CN109692649A - Remove the adsorbent and preparation method thereof of chromate ion in water - Google Patents

Remove the adsorbent and preparation method thereof of chromate ion in water Download PDF

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Publication number
CN109692649A
CN109692649A CN201710982595.9A CN201710982595A CN109692649A CN 109692649 A CN109692649 A CN 109692649A CN 201710982595 A CN201710982595 A CN 201710982595A CN 109692649 A CN109692649 A CN 109692649A
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China
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adsorbent
solution
chromate ion
preparation
water
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CN201710982595.9A
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Chinese (zh)
Inventor
李旭光
孔德金
陈燕
邹薇
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical Technology
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China Petroleum and Chemical Corp
Sinopec Shanghai Research Institute of Petrochemical 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
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
    • 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
    • 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
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/22—Chromium or chromium compounds, e.g. chromates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The present invention relates to a kind of adsorbents and preparation method thereof of chromate ion in removing water.Mainly solve the problems, such as that chromate ion removal efficiency is not high in industrial wastewater existing in the prior art.The present invention prepares metal composite Co by using the method for co-precipitation plus hydro-thermal processxZn6‑xFe2(OH)18.4H2O, wherein x=2~5 are that the technical solution of adsorbent preferably solves the problems, such as this.The adsorbent of the method for the present invention preparation has the characteristics that chromate ion is high-efficient in removing water, can be used for environment protection field.

Description

Remove the adsorbent and preparation method thereof of chromate ion in water
Technical field
The present invention relates to a kind of adsorbents and preparation method thereof of chromate ion in removing water.
Background technique
Chromium is a kind of harmful pollutant, it mainly exists in the form of 2 kinds of+trivalent and+6 valence in the natural environment.6 valence chromium Toxicity and activity it is bigger than trivalent chromium.In chromate waste water, chromium is usually with CrO4 2-And Cr2O7 2-Equal anionic forms exist. Into the chromium in environment not only contaminated soil, earth's surface and underground water, but also can be detrimental to health by food chain.It uses at present Mainly have in the technology for administering the sewage containing chromate ion: reduction precipitation method, ion-exchange, evaporation absorption method and absorption method Deng.To develop efficient, cheap adsorbent, removing the pollutant in water body by absorption method is to grind in recent years for each environmentally friendly mechanism The hot spot studied carefully.
CN103342787A discloses a kind of for adsorbing the preparation method of chromate material.The following steps are included: surface Modified aerosil particles: silica particle surface chemical graft polymethylacrylic acid dimethylamino ethyl ester DMAEMA: by 1.5- The modified aerosil particles AMPS-SiO in the surface of 1.6g2, add 80-85mL water, 15-16mL monomer DMAEMA, 20mL dissolved with The aqueous solution of 0.150-0.155g ammonium persulfate, reaction obtain grafting particle PDMAEMA/SiO2；It is grafted particle PDMAEMA/SiO2 Quaternized transformation: by the grafting particle PDMAEMA/SiO of 1-1.2g2Middle addition 50-55mL epoxychloropropane, reaction obtain function It can particle QPDMAEMA/SiO2.The invention overcomes the dependence to PH values, high to chromate ion adsorption capacity；Belong to Polymer/inorganic functional composite material has excellent physical and chemical performance, at low cost.
CN105541888A discloses a kind of coordination polymer with selective ion exchange performance and its preparation and answers With.Its complex are as follows: [Ag (L)] (BF4)(DMF)2, wherein L=3- (4- pyridyl group) -4,5- bis- (3- pyridyl groups) -1,2,4- tri- Azoles, DMF=N, N '-dimethyl formamide.It is by AgBF4DMF solution be placed in test tube bottom, then add above bottom solution Add ethyl acetate buffer layer, the upper layer of above-mentioned ethyl acetate buffer layer is slowly placed in after then dissolving ligand L with methanol, it is quiet It sets volatilization 5~7 days and obtains colourless bulk-shaped monocrystal product.Experiments have shown that: the tetrafluoroborate to dissociate in the material is weighed with water In the exchange process of chromate pollutant, biggish exchange capacity (297.2mg/g) not only may be implemented, be the Cr being currently known (VI) adsorbance is maximum in adsorbent material, and its detection is limited to 0.1ppm, has reached the cleaning water gauge of Environmental Protection Agency EPA It is quasi-.
CN105457599A discloses a kind of synthesis of magnetic nano adsorption material and its for handling heavy metal waste liquid Method.The invention synthesized first it is a kind of can in specific complex water heavy metal magnetic nano-particle material, it can and water Middle heavy metal ion forms complex compound, and in exterior magnetic field, complex compound quickly is assembled to form solid phase from waste liquid to magnetic direction, The separation of water solid phase is carried out, to realize the removal of heavy metal ion in water.Meanwhile the invention is given up for what COD detector generated Liquid contains the characteristics of high concentration heavy metal and strong acid environment, develops reduction-adsorption-regeneration process flow: using reproducibility Dichromate ion is reduced into trivalent chromic ion in acid condition by iron powder, then with magnetic adsorptive material, under the conditions of alkalescence Adsorption of metal ions is removed, last adsorbent material realizes regeneration in acid condition.It through the invention can be quick, efficient, low At heavy metal ion in local removal water, new method is provided for heavy metal pollution liquid waste processing.
CN104402090A discloses method that is a kind of while removing chromate and trichloro ethylene in water removal, including following step Rapid: (1) nonionic surface active agent and cationic surfactant micelle strengthen (2) ultrafiltration.The present invention is using non-ionic After surfactant is compounded with cationic surfactant, the performance of surfactant can not only be improved, reduces surface-active The CMC of agent finally reduces cost to reduce the dosage of surfactant；Section of surfactant in penetrating fluid is improved simultaneously Rate is stayed, the secondary pollution to environment is reduced.It is demonstrated experimentally that removing CrO simultaneously4 2-85% is reached as high as, removal TCE is reached as high as 72%, permeation flux is 1.8L/ (m2.s), the rejection of surfactant is up to 85%.
Although above-mentioned technological invention has certain effect, there is deficiency, as adsorbent preparation is complicated or adsorption efficiency is not high The problems such as be difficult to apply in practical situations, in view of the above deficiencies, propose that preparation is simple, the high new adsorbent of adsorption efficiency is de- Except the chromate ion in waste water.
Summary of the invention
The first technical problem to be solved by the present invention is to overcome in industrial wastewater existing in the prior art The not high problem of chromate ion removal efficiency provides a kind of new adsorbent for removing chromate ion in water.The adsorbent It is high-efficient to have the characteristics that remove chromate ion in water.
The second technical problem to be solved by the present invention is to provide the corresponding removing of one of one kind and solution technical problem The preparation method of the adsorbent of chromate ion in water.
The third technical problem to be solved by the present invention is to provide the corresponding removing of one of one kind and solution technical problem The application method of the adsorbent of chromate ion in water.
One of to solve above-mentioned technical problem, The technical solution adopted by the invention is as follows: in a kind of removing water chromate from The adsorbent of son, composition include CoxZn6-xFe2(OH)18·4H2O, wherein x=2~5.
In above-mentioned technical proposal, the adsorbent has hydrotalcite-like compound.Preferably, the hydrotalcite-like compound is nitre Acid group intercalation.
In above-mentioned technical proposal, the crystal grain of the adsorbent is less than 500nm, preferably 100-500nm.
In above-mentioned technical proposal, the CoxZn6-xFe2(OH)18·4H2O, wherein preferably 3~5 x.
To solve above-mentioned technical problem two, The technical solution adopted by the invention is as follows: chromate ion in removing water The preparation method of adsorbent, comprising the following steps:
1. it is soluble in water after cobalt salt, zinc salt, molysite are weighed, it is denoted as solution A；
2. alkali source is soluble in water, it is denoted as solution B；
3. solution B is added in solution A, solution ph is 6~11, and stirring pours into solution in crystallizing kettle in 60~150 DEG C 1~36h of hydro-thermal process, is filtered, washed, is drying to obtain adsorbent product.
In above-mentioned technical proposal, the cobalt salt is at least one of cobalt nitrate, cobalt acetate or cobalt chloride.
In above-mentioned technical proposal, the zinc salt is at least one of zinc acetate, zinc nitrate or zinc chloride.
In above-mentioned technical proposal, the molysite is at least one of ferric nitrate or iron chloride.
In above-mentioned technical proposal, the molar ratio of the cobalt salt and zinc salt is 1:2~5:1, and preferred molar ratio is 1:1~5:1.
In above-mentioned technical proposal, the alkali source is at least one of sodium hydroxide, potassium hydroxide or ammonium hydroxide.
In above-mentioned technical proposal, mixed solution pH value 6~10 is controlled.
In above-mentioned technical proposal, hydro-thermal process temperature is 65~120 DEG C, 3~12h of time.It is further preferable that 90-120 DEG C, time 3-5h.To obtain the houghite crystal grain less than 500 nanometers, adsorption efficiency is helped to improve.
In above-mentioned technical proposal, the drying condition is 60-150 DEG C, 1-24h.
In above-mentioned technical proposal, the step is stopped 3. by solution B fast drop into solution A, to solution ph to 6~11 Only.
To solve above-mentioned technical problem three, The technical solution adopted by the invention is as follows: in a kind of removing water chromate from The method of son, adsorbent is mixed with the aqueous solution containing chromate ion at 5~35 DEG C and mixes slowly 10~30min Remove chromate ion in water.
In above-mentioned technical proposal, the concentration ratio of chromate ion is 7~30:1 in adsorbent and water.
Adsorbent provided by the invention can chromate ion in efficient removal water, can be used for environment protection field.
Using technical solution of the present invention, to be co-precipitated the metal composite for adding the method for hydro-thermal process to prepare CoxZn6-xFe2(OH)18·4H2O is active component, and since it is with layer structure, and interlayer can accommodate exchange anion, because This shows the good adsorption properties to anion.In the metal composite that cobalt, zinc, iron form, cobalt, zinc are under certain proportion With synergistic effect, has compared with other adsorbent materials more preferably to the adsorption capacity of chromate ion, be embodied in suction Attached dose of dosage is few, and adsorption rate is fast, 10~30min, can remove chromate ion in water, and it is high-efficient to take off chromate.Pass through control The materials synthesis technological parameter is made, the optimization removal efficiency such as crystal form, pore structure can be effectively controlled, achieves preferable technology effect Fruit.
Below by embodiment, the present invention is further elaborated.
Specific embodiment
[embodiment 1]
By cobalt nitrate, zinc nitrate and ferric nitrate, 4:2:2 is dissolved in deionized water in molar ratio, is stirred at room temperature to clear Clearly, it is denoted as solution A；Sodium hydroxide is dissolved in deionized water, is stirred to clarify at room temperature, solution B is denoted as；Solution B is quick It is added dropwise in solution A, stops to solution ph to 9.0, continue to stir 2h, solution is poured into crystallizing kettle at 110 DEG C of hydro-thermals Manage 5h, be filtered, washed, in 110 DEG C of dry 10h up to adsorbent product A.
In the 1L aqueous solution that the chromate ion containing 500mg is added in 20 DEG C in 10g adsorbent A, water is detected after stirring 20min Middle chromate ion content, is as a result listed in table 1.
[embodiment 2]
By cobalt nitrate, zinc nitrate and ferric nitrate, 2:4:2 is dissolved in deionized water in molar ratio, is stirred at room temperature to clear Clearly, it is denoted as solution A；Sodium hydroxide is dissolved in deionized water, is stirred to clarify at room temperature, solution B is denoted as；Solution B is quick It is added dropwise in solution A, stops to solution ph to 9.0, continue to stir 2h, solution is poured into crystallizing kettle at 110 DEG C of hydro-thermals Manage 5h, be filtered, washed, in 110 DEG C of dry 10h up to adsorbent product B.
In the 1L aqueous solution that the chromate ion containing 500mg is added in 20 DEG C in 10g adsorbent B, water is detected after stirring 20min Middle chromate ion content, is as a result listed in table 1.
[embodiment 3]
By cobalt nitrate, zinc nitrate and ferric nitrate, 3:3:2 is dissolved in deionized water in molar ratio, is stirred at room temperature to clear Clearly, it is denoted as solution A；Sodium hydroxide is dissolved in deionized water, is stirred to clarify at room temperature, solution B is denoted as；Solution B is quick It is added dropwise in solution A, stops to solution ph to 9.0, continue to stir 2h, solution is poured into crystallizing kettle at 110 DEG C of hydro-thermals Manage 5h, be filtered, washed, in 110 DEG C of dry 10h up to adsorbent product C.
In the 1L aqueous solution that the chromate ion containing 500mg is added in 20 DEG C in 10g adsorbent C, water is detected after stirring 20min Middle chromate ion content, is as a result listed in table 1.
[embodiment 4]
By cobalt nitrate, zinc nitrate and ferric nitrate, 4:2:2 is dissolved in deionized water in molar ratio, is stirred at room temperature to clear Clearly, it is denoted as solution A；Sodium hydroxide is dissolved in deionized water, is stirred to clarify at room temperature, solution B is denoted as；Solution B is quick It is added dropwise in solution A, stops to solution ph to 6.0, continue to stir 2h, solution is poured into crystallizing kettle at 110 DEG C of hydro-thermals Manage 5h, be filtered, washed, in 110 DEG C of dry 10h up to adsorbent product D.
In the 1L aqueous solution that the chromate ion containing 500mg is added in 20 DEG C in 10g adsorbent D, water is detected after stirring 20min Middle chromate ion content, is as a result listed in table 1.
[embodiment 5]
By cobalt nitrate, zinc nitrate and ferric nitrate, 4:2:2 is dissolved in deionized water in molar ratio, is stirred at room temperature to clear Clearly, it is denoted as solution A；Sodium hydroxide is dissolved in deionized water, is stirred to clarify at room temperature, solution B is denoted as；Solution B is quick It is added dropwise in solution A, stops to solution ph to 8.0, continue to stir 2h, solution is poured into crystallizing kettle at 110 DEG C of hydro-thermals Manage 5h, be filtered, washed, in 110 DEG C of dry 10h up to adsorbent product E.
In the 1L aqueous solution that the chromate ion containing 500mg is added in 20 DEG C in 10g adsorbent E, water is detected after stirring 20min Middle chromate ion content, is as a result listed in table 1.
[embodiment 6]
By cobalt nitrate, zinc nitrate and ferric nitrate, 4:2:2 is dissolved in deionized water in molar ratio, is stirred at room temperature to clear Clearly, it is denoted as solution A；Sodium hydroxide is dissolved in deionized water, is stirred to clarify at room temperature, solution B is denoted as；Solution B is quick It is added dropwise in solution A, stops to solution ph to 10.0, continue to stir 2h, solution is poured into crystallizing kettle at 110 DEG C of hydro-thermals Manage 5h, be filtered, washed, in 110 DEG C of dry 10h up to adsorbent product F.
In the 1L aqueous solution that the chromate ion containing 500mg is added in 20 DEG C in 10g adsorbent F, water is detected after stirring 20min Middle chromate ion content, is as a result listed in table 1.
[embodiment 7]
By cobalt nitrate, zinc nitrate and ferric nitrate, 4:2:2 is dissolved in deionized water in molar ratio, is stirred at room temperature to clear Clearly, it is denoted as solution A；Sodium hydroxide is dissolved in deionized water, is stirred to clarify at room temperature, solution B is denoted as；Solution B is quick It is added dropwise in solution A, stops to solution ph to 9.0, continue to stir 2h, solution is poured into crystallizing kettle in 75 DEG C of hydro-thermal process 12h, be filtered, washed, in 110 DEG C of dry 10h up to adsorbent product G.
In the 1L aqueous solution that the chromate ion containing 500mg is added in 20 DEG C in 10g adsorbent G, water is detected after stirring 20min Middle chromate ion content, is as a result listed in table 1.
[comparative example 1]
By cobalt nitrate and ferric nitrate, 6:2 is dissolved in deionized water in molar ratio, is stirred to clarify at room temperature, and solution is denoted as A；Sodium hydroxide is dissolved in deionized water, is stirred to clarify at room temperature, solution B is denoted as；By solution B fast drop to solution A In, stop to solution ph to 9.0, continues to stir 2h, solution is poured into crystallizing kettle in 110 DEG C of hydro-thermal process 5h, filters, wash Wash, in 110 DEG C of dry 10h up to adsorbent product.
In the 1L aqueous solution that the chromate ion containing 500mg is added in 20 DEG C in 10g adsorbent, water is detected after stirring 20min Middle chromate ion content, is as a result listed in table 1.
[comparative example 2]
By zinc nitrate and ferric nitrate, 6:2 is dissolved in deionized water in molar ratio, is stirred to clarify at room temperature, and solution is denoted as A；Sodium hydroxide is dissolved in deionized water, is stirred to clarify at room temperature, solution B is denoted as；By solution B fast drop to solution A In, stop to solution ph to 9.0, continues to stir 2h, solution is poured into crystallizing kettle in 110 DEG C of hydro-thermal process 5h, filters, wash Wash, in 110 DEG C of dry 10h up to adsorbent product.
In the 1L aqueous solution that the chromate ion containing 500mg is added in 20 DEG C in 10g adsorbent, water is detected after stirring 20min Middle chromate ion content, is as a result listed in table 1.
Table 1
[embodiment 8~10]
Adsorbent A is carried out to chromate ion in removing water to test under conditions of different amounts, temperature, mixing time, As a result it is listed in table 2.
Table 2

Claims (10)

1. the adsorbent of chromate ion, composition include Co in a kind of removing waterxZn6-xFe2(OH)18.4H2O, wherein x=2~ 5。
2. the preparation method of the adsorbent of chromate ion in removing water described in claim 1, comprising the following steps:
1. cobalt salt, zinc salt, molysite is soluble in water, it is denoted as solution A；
2. alkali source is soluble in water, it is denoted as solution B；
3. solution B is added in solution A, solution ph is 6~11, and stirring pours into solution in crystallizing kettle in 60~150 DEG C of water It is heat-treated 1~36h, is filtered, washed, is drying to obtain adsorbent product.
3. the preparation method of the adsorbent of chromate ion in removing water according to claim 2, it is characterised in that described Cobalt salt be at least one of cobalt nitrate, cobalt acetate or cobalt chloride.
4. the preparation method of the adsorbent of chromate ion in removing water according to claim 2, it is characterised in that described Zinc salt be at least one of zinc acetate, zinc nitrate or zinc chloride.
5. the preparation method of the adsorbent of chromate ion in removing water according to claim 2, it is characterised in that described Molysite be at least one of ferric nitrate or iron chloride.
6. the preparation method of the adsorbent of chromate ion in removing water according to claim 2, it is characterised in that described Alkali source be at least one of sodium hydroxide, potassium hydroxide or ammonium hydroxide.
7. the preparation method of the adsorbent of chromate ion in removing water according to claim 2, it is characterised in that control Mixed solution pH value 6~10.
8. the preparation method of the adsorbent of chromate ion in removing water according to claim 2, it is characterised in that hydro-thermal Treatment temperature is 65~120 DEG C, 3~12h of time.
9. a kind of method of chromate ion in removing water, by adsorbent and the aqueous solution containing chromate ion at 5~35 DEG C 10~30min is mixed, chromate ion in water can be removed.
10. the method for chromate ion in removing water according to claim 9, it is characterised in that chromic acid in adsorbent and water The concentration ratio of radical ion is 7~30:1.
CN201710982595.9A 2017-10-20 2017-10-20 Remove the adsorbent and preparation method thereof of chromate ion in water Pending CN109692649A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115814767A (en) * 2022-12-13 2023-03-21 昆明理工大学 Preparation method and application of coordination polymer adsorbent CPs-ECL
CN115814767B (en) * 2022-12-13 2024-05-03 昆明理工大学 Preparation method and application of coordination polymer adsorbent CPs-ECL

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