CN114558880B - Surfactant suitable for dealkalization of red mud and dealkalization method of red mud - Google Patents
Surfactant suitable for dealkalization of red mud and dealkalization method of red mud Download PDFInfo
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- CN114558880B CN114558880B CN202210243986.XA CN202210243986A CN114558880B CN 114558880 B CN114558880 B CN 114558880B CN 202210243986 A CN202210243986 A CN 202210243986A CN 114558880 B CN114558880 B CN 114558880B
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- red mud
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- lignin sulfonate
- sodium lignin
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- 239000004094 surface-active agent Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 24
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims abstract description 39
- 239000000843 powder Substances 0.000 claims abstract description 29
- 239000002131 composite material Substances 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 230000001590 oxidative effect Effects 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000007800 oxidant agent Substances 0.000 claims abstract description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 150000003385 sodium Chemical class 0.000 claims abstract description 7
- 229920005552 sodium lignosulfonate Polymers 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000002002 slurry Substances 0.000 claims description 62
- 238000003756 stirring Methods 0.000 claims description 45
- 239000002994 raw material Substances 0.000 claims description 39
- 238000000498 ball milling Methods 0.000 claims description 33
- 239000007789 gas Substances 0.000 claims description 25
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical group [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 9
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 9
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 4
- 235000019353 potassium silicate Nutrition 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 239000012948 isocyanate Substances 0.000 claims description 3
- 150000002513 isocyanates Chemical class 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 230000001804 emulsifying effect Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 230000003381 solubilizing effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 7
- 238000013494 PH determination Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a surfactant suitable for dealkalization of red mud, which is prepared by the following steps: adding an oxidant into the sodium lignin sulfonate aqueous solution added with the concentrated sulfuric acid, heating to 70-90 ℃ and reacting for 1-2h; adding a sulfonating agent, keeping the temperature, and continuing to react for 1-2 hours to obtain a modified sodium lignin sulfonate solution; mixing the modified sodium lignosulfonate solution with an inorganic dispersing agent to obtain a composite surfactant suitable for dealkalization of red mud; the composite surfactant is added into the disclosed red mud dealkalization method; according to the invention, sodium lignin sulfonate surfactant is selected for modification, and components with excessive and insufficient molecular weight are removed by a method of oxidizing and vulcanizing, so that modified sodium lignin sulfonate with improved dispersion performance is obtained; the composite surfactant is compounded with an inorganic dispersing agent, has higher interfacial activity, good emulsifying and solubilizing capacity and stronger temperature resistance, and is more suitable for dispersing red mud powder in aqueous solution.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a surfactant and a red mud dealkalization method.
Background
Red mud is the main waste produced in the alumina production process and is also the largest pollution source in alumina factories. With the development of the aluminum industry and the reduction of the bauxite grade, the discharge amount of the red mud is larger and larger, and the dealkalization treatment is a key step in the subsequent treatment application process of the red mud because the red mud contains a large amount of strong alkaline substances. At present, the most widely applied application of red mud dealkalization is wet treatment, and in the process, the red mud is mixed with an aqueous solution, and as the hydrophilic effect of hydroxyl groups on the surface is good, the red mud cannot be fully mixed, the dealkalization efficiency can be inhibited, and the effective utilization and conversion of the red mud are further affected.
The existing inorganic dispersant has strong alkalinity and general dispersion performance; the organic dispersing agent is not suitable for dealkalization treatment of red mud because of the complex molecular structure and large viscosity of slurry due to large relative molecular weight.
Disclosure of Invention
The invention aims to provide a surfactant suitable for dealkalization of red mud, which can effectively promote the dispersibility and uniformity of the red mud slurry and further improve the dealkalization efficiency of the red mud; the second purpose of the invention is to provide a red mud dealkalization method, which solves the problems of environmental pollution and occupation of land caused by red mud, realizes the comprehensive utilization of the red mud and has low process cost.
In order to achieve the above purpose, the following technical scheme is adopted:
the surfactant suitable for dealkalization of red mud is prepared by the following steps:
adding an oxidant into the sodium lignin sulfonate aqueous solution added with the concentrated sulfuric acid, heating to 70-90 ℃ and reacting for 1-2h;
adding a sulfonating agent, keeping the temperature, and continuing to react for 1-2 hours to obtain a modified sodium lignin sulfonate solution;
and mixing the modified sodium lignosulfonate solution with an inorganic dispersing agent to obtain the composite surfactant suitable for dealkalization of the red mud.
According to the scheme, the concentration of the aqueous solution of the sodium lignin sulfonate is 0.3-0.5g/ml, and the consumption of the concentrated sulfuric acid is 1-5% of the mass of the sodium lignin sulfonate.
According to the scheme, the oxidant is hydrogen peroxide, potassium permanganate, ammonium persulfate, sulfite, formaldehyde, phenol or isocyanate; the amount of the oxidant is 5% of the mass of the sodium lignin sulfonate.
According to the scheme, the sulfonating agent is sodium sulfite; the dosage of the sulfonating agent is 10-50% of the mass of the sodium lignin sulfonate.
According to the scheme, the inorganic dispersing agent is one of sodium hexametaphosphate, sodium tripolyphosphate and water glass; the mass ratio of the modified sodium lignosulfonate to the inorganic dispersant is (1-3): 1.
The red mud dealkalization method comprises the following steps:
(1) Drying, ball milling and sieving red mud raw materials to prepare red mud powder;
(2) Mixing the obtained red mud powder with deionized water, adding the composite surfactant, and stirring and dispersing to obtain red mud slurry;
(3) And (3) dealkalizing the obtained red mud.
According to the scheme, the ball milling rotating speed in the step 1 is 500-600r/min, and the ball milling time is 24-36h.
According to the scheme, the mass ratio of the red mud powder to the deionized water in the step 2 is 1: (3-10).
According to the scheme, the adding amount of the composite surfactant in the step 2 accounts for 0.1-1% of the total mass of the obtained red mud slurry.
According to the scheme, the stirring and dispersing temperature in the step 2 is 70-100 ℃; the stirring speed is 150-300r/min, and the stirring time is 3-10h.
According to the scheme, the dealkalization treatment in the step 3 is CO 2 Gas dealkalization method. In the optimized scheme, CO 2 The flow rate of the gas is 0.5-2L/min; CO 2 Concentration of gas>90％。
Compared with the prior art, the invention has the beneficial effects that:
the sodium lignin sulfonate surfactant with better slurry dispersion performance is selected for modification, and components with excessive and insufficient molecular weight are removed by a method of oxidizing and vulcanizing, so that the modified sodium lignin sulfonate with improved dispersion performance is obtained.
The modified sodium lignin sulfonate is compounded with an inorganic dispersing agent, and the obtained compound surfactant has higher interfacial activity, good emulsifying and solubilizing capacity and stronger temperature resistance, and is more suitable for the dispersion of red mud powder in aqueous solution.
Detailed Description
The following examples further illustrate the technical aspects of the present invention, but are not to be construed as limiting the scope of the invention; the endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
The specific embodiment provides a surfactant suitable for dealkalization of red mud, which is prepared by the following steps:
adding an oxidant into the sodium lignin sulfonate aqueous solution added with the concentrated sulfuric acid, heating to 70-90 ℃ and reacting for 1-2h; the concentration of the aqueous solution of the sodium lignin sulfonate is 0.3-0.5g/ml, and the dosage of the concentrated sulfuric acid is 1-5% of the mass of the sodium lignin sulfonate;
adding a sulfonating agent, keeping the temperature, and continuing to react for 1-2 hours to obtain a modified sodium lignin sulfonate solution;
and mixing the modified sodium lignosulfonate solution with an inorganic dispersing agent to obtain the composite surfactant suitable for dealkalization of the red mud.
Wherein the oxidant is hydrogen peroxide, potassium permanganate, ammonium persulfate, sulfite, formaldehyde, phenol or isocyanate; the consumption of the oxidant is 5% of the mass of the sodium lignin sulfonate; the sulfonating agent is sodium sulfite; the dosage of the sulfonating agent is 10-50% of the mass of the sodium lignin sulfonate.
In the optimized scheme, the inorganic dispersant is one of sodium hexametaphosphate, sodium tripolyphosphate and water glass; the mass ratio of the modified sodium lignosulfonate solution to the inorganic dispersant is (1-3): 1.
The specific embodiment also provides a red mud dealkalization method:
(1) Drying, ball milling and sieving red mud raw materials to prepare red mud powder;
(2) Mixing the obtained red mud powder with deionized water, adding the composite surfactant, and stirring and dispersing to obtain red mud slurry;
(3) And (3) dealkalizing the obtained red mud.
In the optimized scheme, the ball milling rotating speed in the step 1 is 500-600r/min, and the ball milling time is 24-36h.
In the optimized scheme, the mass ratio of the red mud powder to the deionized water in the step 2 is 1: (3-10).
In the optimized scheme, the adding amount of the composite surfactant in the step 2 accounts for 0.1-1% of the total mass of the obtained red mud slurry.
In the optimized scheme, the stirring and dispersing temperature in the step 2 is 70-100 ℃; the stirring speed is 150-300r/min, and the stirring time is 3-10h.
In the optimized scheme, the dealkalization treatment in the step 3 is CO 2 Gas dealkalization method. In the optimized scheme, CO 2 The flow rate of the gas is 0.5-2L/min; CO 2 Concentration of gas>90％。
Comparative example 1
(1) Preparing red mud powder: weighing red mud raw materials, placing the red mud raw materials in a muffle furnace, drying the red mud raw materials for 24 hours at 110 ℃ to obtain dried red mud, crushing and ball milling the dried red mud raw materials by adopting an XGB2 type planetary ball mill, wherein the ball milling speed is 500r/min, the ball milling time is 12 hours, and the balls are formed by the steps of: the raw material ratio is 2:1, and the raw materials after ball milling are sieved by a 400-mesh sieve to prepare red mud powder for standby.
(2) Preparing slurry: and (3) putting the obtained red mud powder and deionized water into a stirring container according to a solid-to-liquid ratio of 1:5, and stirring by using a 78HW-1 constant temperature magnetic stirrer to obtain the red mud slurry, wherein the stirring temperature is 60 ℃, the stirring speed is 200r/min, and the stirring time is 5h.
(3) Measurement of initial slurry pH value and Zeta potential value: the pH value and the Zeta potential value of the slurry are respectively measured by a PHS-3C acidometer and a Nanoplus Zeta potential analyzer.
(4) Dealkalization: introducing CO with concentration more than 90% into the prepared red mud slurry by using a gas flowmeter 2 The flow rate of the gas is 0.8L/min, and the dealkalized slurry is obtained after dealkalization reaction is carried out for 2 hours at 70 ℃.
(5) Determination of pH value of dealkalized mud: the pH value of the dealkalized slurry is measured by a PHS-3C acidometer.
In a control experiment group of red mud slurry without adding surfactant, the pH value of the initial slurry is 10.57, the Zeta potential value is 23.88mV, and CO is processed for 2 hours 2 After the dealkalization reaction of the gas, the pH value of the dealkalized mud is 8.93.
Comparative example 2
(1) Preparing red mud powder: weighing red mud raw materials, placing the red mud raw materials in a muffle furnace, drying the red mud raw materials for 24 hours at 110 ℃ to obtain dried red mud, crushing and ball milling the dried red mud raw materials by adopting an XGB2 type planetary ball mill, wherein the ball milling speed is 500r/min, the ball milling time is 12 hours, and the balls are formed by the steps of: the raw material ratio is 2:1, and the raw materials after ball milling are sieved by a 400-mesh sieve to prepare red mud powder for standby.
(2) Preparing slurry: the obtained red mud powder and deionized water are put into a stirring container according to a solid-to-liquid ratio of 1:5, 0.6wt% of sodium lignin sulfonate aqueous solution with concentration of 0.4g/ml is added as a surfactant, and a 78HW-1 constant temperature magnetic stirrer is used for stirring to prepare the red mud slurry, wherein the stirring temperature is 60 ℃, the stirring speed is 200r/min, and the stirring time is 5h.
(3) Measurement of initial slurry pH value and Zeta potential value: the pH value and the Zeta potential value of the slurry are respectively measured by a PHS-3C acidometer and a Nanoplus Zeta potential analyzer.
(4) Dealkalization: introducing CO with concentration more than 90% into the prepared red mud slurry by using a gas flowmeter 2 The flow rate of the gas is 0.8L/min, and the dealkalized slurry is obtained after dealkalization reaction is carried out for 2 hours at 70 ℃.
(5) Determination of pH value of dealkalized mud: the pH value of the dealkalized slurry is measured by a PHS-3C acidometer.
After adding the surfactantIn the red mud slurry, the pH value of the initial slurry is 10.64, the Zeta potential value is 24.76mV, and the CO is treated for 2 hours 2 After the dealkalization reaction of the gas, the pH value of the dealkalized mud is 8.65.
Comparative example 3
(1) Preparing red mud powder: weighing red mud raw materials, placing the red mud raw materials in a muffle furnace, drying the red mud raw materials for 24 hours at 110 ℃ to obtain dried red mud, crushing and ball milling the dried red mud raw materials by adopting an XGB2 type planetary ball mill, wherein the ball milling speed is 500r/min, the ball milling time is 12 hours, and the balls are formed by the steps of: the raw material ratio is 2:1, and the raw materials after ball milling are sieved by a 400-mesh sieve to prepare red mud powder for standby.
(2) Preparation of the composite surfactant: adding inorganic dispersant sodium hexametaphosphate into sodium lignin sulfonate aqueous solution with the concentration of 0.4g/ml, and mixing according to the following steps: sodium hexametaphosphate=2:1 mass ratio, and a 78HW-1 constant temperature magnetic stirrer is used for stirring to prepare the composite surfactant for standby.
(3) Preparing slurry: and (3) putting the obtained red mud powder and deionized water into a stirring container according to a solid-to-liquid ratio of 1:5, adding 0.6wt% of the composite surfactant prepared in the step (2), and stirring by using a 78HW-1 constant temperature magnetic stirrer to prepare the red mud slurry, wherein the stirring temperature is 60 ℃, the stirring speed is 200r/min, and the stirring time is 5h.
(4) Measurement of initial slurry pH value and Zeta potential value: the pH value and the Zeta potential value of the slurry are respectively measured by a PHS-3C acidometer and a Nanoplus Zeta potential analyzer.
(5) Dealkalization: introducing CO with concentration more than 90% into the prepared red mud slurry by using a gas flowmeter 2 The flow rate of the gas is 0.8L/min, and the dealkalized slurry is obtained after dealkalization reaction is carried out for 2 hours at 70 ℃.
(6) Determination of pH value of dealkalized mud: the pH value of the dealkalized slurry is measured by a PHS-3C acidometer.
In the red mud slurry added with the surfactant, the pH value of the initial slurry is 10.89, the Zeta potential value is 34.58mV, and the CO is processed for 2 hours 2 After the dealkalization reaction of the gas, the pH value of the dealkalized mud is 8.34.
Example 4
(1) Preparing red mud powder: weighing red mud raw materials, placing the red mud raw materials in a muffle furnace, drying the red mud raw materials for 24 hours at 110 ℃ to obtain dried red mud, crushing and ball milling the dried red mud raw materials by adopting an XGB2 type planetary ball mill, wherein the ball milling speed is 500r/min, the ball milling time is 12 hours, and the balls are formed by the steps of: the raw material ratio is 2:1, and the raw materials after ball milling are sieved by a 400-mesh sieve to prepare red mud powder for standby.
(2) Preparation of modified sodium lignin sulfonate: the modified sodium lignin sulfonate solution is obtained by taking 0.4g/ml of sodium lignin sulfonate aqueous solution as a reaction solution, sequentially adding 3% of concentrated sulfuric acid, 5% of potassium permanganate as an oxidant and 30% of sodium sulfite as a sulfonating agent, reacting at 80 ℃ for 3 hours, and adopting a method of oxidizing and then vulcanizing.
(3) Preparation of the composite surfactant: adding inorganic dispersant sodium hexametaphosphate into the obtained modified sodium lignin sulfonate solution according to the following steps: sodium hexametaphosphate=2:1 mass ratio, and a 78HW-1 constant temperature magnetic stirrer is used for stirring to prepare the composite surfactant for standby.
(4) Preparing slurry: and (3) putting the obtained red mud powder and deionized water into a stirring container according to a solid-to-liquid ratio of 1:5, adding 0.6wt% of the composite surfactant prepared in the step (3), and stirring by using a 78HW-1 constant temperature magnetic stirrer to prepare the red mud slurry, wherein the stirring temperature is 60 ℃, the stirring speed is 200r/min, and the stirring time is 5h.
(5) Measurement of initial slurry pH value and Zeta potential value: the pH value and the Zeta potential value of the slurry are respectively measured by a PHS-3C acidometer and a Nanoplus Zeta potential analyzer.
(6) Dealkalization: introducing CO with concentration more than 90% into the prepared red mud slurry by using a gas flowmeter 2 The flow rate of the gas is 0.8L/min, and the dealkalized slurry is obtained after dealkalization reaction is carried out for 2 hours at 70 ℃.
(7) Determination of pH value of dealkalized mud: the pH value of the dealkalized slurry is measured by a PHS-3C acidometer.
In the red mud slurry added with the surfactant, the pH value of the initial slurry is tested to be 10.89, the Zeta potential value is 36.17mV, and CO is treated for 2 hours 2 After the dealkalization reaction of the gas, the pH value of the dealkalized mud is 7.54.
Example 5
(1) Preparing red mud powder: weighing red mud raw materials, placing the red mud raw materials in a muffle furnace, drying the red mud raw materials for 24 hours at 110 ℃ to obtain dried red mud, crushing and ball milling the dried red mud raw materials by adopting an XGB2 type planetary ball mill, wherein the ball milling speed is 500r/min, the ball milling time is 12 hours, and the balls are formed by the steps of: the raw material ratio is 2:1, and the raw materials after ball milling are sieved by a 400-mesh sieve to prepare red mud powder for standby.
(2) Preparation of modified sodium lignin sulfonate: the modified sodium lignin sulfonate solution is prepared by taking 0.5g/ml of sodium lignin sulfonate aqueous solution as a reaction solution, sequentially adding 3% of concentrated sulfuric acid, 5% of hydrogen peroxide as an oxidant and 50% of sodium sulfite as a sulfonating agent, reacting at 90 ℃ for 2 hours, and adopting a method of oxidizing and then vulcanizing.
(3) Preparation of the composite surfactant: adding inorganic dispersant sodium hexametaphosphate into the obtained modified sodium lignin sulfonate solution according to the following steps: the mass ratio of the sodium tripolyphosphate=3:1 is proportioned, and the 78HW-1 constant temperature magnetic stirrer is used for stirring to prepare the composite surfactant for standby.
(4) Preparing slurry: and (3) putting the obtained red mud powder and deionized water into a stirring container according to a solid-to-liquid ratio of 1:5, adding 0.6wt% of the composite surfactant prepared in the step (3), and stirring by using a 78HW-1 constant temperature magnetic stirrer to prepare the red mud slurry, wherein the stirring temperature is 60 ℃, the stirring speed is 200r/min, and the stirring time is 5h.
(5) Measurement of initial slurry pH value and Zeta potential value: the pH value and the Zeta potential value of the slurry are respectively measured by a PHS-3C acidometer and a Nanoplus Zeta potential analyzer.
(6) Dealkalization: introducing CO with concentration more than 90% into the prepared red mud slurry by using a gas flowmeter 2 The flow rate of the gas is 0.8L/min, and the dealkalized slurry is obtained after dealkalization reaction is carried out for 2 hours at 70 ℃.
(7) Determination of pH value of dealkalized mud: the pH value of the dealkalized slurry is measured by a PHS-3C acidometer.
After the addition of the surfactantIn the red mud, the pH value of the initial mud is 10.76, the Zeta potential value is 46.87mV, and CO is treated for 2 hours 2 After the dealkalization reaction of the gas, the pH value of the dealkalized mud is 7.76.
Example 6
(1) Preparing red mud powder: weighing red mud raw materials, placing the red mud raw materials in a muffle furnace, drying the red mud raw materials for 24 hours at 110 ℃ to obtain dried red mud, crushing and ball milling the dried red mud raw materials by adopting an XGB2 type planetary ball mill, wherein the ball milling speed is 500r/min, the ball milling time is 12 hours, and the balls are formed by the steps of: the raw material ratio is 2:1, and the raw materials after ball milling are sieved by a 400-mesh sieve to prepare red mud powder for standby.
(2) Preparation of modified sodium lignin sulfonate: the method comprises the steps of taking 0.3g/ml of sodium lignin sulfonate aqueous solution as a reaction solution, sequentially adding 3% of concentrated sulfuric acid, 5% of formaldehyde and hydrogen peroxide as a composite oxidant and 10% of sodium sulfite as a sulfonating agent, reacting at 70 ℃ for 4 hours, and obtaining a modified sodium lignin sulfonate solution by adopting a method of oxidizing and then vulcanizing.
(3) Preparation of the composite surfactant: adding inorganic dispersant sodium hexametaphosphate into the obtained modified sodium lignin sulfonate solution according to the following steps: the mass ratio of water glass=1:1 is mixed by using a 78HW-1 constant temperature magnetic stirrer to prepare the composite surfactant for standby.
(4) Preparing slurry: and (3) putting the obtained red mud powder and deionized water into a stirring container according to a solid-to-liquid ratio of 1:5, adding 0.8wt% of the composite surfactant prepared in the step (3), and stirring by using a 78HW-1 constant temperature magnetic stirrer to prepare the red mud slurry, wherein the stirring temperature is 60 ℃, the stirring speed is 200r/min, and the stirring time is 5h.
(5) Measurement of initial slurry pH value and Zeta potential value: the pH value and the Zeta potential value of the slurry are respectively measured by a PHS-3C acidometer and a Nanoplus Zeta potential analyzer.
(6) Dealkalization: introducing CO with concentration more than 90% into the prepared red mud slurry by using a gas flowmeter 2 The flow rate of the gas is 0.8L/min, and the dealkalized slurry is obtained after dealkalization reaction is carried out for 2 hours at 70 ℃.
(7) Determination of pH value of dealkalized mud: the pH value of the dealkalized slurry is measured by a PHS-3C acidometer.
In the red mud slurry added with the surfactant, the pH value of the initial slurry is tested to be 10.75, the Zeta potential value is tested to be 43.12mV, and CO is tested to be carried out for 2 hours 2 After the dealkalization reaction of the gas, the pH value of the dealkalized mud is 7.85.
Claims (5)
1. The red mud dealkalization method is characterized by comprising the following steps of:
(1) Drying, ball milling and sieving red mud raw materials to prepare red mud powder;
(2) Mixing the obtained red mud powder with deionized water, adding a surfactant suitable for dealkalization of the red mud, and stirring and dispersing to obtain red mud slurry;
(3) Dealkalizing the obtained red mud slurry;
the surfactant suitable for dealkalizing red mud is prepared by the following steps:
adding an oxidant into the sodium lignin sulfonate aqueous solution added with the concentrated sulfuric acid, heating to 70-90 ℃ and reacting for 1-2h; the concentration of the sodium lignin sulfonate solution is 0.3-0.5g/ml, and the consumption of the concentrated sulfuric acid is 1-5% of the mass of the sodium lignin sulfonate; the oxidant is hydrogen peroxide, potassium permanganate, ammonium persulfate, sulfite, formaldehyde, phenol or isocyanate; the consumption of the oxidant is 5% of the mass of the sodium lignin sulfonate;
adding a sulfonating agent, keeping the temperature, and continuing to react for 1-2 hours to obtain a modified sodium lignin sulfonate solution; the sulfonating agent is sodium sulfite; the dosage of the sulfonating agent is 10-50% of the mass of the sodium lignin sulfonate;
mixing the modified sodium lignosulfonate solution with an inorganic dispersing agent to obtain a composite surfactant suitable for dealkalization of red mud; the inorganic dispersant is one of sodium hexametaphosphate, sodium tripolyphosphate and water glass; the mass ratio of the modified sodium lignosulfonate to the inorganic dispersant is (1-3): 1.
2. The method for dealkalizing red mud according to claim 1, wherein the ball milling rotating speed in the step 1 is 500-600r/min, and the ball milling time is 24-36h.
3. The red mud dealkalization method as claimed in claim 1, wherein in the step 2, the mass ratio of the red mud powder to the deionized water is 1: (3-10); the addition amount of the composite surfactant accounts for 0.1-1% of the total mass of the red mud slurry.
4. The red mud dealkalization method as claimed in claim 1, wherein the stirring and dispersing temperature in the step 2 is 70-100 ℃; the stirring speed is 150-300r/min, and the stirring time is 3-10h.
5. The method for dealkalizing red mud as claimed in claim 1, wherein the dealkalizing treatment in the step 3 is CO 2 Gas dealkalization method.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141264A (en) * | 1995-07-27 | 1997-01-29 | 山东铝业公司 | Sinter method for red mud dealkalization and surface modification treatment process |
| CN101147480A (en) * | 2007-09-13 | 2008-03-26 | 华南理工大学 | Modified lignosulfonate pesticide dispersing agent and its preparation method |
| CN101665339A (en) * | 2009-09-10 | 2010-03-10 | 惠州市富力新技术有限公司 | Enhanced cement composite grinding aid |
| CN102172598A (en) * | 2011-01-11 | 2011-09-07 | 天津城市建设学院 | Red mud slurrying multistage circulating dealkalization method |
| CN102441339A (en) * | 2011-09-06 | 2012-05-09 | 福州大学 | Dissolving pulp sodium lignosulfonate dispersant, and reducing preparation method and application thereof |
| CN103045317A (en) * | 2012-12-26 | 2013-04-17 | 中国东方电气集团有限公司 | Lignin serial coal water slurry dispersing agent and preparation method thereof |
| CN103131020A (en) * | 2013-01-22 | 2013-06-05 | 华南理工大学 | Carboxylic sulfonic-acid-group lignin dye dispersing agent and preparation method thereof |
| CN104659369A (en) * | 2015-03-26 | 2015-05-27 | 天能集团江苏科技有限公司 | Preparation method of modified sodium lignosulfonate for lead-acid battery |
| CN105018160A (en) * | 2015-06-24 | 2015-11-04 | 济南圣泉集团股份有限公司 | Coal water slurry dispersant and its preparation method and use |
-
2022
- 2022-03-14 CN CN202210243986.XA patent/CN114558880B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141264A (en) * | 1995-07-27 | 1997-01-29 | 山东铝业公司 | Sinter method for red mud dealkalization and surface modification treatment process |
| CN101147480A (en) * | 2007-09-13 | 2008-03-26 | 华南理工大学 | Modified lignosulfonate pesticide dispersing agent and its preparation method |
| CN101665339A (en) * | 2009-09-10 | 2010-03-10 | 惠州市富力新技术有限公司 | Enhanced cement composite grinding aid |
| CN102172598A (en) * | 2011-01-11 | 2011-09-07 | 天津城市建设学院 | Red mud slurrying multistage circulating dealkalization method |
| CN102441339A (en) * | 2011-09-06 | 2012-05-09 | 福州大学 | Dissolving pulp sodium lignosulfonate dispersant, and reducing preparation method and application thereof |
| CN103045317A (en) * | 2012-12-26 | 2013-04-17 | 中国东方电气集团有限公司 | Lignin serial coal water slurry dispersing agent and preparation method thereof |
| CN103131020A (en) * | 2013-01-22 | 2013-06-05 | 华南理工大学 | Carboxylic sulfonic-acid-group lignin dye dispersing agent and preparation method thereof |
| CN104659369A (en) * | 2015-03-26 | 2015-05-27 | 天能集团江苏科技有限公司 | Preparation method of modified sodium lignosulfonate for lead-acid battery |
| CN105018160A (en) * | 2015-06-24 | 2015-11-04 | 济南圣泉集团股份有限公司 | Coal water slurry dispersant and its preparation method and use |
Non-Patent Citations (1)
| Title |
|---|
| 郭腊梅.纺织品整理学.中国纺织出版社,2005,41-46. * |
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