CN110756162A - Synthesis of P5O7 composite carbon fiber material and method for adsorbing and separating indium in liquid crystal panel by using same - Google Patents
Synthesis of P5O7 composite carbon fiber material and method for adsorbing and separating indium in liquid crystal panel by using same Download PDFInfo
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- CN110756162A CN110756162A CN201911017802.2A CN201911017802A CN110756162A CN 110756162 A CN110756162 A CN 110756162A CN 201911017802 A CN201911017802 A CN 201911017802A CN 110756162 A CN110756162 A CN 110756162A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28023—Fibres or filaments
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for synthesizing an extractant P5O7 composite carbon fiber material and for adsorbing and separating indium in a liquid crystal panel. The invention belongs to the technical field of indium recycling, and particularly relates to a method for recycling indium from a waste liquid crystal display screen panel. The method comprises the following steps: (1) soaking carbon fibers in acetone, removing epoxy resin glue on the surface, drying the carbon fibers in a drying oven at 60 ℃, taking out the carbon fibers, cooling the carbon fibers, fully soaking the carbon fibers in P5O7, taking out the carbon fibers, cleaning the carbon fibers with deionized water for 3 times, and drying the carbon fibers in the drying oven at 110 ℃ to obtain a P5O7-C fiber composite material; (2) preparing 0-1000ppm InCl3 aqueous solution, adding 0.1-4 g/L P5O7/C fiber composite material, adsorbing and separating indium at 25-45 ℃ of a shaking table at 200-300rpm and at the pH value of 0-3, wherein the recovery rate of In3+ is more than 95%, desorption of In3+ can be realized by using 3mol/L hydrochloric acid, and the desorption efficiency can reach 80%. The composite material can be repeatedly used, and the recovery rate of the P5O7/C fiber composite material to In3+ is basically kept unchanged after 7 cycle tests.
Description
Technical Field
The invention belongs to the technical field of indium recycling, and particularly relates to a method for recycling indium from a waste liquid crystal display screen panel.
Background
Indium is a valuable strategic metal resource and is the main component of ITO films in Liquid Crystal Displays (LCDs) on Liquid crystal panels. With the development of science, the service life of a liquid crystal panel is generally 3-5 years. With the upgrade of electronic products, a large amount of waste liquid crystal panels will be generated. These electronic wastes contain a considerable amount of indium metal. Statistically, more than half of the indium metal is recovered from the secondary resource. When the indium content in the secondary resource reaches 0.002%, it is worth recovering indium. In a waste liquid crystal panel, the indium content exceeds 0.03%. Therefore, the discarded liquid crystal panel is an important secondary resource in the indium recovery process. Indium is a toxic metal, and if electronic waste is directly put into the environment, lung cancer or lung diseases are easily caused. And the recovered In3+ not only reduces the pollution caused by directly discharging the metal into the garbage, but also can generate good economic benefit.
The traditional method for recovering indium in the liquid crystal panel mainly adopts a cation exchange resin method, an acid leaching extraction mode, a coprecipitation method, replacement or electrolysis, a solvent extraction method and the like. Among them, the solvent extraction method has many advantages such as high selectivity, good effect, low energy consumption, and is suitable for separation of heat-sensitive substances. The related patents mainly include: in the patent of a method for extracting and separating indium and tin from indium-containing leaching slag (Redanhua and the like, application number CN 201510149137.8), indium and tin are extracted simultaneously by adopting P2O4, tin is complexly and reversely extracted by adopting fluoride, and then indium is reversely extracted by hydrochloric acid, so that a large amount of raffinate generated by the method is difficult to treat, and environmental protection is influenced; in the patent of a method for recovering indium from indium-containing neutralized sediments obtained by directly leaching zinc concentrate (Tang Aiyong et al, application No. 200910311599. X), sponge indium is prepared by adopting a plurality of steps of primary sulfuric acid leaching, zinc powder enrichment, secondary sulfuric acid leaching, iron powder essence, P2O4 extraction, hydrochloric acid back extraction, chip replacement and the like.
The technologies of the patents adopt the chelating agent P2O4 for extraction, a large amount of organic solvent is needed for assisting the extraction, and the subsequent back extraction process has the problems of easy loss of the organic solvent, difficult solid-liquid separation and the like.
In the patent of preparation method of impregnating resin for adsorbing scattered metal indium (III) (Liu military deep et al, application number CN 201811102086.3), styrene-divinyl macroporous adsorption resin is used as a carrier, and a mixed extraction agent of N1923 and phytic acid is used as an adsorption site to adsorb the scattered metal indium (III) in an acid solution system.
The synthesis of P2O4 composite UiO-66 material and the method for adsorbing and separating indium in liquid crystal panel (Deming et al, application No. 201910851278.2) adopts P2O4 composite UiO-66 material, the used UiO-66 material is MOFs material, the UiO-66 is powder porous material, the powder needed to be coated is more, and the cost is higher.
Carbon fiber has the excellent characteristics of strong acid resistance, strong alkali resistance, high temperature resistance, no harm to organisms and the like. The aluminum alloy is lighter than metal aluminum, but has higher strength than steel and corrosion resistance. The carbon fiber is compounded with P5O7, and after the indium is adsorbed, the carbon fiber can be desorbed in strong acid, so that the effect of recycling is achieved.
Disclosure of Invention
[1] The technical problem to be solved by the invention is to provide a preparation method of a P5O7 composite C fiber material with low cost, simple manufacture, excellent performance and acid resistance and an In3+ of an LCD In an adsorption separation liquid crystal panel. Has the advantages of high efficiency, energy saving, convenient operation, etc.
[2] In order to solve the technical problem, the synthesized material comprises the following steps:
the method comprises the following steps: soaking carbon fibers in acetone, removing epoxy resin glue on the surface, drying in an oven at 60 ℃, taking out, cooling, soaking in P5O7, taking out, washing with deionized water for 3 times, and drying in an oven at 110 ℃. Obtaining the P5O7-C fiber composite material;
step two: a 23ppm indium chloride solution was prepared and used for adsorption studies.
[3] The P5O7/C fiber composite material synthesized by the steps has acid resistance and stable structure under the strong acid condition.
[4] Compared with the prior art, the invention has the beneficial effects that: the invention has simple preparation and acid resistance, and can be applied to acidic solution to absorb In3 +; 2 compared with the traditional method for recovering In3+, the method of the invention comprises the following steps: the method is simple to operate and recover, does not generate new chemical pollution, has good anti-interference performance, and can also recover In3+ under an acidic condition.
Drawings
Fig. 1 pure C fiber XRD pattern.
FIG. 2 is a FT-IR chart of a P5O7/C fiber composite prepared from pure C fibers and example 1 of the invention.
FIG. 3 is a photograph of a P5O7/C fiber composite prepared in example 1 of the present invention.
The upper left and upper right of the figure 4 are scanning electron micrographs of pure C fiber samples, and the lower left and lower right are scanning electron micrographs of P5O7/C fiber composite materials.
FIG. 5 the cyclic performance of the P5O7/C fiber composite material prepared In the embodiment 1 of the present invention for In3 +.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings and specific embodiments, which are merely illustrative of the present invention and are not limited to the present invention.
Example 1 was carried out.
The technical problem to be solved by the invention is to provide a preparation method of a P5O7 composite C fiber material with low cost, simple manufacture, excellent performance and acid resistance and an In3+ of an LCD In an adsorption separation liquid crystal panel. Has the advantages of high efficiency, energy saving, convenient operation, etc.
Fig. 1 pure C fiber XRD pattern, 25.8 degree is d002 crystal face of carbon fiber.
FIG. 2 is a FT-IR chart of a P5O7/C fiber composite prepared by pure C fiber and the embodiment 1 of the invention; . Only 1382 cm-1 of pure C fiber has a characteristic peak, and the P5O7/C fiber composite material also has 1041 cm-1 characteristic peak P-O-C bond and 1203 cm-1 characteristic peak P = O bond besides the 1384 cm-1 carbon fiber characteristic peak. The characteristic peaks of 2865 cm-1 and 2956 cm-1 are C-H bonds. This indicates successful compounding of the P5O7-C fiber.
FIG. 3 is a photograph of a P5O7/C fiber composite material prepared in example 1 of the present invention, from which it can be seen that the P5O7/C fiber composite material is a net-like material.
In FIG. 4, the upper left and upper right images are scanning electron micrographs of pure C fiber samples, each fiber is, the lower left and lower right are scanning electron micrographs of P5O7/C fiber composite material, and the surface becomes smooth after surface compounding. This is due to the coverage of P5O7 on the surface of the C fiber.
Example 2 was carried out.
A23 ppm aqueous solution of InCl3 was prepared for use. Adsorption experiment: 20mL of the indium solution were added to 0.15 g of the P5O7/C fiber composite prepared in case 1, with the table parameters: 25 ℃, 200r/min, pH = 3. The reaction time was 15 min. Desorption parameters: at 25 ℃, 200r/min, the reaction time is 15min, and 7ml of hydrochloric acid solution with the thickness of 3m is used for desorption. The above samples were quantified by ICP-OES analysis and plotted as a cycle curve in FIG. 5. As can be seen from FIG. 5, the P5O7/C fiber composite material has the advantages of excellent adsorption performance, short reaction time and good regeneration cycle performance. After 7 cycles, the adsorption rate of 98 percent can still be maintained.
Claims (7)
1. A method for synthesizing a P5O7/C fiber composite material and using the composite material for adsorbing and separating indium in a liquid crystal panel is characterized by comprising the following steps of synthesizing the P5O7/C fiber composite material: soaking the carbon fiber in acetone, removing epoxy resin glue on the surface, drying the carbon fiber in a 60 ℃ drying oven, taking out the carbon fiber, cooling, soaking the carbon fiber in P5O7, taking out the carbon fiber, cleaning the carbon fiber with deionized water for 3 times, and drying the carbon fiber in a 110 ℃ drying oven to obtain the P5O7/C fiber composite material.
2. A P5O7/C fiber composite material synthesis and method for using the composite material P5O7/C fiber in adsorption separation of indium in a liquid crystal panel are characterized in that the composite material P5O7/C fiber is a reticular fiber, and after the indium is adsorbed and separated, the separation is easy, and the separation and recovery can be realized without centrifugation or filtration.
3. A P5O7/C fiber composite material synthesis and a method for absorbing and separating indium in a liquid crystal panel are characterized in that the material has high indium absorption speed, the recovery rate can reach more than 98% within 15 minutes, and the desorption rate is also high.
4. The synthesis of the P5O7/C fiber composite material and the method for adsorbing and separating indium In the liquid crystal panel are characterized In that the concentration of the In3+ solution is 1-1000 mg/L.
5. A P5O7/C fiber composite material synthesis and a method for using the composite material to absorb and separate indium in a liquid crystal panel are characterized in that the adding amount of the composite material is 0.1-4 g/L.
6. A P5O7/C fiber composite material synthesis and a method for using the material In adsorption and separation of indium In a liquid crystal panel are characterized In that the material can be used In an actual liquid crystal panel to adsorb and separate In3 +.
7. A P5O7/C fiber composite material synthesis and a method for using the composite material in adsorption separation of indium in a liquid crystal panel are characterized in that the composite material has good recycling performance, and can still maintain 98% of indium recovery rate after 7 times of recycling.
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Application publication date: 20200207 |