CN108607523B - Adsorbent material for selective separation of indium and preparation method thereof - Google Patents

Adsorbent material for selective separation of indium and preparation method thereof Download PDF

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CN108607523B
CN108607523B CN201810562152.9A CN201810562152A CN108607523B CN 108607523 B CN108607523 B CN 108607523B CN 201810562152 A CN201810562152 A CN 201810562152A CN 108607523 B CN108607523 B CN 108607523B
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CN108607523A (en
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李敏
冯建
孟晓静
唐思
汪麒麟
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Chongqing Jack Environmental Protection Co ltd
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    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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Abstract

本发明公开了一种选择性分离铟的吸附材料，所述吸附材料包括基质以及在基质表面修饰的能于铟离子配位的功能单体。本发明还公开了一种选择性分离铟的吸附材料的制备方法，包括如下步骤：1)在二氧化硅表面修饰羧基，标记为SG‑COOH；2)将硫酸铟溶解于二甲基亚砜中，并加入乙烯基磷酸和烯丙基硫醇，搅拌一段时间，得到溶液A；3)将步骤1)所得SG‑COOH与步骤2)所得溶液A混合，再加入二甲基丙烯酸乙二醇酯和偶氮二异丁腈，在无氧条件下，发生聚合反应，得到聚合物B；4)将得到的聚合物B使用酸洗脱出铟离子，依次用去离子水洗至中性，再烘干，即得选择性分离铟的吸附材料。所述吸附材料制备方法简单，并且所述吸附材料针对低浓度铟离子的吸附效率高。The invention discloses an adsorption material for selective separation of indium. The adsorption material comprises a matrix and a functional monomer capable of coordinating with indium ions modified on the surface of the matrix. The invention also discloses a preparation method of an adsorption material for selectively separating indium, comprising the following steps: 1) modifying carboxyl groups on the surface of silica, marked as SG-COOH; 2) dissolving indium sulfate in dimethyl sulfoxide , and add vinyl phosphoric acid and allyl mercaptan, and stir for a period of time to obtain solution A; 3) mix the SG-COOH obtained in step 1) with the solution A obtained in step 2), and then add ethylene glycol dimethacrylate Ester and azobisisobutyronitrile, under anaerobic conditions, undergo a polymerization reaction to obtain polymer B; 4) use acid to elute the indium ion from the obtained polymer B, wash it with deionized water to neutrality, and then After drying, an adsorbent for selectively separating indium can be obtained. The preparation method of the adsorption material is simple, and the adsorption efficiency of the adsorption material for low-concentration indium ions is high.

Description

Adsorption material for selectively separating indium and preparation method thereof
Technical Field
The invention belongs to the field of environmental pollution control and rare material recovery, and particularly relates to an adsorption material for selectively separating indium and a preparation method thereof.
Background
Indium, a very low-content rare-earth element in the earth's crust, is widely dispersed in nature, and so far no deposit with indium as an independent or main component has been found to exist in other minerals in the form of impurities. However, indium and its compounds are widely used in the fields of aviation, electronics, and military industry. In addition, indium ions in the aqueous solution are a heavy metal ion which poses serious threats to the environment and human health, so that the method has important significance for selective separation and recovery of indium ions in the aqueous solution from the perspective of resource recycling and the perspective of removing the metal ions in the aqueous solution.
Currently, there are mainly chemical precipitation and liquid-liquid extraction methods for indium separation and recovery. Patent CN 106086410 a discloses a method for separating and recovering indium and zinc from a solution after indium extraction and substitution, which requires that indium and zinc are separated by adjusting the pH value, and then indium is recovered by back extraction. This method of chemical precipitation is often used in systems where the concentration of indium ions is high, and as mentioned above, indium is a very low-dispersion element, and therefore its concentration in aqueous solution is generally low, and other interfering metal ions are also present. The method has certain limitations. Patent CN 103620070 a discloses a method for recovering indium, which adopts a method of strain to recover indium, and this method generally has a small amount of treatment, a long time and a relatively high cost; patent CN 102061398A mentions that indium is recovered by directly adopting a step-by-step extraction method, and although the liquid-liquid extraction method is the main method for recovering indium at present, there are many disadvantages, such as organic phase residue, complex operation, and serious environmental pollution. CN201380050353 discloses a method for producing a complex-forming adsorbent for selective extraction of indium. The technical scheme uses spherical and granular cross-linked macroporous acrylonitrile as a carrier and an organic carrier, and has high cost and complicated modification operation steps.
Therefore, in the field of indium separation and recovery, it is necessary to develop a simpler and easier adsorbent.
Disclosure of Invention
In view of the above problems in the prior art, an object of the present invention is to provide an adsorbent that can efficiently adsorb and recover indium ions when the indium ion concentration is low, and that has a simple preparation method and a high adsorption efficiency for low-concentration indium ions.
In order to achieve the above purpose, the following technical solutions are specifically provided:
1. an adsorption material for selectively separating indium, which comprises a silicon dioxide matrix and a functional monomer modified on the surface of the silicon dioxide matrix and capable of coordinating with indium ions.
2. A preparation method of an adsorption material for selectively separating indium comprises the following steps:
1) modifying carboxyl on the surface of the silicon dioxide, and marking the carboxyl as SG-COOH;
2) dissolving indium sulfate in dimethyl sulfoxide, adding vinylphosphonic acid and allyl mercaptan, and stirring for a period of time to obtain a solution A;
3) mixing SG-COOH obtained in the step 1) with the solution A obtained in the step 2), adding ethylene glycol dimethacrylate and azobisisobutyronitrile, and carrying out polymerization reaction under an anaerobic condition to obtain a polymer B;
4) and removing indium ions from the obtained polymer B by using acid washing, washing the polymer B to be neutral by using deionized water in sequence, and drying to obtain the adsorption material for selectively separating indium.
In a preferred technical scheme, the step 1) is carried out according to the following method: firstly, modifying amino on the surface of silicon dioxide, and marking the amino as SG-NH2And further reacting to obtain SG-COOH.
The technical scheme for modifying amino on the surface of silicon dioxide comprises the following steps: toluene is used as a dispersing agent to prepare silicon dioxide nano-particle turbid liquid with the solid-liquid mass volume ratio of 1-60 percent and the particle size of 40-400 meshes, gamma-aminopropyltriethoxysilane is added into the silicon dioxide nano-particle turbid liquid and is stirred uniformly, and the solid-liquid mass of the gamma-aminopropyltriethoxysilane and the silicon dioxide nano-particle turbid liquid is addedThe volume ratio is 30-100%, the temperature is controlled to be 20-110 ℃ for reaction for 24h, and SG-NH is obtained after filtration and washing2。
Further, SG-COOH was prepared by the following reaction method, and obtained SG-NH250g of the mixture is dispersed in tetrahydrofuran, 15g of maleic anhydride is added, the mixture reacts for 24 hours at room temperature, and SG-COOH is obtained after filtration, washing and drying.
Further, indium sulfate is dissolved in dimethyl sulfoxide, mixed liquid of vinyl phosphoric acid and allyl mercaptan is added, stirring is carried out for reaction for 2 hours, and solution A is obtained, wherein the mass ratio of indium sulfate to dimethyl sulfoxide is 0.1% -20%, vinyl phosphoric acid and allyl mercaptan can be mixed in any ratio, the mass ratio of the mixed liquid to indium sulfate is 0.1% -0.4%, and the reaction temperature of the system is 10-70 ℃.
Further, the synthesis method of the polymer B comprises the following steps: mixing SG-COOH obtained in the step 1) with the solution A obtained in the step 2), adding ethylene glycol dimethacrylate and azobisisobutyronitrile, and carrying out polymerization reaction at the temperature of 20-70 ℃ under an anaerobic condition to obtain a polymer B.
Further, the acid used in the acid washing in the step 4) is one or more of sulfuric acid, hydrochloric acid or nitric acid.
The invention has the beneficial effects that: according to the invention, the adsorption material is prepared by modifying the surface of silicon dioxide into a functional monomer capable of coordinating with indium ions by using a widely-existing inorganic material, and the adsorption material can realize the effect of effectively recovering indium from low-concentration indium ion wastewater. In addition, the preparation method of the adsorption material has the advantages that the cost of all materials is low, the matrix material is widely available, and the price of the used modification material is low; in addition, the preparation process conditions are not harsh, and the operation is simple and easy.
Detailed Description
The present invention will be explained in more detail with reference to specific examples.
Example 1
In a 1000mL flask, 50g of 50 mesh silica was added and dispersed in 350mL of tolueneAdding 50mL of gamma-aminopropyltriethoxysilane, reacting and refluxing for 24h at 70 ℃, filtering, washing and drying to obtain SG-NH2(ii) a The obtained SG-NH2Dispersing 50g of the mixture in tetrahydrofuran, adding 15g of maleic anhydride, reacting for 24 hours at room temperature, and filtering, washing and drying to obtain SG-COOH;
dissolving indium sulfate in dimethyl sulfoxide to prepare a solution with the mass fraction of 10%, adding a mixed solution of 10 wt% of vinylphosphoric acid and allyl mercaptan, and stirring for reacting for 2h to obtain a solution A. Weighing 40g of the obtained SG-COOH, adding the SG-COOH into 150ml of the solution A, then adding 0.4g of ethylene glycol dimethacrylate and 0.4g of azobisisobutyronitrile, introducing nitrogen and discharging oxygen for 20min, and reacting for 24h at the temperature of 60 ℃ to obtain a polymer B; and eluting the obtained polymer A with sulfuric acid to obtain indium ions, sequentially washing with deionized water to neutrality, and drying to obtain the novel adsorption material for selectively separating indium. Weighing 1.50g of the obtained adsorbing material, placing In an adsorbing column with diameter of 1cm and height of 10cm, and using for In3+In the mining and metallurgy wastewater (the wastewater contains a large amount of Fe3+、Zn2+、Ca2+、Mg2+、Al3+K +, Na +, and the like) and selective separation and recovery of In3+, and the result shows that the material can realize In the wastewater3+The adsorption capacity reaches 82.53mg/g and the recovery rate reaches more than 98 percent.
Example 2
Adding 50g of chromatographic silica gel into a 1000mL flask, dispersing the chromatographic silica gel into 350mL of toluene, adding 50mL of gamma-aminopropyltriethoxysilane, reacting and refluxing for 24 hours, filtering, washing and drying to obtain SG-NH2(ii) a The obtained SG-NH2Dispersing 50g of the mixture in tetrahydrofuran, adding 15g of maleic anhydride, reacting for 24 hours at room temperature, and filtering, washing and drying to obtain SG-COOH;
dissolving indium sulfate in dimethyl sulfoxide to prepare a solution with the mass fraction of 10%, adding a mixed solution of 10 wt% of vinyl phosphoric acid and allyl mercaptan into the solution, and stirring at 70 ℃ for reacting for 2 hours to obtain a solution A; 50g of the obtained SG-COO was weighed outAdding H into 240ml of the solution A, then adding 0.5g of ethylene glycol dimethacrylate and 0.5g of azobisisobutyronitrile, introducing nitrogen and discharging oxygen for 20min, and reacting for 24H at the temperature of 60 ℃ to obtain a polymer A; and removing indium ions from the obtained polymer A through nitric acid washing, sequentially washing with deionized water to be neutral, and drying to obtain the novel adsorption material for selectively separating indium. Weighing 1.50g of the obtained adsorbing material, placing In an adsorbing column with diameter of 1cm and height of 10cm, and using for In3+In the mining and metallurgy wastewater (the wastewater contains a large amount of Fe3+、Zn2+、Ca2+、Mg2+、Al3+、K+、Na+Etc.), In3+The result shows that the material can realize In the wastewater3+The adsorption capacity reaches 76.63mg/g and the recovery rate reaches 99.65 percent.
Example 3
Adding 50g of fly ash into a 1000mL flask, dispersing the fly ash into 350mL of toluene, adding 50mL of gamma-aminopropyltriethoxysilane, reacting and refluxing for 24 hours, filtering, washing and drying to obtain SG-NH2(ii) a The obtained SG-NH2Dispersing 50g of the mixture in acetic acid, adding 15g of maleic anhydride, reacting for 24 hours at room temperature, and filtering, washing and drying to obtain SG-COOH;
dissolving indium sulfate in dimethyl sulfoxide to prepare a solution with the mass fraction of 15%, adding a mixed solution of 10 wt% of vinylphosphoric acid and vinylmercaptan, and stirring for reacting for 2 hours to obtain a solution A; weighing 50 parts of SG-COOH obtained above, adding the SG-COOH into the solution A, then adding 0.5 part of ethylene glycol dimethacrylate and 0.5 part of azodiisobutyronitrile, introducing nitrogen and discharging oxygen for 20min, and reacting for 24h at the temperature of 60 ℃ to obtain a polymer A; and removing indium ions from the obtained polymer A through nitric acid washing, sequentially washing with deionized water to be neutral, and drying to obtain the novel adsorption material for selectively separating indium. Weighing 1.50g of the obtained adsorbing material, placing In an adsorbing column with diameter of 1cm and height of 10cm, and using for In3+In the mining and metallurgy wastewater (the wastewater contains a large amount of Fe3+、Zn2+、Ca2+、Mg2+、Al3+、K+、Na+Etc.), In3+The result shows that the material can realize In the wastewater3+The adsorption capacity reaches 25.38mg/g, and the recovery rate reaches 93.61%.
The above examples further illustrate the present invention by modifying the surface of silica component with a functional monomer capable of coordinating with indium ions by using a widely available inorganic material to prepare an adsorbing material, which can achieve the effect of efficiently recovering indium from low-concentration indium ion wastewater.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.

Claims (8)

1.一种选择性分离铟的吸附材料，其特征在于，所述吸附材料包括基质以及在基质表面修饰的能与铟离子配位的功能单体，所述基质包括主要成分二氧化硅；1. An adsorbent material for selectively separating indium, characterized in that the adsorbent material comprises a matrix and a functional monomer capable of coordinating with indium ions modified on the surface of the matrix, and the matrix comprises a main component silicon dioxide; 所述选择性分离铟的吸附材料的制备方法，包括如下步骤：The preparation method of the adsorbent material for selectively separating indium comprises the following steps: 1)首先在二氧化硅表面修饰氨基，标记为SG-NH2，再进一步反应得到SG-COOH；1) First, modify the amino group on the surface of silica, marked as SG-NH 2 , and then further react to obtain SG-COOH; 2)将硫酸铟溶解于二甲基亚砜中，并加入乙烯基磷酸和烯丙基硫醇，搅拌一段时间，得到溶液A；2) dissolving indium sulfate in dimethyl sulfoxide, adding vinyl phosphoric acid and allyl mercaptan, and stirring for a period of time to obtain solution A; 3)将步骤1)所得SG-COOH与步骤2)所得溶液A混合，再加入二甲基丙烯酸乙二醇酯和偶氮二异丁腈，在无氧条件下，发生聚合反应，得到聚合物B；3) Mix the SG-COOH obtained in step 1) with the solution A obtained in step 2), then add ethylene glycol dimethacrylate and azobisisobutyronitrile, and under anaerobic conditions, a polymerization reaction occurs to obtain a polymer B; 4)将得到的聚合物B使用酸洗脱出铟离子，依次用去离子水洗至中性，再烘干，即得选择性分离铟的吸附材料；4) using acid to elute out indium ions from the obtained polymer B, washing with deionized water until neutrality in turn, and drying again to obtain an adsorbent material for selectively separating indium; 在二氧化硅表面修饰氨基的技术方案为：以甲苯作为分散剂，配制固液质量体积比为1％～60％粒径为40～400目的二氧化硅纳米颗粒浊液，向二氧化硅纳米颗粒浊液中加入γ-氨丙基三乙氧基硅烷并搅匀，所加入γ-氨丙基三乙氧基硅烷与二氧化硅纳米颗粒浊液的固液质量体积比为30％～100％，控制温度20℃～110℃反应24h，经过滤、洗涤即得SG-NH2。The technical scheme of modifying amino groups on the surface of silica is as follows: using toluene as a dispersant, preparing a turbid liquid of silica nanoparticles with a solid-liquid mass volume ratio of 1% to 60% and a particle size of 40 to 400 meshes, and adding silica nanoparticles Add γ-aminopropyltriethoxysilane to the cloudy particle liquid and stir it evenly, and the solid-liquid mass-volume ratio of the added γ-aminopropyltriethoxysilane to the cloudy silica nanoparticle liquid is 30% to 100%. %, control the temperature to 20℃～110℃ and react for 24h, then filter and wash to obtain SG-NH 2 . 2.根据权利要求1所述一种选择性分离铟的吸附材料，其特征在于，所述基质为二氧化2 . The adsorbent material for selective separation of indium according to claim 1 , wherein the matrix is a carbon dioxide. 3 . 硅、硅胶、粉煤灰。Silicon, silica gel, fly ash. 3.一种选择性分离铟的吸附材料的制备方法，其特征在于，包括如下步骤：3. A preparation method of an adsorbent material for selective separation of indium, characterized in that it comprises the following steps: 1)在二氧化硅表面修饰羧基，标记为SG-COOH；1) Modification of carboxyl groups on the surface of silica, marked as SG-COOH; 2)将硫酸铟溶解于二甲基亚砜中，并加入乙烯基磷酸和烯丙基硫醇，搅拌一段时间，得到溶液A；2) dissolving indium sulfate in dimethyl sulfoxide, adding vinyl phosphoric acid and allyl mercaptan, and stirring for a period of time to obtain solution A; 3)将步骤1)所得SG-COOH与步骤2)所得溶液A混合，再加入二甲基丙烯酸乙二醇酯和偶氮二异丁腈，在无氧条件下，发生聚合反应，得到聚合物B；3) Mix the SG-COOH obtained in step 1) with the solution A obtained in step 2), then add ethylene glycol dimethacrylate and azobisisobutyronitrile, and under anaerobic conditions, a polymerization reaction occurs to obtain a polymer B; 4)将得到的聚合物B使用酸洗脱出铟离子，依次用去离子水洗至中性，再烘干，即得选择性分离铟的吸附材料。4) The obtained polymer B is eluted with acid to remove indium ions, washed with deionized water until neutral, and then dried to obtain an adsorption material for selectively separating indium. 4.根据权利要求3所述一种选择性分离铟的吸附材料的制备方法，其特征在于，步骤1)4. the preparation method of the adsorbent material of a kind of selective separation of indium according to claim 3, is characterized in that, step 1) 制备方法为：首先在二氧化硅表面修饰氨基，标记为SG-NH2，再进一步反应得到SG-COOH。The preparation method is as follows: firstly, an amino group is modified on the surface of silica, which is marked as SG-NH 2 , and then SG-COOH is obtained by further reaction. 5.根据权利要求4所述一种选择性分离铟的吸附材料的制备方法，其特征在于，所述SG-COOH按如下方法反应制备，取50g SG-NH2分散在四氢呋喃中，并加入15g顺丁烯二酸酐，在室温条件下反应24h，经过滤、洗涤和烘干即得到SG-COOH。5. the preparation method of the adsorbent material of a kind of selective separation of indium according to claim 4, is characterized in that, described SG-COOH reacts and prepares as follows, get 50g SG - NH Disperse in tetrahydrofuran, and add 15g Maleic anhydride, reacted at room temperature for 24h, filtered, washed and dried to obtain SG-COOH. 6.根据权利要求3所述一种选择性分离铟的吸附材料的制备方法，其特征在于，所述溶液A的合成方法为：将硫酸铟溶解于二甲基亚砜中，并加入乙烯基磷酸和烯丙基硫醇的混合液，搅拌反应2h，得到溶液A，其中，硫酸铟与二甲基亚砜之间的质量比例为0.1％～20％，乙烯基磷酸、烯丙基硫醇之间可以任意比例混合，其组成的混合液与硫酸铟的质量比为0.1％～0.4％，体系的反应温度为10℃～70℃。6 . The method for preparing an adsorbent for selectively separating indium according to claim 3 , wherein the method for synthesizing the solution A is: dissolving indium sulfate in dimethyl sulfoxide, adding vinyl The mixed solution of phosphoric acid and allyl mercaptan is stirred and reacted for 2 hours to obtain solution A, wherein the mass ratio between indium sulfate and dimethyl sulfoxide is 0.1% to 20%, vinyl phosphoric acid, allyl mercaptan They can be mixed in any proportion, the mass ratio of the mixed solution and indium sulfate is 0.1% to 0.4%, and the reaction temperature of the system is 10°C to 70°C. 7.根据权利要求3所述一种选择性分离铟的吸附材料的制备方法，其特征在于，所述聚合物B的合成方法为：将步骤1)所得SG-COOH与步骤2)所得溶液A混合，再加入二甲基丙烯酸乙二醇酯和偶氮二异丁腈，在无氧条件下，在20～70℃温度条件下发生聚合反应，得到聚合物B。7. The method for preparing an adsorbent material for selectively separating indium according to claim 3, wherein the method for synthesizing the polymer B is: combining the SG-COOH obtained in step 1) with the solution A obtained in step 2). Mixing, then adding ethylene glycol dimethacrylate and azobisisobutyronitrile, and under anaerobic conditions, a polymerization reaction occurs at a temperature of 20-70° C. to obtain polymer B. 8.根据权利要求3所述一种选择性分离铟的吸附材料的制备方法，其特征在于，步骤4)所述酸洗使用酸为硫酸、盐酸或硝酸的一种或几种。8 . The method for preparing an adsorbent material for selectively separating indium according to claim 3 , wherein the acid used in the pickling in step 4) is one or more of sulfuric acid, hydrochloric acid or nitric acid. 9 .
CN201810562152.9A 2018-06-04 2018-06-04 Adsorbent material for selective separation of indium and preparation method thereof Active CN108607523B (en)

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