CN105561942A - Method for preparing arsenic-removing adsorbent by using cerous nitrate modified crustacean waste - Google Patents
Method for preparing arsenic-removing adsorbent by using cerous nitrate modified crustacean waste Download PDFInfo
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- CN105561942A CN105561942A CN201610128299.8A CN201610128299A CN105561942A CN 105561942 A CN105561942 A CN 105561942A CN 201610128299 A CN201610128299 A CN 201610128299A CN 105561942 A CN105561942 A CN 105561942A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a method for preparing an arsenic-removing adsorbent by using a cerous nitrate modified crustacean waste. The method comprises the following steps of (1), putting the crustacean waste into a NaOH solution for soaking, cleaning the soaked crustacean waste, and drying the cleaned crustacean waste; (2), pulverizing the dried crustacean waste; (3), soaking the pulverized crustacean waste in a HCl solution, carrying out vacuum filtration, cleaning the crustacean waste, and drying the crustacean waste; (4), soaking the crustacean waste in a cerous nitrate solution; (5), cooling obtained mixed liquid to a room temperature, filtering the mixed liquid, drying a solid particle, and then carrying out heat treatment on the dried solid particle, cooling the solid particle subjected to the heat treatment, cleaning the cooled solid particle, and drying the cleaned solid particle, to prepare the arsenic-removing adsorbent by using the cerous nitrate modified crustacean waste. According to the method for preparing the arsenic-removing adsorbent by using the cerous nitrate modified crustacean waste, the crustacean waste and cerium salt are selected as raw materials, not only have the heat stability of an inorganic material, but also have the advantages of the polyfunctionality of an organic material; the prepared arsenic-removing adsorbent can be used for realizing the removal of arsenic in waste water and a drinking water source; when the initial concentration of the arsenic is below 20mg/L, the adsorption capacity to the arsenic can be up to 69.4mg/g; the removal efficiency of the arsenic can be up to not less than 95 percent.
Description
Technical field
The present invention relates to a kind of method being prepared arsenic-removing adsorption agent by cerium salt (cerous nitrate) modification shell-fish discarded object, belong to absorbent preparation technical field.
Background technology
At present, Heavy Metals in Waters contamination hazard has become a global problem.Wherein, arsenic has high toxicity, widespread feature, is considered to No. 1 toxin in USEPA list.Arsenic in environment is mainly derived from the weathering of occurring in nature arsenic mineral and the activity in production of the mankind, the discharge as Industrial " three Waste "s such as chemical industry, mining, metallurgy, generatings and the application containing arsenic Insecticides (tech) & Herbicides (tech).Arsenic, after water, food and the air polluted enters human body, can cause acute or slow poisoning, can cause multiple organ tissue and abnormal change functionally.Therefore how to administer arsenic pollution and receive showing great attention to of Environmental Studies person.
The method of conventional process arsenic-containing waste water mainly contains the precipitation method, absorption method, oxidizing process, ion-exchange, biochemical process etc.In these traditional dearsenicating methods, absorption method is considered to the most cost-effective method.In recent years, scientific research finds rare earth element such as lanthanum and cerium, has stronger affinity to arsenic.Main component be the commercial sorbents (READ) of cerium oxide for a process for waste water containing arsenic, and show good performance in adsorption capacity and regeneration.But its processing cost is higher, limit its application in water treatment field.
Summary of the invention
The present invention is directed to the deficiency that existing arsenic-removing adsorption agent exists, provide a kind of cerous nitrate modification shell-fish discarded object to prepare the method for arsenic-removing adsorption agent, to solve the problem utilizing merely cerium process arsenic pollution cost higher.
Cerous nitrate modification shell-fish discarded object of the present invention prepares the method for arsenic-removing adsorption agent, comprises the following steps:
(1) NaOH solution shell-fish discarded object (crab shell, shrimp shell etc.) being placed in concentration 0.5 ~ 1mol/L is soaked 2 ~ 3 hours, then repeatedly cleans to pH value 6.5 ~ 7 with clear water, dries;
(2) shell-fish discarded object to 60 ~ 80 order after drying is pulverized;
(3) the shell-fish discarded object of pulverizing is soaked in the HCl solution of mass concentration 6%, vacuum filtration, clean to water outlet pH value 6.5 ~ 7.0, dry;
(4) under bath temperature 40 ~ 60 DEG C of conditions, step (3) gained shell-fish discarded object is soaked 3 ~ 4 hours in the cerium nitrate solution of mass concentration 8% ~ 12%; The mass ratio of shell-fish discarded object particle and cerous nitrate is 2:1 ~ 4:1;
(5) step (4) gained mixed liquor is cooled to room temperature, filter, solid particle was 60 ~ 70 DEG C of dryings 20 ~ 25 hours, then heat treatment, cooling, cleans with distilled water, dry, obtained cerous nitrate modification shell-fish discarded object arsenic-removing adsorption agent.
In described step (1), the ratio of shell-fish discarded object and NaOH solution is 1g:20mL ~ 1g:25mL.
Bake out temperature in described step (1), step (3) and step (5) is 65 ~ 75 DEG C.
In described step (3), the mass ratio of shell-fish discarded object particle and hydrochloric acid solution is 1:10 ~ 1:20.
Heat treatment to refer under argon shield 100 ~ 120 DEG C of heat treatments 30 ~ 60 minutes in described step (5), in atmosphere 80 ~ 100 DEG C of heat treatment 60 ~ 90 minutes.
In described step (5), heat treatment refers to that the heat treatment temperature under argon shield is 120 DEG C, and heat treatment time is 45 minutes; Aerial heat treatment temperature is 100 DEG C, and heat treatment time is 60 minutes.
Compared with prior art, the invention has the advantages that:
(1) choose shell-fish discarded object and cerium salt is raw material, on the one hand, the utilization of shell-fish discarded object not only improves the value of shell class marine product but also decreases the environmental pollution that waste discharge causes; On the other hand, China's Ce elements aboundresources, reserves occupy first place in the world, and Ce elements Quality Research is of great importance for exploitation China superior resources.
(2) removal to arsenic in waste water and drinking water source can be realized, arsenic initial concentration is when below 20mg/L, can reach 69.4mg/g to arsenic adsorption capacity, arsenic removal efficiency can reach more than 95%, has great importance for the process of industrial wastewater and the improvement of water environment.
(3) choose shell-fish discarded object and cerium salt is raw material, have inorganic material heat endurance concurrently on the one hand, have again the polyfunctional advantage of organic material on the other hand.
Accompanying drawing explanation
Fig. 1 is the microstructure schematic diagram of crab shell particle under electron scanning Electronic Speculum of non-modified.
Fig. 2 is the microstructure schematic diagram of cerous nitrate modification crab shell arsenic-removing adsorption agent under electron scanning Electronic Speculum prepared by embodiment 1.
Fig. 3 is that the cerous nitrate modification shrimp shell arsenic-removing adsorption agent of embodiment 2 preparation is at various ph values to the adsorption capacity schematic diagram of arsenic.
Fig. 4 be embodiment 3 prepare cerous nitrate modification fresh-water turtle shell arsenic-removing adsorption agent under the different disposal time to the adsorbance schematic diagram of arsenic.
Detailed description of the invention
Embodiment 1
(1) NaOH solution 50g crab shell being placed in 1000mL concentration 1mol/L is soaked 2 hours, then repeatedly cleans to pH value 6.5 with clear water, is placed in 70 DEG C of baking ovens and dries.
(2) pulverization process is done to crab shell, cross 80 order screens.
(3) hydrochloric acid crab shell sieved being placed in mass concentration 6% soaks (mass ratio of crab shell and hydrochloric acid solution is 1:10), and vacuum filtration, cleans and dry under water outlet pH value is 6.5,70 DEG C of temperature conditions.
(4) under bath temperature 50 DEG C of conditions by crab shell in mass concentration be 8% cerium nitrate solution in soak 4 hours (mass ratio of crab shell and cerous nitrate is 3:1).
(5) above-mentioned mixed liquor is cooled to room temperature; filter; solid particle is placed in Constant Temp. Oven; temperature controls 65 DEG C of dryings after 23 hours, 110 DEG C of heat treatment 30 minutes under argon shield, in atmosphere 90 DEG C of heat treatment 75 minutes; cooling; with distilled water cleaning, be placed in 70 DEG C of baking ovens and dry, obtained cerous nitrate modification crab shell arsenic-removing adsorption agent (CC1).
Under arsenic-removing adsorption agent CC1 prepared by crab shell particle and the present embodiment of non-modified is placed in electron scanning Electronic Speculum respectively, observe before modified and the surface pore structure of modified crab shell, as depicted in figs. 1 and 2, contained in the forward and backward adsorbent of contrast modification elemental constituent.
Can find out that from Fig. 1 and Fig. 2 the crab shell particle surface through modification is uneven, in layered laminate open structure, space increase.Compared with raw material crab shell, in the CC1 of modified preparation, Ca, Mg, P element content sharply reduce, and charcoal oxygen content increases, and reason is that calcareous, magnesia, phosphorus matter has had dissolving in various degree in hydrochloric acid; In addition, in CC1, the appearance of Ce element shows its successful load Ce elements, is conducive to improving its adsorption effect to arsenate.
Embodiment 2
(1) NaOH solution 50g shrimp shell being placed in 1100mL concentration 0.8mol/L is soaked 2.5 hours, then repeatedly cleans to pH value 7 with clear water, is placed in 65 DEG C of baking ovens and dries.
(2) prawn shell does pulverization process, crosses 60 order screens.
(3) hydrochloric acid shrimp shell sieved being placed in mass concentration 6% soaks (mass ratio of shrimp shell and hydrochloric acid solution is 1:20), vacuum filtration, cleans under being 7.0,65 DEG C of temperature conditions to water outlet pH value dry.
(4) under bath temperature 40 DEG C of conditions by shrimp shell in mass concentration be 12% cerium nitrate solution in soak 3 hours (mass ratio of shrimp shell and cerous nitrate is 4:1).
(5) above-mentioned mixed liquor is cooled to room temperature; filter; solid particle is placed in Constant Temp. Oven; temperature controls 70 DEG C of dryings after 20 hours, 120 DEG C of heat treatment 45 minutes under argon shield, in atmosphere 100 DEG C of heat treatment 60 minutes; cooling; with distilled water cleaning, be placed in 65 DEG C of baking ovens and dry, obtained cerous nitrate modification shrimp shell arsenic-removing adsorption agent (CC2).
The adsorption test of cerous nitrate modification shrimp shell arsenic-removing adsorption agent (CC2) the heavy metal arsenic that the present embodiment is obtained and removal effect thereof:
(1), under room temperature, 0.2gCC2 is placed in 100mL arsenic-containing waste water (arsenic initial concentration is 2mg/L, and initial pH on wastewater is respectively 1,2,3,4,5,6,7,8,9,10,11,12); Carry out oscillating reactions to above-mentioned water sample, temperature controls at 35 ° of C, and rotating speed is 120rpm; After 12h, extract supernatant, the PTFE film crossing 0.45 μm is filtered, and measures in filtrate remain arsenic ion concentration with atomic absorption spectrophotometer.Thus calculating the clearance of CC2 to arsenic, experimental result is shown in Fig. 3.
(2), under room temperature, 0.2g shrimp shell is placed in 100mL arsenic-containing waste water (arsenic initial concentration is 2mg/L, and initial pH on wastewater is respectively 1,2,3,4,5,6,7,8,9,10,11,12); Carry out oscillating reactions to above-mentioned water sample, temperature controls at 35 ° of C, and rotating speed is 120rpm; After 12h, extract supernatant, the PTFE film crossing 0.45 μm is filtered, and measures in filtrate remain arsenic ion concentration with atomic absorption spectrophotometer.Thus calculating the clearance of shrimp shell to arsenic, experimental result is shown in Fig. 3.
As shown in Figure 3, when pH value is 6, compared with shrimp shell, the clearance of adsorbent CC2 to arsenic has the lifting of 55%, and adsorption effect is significantly improved.
Embodiment 3
(1) NaOH solution 40g fresh-water turtle shell being placed in 1000mL concentration 0.5mol/L is soaked 3 hours, then repeatedly cleans to pH value 6.8 with clear water, is placed in 75 DEG C of baking ovens and dries.
(2) pulverization process is done to fresh-water turtle shell, cross 70 order screens.
(3) hydrochloric acid fresh-water turtle shell sieved being placed in mass concentration 6% soaks (mass ratio of fresh-water turtle shell and hydrochloric acid solution is 1:15), vacuum filtration, cleans under being 6.8,75 DEG C of temperature conditions to water outlet pH value dry.
(4) under bath temperature 60 DEG C of conditions by fresh-water turtle shell in mass concentration be 10% cerium nitrate solution in soak 3.5 hours (mass ratio of fresh-water turtle shell and cerous nitrate is 2:1).
(5) above-mentioned mixed liquor is cooled to room temperature; filter; solid particle is placed in Constant Temp. Oven; temperature controls 60 DEG C of dryings after 25 hours, 100 DEG C of heat treatment 60 minutes under argon shield, in atmosphere 80 DEG C of heat treatment 90 minutes; cooling; with distilled water cleaning, be placed in 75 DEG C of baking ovens and dry, obtained cerous nitrate modification fresh-water turtle shell arsenic-removing adsorption agent (CC3).
The adsorption test of cerous nitrate modification fresh-water turtle shell arsenic-removing adsorption agent (CC3) heavy metal arsenic prepared by the present embodiment and removal effect thereof:
(1), under room temperature, 0.2g adsorbent CC3 is placed in 100mL arsenic-containing waste water (arsenic initial concentration is 2mg/L, and initial pH on wastewater value is 6.5); Carry out oscillating reactions to above-mentioned water sample, temperature controls at 35 ° of C, and rotating speed is 120rpm; After 0.25 hour, 0.5 hour, 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours, 12 hours and 14 hours, extract supernatant, the PTFE film crossing 0.45 μm is filtered, and measures in filtrate remain arsenic ion concentration with atomic absorption spectrophotometer.Thus calculating the clearance of adsorbent CC3 to arsenic, experimental result is as shown in Figure 4.
(2), under room temperature, 0.2g fresh-water turtle shell is placed in 100mL arsenic-containing waste water (arsenic initial concentration is 2mg/L, and initial pH on wastewater is respectively 6.5); Carry out oscillating reactions to above-mentioned water sample, temperature controls at 35 ° of C, and rotating speed is 120rpm; After 0.25 hour, 0.5 hour, 1 hour, 2 hours, 4 hours, 6 hours, 8 hours, 10 hours, 12 hours and 14 hours, extract supernatant, the PTFE film crossing 0.45 μm is filtered, and measures in filtrate remain arsenic ion concentration with atomic absorption spectrophotometer.Thus calculating the clearance of fresh-water turtle shell to arsenic, experimental result is shown in Fig. 4.
As shown in Figure 4, the adsorbance of fresh-water turtle shell adsorbent CC3 to arsenic increases along with the increase in reaction time, and the reaction time is after 12h, little to the adsorption effect change of arsenic.Therefore, in actual application, reaction contact time should be no less than 12 hours.In addition, under the same conditions, compared with fresh-water turtle shell, the adsorption effect of adsorbent CC3 to arsenic is significantly improved.
Claims (6)
1. cerous nitrate modification shell-fish discarded object prepares a method for arsenic-removing adsorption agent, it is characterized in that, comprises the following steps:
(1) NaOH solution shell-fish discarded object being placed in concentration 0.5 ~ 1mol/L is soaked 2 ~ 3 hours, then repeatedly cleans to pH value 6.5 ~ 7 with clear water, dries;
(2) shell-fish discarded object to 60 ~ 80 order after drying is pulverized;
(3) the shell-fish discarded object of pulverizing is soaked in the HCl solution of mass concentration 6%, vacuum filtration, clean to water outlet pH value 6.5 ~ 7.0, dry;
(4) under bath temperature 40 ~ 60 DEG C of conditions, step (3) gained shell-fish discarded object is soaked 3 ~ 4 hours in the cerium nitrate solution of mass concentration 8% ~ 12%; The mass ratio of shell-fish discarded object particle and cerous nitrate is 2:1 ~ 4:1;
(5) step (4) gained mixed liquor is cooled to room temperature, filter, solid particle was 60 ~ 70 DEG C of dryings 20 ~ 25 hours, then heat treatment, cooling, cleans with distilled water, dry, obtained cerous nitrate modification shell-fish discarded object arsenic-removing adsorption agent.
2. cerous nitrate modification shell-fish discarded object according to claim 1 prepares the method for arsenic-removing adsorption agent, it is characterized in that, in described step (1), the ratio of shell-fish discarded object and NaOH solution is 1g:20mL ~ 1g:25mL.
3. cerous nitrate modification shell-fish discarded object according to claim 1 prepares the method for arsenic-removing adsorption agent, it is characterized in that, the bake out temperature in described step (1), step (3) and step (5) is 65 ~ 75 DEG C.
4. cerous nitrate modification shell-fish discarded object according to claim 1 prepares the method for arsenic-removing adsorption agent, it is characterized in that, in described step (3), the mass ratio of shell-fish discarded object particle and hydrochloric acid solution is 1:10 ~ 1:20.
5. cerous nitrate modification shell-fish discarded object according to claim 1 prepares the method for arsenic-removing adsorption agent; it is characterized in that; heat treatment to refer under argon shield 100 ~ 120 DEG C of heat treatments 30 ~ 60 minutes in described step (5), in atmosphere 80 ~ 100 DEG C of heat treatment 60 ~ 90 minutes.
6. cerous nitrate modification shell-fish discarded object according to claim 1 prepares the method for arsenic-removing adsorption agent, it is characterized in that, in described step (5), heat treatment refers to that the heat treatment temperature under argon shield is 120 DEG C, and heat treatment time is 45 minutes; Aerial heat treatment temperature is 100 DEG C, and heat treatment time is 60 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116002909A (en) * | 2022-12-29 | 2023-04-25 | 贵州亚太矿业有限公司 | Method for recovering iron from gold concentrate biological oxidation waste liquid |
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| CN101708461A (en) * | 2009-12-01 | 2010-05-19 | 辽宁石油化工大学 | Adsorbent of immobilized rare earth metal cerium and preparation method thereof |
| CN102500337A (en) * | 2011-11-21 | 2012-06-20 | 大连理工大学 | Phosphorus removal adsorbent for modifying oyster shell with iron salt and preparation method as well as application thereof |
| CN103394325A (en) * | 2013-08-14 | 2013-11-20 | 山东建筑大学 | Method for preparing arsenic removal adsorbent by use of marine product waste |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2003062457A (en) * | 2001-08-29 | 2003-03-04 | Nkk Plant Engineering Corp | Fluorine adsorbent and method for removing fluorine by using the same |
| CN1817439A (en) * | 2006-01-17 | 2006-08-16 | 昆明理工大学 | Rare earth adsorbent and production thereof |
| CN101708461A (en) * | 2009-12-01 | 2010-05-19 | 辽宁石油化工大学 | Adsorbent of immobilized rare earth metal cerium and preparation method thereof |
| CN102500337A (en) * | 2011-11-21 | 2012-06-20 | 大连理工大学 | Phosphorus removal adsorbent for modifying oyster shell with iron salt and preparation method as well as application thereof |
| CN103394325A (en) * | 2013-08-14 | 2013-11-20 | 山东建筑大学 | Method for preparing arsenic removal adsorbent by use of marine product waste |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116002909A (en) * | 2022-12-29 | 2023-04-25 | 贵州亚太矿业有限公司 | Method for recovering iron from gold concentrate biological oxidation waste liquid |
| CN116002909B (en) * | 2022-12-29 | 2023-07-28 | 贵州亚太矿业有限公司 | Method for recovering iron from gold concentrate biological oxidation waste liquid |
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