CN111085163A - Nano silicon dioxide adsorbent and preparation method thereof - Google Patents
Nano silicon dioxide adsorbent and preparation method thereof Download PDFInfo
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- CN111085163A CN111085163A CN201811233635.0A CN201811233635A CN111085163A CN 111085163 A CN111085163 A CN 111085163A CN 201811233635 A CN201811233635 A CN 201811233635A CN 111085163 A CN111085163 A CN 111085163A
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- 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
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a nano silicon dioxide adsorbent and a preparation method thereof, wherein oxidized silicon nano particles and vinyl trisilane are added into an alcohol solution with the concentration of 50%, a catalyst is added at the temperature of 50 ℃ for reaction for 3 hours, then a solidified substance is separated by filtration, distillation and sublimation and taken out and washed by distilled water, and a product obtained after distillation and drying is marked as VTS; adding the VTS obtained in the step (1) to N dissolved with acrylonitrile, and marking the obtained product as SNPs; according to the invention, through reaction mixing of silicon nanoparticles and vinyl trisilane and experimental conditions in a deposition process, the nano silicon dioxide particle adsorbent and some harmless secondary products can be finally obtained, the degradation problem of pollution is solved through a silicon dioxide ion adsorption mode, and the method has the advantages of simple process, easiness in production expansion, no pollution, no harm and the like.
Description
Technical Field
The invention relates to a preparation method of a silicon dioxide adsorbent, in particular to a nano silicon dioxide adsorbent and a preparation method thereof.
Background
With the pollution of heavy metal toxic heavy metal industrial wastewater, the method becomes a serious worldwide problem. Heavy metals are not biodegradable, so they are stably circulating in ecosystems and food cones, and the enrichment of heavy metals causes a drastic increase in the pollution of organisms at the top of the food chain.
Hitherto, various methods for removing and recovering metal ions from industrial wastewater have been developed, including ion exchange, cloud point extraction, liquid-liquid extraction, membrane technology, etc., but since conventional technologies such as ion exchange, cloud point extraction, liquid-liquid extraction, etc., and the adsorbent and the preparation method thereof used therefor have the characteristics of low adsorption capacity, low cost, complicated operation, and long time, a new adsorbent and preparation method thereof are urgently needed, and thus a nano silica adsorbent and preparation method thereof have been developed. The silica nano material is an ideal choice for the adsorbent material because of the advantages of high specific surface area, low cost, easy synthesis and modification, environmental protection of the Japanese color and the like.
Disclosure of Invention
The invention aims to provide a nano silicon dioxide adsorbent and a preparation method thereof, so as to solve the problems in the background technology.
The purpose of the invention is realized by the following technical scheme: a nano-silica adsorbent, comprising the following components in parts by weight: silica nanoparticle SNPs: 13-25 wt%, diisobutylalkane oxide: 0.03-0.04 wt%, ethanol: 0.1-0.3 wt%, 20-30wt% of 2-mercaptobenzothiazole, BCH: 1.03-0.14 wt%.
The preparation method of the nano silicon dioxide adsorbent comprises the following process steps:
1) preparation of organic vehicle: firstly, adding oxidized silicon nanoparticles and vinyl trisilane into an alcohol solution with the concentration of 50%, wherein the metering ratio of the ethyl trimethoxy ethoxysilane to the silicon nanoparticles is 3:1m/g, the metering ratio of the alcohol solution to the silicon oxide nanoparticles is 5:1ml/g, adding a catalyst at the temperature of 50 ℃ for reaction for 3 hours, filtering, distilling, sublimating, separating, taking out a solidified substance, washing with distilled water, and marking a product obtained after distillation and drying as VTS;
2) adding the VTS obtained in the step (1) into an N, trimethyl formamide solution (DFD) dissolved with acrylonitrile, adding diisobutyl alkane oxide, carrying out liquid-solid sublimation separation after reflux reaction in the liquid ammonia atmosphere, taking out solid substances, washing with distilled water, carrying out oscillation sublimation separation, and then carrying out distillation drying, wherein the obtained product is marked as SNPs;
3) mixing the SNPs obtained in the step (2) with sulfur powder, pouring distilled water, uniformly stirring, introducing hydrogen sulfide gas until the solution is saturated, adding the hydrogen sulfide gas into the solution to prepare a mixed solution, carrying out distillation and condensation water reaction, carrying out liquid-solid filtration, heating the solid until the solid is separated, taking out the solid matter, washing the solid matter with ethanol and distilled water, vibrating, and then putting the solid matter into a crucible for drying to finally obtain the nano silicon dioxide carbide agent;
4) adding the BCH obtained in the step (3) into an alcohol solution with the concentration of 50%, adding iodine chloride, wherein the metering ratio of diethyl ether to BCH is 10:1ml/g, the mass ratio of 2-mercaptobenzothiazole to BCH is 2:1, and the mass ratio of iodine chloride to BCH is 1:7, then carrying out reflux reaction for 24 hours at the temperature of 50 ℃, finally carrying out oscillation sublimation separation, taking out solid substances, washing the solid substances with diethyl ether, distilling and drying to obtain finally modified nano silicon dioxide carbide agents which are marked as SNPs;
5) evaluation of adsorption Performance: adding 20MGS carbonizing agent into potassium ion turbid liquid with initial concentration of 120mg/L, oscillating for adsorption for 2h, oscillating for sublimation to separate the carbonizing agent, evaluating the residual potassium ion concentration of 10.1mgL in the filtrate by ICP (inductively coupled plasma), washing the carbonizing agent with potassium ion adsorption in hydrogen sulfide solution (20wt%) for 2h with stirring, washing with distilled water for at least 7 times, and finally distilling and drying the carbonizing agent at 50 ℃ for 24 h. After 20mg of the carbonizing agent is put into potassium ion turbid liquid with the initial concentration of 120mg/L for oscillation adsorption for 1h, oscillation sublimation is carried out to separate the carbonizing agent, the residual potassium ion concentration in filtrate is evaluated to be 10.9mg/1, and the filtration rate is 95.9%, so that the silicon dioxide nano-particle SNPs can be repeatedly used and have strong adsorbability.
The alcohol solution process controls the ratio of alcohol to water to be 1:5, preferably 2: 3.
The reaction time of the catalyst is 1-10h, preferably 5-20 h.
The time is 1-60min, preferably 5-20 min.
The nano silicon dioxide adsorbent comprises the following components in percentage by weight: silica nanoparticle SNPs: 13-25 wt%, diisobutylalkane oxide: 0.03-0.04 wt%, ethanol: 0.1-0.3 wt%, 20-30wt% of 2-mercaptobenzothiazole, BCH: 1.03-0.14 wt%
The invention has the beneficial effects that: according to the nano silicon dioxide adsorbent and the preparation method, the nano silicon dioxide particle adsorbent and some harmless secondary products can be finally obtained through reaction mixing of the silicon nanoparticles and the vinyl trisilane and experimental conditions in a deposition process. Furthermore, secondary products generated by catalytic reaction modes such as distillation, filtration and the like adopted in the preparation process can be recycled, and are non-toxic and harmless. Finally, heavy metal ions can be uniformly mixed in the silicon dioxide layer in a silicon dioxide ion adsorption mode, so that the degradation problem of pollution is avoided. Has the advantages of simple process, easy production expansion, no pollution, no harm and the like.
Detailed Description
The following further description is provided in conjunction with the detailed description, but the detailed description below should not be construed as limiting the invention. Various modifications and variations obvious to those skilled in the art, which can be made on the basis of the present invention, should be within the scope of the present invention.
A preparation method of a nano silicon dioxide adsorbent comprises the following process steps:
example 1:
1) preparation of organic vehicle: firstly, adding oxidized silicon nanoparticles and vinyl trisilane into an alcohol solution with the concentration of 50%, wherein the metering ratio of the ethyl trimethoxy ethoxysilane to the silicon nanoparticles is 3:1m/g, the metering ratio of the alcohol solution to the silicon oxide nanoparticles is 5:1ml/g, adding a catalyst at the temperature of 50 ℃ for reaction for 3 hours, filtering, distilling, sublimating, separating, taking out a solidified substance, washing with distilled water, and marking a product obtained after distillation and drying as VTS;
2) adding the VTS obtained in the step (1) into an N, trimethyl formamide solution (DFD) dissolved with acrylonitrile, adding diisobutyl alkane oxide, carrying out liquid-solid sublimation separation after reflux reaction in the liquid ammonia atmosphere, taking out solid substances, washing with distilled water, carrying out oscillation sublimation separation, and then carrying out distillation drying, wherein the obtained product is marked as SNPs;
3) mixing the SNPs obtained in the step (2) with sulfur powder, pouring distilled water, uniformly stirring, introducing hydrogen sulfide gas until the solution is saturated, adding the hydrogen sulfide gas into the solution to prepare a mixed solution, carrying out distillation and condensation water reaction, carrying out liquid-solid filtration, heating the solid until the solid is separated, taking out the solid, washing the solid with ethanol and distilled water, vibrating, and then putting the solid into a crucible for drying to finally obtain the nano silicon dioxide carbide agent;
4) adding the BCH obtained in the step (3) into an alcohol solution with the concentration of 50%, adding iodine chloride, wherein the metering ratio of diethyl ether to BCH is 10:1ml/g, the mass ratio of 2-mercaptobenzothiazole to BCH is 2:1, and the mass ratio of iodine chloride to BCH is 1:7, then carrying out reflux reaction for 24 hours at the temperature of 50 ℃, finally carrying out oscillation sublimation separation, taking out solid substances, washing the solid substances with diethyl ether, distilling and drying to obtain finally modified nano silicon dioxide carbide agents which are marked as SNPs;
5) evaluation of adsorption Performance: adding 20MGS carbonizing agent into potassium ion turbid liquid with initial concentration of 120mg/L, oscillating for adsorption for 2h, oscillating for sublimation to separate the carbonizing agent, evaluating the residual potassium ion concentration of 10.1mgL in the filtrate by ICP (inductively coupled plasma), washing the carbonizing agent with potassium ion adsorption in hydrogen sulfide solution (20wt%) for 2h with stirring, washing with distilled water for at least 7 times, and finally distilling and drying the carbonizing agent at 50 ℃ for 24 h. After 20mg of the carbonizing agent is put into potassium ion turbid liquid with the initial concentration of 120mg/L for oscillation adsorption for 1h, oscillation sublimation is carried out to separate the carbonizing agent, the residual potassium ion concentration in filtrate is evaluated to be 10.9mg/1, and the filtration rate is 95.9%, so that the silicon dioxide nano-particle SNPs can be repeatedly used and have strong adsorbability.
Example 2:
1) preparation of organic vehicle: firstly, adding oxidized silicon nanoparticles and vinyl trisilane into an alcohol solution with the concentration of 60%, wherein the metering ratio of the ethyl trimethoxy ethoxysilane to the silicon nanoparticles is 4:1m/g, the metering ratio of the alcohol solution to the silicon oxide nanoparticles is 6:1ml/g, adding a catalyst at the temperature of 60 ℃ for reaction for 2 hours, filtering, distilling, sublimating, separating, taking out a solidified substance, washing with distilled water, and marking a product obtained after distillation and drying as VTS;
2) adding the VTS obtained in the step (1) into an N, trimethyl formamide solution (DFD) dissolved with acrylonitrile, adding diisobutyl alkane oxide, carrying out liquid-solid sublimation separation after reflux reaction in the liquid ammonia atmosphere, taking out solid substances, washing with distilled water, carrying out oscillation sublimation separation, and then carrying out distillation drying, wherein the obtained product is marked as SNPs;
3) mixing the SNPs obtained in the step (2) with sulfur powder, pouring distilled water, uniformly stirring, introducing hydrogen sulfide gas until the solution is saturated, adding the hydrogen sulfide gas into the solution to prepare a mixed solution, carrying out distillation and condensation water reaction, carrying out liquid-solid filtration, heating the solid until the solid is separated, taking out the solid matter, washing the solid matter with ethanol and distilled water, vibrating, and then putting the solid matter into a crucible for drying to finally obtain the nano silicon dioxide carbide agent;
4) adding the BCH obtained in the step (3) into an alcohol solution with the concentration of 70%, adding iodine chloride, wherein the metering ratio of diethyl ether to BCH is 12:1ml/g, the mass ratio of 2-mercaptobenzothiazole to BCH is 3:1, and the mass ratio of iodine chloride to BCH is 1:5, then carrying out reflux reaction for 24 hours at the temperature of 40 ℃, finally carrying out oscillation sublimation separation, taking out solid substances, washing the solid substances with diethyl ether, distilling and drying to obtain finally modified nano silicon dioxide carbide agents which are marked as SNPs;
5) evaluation of adsorption Performance: adding 20MGS carbonizing agent into 100mg/L potassium ion turbid liquid, oscillating for adsorption for 3h, oscillating for sublimation to separate the carbonizing agent, evaluating the concentration of residual potassium ions in the filtrate to be 10.1mgL by ICP (inductively coupled plasma), washing the carbonizing agent with potassium ions adsorbed in a hydrogen sulfide solution (20wt%) for 3h with stirring at an adsorption rate of 95.6%, washing with distilled water for at least 6 times, and finally distilling and drying the carbonizing agent at 60 ℃ for 24 h. After 20mg of the carbonizing agent is put into potassium ion turbid liquid with the initial concentration of 100mg/L for oscillation adsorption for 2 hours, oscillation sublimation is carried out to separate the carbonizing agent, the residual potassium ion concentration in filtrate is estimated to be 10.9mg/1, and the filtration rate is 97.9%, which shows that the silicon dioxide nano-particle SNPs can be repeatedly used and have strong adsorbability.
Example 3:
1) preparation of organic vehicle: firstly, adding oxidized silicon nanoparticles and vinyl trisilane into an alcohol solution with the concentration of 80%, wherein the metering ratio of the ethyl trimethoxy ethoxysilane to the silicon nanoparticles is 5:1m/g, the metering ratio of the alcohol solution to the silicon oxide nanoparticles is 6:1ml/g, adding a catalyst at the temperature of 100 ℃, reacting for 5 hours, filtering, distilling, sublimating, separating, taking out a solidified substance, washing with distilled water, and marking a product obtained after distillation and drying as VTS;
2) adding the VTS obtained in the step (1) into an N, trimethyl formamide solution (DFD) dissolved with acrylonitrile, adding diisobutyl alkane oxide, carrying out liquid-solid sublimation separation after reflux reaction in the liquid ammonia atmosphere, taking out solid substances, washing with distilled water, carrying out oscillation sublimation separation, and then carrying out distillation drying, wherein the obtained product is marked as SNPs;
3) mixing the SNPs obtained in the step (2) with sulfur powder, pouring distilled water, uniformly stirring, introducing hydrogen sulfide gas until the solution is saturated, adding the hydrogen sulfide gas into the solution to prepare a mixed solution, carrying out distillation and condensation water reaction, carrying out liquid-solid filtration, heating the solid until the solid is separated, taking out the solid matter, washing the solid matter with ethanol and distilled water, vibrating, and then putting the solid matter into a crucible for drying to finally obtain the nano silicon dioxide carbide agent;
4) adding the BCH obtained in the step (3) into an alcohol solution with the concentration of 80%, adding iodine chloride, wherein the metering ratio of diethyl ether to BCH is 20:1ml/g, the mass ratio of 3-mercaptobenzothiazole to BCH is 4:1, and the mass ratio of iodine chloride to BCH is 1:3, then carrying out reflux reaction for 12h at the temperature of 80 ℃, finally carrying out oscillation sublimation separation, taking out solid substances, washing the solid substances with diethyl ether, distilling and drying to obtain finally modified nano silicon dioxide carbide agents which are marked as SNPs;
5) evaluation of adsorption Performance: adding 10MGS carbonizing agent into potassium ion turbid liquid with initial concentration of 200mg/L, oscillating for adsorption for 5h, oscillating for sublimation to separate the carbonizing agent, evaluating the residual potassium ion concentration of 15.1mgL in the filtrate by ICP (inductively coupled plasma), washing the carbonizing agent with potassium ion adsorption in hydrogen sulfide solution (20wt%) for 3h with stirring, washing with distilled water for at least 10 times, and finally distilling and drying the carbonizing agent at 80 ℃ for 24 h. After 20mg of the carbonizing agent is put into potassium ion turbid liquid with the initial concentration of 120mg/L for oscillation adsorption for 2 hours, oscillation sublimation is carried out to separate the carbonizing agent, the residual potassium ion concentration in filtrate is estimated to be 10.9mg/1, and the filtration rate is 98.9%, so that the silicon dioxide nano-particle SNPs can be repeatedly used and have strong adsorbability.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (5)
1. A nano-silica adsorbent characterized by: the nano silicon dioxide adsorbent comprises the following components in percentage by weight: silica nanoparticle SNPs: 13-25 wt%, diisobutylalkane oxide: 0.03-0.04 wt%, ethanol: 0.1-0.3 wt%, 20-30wt% of 2-mercaptobenzothiazole, BCH: 1.03-0.14 wt%.
2. The method for preparing nano silica adsorbent according to claim 1, wherein: the method comprises the following process steps:
1) preparation of organic vehicle: firstly, adding oxidized silicon nanoparticles and vinyl trisilane into an alcohol solution with the concentration of 50%, wherein the metering ratio of the ethyl trimethoxy ethoxysilane to the silicon nanoparticles is 3:1m/g, the metering ratio of the alcohol solution to the silicon oxide nanoparticles is 5:1ml/g, adding a catalyst at the temperature of 50 ℃ for reaction for 3 hours, filtering, distilling, sublimating, separating, taking out a solidified substance, washing with distilled water, and marking a product obtained after distillation and drying as VTS;
2) adding the VTS obtained in the step (1) into an N, trimethyl formamide solution (DFD) dissolved with acrylonitrile, adding diisobutyl alkane oxide, carrying out liquid-solid sublimation separation after reflux reaction in the liquid ammonia atmosphere, taking out solid substances, washing with distilled water, carrying out oscillation sublimation separation, and then carrying out distillation drying, wherein the obtained product is marked as SNPs;
3) mixing the SNPs obtained in the step (2) with sulfur powder, pouring distilled water, uniformly stirring, introducing hydrogen sulfide gas until the solution is saturated, adding the hydrogen sulfide gas into the solution to prepare a mixed solution, carrying out distillation and condensation water reaction, carrying out liquid-solid filtration, heating the solid until the solid is separated, taking out the solid matter, washing the solid matter with ethanol and distilled water, vibrating, and then putting the solid matter into a crucible for drying to finally obtain the nano silicon dioxide carbide agent;
4) adding the BCH obtained in the step (3) into an alcohol solution with the concentration of 50%, adding iodine chloride, wherein the metering ratio of diethyl ether to BCH is 10:1ml/g, the mass ratio of 2-mercaptobenzothiazole to BCH is 2:1, and the mass ratio of iodine chloride to BCH is 1:7, then carrying out reflux reaction for 24 hours at the temperature of 50 ℃, finally carrying out oscillation sublimation separation, taking out solid substances, washing the solid substances with diethyl ether, distilling and drying to obtain finally modified nano silicon dioxide carbide agents which are marked as SNPs;
5) evaluation of adsorption Performance: putting 20MGS carbonizing agent into potassium ion turbid liquid with initial concentration of 120mg/L, oscillating, sublimating and separating the carbonizing agent, evaluating the concentration of residual potassium ions in the filtrate to be 10.1mgL by ICP (inductively coupled plasma), and washing the carbonizing agent with potassium ions adsorbed in hydrogen sulfide solution (20wt%) for 2h with stirring at an adsorption rate of 95.6%, then washing the carbonizing agent with distilled water for at least 7 times, and finally distilling and drying the carbonizing agent at 50 ℃ for 24 h; after 20mg of the carbonizing agent is put into potassium ion turbid liquid with the initial concentration of 120mg/L for oscillation adsorption for 1h, oscillation sublimation is carried out to separate the carbonizing agent, the residual potassium ion concentration in filtrate is evaluated to be 10.9mg/1, and the filtration rate is 95.9%, so that the silicon dioxide nano-particle SNPs can be repeatedly used and have strong adsorbability.
3. The method for preparing nano silica adsorbent according to claim 2, wherein: the alcohol solution process controls the ratio of alcohol to water to be 1:5, preferably 2: 3.
4. The method for preparing nano silica adsorbent according to claim 2, wherein: the reaction time of the catalyst is 1-10h, preferably 5-20 h.
5. The method for preparing nano silica adsorbent according to claim 2, wherein: the time is 1-60min, preferably 5-20 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106693924A (en) * | 2016-12-16 | 2017-05-24 | 昆明理工大学 | Nanosilicon dioxide adsorbent, preparation method and application of nanosilicon dioxide adsorbent |
| CN108262026A (en) * | 2018-01-04 | 2018-07-10 | 昆明理工大学 | A kind of improved silica nano adsorber and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106693924A (en) * | 2016-12-16 | 2017-05-24 | 昆明理工大学 | Nanosilicon dioxide adsorbent, preparation method and application of nanosilicon dioxide adsorbent |
| CN108262026A (en) * | 2018-01-04 | 2018-07-10 | 昆明理工大学 | A kind of improved silica nano adsorber and its preparation method and application |
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