CN109603736B - Preparation method and application of modified silica gel material - Google Patents

Preparation method and application of modified silica gel material Download PDF

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CN109603736B
CN109603736B CN201811479657.5A CN201811479657A CN109603736B CN 109603736 B CN109603736 B CN 109603736B CN 201811479657 A CN201811479657 A CN 201811479657A CN 109603736 B CN109603736 B CN 109603736B
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silica gel
modified
gel material
modified silica
drying
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CN109603736A (en
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字富庭
陈树梁
胡显智
陈云龙
刘洋
杨朋
胡德琼
何易
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Kunming University of Science and Technology
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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
    • B01J20/10—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
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • 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
    • C22B11/00—Obtaining noble metals
    • 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
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    • 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

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Abstract

The invention discloses a preparation method and application of a modified silica gel material, and belongs to the technical field of silica gel. The method overcomes the defects of organic solvent and long time consumption in the common silica gel modification method, shortens the modification time while ensuring the modification effect, and avoids the use of the organic solvent; according to the method, silica gel is used as a substrate, and a modifier is conveyed to the surface of the silica gel in a gas form under a certain condition, so that the surface property of the silica gel is changed, and the modified silica gel material is obtained. In addition, the silica gel material modified by the sulfhydryl-containing silane coupling agent prepared by the invention is p [ Au (S)2O3)2]3‑The complex ions have adsorption effect and can effectively recover gold in the thiosulfate gold leaching solution. The method of the invention does not use organic solvent, effectively avoids the environmental problem caused by using organic solvent, shortens the modification time, reduces the time cost and the expense in practical application, and has wide application prospect.

Description

Preparation method and application of modified silica gel material
Technical Field
The invention relates to a preparation method and application of a modified silica gel material, and belongs to the fields of hydrometallurgy and metal recovery.
Background
As a rare and precious metal which symbolizes the wealth of human beings, gold is often associated with minerals such as quartz, pyrite, arsenopyrite and the like in nature, and has stable property. When gold is extracted by a cyanidation method, the use of cyanide is influenced because the cyanide has extremely high toxicity. Therefore, the thiosulfate gold extraction technology is attracting attention as a nontoxic gold extraction technology which can possibly replace a cyanidation method. However, in the thiosulfate gold extraction technology, gold recovery from the gold leaching solution is difficult, and the development of the technology is limited. When the carbon pulp method (CIL) or the carbon leaching method (CIP) in the cyanidation method extraction process is applied to the thiosulfate method for recovering gold, the gold can hardly be recovered by the activated carbon or the effect is not obvious. Therefore, a suitable safe and nontoxic adsorbing material needs to be found for recovering gold from thiosulfate gold leaching solution.
Silica gel is used as a non-toxic amorphous substance with rich void structure, is commonly used as an adsorption material, and is widely used in the aspects of metal ion separation, solid phase extraction, catalysis, medicine and the like. The adsorption characteristic of silica gel mainly comes from silicon hydroxyl groups which are rich on the surface of the silica gel, but the silica gel has poor adsorption selectivity and adsorption capacity, and can react with alkali, so that the application of the silica gel is limited. However, the silicon hydroxyl functional group on the surface of the silica gel can introduce other functional groups by a modification or surface modification method, so that the selective adsorption of the silica gel can be effectively improved. In patent cn201010191116.x, a silica gel modified adsorption material modified by bifunctional groups with high content is prepared. In patent CN201510901916.9, 3-aminopropyl trisiloxysilane is used as a modifier to prepare a modified silica gel adsorption material for treating anionic dye wastewater. Therefore, it is feasible to recover metal ions after surface modification by using silica gel as a matrix.
Disclosure of Invention
The invention aims to provide a preparation method of a modified silica gel material, which takes a silane coupling agent as a silica gel modifier to carry out surface modification on silica gel under the condition of not using organic solution, so that a target functional group is grafted on the surface of the silica gel to prepare the modified silica gel material; in the whole modification process, the used modifier can be recycled, and an organic solvent is not used, so that the method is environment-friendly and has no influence; the process is simple and easy to operate; the prepared modified silica gel material has wide application prospect in the fields of metal ion separation, adsorption recovery and the like, and specifically comprises the following steps:
(1) washing a proper amount of silica gel with deionized water, removing impurities of the silica gel, filtering and drying;
(2) putting the silica gel obtained in the step (1) into a hydrochloric acid solution (6 mol/L) according to a ratio of 20-150 g/L, soaking for 6-24 h, filtering, washing to be neutral, and drying;
(3) sequentially adding a modifier and a catalyst into a high-pressure reaction kettle, then placing the silica gel obtained in the step (2) into a crucible, then placing the crucible into the reaction kettle, sealing, placing the reaction kettle at 120-260 ℃ for reacting for 0.5-8 h, taking out and naturally cooling; the silica gel is not directly contacted with a modifier and a catalyst, wherein the modifier is a silane coupling agent;
(4) and (4) drying the modified silica gel obtained in the step (3) in vacuum to obtain the modified silica gel material.
Preferably, the drying condition in the step (1) is drying at 60-180 ℃ for 12-24 h.
Preferably, the liquid-solid ratio of the silane coupling agent to the silica gel is 0.1-5.
Preferably, the catalyst is one of triethylamine, ethylenediamine and ammonia water.
Preferably, the modifier of the invention can be common organosilane coupling agent containing sulfydryl, amino, chlorine and the like, and has the structure: SiH3-m(OCnH2n+1)mCH2CH2CH2X, wherein m is 1,2,3, n may be 1,2, X is-SH, -NH2，-Cl。
The modified silica gel material containing sulfydryl prepared by the method can be directly used for adsorbing and recovering dithio-sulfuric acid alloy (I) complex ions from thiosulfate gold leaching solution so as to realize the purpose of absorbing and recovering Au (S) in the thiosulfate gold leaching solution2O3)2]3-The purpose of complex ion separation and enrichment.
The invention has the beneficial effects that:
(1) according to the method, the surface property of the silica gel is changed by chemically modifying the surface of the silica gel, the modified silica gel is chemically bonded, the modified silica gel is stable in property, the modified silica gel is wide in pH range suitable for an adsorption solution, and the method has a wide application prospect in the fields of metal ion separation, adsorption recovery and the like.
(2) The silica gel material modified by the mercapto silane coupling agent prepared by the invention is p [ Au (S)2O3)2]3-The complex ions have an adsorption effect and can effectively recover gold in the thiosulfate gold leaching solution; the method is a chemical modification method, and the modified silica gel has stable property; the pH range of the adsorption solution is wide, and the adsorption effect in the weak alkaline solution is good.
(3) The method has the advantages of simple process, low modification cost and high gold recovery rate, and the used modifier can be recycled in the whole modification process, and the method does not use an organic solvent and has no influence on the environment.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the examples.
Example 1
A preparation method of a modified silica gel material specifically comprises the following steps:
(1) weighing 2g of granular silica gel, washing with deionized water, removing impurities of the silica gel, filtering and drying.
(2) Adding the silica gel obtained in the step (1) into a hydrochloric acid solution with the concentration of 6mol/L according to the proportion of 20g/L, soaking for 24 hours, filtering, washing to be neutral, and drying for 24 hours at the temperature of 60 ℃.
(3) And (3-mercaptopropyl) trimethoxysilane of 5ml and triethylamine of 0.1ml are sequentially added into the lining of the high-pressure reaction kettle, then the silica gel obtained in the step (2) is placed in a crucible, the crucible is placed in the lining of the reaction kettle, and the silica gel and the silane coupling agent are not directly contacted and sealed.
(4) And (4) placing the reaction kettle in the step (3) at 260 ℃ for reaction for 4h, taking out, and naturally cooling.
(5) And (5) placing the silica gel obtained in the step (4) in a vacuum oven, sealing and storing for 2h at the temperature of 80 ℃, and taking out to obtain the mercaptopropyl modified silica gel material.
0.5g of the silica gel obtained in step (5) was weighed into 100mL of 10. mu.g/mL of Au (S) at pH 92O3)2 3-Adsorbing in solution (adsorption solution for short) for 12 hr, and filtering; the adsorption rate was found to be 35% and the loading was found to be 0.7 kg/t.
Example 2
A preparation method of a modified silica gel material specifically comprises the following steps:
(1) weighing 2g of column chromatography silica gel, washing with deionized water, removing impurities of the silica gel, filtering and drying.
(2) Adding the silica gel obtained in the step (1) into a hydrochloric acid solution with the concentration of 6mol/L according to the proportion of 90g/L, soaking for 18h, filtering, washing to be neutral, and drying for 18h at 120 ℃.
(3) And (3-mercaptopropyl) triethoxysilane 0.2ml and ethylenediamine 0.1ml are sequentially added into the lining of the high-pressure reaction kettle, then the silica gel obtained in the step (2) is placed in a crucible, the crucible is placed in the lining of the reaction kettle, and the silica gel and the silane coupling agent are not directly contacted and sealed.
(4) And (4) placing the reaction kettle in the step (3) at 120 ℃ for reacting for 8h, taking out, and naturally cooling.
(5) And (5) placing the silica gel obtained in the step (4) in a vacuum oven, sealing and storing for 2h at the temperature of 80 ℃, and taking out to obtain the mercaptopropyl modified silica gel material.
0.5g of the silica gel obtained in step (5) was weighed into 100mL of 10. mu.g/mL of Au (S) having a pH of 102O3)2 3-Adsorbing in solution (adsorption solution for short) for 48 hr, and filtering; the adsorption rate was found to be 65% with a loading of 1.3 kg/t.
Example 3
A preparation method of a modified silica gel material specifically comprises the following steps:
(1) weighing 2g of powdered silica gel, washing with deionized water, removing impurities of the silica gel, filtering and drying.
(2) Adding the silica gel obtained in the step (1) into a hydrochloric acid solution with the concentration of 6mol/L according to the proportion of 150g/L, soaking for 6h, filtering, washing to be neutral, and drying for 12h at 180 ℃.
(3) And (3-mercaptopropyl) diethoxysilane 5ml and ammonia water 0.1ml are sequentially added into the lining of the high-pressure reaction kettle, then the silica gel obtained in the step (2) is placed into a crucible, the crucible is placed into the lining of the reaction kettle, and the silica gel and the silane coupling agent are not directly contacted and sealed.
(4) And (4) placing the reaction kettle in the step (3) at 200 ℃ for reaction for 0.5h, taking out, and naturally cooling.
(5) And (5) placing the silica gel obtained in the step (4) in a vacuum oven, sealing and storing for 2h at the temperature of 80 ℃, and taking out to obtain the mercaptopropyl modified silica gel material.
Taking an ore leach solution containing about 20.69 g/t gold as an example, Au (S) is contained in the ore leach solution2O3)2 3-Has a concentration of 3.3mg/L, Cu2+Concentration of 5mmol/L, NH3/NH4 +The concentration is 0.5 mol/L, and the pH is 10; a500 mL portion of this leachate was prepared, and 1g of the silica gel of step (3) was added to the leachate, adsorbed for 12h and filtered. The adsorption rate was 29%, and the loading amount of gold on silica gel was 0.479 kg/t.
Example 4
A preparation method of a modified silica gel material specifically comprises the following steps:
(1) weighing 2g of column chromatography silica gel, washing with deionized water, removing impurities of the silica gel, filtering and drying.
(2) Adding the silica gel obtained in the step (1) into a hydrochloric acid solution with the concentration of 6mol/L according to the proportion of 100g/L, soaking for 12h, filtering, washing to be neutral, and drying for 12h at 120 ℃.
(3) And (3-mercaptopropyl) trimethoxysilane of 5ml and triethylamine of 0.1ml are sequentially added into the lining of the high-pressure reaction kettle, then the silica gel obtained in the step (2) is placed in a crucible, the crucible is placed in the lining of the reaction kettle, and the silica gel and the silane coupling agent are not directly contacted and sealed.
(4) And (4) placing the reaction kettle in the step (3) at 220 ℃ for reaction for 4h, taking out, and naturally cooling.
(5) And (5) placing the silica gel obtained in the step (4) in a vacuum oven, sealing and storing for 2h at the temperature of 80 ℃, and taking out to obtain the mercaptopropyl modified silica gel material.
Taking an ore leach solution containing about 20.69 g/t gold as an example, Au (S) is contained in the ore leach solution2O3)2 3-Has a concentration of 3.3mg/L，Cu2+Concentration of 5mmol/L, NH3/NH4 +The concentration is 0.5 mol/L, and the pH is 10; a500 mL portion of this leachate was prepared, and 1g of the silica gel of step (3) was added to the leachate, adsorbed for 12h and filtered. The adsorption rate was 56%, and the loading of gold on silica gel was 0.924 kg/t.
Example 5
A preparation method of a modified silica gel material specifically comprises the following steps:
(1) weighing 2g of column chromatography silica gel, washing with deionized water to remove impurities of the silica gel, filtering and drying.
(2) Adding the silica gel obtained in the step (1) into a hydrochloric acid solution with the concentration of 6mol/L according to the proportion of 100g/L, soaking for 24 hours, filtering, washing to be neutral, and drying for 24 hours at 120 ℃.
(3) And (3-chloropropyl) trimethoxy silane 5ml and triethylamine 0.1ml are sequentially added into the lining of the high-pressure reaction kettle, then the silica gel obtained in the step (2) is placed into a crucible, the crucible is placed into the lining of the reaction kettle, and the silica gel and the silane coupling agent are not directly contacted and sealed.
(4) And (4) placing the reaction kettle in the step (3) at 260 ℃ for reaction for 0.5h, taking out, and naturally cooling.
(5) And (5) placing the silica gel obtained in the step (4) in a vacuum oven, sealing and storing for 2h at the temperature of 80 ℃, and taking out to obtain the chloropropyl modified silica gel material. The content of chlorine element is 1.12% by energy spectrum analysis. The prepared chloropropyl modified silica gel can be used for determining trace manganese, cobalt and nickel in a water sample by flame atomic absorption spectrometry.
Example 6
A preparation method of a modified silica gel material specifically comprises the following steps:
(1) weighing 2g of column chromatography silica gel, washing with deionized water to remove impurities of the silica gel, filtering and drying.
(2) Adding the silica gel obtained in the step (1) into a hydrochloric acid solution with the concentration of 6mol/L according to the proportion of 100g/L, soaking for 12h, filtering, washing to be neutral, and drying for 12h at 120 ℃.
(3) And (3-aminopropyl) trimethoxy silane 5ml and ammonia water 0.1ml are sequentially added into the lining of the high-pressure reaction kettle, then the silica gel obtained in the step (2) is placed into a crucible, the crucible is placed into the lining of the reaction kettle, and the silica gel and the silane coupling agent are not directly contacted and sealed.
(4) And (4) placing the reaction kettle in the step (3) at 200 ℃ for reacting for 8h, taking out, and naturally cooling.
(5) And (5) placing the silica gel obtained in the step (4) in a vacuum oven, sealing and storing for 2h at the temperature of 80 ℃, and taking out to obtain the aminopropyl modified silica gel material. The content of nitrogen element is 0.94% by energy spectrum analysis. The aminopropyl modified silica gel prepared by the experiment can be used for measuring trace copper, cobalt and nickel in a water sample by flame atomic absorption spectrometry.
Example 7
A preparation method of a modified silica gel material specifically comprises the following steps:
(1) weighing 2g of column chromatography silica gel, washing with deionized water to remove impurities of the silica gel, filtering and drying.
(2) Adding the silica gel obtained in the step (1) into a hydrochloric acid solution with the concentration of 6mol/L according to the proportion of 100g/L, soaking for 12 hours, filtering, washing to be neutral, and drying for 12 hours at 120 ℃.
(3) And (3-aminopropyl) triethoxysilane 5ml and triethylamine 0.1ml are sequentially added into the lining of the high-pressure reaction kettle, then the silica gel obtained in the step (2) is placed in a crucible, the crucible is placed in the lining of the reaction kettle, and the silica gel and the silane coupling agent are not directly contacted and sealed.
(4) And (4) placing the reaction kettle in the step (3) at 160 ℃ for reaction for 3h, taking out, and naturally cooling.
(5) And (5) placing the silica gel obtained in the step (4) in a vacuum oven, sealing and storing for 2h at the temperature of 80 ℃, and taking out to obtain the aminopropyl modified silica gel material. The content of nitrogen element is 0.85% by energy spectrum analysis. The aminopropyl modified silica gel prepared by the experiment can be used for measuring trace copper, cobalt and nickel in a water sample by flame atomic absorption spectrometry.

Claims (3)

1. Method for adsorbing and recovering Au (S) from thiosulfate gold leaching solution2O3)2]3-Preparation of modified silica gel material with complex ionThe method is characterized by comprising the following steps:
(1) washing a proper amount of silica gel with deionized water, removing impurities of the silica gel, filtering and drying;
(2) putting the silica gel obtained in the step (1) into a hydrochloric acid solution according to the proportion of 20-150 g/L, soaking for 6-24 h, filtering, washing to be neutral, and drying;
(3) sequentially adding a modifier and a catalyst into a high-pressure reaction kettle, then placing the silica gel obtained in the step (2) into a crucible, then placing the crucible into the reaction kettle, sealing, placing the reaction kettle at 120-260 ℃ for reacting for 0.5-8 h, taking out and naturally cooling; the silica gel is not directly contacted with a modifier and a catalyst, wherein the modifier is a mercapto-containing silane coupling agent;
(4) vacuum drying the modified silica gel obtained in the step (3) to obtain a modified silica gel material;
the catalyst is one of triethylamine, ethylenediamine and ammonia water.
2. The method for preparing a modified silica gel material according to claim 1, wherein: the drying condition in the step (1) is drying for 12-24 h at 60-180 ℃.
3. The method for preparing a modified silica gel material according to claim 1, wherein: the concentration of the hydrochloric acid solution is 6mol/L, and the liquid-solid ratio of the mercapto-containing silane coupling agent to the silica gel is 0.1-5.
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CN113457629A (en) * 2020-03-30 2021-10-01 深圳思创环保科技有限公司 Polyamine-based composite purification material and preparation method and application thereof
CN111841492A (en) * 2020-06-19 2020-10-30 昆明理工大学 For adsorbing and recovering Au (S)2O3)2]3-Preparation method of ionic carbonaceous material
CN111889068A (en) * 2020-06-19 2020-11-06 昆明理工大学 For adsorbing and recovering Au (S)2O3)2]3-Modification method of ion-complexed active carbon
CN112642401A (en) * 2020-12-02 2021-04-13 昆明理工大学 Preparation method of composite material for extracting gold from thiosulfate
CN113546601B (en) * 2021-07-19 2022-11-11 昆明理工大学 Method for recovering Au (I) from thiosulfate solution
CN115282923B (en) * 2022-07-06 2023-04-28 东莞永成新材料有限公司 Modified silica gel material convenient to clean and preparation method thereof

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