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CN-121976042-A - Extractant and extraction method

CN121976042ACN 121976042 ACN121976042 ACN 121976042ACN-121976042-A

Abstract

The application relates to an extracting agent and an extracting method, and relates to the technical field of industrial solid waste wet extraction, wherein the extracting agent comprises an extracting main agent, an impurity-resistant stabilizer and an extraction aid in parts by weight, the extracting main agent comprises di (2-ethylhexyl) phosphate and mono (2-ethylhexyl) phosphate, the impurity-resistant stabilizer comprises an imidazoline derivative, a triazine derivative and dimethyl methylphosphonate, the extraction aid comprises isooctanol, and the extracting method comprises the steps of ash ball preparation, impurity removal, extraction and the like. According to the extractant and the extraction method, trace heavy metal ions, sulfides, cyanides and other interference impurities generated by component fluctuation in the purified ash of the calcium carbide furnace are selectively chelated, so that the combination of the impurities and the extraction main agent is prevented, the anti-interference stability of the extractant under the fluctuation of the impurity content of the purified ash of the calcium carbide furnace is further improved, and the control difficulty in the production process is reduced.

Inventors

  • ZHANG YULONG
  • GUO XINMING
  • ZHANG TAO
  • ZHANG XIAOXU
  • FU RUI
  • LIU KANGWEI
  • SHAO LEI
  • HE GUANGLIN

Assignees

  • 聊城研聚新材料有限公司

Dates

Publication Date
20260505
Application Date
20260212

Claims (9)

  1. 1. The extractant is characterized by comprising, by mass, 45-55 parts of an extraction main agent, 7-10 parts of an anti-impurity stabilizer and 35-48 parts of an extraction auxiliary agent; the extraction main agent comprises di (2-ethylhexyl) phosphate and mono (2-ethylhexyl) phosphate, wherein the mass ratio of the di (2-ethylhexyl) phosphate to the mono (2-ethylhexyl) phosphate is 3-5:1; The anti-impurity stabilizer comprises an imidazoline derivative, a triazine derivative and dimethyl methylphosphonate, wherein the mass ratio of the imidazoline derivative to the triazine derivative to the dimethyl methylphosphonate is 1-2:1:0.8-1.2; The extraction aid comprises isooctyl alcohol.
  2. 2. The extractant of claim 1, further comprising 2-3 parts of a polyether-silicone composite anti-emulsifying agent.
  3. 3. The extractant according to claim 1, wherein the extraction main agent further comprises tributyl citrate and laurylamine polyoxyethylene ether, and wherein the mass ratio of di (2-ethylhexyl) phosphate to mono (2-ethylhexyl) phosphate to tributyl citrate to laurylamine polyoxyethylene ether is 3-5:1:0.1-0.2:0.05-0.1.
  4. 4. The extractant according to claim 1, wherein the extraction aid further comprises polyethylene glycol octyl phenyl ether, wherein the mass ratio of isooctyl alcohol to polyethylene glycol octyl phenyl ether is 5-8:1.
  5. 5. The extractant according to claim 1, wherein the extraction aid further comprises ethyl acetate, wherein the mass ratio of isooctyl alcohol to ethyl acetate is 5-7:1.
  6. 6. An extraction method using the extractant according to any one of claims 1 to 5, comprising the steps of: The preparation of ash balls comprises the steps of mixing the purified ash of a calcium carbide furnace with a binder according to a mass ratio of 8-10:1, pyrolyzing for 1-2 hours at 300-350 ℃, adding water, stirring uniformly, extruding into spheres with diameters of 7.5+/-2.5 mm, and drying for 2-4 hours at 110-120 ℃, wherein the binder is one or two of sodium carboxymethyl cellulose or polyvinyl alcohol; Mixing ash balls with 1.0-1.5 mol/L hydrochloric acid solution according to a solid-liquid volume ratio of 1:4-6, stirring for 20-30 min at a temperature of 30-40 ℃, sequentially adding ferric chloride accounting for 0.3-0.5wt% of the water phase and ferrous sulfate accounting for 0.2-0.4wt% of the water phase into the leached water phase, stirring and reacting for 10-15 min, adding aminophosphonic acid type chelating microspheres accounting for 0.5-0.8wt% of the water phase into the water phase, stirring and adsorbing for 15-20 min at a temperature of 30-40 ℃, filtering, and removing sediment and chelating microspheres to obtain a water phase after impurity removal; mixing an extractant and sulfonated kerosene to form an organic phase, carrying out countercurrent contact extraction on the organic phase and the water phase after impurity removal, extracting for 50-70 min at 30-50 ℃, standing for 10-15 min, and separating to obtain a calcium-magnesium ion loaded organic phase and a raffinate water phase; The extractant occupies 25-35 wt% of the mass of the organic phase, and the volume ratio of the organic phase to the water phase after impurity removal is 2.0-3.0:1.
  7. 7. The method according to claim 6, further comprising a back-extraction step, the back-extraction step being provided after the extraction step, the back-extraction step comprising: Performing calcium ion stripping, namely stripping for 20-40 min at 45-55 ℃ by adopting a sulfuric acid solution with the concentration of 0.8-1.2 mol/L as a calcium stripping agent to obtain a calcium-rich stripping solution, wherein the volume ratio of the calcium stripping agent to a calcium-magnesium ion loaded organic phase is 1:1.2-1.8; and magnesium ion stripping, namely, adopting sulfuric acid-phosphoric acid mixed solution as a magnesium stripping agent, and carrying out stripping for 15-25 min at 55-60 ℃ to obtain magnesium-rich stripping solution, wherein the volume ratio of the magnesium stripping agent to a calcium-magnesium ion loaded organic phase subjected to calcium ion stripping is 1:1.5-1.8, the sulfuric acid concentration in the sulfuric acid-phosphoric acid mixed solution is 1.5-2.5 mol/L, and phosphoric acid accounts for 10-15 wt% of the mass of the mixed solution.
  8. 8. The method according to claim 7, further comprising a strip liquor control step, the strip liquor control step being disposed after the strip step, the strip liquor control step comprising: Adding barium chloride solution accounting for 0.8-1.2wt% of the calcium-rich strip liquor into the calcium-rich strip liquor, stirring and reacting for 15-20 min at 30-40 ℃, filtering to remove barium sulfate precipitate and obtain desulphated calcium-rich liquor; and adding ammonia water into the magnesium-rich strip liquor until the pH value is 9.0-9.5, and stirring under the ultrasonic conditions of 150-200W and 20kHz to generate a precipitate.
  9. 9. Use of an extractant according to any one of claims 1 to 5 or an extraction process according to any one of claims 6 to 8 for extracting calcium and magnesium ions from trace sulfide, cyanide furnace cleaning ash for the preparation of high purity magnesium hydroxide and calcium carbonate.

Description

Extractant and extraction method Technical Field The invention relates to the technical field of industrial solid waste wet extraction, in particular to an extractant and an extraction method. Background The calcium carbide furnace is used as core equipment for calcium carbide production, a large amount of calcium carbide furnace purification ash can be generated in the production process, the ash slag is rich in magnesium oxide, calcium oxide and other effective components, and simultaneously contains trace sulfide and cyanide, so that the calcium carbide furnace has the characteristics of fine granularity, light specific gravity, easiness in spontaneous combustion, high powder fineness, easiness in dust raising, easiness in blocking a pipeline when being sticky when meeting damp and the like. Along with the continuous expansion of the productivity of the calcium carbide industry, the production amount of the purified ash of the calcium carbide furnace synchronously increases, and the harmless treatment and the recycling utilization of the purified ash become important subjects for restricting the development of the industry. At present, the treatment of the purification ash of the calcium carbide furnace in the industry mainly takes landfill, and the method not only occupies a large amount of land resources, but also can cause soil and water pollution due to dust diffusion and harmful substance leakage, and further causes waste of high-quality resources such as magnesium oxide, calcium oxide and the like, which is contrary to the development demands of clean production and resource circulation in the industry. Aiming at the problems, the Chinese patent application with publication number of CN114477249A and publication number of 2022 and 5/13 proposes a method for preparing high-purity magnesium hydroxide and calcium sulfate by adopting calcium carbide furnace purification ash, which comprises the steps of carrying out dipping treatment on the purification ash by adopting ammonium carboxylate/amine salt solution and then filtering to obtain ammonia/amine gas, calcium carboxylate solution and crude magnesium hydroxide, carrying out reaction on the ammonia/amine gas and magnesium carboxylate solution and then filtering to obtain wet Mg (OH) 2 solid and ammonium carboxylate/amine salt solution, carrying out double decomposition reaction on the calcium carboxylate solution and sulfuric acid and then filtering to obtain calcium sulfate and carboxylic acid solution, carrying out reaction on crude magnesium hydroxide and carboxylic acid solution to obtain magnesium carboxylate solution and residues, wherein the magnesium carboxylate solution is used for synthesizing Mg (OH) 2. However, the inventor finds that, because the purifying ash component of the calcium carbide furnace is complex, when the impurity content fluctuates, the anti-interference capability of the extractant in the scheme is obviously insufficient, thereby directly increasing the difficulty of production control and affecting the quality stability of the product. Disclosure of Invention The invention provides an extractant and an extraction method for solving the problem that the extractant has weak anti-interference capability due to complex components and fluctuation of impurity content of purified ash. In a first aspect, the invention provides an extractant, which adopts the following technical scheme: the extractant comprises, by mass, 45-55 parts of an extraction main agent, 7-10 parts of an anti-impurity stabilizer and 35-48 parts of an extraction auxiliary agent; the extraction main agent comprises di (2-ethylhexyl) phosphate and mono (2-ethylhexyl) phosphate, wherein the mass ratio of the di (2-ethylhexyl) phosphate to the mono (2-ethylhexyl) phosphate is 3-5:1; The anti-impurity stabilizer comprises an imidazoline derivative, a triazine derivative and dimethyl methylphosphonate, wherein the mass ratio of the imidazoline derivative to the triazine derivative to the dimethyl methylphosphonate is 1-2:1:0.8-1.2; The extraction aid comprises isooctyl alcohol. By adopting the technical scheme, the extraction main agent adopts di (2-ethylhexyl) phosphate and mono (2-ethylhexyl) phosphate, phosphate groups in the molecular structure of the extraction main agent can form stable complexes with calcium and magnesium ions, and meanwhile, the phosphate groups and the calcium and magnesium ions are mixed to reduce competitive adsorption of impurity ions, the imidazoline derivative and the triazine derivative in the anti-impurity stabilizer have stronger impurity chelating capability, and the impurity stabilizer can selectively chelate trace heavy metal ions, sulfides, cyanides and other interference impurities generated by component fluctuation in the purified ash, prevent the trace heavy metal ions, sulfides, cyanides and other interference impurities from being combined with the extraction main agent, and the methyl phosphonic acid dimethyl ester e