: The preparation process of the gangue-modified environmentally friendly adsorption material comprises the following steps:

[0080] Step 1: The crushed gangue is passed through a 190-mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0081] Step 2: The gangue particles after magnetic separation are sequentially subjected to acid washing, deionized water washing and high-speed centrifugation, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue, wherein the solution used for acid washing is hydrochloric acid with a concentration of 6 mol / L, and stirred at 80°C for 2 hours;

[0082] Step 3: Physically activate the pretreated gangue obtained in the second step to obtain modified gangue, crush it again, and pass it through a 110-mesh sieve to obtain gangue-modified environmentally friendly adsorption material.

[0083] The steps of physically activating the pretreated gangue are as follows:

[0084] S1. Laying the pretreated coal gangue in a corundum crucible according to a set layer thickness, wherein the set layer thickness is 4.5 mm;

[0085] S2. Under nitrogen protection, the corundum crucible is heated at a set heating rate. When the set temperature is reached, the nitrogen is switched to carbon dioxide, and carbon dioxide is continuously introduced at a constant temperature for 58 minutes. The heating rate is set to 5°C / min, the set temperature is 850°C, and the flow rate of carbon dioxide into the corundum crucible is 200 mL / min.

[0086] S3. Re-introduce nitrogen into the corundum crucible until it cools to room temperature.

[0087] Example 6: The preparation process of the gangue-modified environmentally friendly adsorption material comprises the following steps:

[0088] Step 1: The crushed gangue is passed through a 190-mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0089] Step 2: The gangue particles after magnetic separation are sequentially subjected to acid washing, deionized water washing and high-speed centrifugation, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue, wherein the solution used for acid washing is hydrochloric acid with a concentration of 6 mol / L, and stirred at 80°C for 2 hours;

[0090] Step 3: calcining the pretreated gangue in a calcining furnace for 3 hours under nitrogen protection at a calcination temperature of 780°C to obtain calcined gangue;

[0091] Step 4: Immersing the calcined gangue in a composite modifier, ultrasonically treating for 40 minutes to obtain a gangue mixture, then drying the obtained gangue mixture, washing with deionized water, and centrifuging at high speed, and drying the precipitate obtained by centrifugation to obtain preliminary modified gangue;

[0092] Wherein, the preparation method of the composite modifier is:

[0093] Step 1: Take cetyltrimethylammonium bromide and sodium dodecylsulfonate in a mass ratio of 1:1.8;

[0094] Step 2: dissolving it in a mixed solvent of deionized water and ethanol in a volume ratio of 7:5, and mixing evenly to obtain a modified material mixed solution;

[0095] Step 3: Add a sodium hydroxide solution with a concentration of 0.9 mol / L to the modified material mixture, adjust the mixture to pH = 9, and mix evenly to obtain a composite modifier with a mass concentration of hexadecyltrimethylammonium bromide and sodium dodecylsulfonate of 2 mol / L.

[0096] The specific impregnation process is:

[0097] The calcined gangue was mixed with the composite modifier at a solid-liquid ratio of 1:9, placed in a water bath at 65°C, centrifuged after 55 minutes, and vacuum dried at 70°C for 12 hours.

[0098] Step 5: The preliminarily modified gangue obtained in the fourth step is crushed again and passed through a 110-mesh sieve to obtain a gangue-modified environmentally friendly adsorption material.

[0099] Example 7: The preparation process of the gangue-modified environmentally friendly adsorption material comprises the following steps:

[0100] Step 1: The crushed gangue is passed through a 190-mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0101] Step 2: The gangue particles after magnetic separation are sequentially subjected to acid washing, deionized water washing and high-speed centrifugation, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue, wherein the solution used for acid washing is hydrochloric acid with a concentration of 6 mol / L, and stirred at 80°C for 2 hours;

[0102] Step 3: calcining the pretreated gangue in a calcining furnace for 3 hours under nitrogen protection at a calcination temperature of 780°C to obtain calcined gangue;

[0103] Step 4: Physically activate the calcined gangue obtained in the third step to obtain re-modified gangue, crush it again, and pass it through a 110-mesh sieve to obtain gangue-modified environmentally friendly adsorption material.

[0104] The steps of physically activating the calcined gangue are as follows:

[0105] S1. Laying the calcined coal gangue in a corundum crucible according to a set layer thickness, wherein the set layer thickness is 4.5 mm;

[0106] S2. Under nitrogen protection, the corundum crucible is heated at a set heating rate. When the set temperature is reached, the nitrogen is switched to carbon dioxide, and carbon dioxide is continuously introduced at a constant temperature for 58 minutes. The heating rate is set to 5°C / min, the set temperature is 850°C, and the flow rate of carbon dioxide into the corundum crucible is 200 mL / min.

[0107] S3. Re-introduce nitrogen into the corundum crucible until it cools to room temperature.

[0108] Example 8: The preparation process of the gangue-modified environmentally friendly adsorption material comprises the following steps:

[0109] Step 1: The crushed gangue is passed through a 190-mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0110] Step 2: The gangue particles after magnetic separation are sequentially subjected to acid washing, deionized water washing and high-speed centrifugation, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue, wherein the solution used for acid washing is hydrochloric acid with a concentration of 6 mol / L, and stirred at 80°C for 2 hours;

[0111] Step 3: Immersing the obtained pretreated gangue in a composite modifier, ultrasonically treating for 40 minutes to obtain a gangue mixture, then drying the obtained gangue mixture, washing with deionized water, and high-speed centrifuging, and drying the precipitate obtained by centrifugation to obtain preliminary modified gangue;

[0112] Wherein, the preparation method of the composite modifier is:

[0113] Step 1: Take cetyltrimethylammonium bromide and sodium dodecylsulfonate in a mass ratio of 1:1.8;

[0114] Step 2: dissolving it in a mixed solvent of deionized water and ethanol in a volume ratio of 7:5, and mixing evenly to obtain a modified material mixed solution;

[0115] Step 3: Add a sodium hydroxide solution with a concentration of 0.9 mol / L to the modified material mixture, adjust the mixture to pH = 9, and mix evenly to obtain a composite modifier with a mass concentration of hexadecyltrimethylammonium bromide and sodium dodecylsulfonate of 2 mol / L.

[0116] The specific impregnation process is:

[0117] The pretreated gangue was mixed with the composite modifier at a solid-liquid ratio of 1:9, placed in a water bath at 65°C, centrifuged after 55 minutes, and vacuum dried at 70°C for 12 hours.

[0118] Step 4: Physically activate the preliminarily modified gangue obtained in the third step to obtain a second modified gangue, crush it again, and pass it through a 110 mesh sieve to obtain a gangue modified environmentally friendly adsorption material.

[0119] The steps of physically activating the preliminarily modified coal gangue are as follows:

[0120] S1. Laying the preliminarily modified coal gangue in a corundum crucible according to a set layer thickness, wherein the set layer thickness is 4.5 mm;

[0121] S2. Under nitrogen protection, the corundum crucible is heated at a set heating rate. When the set temperature is reached, the nitrogen is switched to carbon dioxide, and carbon dioxide is continuously introduced at a constant temperature for 58 minutes. The heating rate is set to 5°C / min, the set temperature is 850°C, and the flow rate of carbon dioxide into the corundum crucible is 200 mL / min.

[0122] S3. Re-introduce nitrogen into the corundum crucible until it cools to room temperature.

[0123] Comparative Example 1: The preparation process of the gangue adsorption material comprises the following steps:

[0124] Step 1: The crushed gangue is passed through a 190-mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron;

[0125] Step 2: The gangue particles after magnetic separation are sequentially subjected to acid washing, deionized water washing and high-speed centrifugation, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue, wherein the solution used for acid washing is hydrochloric acid with a concentration of 6 mol / L, and stirred at 80°C for 2 hours;

[0126] Step 3: The pretreated gangue obtained in the second step is crushed again and passed through a 110-mesh sieve to obtain a gangue-modified environmentally friendly adsorption material.

[0127] Table 1:

[0128]

[0129] It can be seen from Table 1 that the specific surface area of the modified gangue is the largest, which is 30.7 times that of the original gangue, and its average pore size is 0.14 times that of the original gangue. Under the same adsorption conditions, the larger the specific surface area, the larger the contact area with the sewage, and the better the adsorption effect.

[0130] Table 2: Pb concentration of 100 mg / L 2+ Solution, Cd 2+ Solution, Cr2O7 2- Solution and methyl orange solution, the gangue modified environmentally friendly adsorption material prepared in Examples 1 to 8 and Comparative Example 1 was added to each solution at an addition amount of 10 g / L, stirred and allowed to stand for 60 minutes, adsorbed at room temperature, and then the concentration of the substance in each group was detected, and the removal rate of each substance was calculated. The results are shown in the following table:

[0131]

[0132]

[0133] As shown in Table 2, the coal gangue modified environmentally friendly adsorption material prepared in this scheme has an effective effect on the Pb content in the solution. 2+ 、Cd 2+ 、Cr2O7 2- and methyl orange have better adsorption effects.

[0134] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

Claims

1. The preparation process of coal gangue modified environmentally friendly adsorption material is characterized by: The following steps are involved: The first step: the crushed gangue is passed through a 100-200 mesh sieve to obtain gangue particles, and the gangue particles are subjected to magnetic separation to remove iron; Step 2: The gangue particles after magnetic separation are acid-washed, washed with deionized water and centrifuged at high speed, and the precipitate obtained by centrifugation is dried to obtain pretreated gangue; Step 3: calcining the pretreated gangue in a calcining furnace for 1-3 hours under nitrogen protection at a calcination temperature of 600-800°C to obtain calcined gangue; Step 4: Immersing the calcined gangue in a composite modifier, ultrasonically treating for 20-40 minutes to obtain a gangue mixture, then drying the obtained gangue mixture, washing with deionized water, and high-speed centrifuging, and drying the precipitate obtained by centrifugation to obtain preliminary modified gangue; Step 5: Physically activate the preliminarily modified gangue obtained in the fourth step to obtain a second modified gangue, crush it again, and pass it through a 100-200 mesh sieve to obtain a gangue modified environmentally friendly adsorption material.

2. The preparation process of the gangue-modified environmentally friendly adsorption material according to claim 1, characterized in that: The pickling solution in the second step is hydrochloric acid with a concentration of 3-6 mol / L, and is stirred at 60-80° C. for 2 h.

3. The preparation process of the gangue-modified environmentally friendly adsorption material according to claim 1, characterized in that: The preparation method of the composite modifier is: Step 1: Take cetyltrimethylammonium bromide and sodium dodecylsulfonate in a mass ratio of 1:1-2; Step 2: dissolving it in a mixed solvent of deionized water and ethanol in a volume ratio of 7:2-5, and mixing evenly to obtain a modified material mixture; Step 3: Add a sodium hydroxide solution with a concentration of 0.5-1 mol / L to the modified material mixture, adjust the mixture to pH = 8-9, and mix evenly to obtain a composite modifier with a mass concentration of hexadecyltrimethylammonium bromide and sodium dodecylsulfonate of 1-2 mol / L.

4. The preparation process of the gangue-modified environmentally friendly adsorption material according to claim 3, characterized in that: The impregnation process in the fourth step is: The calcined gangue is mixed with the composite modifier at a solid-liquid ratio of 1:5-10, placed in a water bath at 55-65°C, centrifuged after 30-60 minutes, and vacuum dried at 50-70°C for 10-12 hours.

5. The preparation process of the gangue-modified environmentally friendly adsorption material according to claim 1, characterized in that: The steps of physically activating the preliminarily modified coal gangue in the fifth step are: S1. Laying the preliminarily modified coal gangue in a corundum crucible according to a set layer thickness; S2. Under nitrogen protection, heat the corundum crucible at a set heating rate. When the set temperature is reached, switch the nitrogen to carbon dioxide, and continue to introduce carbon dioxide at a constant temperature for 30-60 minutes. S3. Re-introduce nitrogen into the corundum crucible until it cools to room temperature.

6. The preparation process of the gangue-modified environmentally friendly adsorption material according to claim 5, characterized in that: The set ply thickness is 2-5 mm.

7. The preparation process of the gangue-modified environmentally friendly adsorption material according to claim 5, characterized in that: The set heating rate is 3-5°C / min.

8. The preparation process of the gangue-modified environmentally friendly adsorption material according to claim 5, characterized in that: The set temperature value is 700-850°C.

9. The preparation process of the gangue-modified environmentally friendly adsorption material according to claim 5, characterized in that: In the step S2, the flow rate of carbon dioxide into the corundum crucible is 100-200 mL / min.

Images