CN109351353A - A kind of preparation method and application carrying iron silica gel arsenic-removing adsorption agent - Google Patents
A kind of preparation method and application carrying iron silica gel arsenic-removing adsorption agent Download PDFInfo
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- CN109351353A CN109351353A CN201811281431.4A CN201811281431A CN109351353A CN 109351353 A CN109351353 A CN 109351353A CN 201811281431 A CN201811281431 A CN 201811281431A CN 109351353 A CN109351353 A CN 109351353A
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- silica gel
- arsenic
- iron
- organic solvent
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 193
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 148
- 239000000741 silica gel Substances 0.000 title claims abstract description 116
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 116
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 103
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 72
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 69
- 239000003960 organic solvent Substances 0.000 claims abstract description 63
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 62
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 62
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000007788 liquid Substances 0.000 claims abstract description 41
- 239000007787 solid Substances 0.000 claims abstract description 30
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 26
- 239000003495 polar organic solvent Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000004140 cleaning Methods 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 238000013019 agitation Methods 0.000 claims abstract description 10
- 150000002505 iron Chemical class 0.000 claims abstract description 3
- 238000010992 reflux Methods 0.000 claims abstract description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 23
- -1 iron ion Chemical class 0.000 claims description 17
- 238000004587 chromatography analysis Methods 0.000 claims description 9
- 229920002379 silicone rubber Polymers 0.000 claims description 9
- 239000004945 silicone rubber Substances 0.000 claims description 9
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 3
- 150000001282 organosilanes Chemical class 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 150000001298 alcohols Chemical group 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical group [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- YAGBAUUBKBTRNY-UHFFFAOYSA-N CO[SiH](OC)OC.C(C=C)(=O)OCCC[SiH2]OCC Chemical compound CO[SiH](OC)OC.C(C=C)(=O)OCCC[SiH2]OCC YAGBAUUBKBTRNY-UHFFFAOYSA-N 0.000 claims 1
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 239000007822 coupling agent Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 abstract description 2
- 239000002250 absorbent Substances 0.000 abstract 1
- 230000002745 absorbent Effects 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 230000010355 oscillation Effects 0.000 description 21
- 239000003463 adsorbent Substances 0.000 description 16
- 238000000034 method Methods 0.000 description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- 238000001514 detection method Methods 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000008929 regeneration Effects 0.000 description 6
- 238000011069 regeneration method Methods 0.000 description 6
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 4
- DJHGAFSJWGLOIV-UHFFFAOYSA-K Arsenate3- Chemical compound [O-][As]([O-])([O-])=O DJHGAFSJWGLOIV-UHFFFAOYSA-K 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 4
- 229940000489 arsenate Drugs 0.000 description 4
- FGIWMSAVEQNPPQ-UHFFFAOYSA-N arsenic;hydrate Chemical compound O.[As] FGIWMSAVEQNPPQ-UHFFFAOYSA-N 0.000 description 4
- OWTFKEBRIAXSMO-UHFFFAOYSA-N arsenite(3-) Chemical compound [O-][As]([O-])[O-] OWTFKEBRIAXSMO-UHFFFAOYSA-N 0.000 description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 4
- 229940087654 iron carbonyl Drugs 0.000 description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 229940006020 arsenite ion Drugs 0.000 description 2
- 239000000701 coagulant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- BMWMWYBEJWFCJI-UHFFFAOYSA-K iron(3+);trioxido(oxo)-$l^{5}-arsane Chemical compound [Fe+3].[O-][As]([O-])([O-])=O BMWMWYBEJWFCJI-UHFFFAOYSA-K 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
Classifications
-
- 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
- B01J20/02—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
-
- 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
- C02F2101/103—Arsenic compounds
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic 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)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of preparation methods for carrying iron silica gel arsenic-removing adsorption agent, belong to arsenic technical field of absorbent.Silica gel is added in hydrochloric acid by the present invention to be uniformly mixed and reflux is activated 8 ~ 10h under agitation, is used distilled water or deionized water to wash silica gel and is dried in vacuo activated silica gel to obtain the final product to neutrality and under the conditions of temperature is 60 ~ 70 DEG C；It is 220 ~ 260 DEG C, under stirring condition in temperature, iron salt dissolved is obtained to Fe- organic solvent mixed liquor A in polar organic solvent, then silane coupling agent is added to constant temperature reflow treatment 1h Fe- organic solvent mixed liquid B derived above in Fe- organic solvent mixed liquor A；By activated silica gel be added in Fe- organic solvent mixed liquid B and temperature be 200 ~ 240 DEG C, reflow treatment 20 under stirring condition ~ for 24 hours；Separation of solid and liquid obtains solid and carries iron silica gel, iron silica gel is carried to neutrality using polar organic solvent washing solid, non-iron-ion is washed into cleaning solution using distilled water or deionized water again, is placed under the conditions of temperature is 60 ~ 70 DEG C and is dried in vacuo up to iron silica gel arsenic-removing adsorption agent is carried.
Description
Technical field
The present invention relates to a kind of preparation method and applications for carrying iron silica gel arsenic-removing adsorption agent, belong to arsenic adsorber technologies neck
Domain.
Background technique
Arsenic and its compound are first kind carcinogenic substance, and excessive contact or intake arsenic can cause damages to human health.Water
The common method of middle arsenic removal has absorption method, coagulant sedimentation, bioanalysis, membrane separation process etc., and absorption method is more commonly used one
Kind method, key technology are to seek efficient low expense and the simple arsenic adsorbent of process flow.
Iron ion has very high compatibility and exclusive adsorptivity to arsenic, is at common arsenic-containing water body using molysite arsenic removal
Reason method studies the removal using arsenic in water of Nanoscale Iron in the method that ferriferous oxide prepares Nanoscale Iron as raw material.But it should
Technics comparing is complicated and needs hot conditions, and operation is more difficult；Iron-containing multiple element composite metal oxidate arsenic removal settling agent
Preparation method, arsenic-containing waste water is handled using molysite as coagulant can generate a large amount of sludge, and Treatment of Sludge is difficult, and Coagulation Method pair
The arsenic removal efficiency of low concentration is lower.Iron is loaded to the surface of active carbon and the arsenic-removing adsorption agent of inside, adsorbent can not
Regeneration.
Summary of the invention
Arsenic adsorbent in the prior art there are aiming at the problem that, the present invention provide it is a kind of carry iron silica gel arsenic-removing adsorption agent system
Preparation Method and application, for the present invention using activated silica gel as matrix, iron ion is immobilized on activated silica gel by silane coupling agent, with
The iron ion on carrier is fixed on as adsorption site, by ligand exchange approach, can reach absorption highly selective to arsenic, high
The absorption of amount.At the low ph, the iron ion on the arsenate in waste water, arsenite ion and carrier forms solubility
The ferric arsenate and iron arsenite of very little, remove arsenic；OH under the conditions of higher ph, in solution-With the iron on carrier
Ion can generate iron carbonyl, and the arsenate and arsenous anion in solution are adsorbed on carrier surface by iron carbonyl, to remove solution
In arsenic.
A kind of preparation method carrying iron silica gel arsenic-removing adsorption agent, the specific steps are as follows:
(1) silica gel is added in hydrochloric acid and is uniformly mixed and 8 ~ 10h of reflux activation processing under agitation, using distilled water or
Deionized water is washed silica gel and is dried in vacuo to neutrality and under the conditions of temperature is 60 ~ 70 DEG C up to activated silica gel；
(2) it is 220 ~ 260 DEG C, under stirring condition in temperature, iron salt dissolved is obtained to Fe- organic solvent in polar organic solvent
Mixed liquor A, then that silane coupling agent is added to constant temperature reflow treatment 1h Fe- derived above in Fe- organic solvent mixed liquor is organic
Solvent mixed liquid B；
(3) activated silica gel of step (1) is added in Fe- organic solvent mixed liquid B obtained by step (2) and is 200 in temperature
~ 240 DEG C, reflow treatment 20 under stirring condition ~ for 24 hours；Separation of solid and liquid obtains solid and carries iron silica gel, is washed using polar organic solvent
Solid carries iron silica gel and washs into cleaning solution non-iron-ion to neutrality, then using distilled water or deionized water, is subsequently placed in temperature
It is dried in vacuo under the conditions of being 60 ~ 70 DEG C up to iron silica gel arsenic-removing adsorption agent is carried；
The polar organic solvent is alcohols or ketone；
The concentration of step (1) hydrochloric acid is 5.5 ~ 6.5 mol/L, and the volume ratio of silica gel and hydrochloric acid is 1:(5 ~ 8)；
Step (1) silica gel is column layer chromatography silicone rubber, and partial size is 60 ~ 100 mesh；
Step (2) molysite is iron chloride or ferric nitrate, and silane coupling agent is the organo silane coupling agent of oxygen-containing group, and Fe- has
The concentration of molysite is 0.1 ~ 0.5g/mL in solvent mixed liquor A, and silane coupling agent dosage is the body of Fe- organic solvent mixed liquor A
Product 0.1% ~ 2%；
Further, the organo silane coupling agent of the oxygen-containing group is gamma-aminopropyl-triethoxy-silane, γ-glycidol ether
Oxygen propyl trimethoxy silicane or γ-methacryloxypropyl trimethoxy silane；
The mass ratio of activated silica gel and iron ion in Fe- organic solvent mixed liquid B is 100:(0.5 ~ 2 in the step (3)).
Load iron silica gel arsenic-removing adsorption agent prepared by the preparation method of the present invention for carrying iron silica gel arsenic-removing adsorption agent is being inhaled
Application in attached arsenic removal: it before load iron silica gel arsenic-removing adsorption agent is adsorbed, needs to contain using lime, sodium hydroxide or hydrochloric acid adjusting
The pH value of arsenic water body is 2 ~ 11；
After the present invention carries the arsenic-removing adsorption agent adsorption saturation of iron silica gel, concentration is used to be desorbed again for 1 ~ 2mol/L hydrochloric acid solution
It is raw.
Beneficial effects of the present invention:
(1) present invention is using activated silica gel as matrix, and it is immobilized on activated silica gel that iron ion passes through silane coupling agent, to be fixed on
Iron ion on carrier is as adsorption site, by ligand exchange approach, can reach suction highly selective to arsenic, high adsorption capacity
It is attached；At the low ph, the iron ion on the arsenate in waste water, arsenite ion and carrier forms solubility very little
Ferric arsenate and iron arsenite, remove arsenic；OH under the conditions of higher ph, in solution-With the iron ion meeting on carrier
Iron carbonyl is generated, the arsenate and arsenous anion in solution are adsorbed on carrier surface by iron carbonyl, to remove the arsenic in solution；
(2) present invention carries iron silica gel arsenic-removing adsorption agent, big to arsenic adsorption capacity, and selectivity is strong, stability is high, has excellent water
Matter purification efficiency；
(3) present invention carries iron silica gel arsenic-removing adsorption agent and can be used multiple times by hydrochloric acid solution desorption and regeneration.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
A kind of embodiment 1: preparation method carrying iron silica gel arsenic-removing adsorption agent, the specific steps are as follows:
(1) silica gel is added in hydrochloric acid to be uniformly mixed and flow back under agitation and is activated 8h, adopted and be washed with distilled water
Silica gel is dried in vacuo to neutrality and under the conditions of temperature is 60 DEG C up to activated silica gel；Wherein the concentration of hydrochloric acid is 6mol/L, silicon
The volume ratio of glue and hydrochloric acid is 1:5；Silica gel is column layer chromatography silicone rubber, and partial size is 60 ~ 80 mesh；
It (2) is 220 DEG C, under stirring condition in temperature, by molysite (FeCl3) be dissolved in polar organic solvent (methanol) and obtain
Fe- organic solvent mixed liquor A, then silane coupling agent (gamma-aminopropyl-triethoxy-silane) is added to Fe- organic solvent and is mixed
Constant temperature reflow treatment 1.2h obtains Fe- organic solvent mixed liquid B in liquid；Wherein in Fe- organic solvent mixed liquor A molysite concentration
For 0.1g/mL, silane coupling agent dosage is the volume 0.1% of Fe- organic solvent mixed liquor A；
(3) activated silica gel of step (1) is added in Fe- organic solvent mixed liquid B obtained by step (2) and is 200 in temperature
DEG C, reflow treatment 20h under stirring condition；Separation of solid and liquid obtains solid and carries iron silica gel, is washed using polar organic solvent (methanol)
Solid carries iron silica gel to neutrality, then adopts and be washed with distilled water to non-iron-ion in cleaning solution, and being subsequently placed in temperature is 60 DEG C of conditions
Under be dried in vacuo up to carry iron silica gel arsenic-removing adsorption agent；The wherein matter of activated silica gel and iron ion in Fe- organic solvent mixed liquid B
Amount is than being 100:0.5；
Arsenic removal performance detection: it is that 10mg/L arsenic-containing water solution is placed in the conical flask of 150mL by 50mL arsenic concentration, adjusts arsenic-containing water
PH value be 4, be added 1 g carry iron silica gel arsenic-removing adsorption agent temperature be 25 DEG C of constant temperature oscillation 10h, after reaching adsorption equilibrium, water
Arsenic concentration is 0.005mg/L in body；
Take the HCl solution that 10 mL concentration are 1mol/L in 100mL conical flask, the load iron silica gel after being up to adsorption equilibrium removes
Arsenic adsorbent is added in conical flask, and temperature is constant temperature oscillation 2h under the conditions of 25 DEG C；After oscillation, adsorbent is filtered, is used
Deionized water is rinsed to cleaning solution and is in neutrality, then being placed in temperature is 70 DEG C of freeze-day with constant temperature 10h, carries iron silica gel arsenic-removing adsorption agent again
It is raw.
A kind of embodiment 2: preparation method carrying iron silica gel arsenic-removing adsorption agent, the specific steps are as follows:
(1) silica gel is added in hydrochloric acid to be uniformly mixed and flow back under agitation and is activated 9h, adopted and be washed with distilled water
Silica gel is dried in vacuo to neutrality and under the conditions of temperature is 65 DEG C up to activated silica gel；The wherein concentration 5.8mol/L of hydrochloric acid, silicon
The volume ratio of glue and hydrochloric acid is 1:6；Silica gel is column layer chromatography silicone rubber, and partial size is 70 ~ 90 mesh；
It (2) is 230 DEG C, under stirring condition in temperature, by molysite (FeCl3) be dissolved in polar organic solvent (acetone) and obtain
Fe- organic solvent mixed liquor A, then silane coupling agent (γ-glycidyl ether oxygen propyl trimethoxy silicane) is added to Fe- has
Constant temperature reflow treatment 1.2h obtains Fe- organic solvent mixed liquid B in solvent mixed liquor；Wherein in Fe- organic solvent mixed liquor A
The concentration of molysite is 0.2g/mL, and silane coupling agent dosage is the volume 0.4% of Fe- organic solvent mixed liquor A；
(3) activated silica gel of step (1) is added in Fe- organic solvent mixed liquid B obtained by step (2) and is 210 in temperature
DEG C, reflow treatment 21h under stirring condition；Separation of solid and liquid obtains solid and carries iron silica gel, is washed using polar organic solvent (acetone)
Solid carries iron silica gel to neutrality, then adopts and be washed with distilled water to non-iron-ion in cleaning solution, and being subsequently placed in temperature is 60 DEG C of conditions
Under be dried in vacuo up to iron silica gel arsenic-removing adsorption agent is carried, wherein in activated silica gel and Fe- organic solvent mixed liquid B iron ion matter
Amount is than being 100:0.8；
Arsenic removal performance detection: it is that 20mg/L arsenic-containing water solution is placed in the conical flask of 100mL by 30mL arsenic concentration, adjusts arsenic-containing water
PH value be 3, be added 1 g carry iron silica gel arsenic-removing adsorption agent temperature be 25 DEG C of constant temperature oscillation 10h, after reaching adsorption equilibrium, water
Arsenic concentration is 0.006mg/L in body；
Take load iron silica gel of the HCl solution in 100mL conical flask, after being up to adsorption equilibrium that 15 mL concentration are 1.5mol/L
Arsenic-removing adsorption agent is added in conical flask, and temperature is constant temperature oscillation 2h under the conditions of 25 DEG C；After oscillation, adsorbent is filtered,
It is rinsed with deionized water to cleaning solution and is in neutrality, then being placed in temperature is 70 DEG C of freeze-day with constant temperature 10h, carries iron silica gel arsenic-removing adsorption agent again
It is raw.
A kind of embodiment 3: preparation method carrying iron silica gel arsenic-removing adsorption agent, the specific steps are as follows:
(1) silica gel is added in hydrochloric acid to be uniformly mixed and flow back under agitation and is activated 10h, adopted and be washed with distilled water
Silica gel is dried in vacuo to neutrality and under the conditions of temperature is 70 DEG C up to activated silica gel；Wherein the concentration of hydrochloric acid is 6.2mol/L,
The volume ratio of silica gel and hydrochloric acid is 1:7；Silica gel is column layer chromatography silicone rubber, and partial size is 60 ~ 70 mesh；
It (2) is 240 DEG C, under stirring condition in temperature, by molysite (FeCl3) be dissolved in polar organic solvent (ethylene glycol) and obtain
Fe- organic solvent mixed liquor A, then silane coupling agent (γ-methacryloxypropyl trimethoxy silane) is added to Fe-
Constant temperature reflow treatment 1.5h obtains Fe- organic solvent mixed liquid B in organic solvent mixed liquor；Wherein Fe- organic solvent mixed liquor A
The concentration of middle molysite is 0.3g/mL, and silane coupling agent dosage is the volume 0.8% of Fe- organic solvent mixed liquor A；
(3) activated silica gel of step (1) is added in Fe- organic solvent mixed liquid B obtained by step (2) and is 220 in temperature
DEG C, reflow treatment is for 24 hours under stirring condition；Separation of solid and liquid obtains solid and carries iron silica gel, is washed using polar organic solvent (ethylene glycol)
It washs solid and carries iron silica gel to neutrality, then adopt and be washed with distilled water to non-iron-ion in cleaning solution, being subsequently placed in temperature is 70 DEG C of items
It is dried in vacuo under part up to iron silica gel arsenic-removing adsorption agent is carried；Wherein activated silica gel and iron ion in Fe- organic solvent mixed liquid B
Mass ratio is 100:1.2；
Arsenic removal performance detection: it is that 15mg/L arsenic-containing water solution is placed in the conical flask of 150mL by 50mL arsenic concentration, adjusts arsenic-containing water
PH value be 4, be added 1.5 g carry iron silica gel arsenic-removing adsorption agent temperature be 25 DEG C of constant temperature oscillation 10h, after reaching adsorption equilibrium,
Arsenic in water body concentration is 0.008mg/L；
Take load iron silica gel arsenic removal of the HCl solution in 100mL conical flask, after being up to adsorption equilibrium that 10mL concentration is 1mol/L
Adsorbent is added in conical flask, and temperature is constant temperature oscillation 2h under the conditions of 25 DEG C；After oscillation, adsorbent is filtered, is spent
Ionized water is rinsed to cleaning solution and is in neutrality, then being placed in temperature is 70 DEG C of freeze-day with constant temperature 10h, carries the regeneration of iron silica gel arsenic-removing adsorption agent.
A kind of embodiment 4: preparation method carrying iron silica gel arsenic-removing adsorption agent, the specific steps are as follows:
(1) silica gel is added in hydrochloric acid to be uniformly mixed and flow back under agitation and is activated 8.5h, using deionized water
Washing silica gel is dried in vacuo to neutrality and under the conditions of temperature is 60 DEG C up to activated silica gel；Wherein the concentration of hydrochloric acid is
The volume ratio of 5.7mol/L, silica gel and hydrochloric acid is 1:8；Silica gel is column layer chromatography silicone rubber, and partial size is 70 ~ 80 mesh；
It (2) is 250 DEG C, under stirring condition in temperature, by molysite (Fe (NO3)3) be dissolved in polar organic solvent (glycerine)
Fe- organic solvent mixed liquor A is obtained, then silane coupling agent (gamma-aminopropyl-triethoxy-silane) is added to Fe- organic solvent
Constant temperature reflow treatment 2h obtains Fe- organic solvent mixed liquid B in mixed liquor；Wherein in Fe- organic solvent mixed liquor A molysite it is dense
Degree is 0.4g/mL, and silane coupling agent dosage is the volume 1.1% of Fe- organic solvent mixed liquor A；
(3) activated silica gel of step (1) is added in Fe- organic solvent mixed liquid B obtained by step (2) and is 230 in temperature
DEG C, reflow treatment 22h under stirring condition；Separation of solid and liquid obtains solid and carries iron silica gel, is washed using polar organic solvent (glycerine)
It washs solid and carries iron silica gel to neutrality, then adopt and non-iron-ion is washed with deionized into cleaning solution, being subsequently placed in temperature is 65 DEG C
Under the conditions of be dried in vacuo up to carry iron silica gel arsenic-removing adsorption agent；Wherein activated silica gel and iron ion in Fe- organic solvent mixed liquid B
Mass ratio be 100:1.6；
Arsenic removal performance detection: it is that 20mg/L arsenic-containing water solution is placed in the conical flask of 100mL by 50mL arsenic concentration, adjusts arsenic-containing water
PH value be 2, be added 2 g carry iron silica gel arsenic-removing adsorption agent temperature be 25 DEG C of constant temperature oscillation 10h, after reaching adsorption equilibrium, water
Arsenic concentration is 0.004mg/L in body；
Take load iron silica gel arsenic removal of the HCl solution in 100mL conical flask, after being up to adsorption equilibrium that 15mL concentration is 1mol/L
Adsorbent is added in conical flask, and temperature is constant temperature oscillation 2h under the conditions of 25 DEG C；After oscillation, adsorbent is filtered, is spent
Ionized water is rinsed to cleaning solution and is in neutrality, then being placed in temperature is 70 DEG C of freeze-day with constant temperature 9h, carries the regeneration of iron silica gel arsenic-removing adsorption agent.
A kind of embodiment 5: preparation method carrying iron silica gel arsenic-removing adsorption agent, the specific steps are as follows:
(1) silica gel is added in hydrochloric acid to be uniformly mixed and flow back under agitation and is activated 12h, adopted and be washed with deionized water
Silica gel is washed to be dried in vacuo to neutrality and under the conditions of temperature is 65 DEG C up to activated silica gel；Wherein the concentration of hydrochloric acid is 6.5mol/
The volume ratio of L, silica gel and hydrochloric acid is 1:7；Silica gel is column layer chromatography silicone rubber, and partial size is 80 ~ 90 mesh；
It (2) is 260 DEG C, under stirring condition in temperature, by molysite (Fe (NO3)3) be dissolved in polar organic solvent (cyclohexanone)
Fe- organic solvent mixed liquor A is obtained, then silane coupling agent (γ-glycidyl ether oxygen propyl trimethoxy silicane) is added to
Constant temperature reflow treatment 1h obtains Fe- organic solvent mixed liquid B in Fe- organic solvent mixed liquor；Wherein Fe- organic solvent mixed liquor
The concentration of molysite is 0.5g/mL in A, and silane coupling agent dosage is the volume 1.4% of Fe- organic solvent mixed liquor A；
(3) activated silica gel of step (1) is added in Fe- organic solvent mixed liquid B obtained by step (2) and is 240 in temperature
DEG C, reflow treatment 21h under stirring condition；Separation of solid and liquid obtains solid and carries iron silica gel, is washed using polar organic solvent (cyclohexanone)
It washs solid and carries iron silica gel to neutrality, then adopt and non-iron-ion is washed with deionized into cleaning solution, being subsequently placed in temperature is 70 DEG C
Under the conditions of be dried in vacuo up to carry iron silica gel arsenic-removing adsorption agent；Wherein activated silica gel and iron ion in Fe- organic solvent mixed liquid B
Mass ratio be 100:2；
Arsenic removal performance detection: it is that 10mg/L arsenic-containing water solution is placed in the conical flask of 100mL by 30mL arsenic concentration, adjusts arsenic-containing water
PH value be 11, be added 1 g carry iron silica gel arsenic-removing adsorption agent temperature be 25 DEG C of constant temperature oscillation 10h, after reaching adsorption equilibrium, water
Arsenic concentration is 0.006mg/L in body；
Take the HCl solution that 15mL concentration is 1.5mol/L in 100mL conical flask, the load iron silica gel after being up to adsorption equilibrium removes
Arsenic adsorbent is added in conical flask, and temperature is constant temperature oscillation 2h under the conditions of 25 DEG C；After oscillation, adsorbent is filtered, is used
Deionized water is rinsed to cleaning solution and is in neutrality, then being placed in temperature is 70 DEG C of freeze-day with constant temperature 8h, carries the regeneration of iron silica gel arsenic-removing adsorption agent.
A kind of embodiment 6: preparation method carrying iron silica gel arsenic-removing adsorption agent, the specific steps are as follows:
(1) silica gel is added in hydrochloric acid to be uniformly mixed and flow back under agitation and is activated 10h, adopted and be washed with deionized water
Silica gel is washed to be dried in vacuo to neutrality and under the conditions of temperature is 70 DEG C up to activated silica gel；Wherein the concentration of hydrochloric acid is 6.4mol/
The volume ratio of L, silica gel and hydrochloric acid is 1:6；Silica gel is column layer chromatography silicone rubber, and partial size is 90 ~ 100 mesh；
It (2) is 245 DEG C, under stirring condition in temperature, by molysite (Fe (NO3)3) be dissolved in polar organic solvent (methyl ethyl ketone)
Fe- organic solvent mixed liquor A is obtained, then silane coupling agent (γ-methacryloxypropyl trimethoxy silane) is added
Into Fe- organic solvent mixed liquor, constant temperature reflow treatment 1.5h obtains Fe- organic solvent mixed liquid B；Wherein Fe- organic solvent is mixed
The concentration for closing molysite in liquid A is 0.4g/mL, and silane coupling agent dosage is the volume 1.7% of Fe- organic solvent mixed liquor A；
(3) activated silica gel of step (1) is added in Fe- organic solvent mixed liquid B obtained by step (2) and is 235 in temperature
DEG C, reflow treatment 21h under stirring condition；Separation of solid and liquid obtains solid and carries iron silica gel, is washed using polar organic solvent (methyl ethyl ketone)
It washs solid and carries iron silica gel to neutrality, then adopt and non-iron-ion is washed with deionized into cleaning solution, be subsequently placed in 65 DEG C of items of temperature
It is dried in vacuo under part up to iron silica gel arsenic-removing adsorption agent is carried；Wherein activated silica gel and iron ion in Fe- organic solvent mixed liquid B
Mass ratio is 100:1.6；
Arsenic removal performance detection: it is that 20mg/L arsenic-containing water solution is placed in the conical flask of 100mL by 20mL arsenic concentration, adjusts arsenic-containing water
PH value 8, be added 1 g carry iron silica gel arsenic-removing adsorption agent temperature be 25 DEG C of constant temperature oscillation 10h, after reaching adsorption equilibrium, water body
Middle arsenic concentration is 0.008mg/L；
Take the HCl solution that 15mL concentration is 1.5mol/L in 100mL conical flask, the load iron silica gel after being up to adsorption equilibrium removes
Arsenic adsorbent is added in conical flask, and temperature is constant temperature oscillation 2h under the conditions of 25 DEG C；After oscillation, adsorbent is filtered, is used
Deionized water is rinsed to cleaning solution and is in neutrality, then being placed in temperature is 70 DEG C of freeze-day with constant temperature 10h, carries iron silica gel arsenic-removing adsorption agent again
It is raw.
A kind of embodiment 7: preparation method carrying iron silica gel arsenic-removing adsorption agent, the specific steps are as follows:
(1) silica gel is added in hydrochloric acid to be uniformly mixed and flow back under agitation and is activated 9h, adopted and be washed with deionized water
Silica gel is washed to be dried in vacuo to neutrality and under the conditions of temperature is 60 DEG C up to activated silica gel；Wherein the concentration of hydrochloric acid is 6mol/L,
The volume ratio of silica gel and hydrochloric acid is 1:6；Silica gel is column layer chromatography silicone rubber, and partial size is 90 ~ 100 mesh；
It (2) is 235 DEG C, under stirring condition in temperature, by molysite (Fe (NO3)3) be dissolved in polar organic solvent (acetone)
It is added to Fe- organic solvent mixed liquor A, then by silane coupling agent (γ-methacryloxypropyl trimethoxy silane)
Constant temperature reflow treatment 2h obtains Fe- organic solvent mixed liquid B in Fe- organic solvent mixed liquor；Wherein Fe- organic solvent mixed liquor
The concentration of molysite is 0.3g/mL in A, and silane coupling agent dosage is the volume 2% of Fe- organic solvent mixed liquor A；
(3) activated silica gel of step (1) is added in Fe- organic solvent mixed liquid B obtained by step (2) and is 215 in temperature
DEG C, reflow treatment is for 24 hours under stirring condition；Separation of solid and liquid obtains solid and carries iron silica gel, is washed using polar organic solvent (acetone)
Solid carries iron silica gel to neutrality, then adopts and non-iron-ion is washed with deionized into cleaning solution, is subsequently placed in temperature 70 C condition
Under be dried in vacuo up to carry iron silica gel arsenic-removing adsorption agent；The wherein matter of activated silica gel and iron ion in Fe- organic solvent mixed liquid B
Amount is than being 100:1.2；
Arsenic removal performance detection: 50mL arsenic concentration 10mg/L arsenic-containing water solution is placed in the conical flask of 150mL, arsenic-containing water is adjusted
PH value 10, it is 25 DEG C of constant temperature oscillation 8h that 1 g, which is added, and carries iron silica gel arsenic-removing adsorption agent in temperature, after reaching adsorption equilibrium, in water body
Arsenic concentration is 0.007mg/L；
Take load iron silica gel arsenic removal of the HCl solution in 100mL conical flask, after being up to adsorption equilibrium that 15mL concentration is 2mol/L
Adsorbent is added in conical flask, and temperature is constant temperature oscillation 2h under the conditions of 25 DEG C；After oscillation, adsorbent is filtered, is spent
Ionized water is rinsed to cleaning solution and is in neutrality, then being placed in temperature is 70 DEG C of freeze-day with constant temperature 10h, carries the regeneration of iron silica gel arsenic-removing adsorption agent.
Claims (8)
1. a kind of preparation method for carrying iron silica gel arsenic-removing adsorption agent, which is characterized in that specific step is as follows:
(1) silica gel is added in hydrochloric acid and is uniformly mixed and 8 ~ 10h of reflux activation processing under agitation, using distilled water or
Deionized water is washed silica gel and is dried in vacuo to neutrality and under the conditions of temperature is 60 ~ 70 DEG C up to activated silica gel；
(2) it is 220 ~ 260 DEG C, under stirring condition in temperature, it is organic molten that iron salt dissolved is obtained to Fe- in polar organic solvent
Agent mixed liquor A, then silane coupling agent is added to constant temperature reflow treatment 1h Fe- derived above in Fe- organic solvent mixed liquor A has
Solvent mixed liquid B；
(3) activated silica gel of step (1) is added in Fe- organic solvent mixed liquid B obtained by step (2) and is 200 in temperature
~ 240 DEG C, reflow treatment 20 under stirring condition ~ for 24 hours；Separation of solid and liquid obtains solid and carries iron silica gel, is washed using polar organic solvent
Solid carries iron silica gel and washs into cleaning solution non-iron-ion to neutrality, then using distilled water or deionized water, is subsequently placed in temperature
It is dried in vacuo under the conditions of being 60 ~ 70 DEG C up to iron silica gel arsenic-removing adsorption agent is carried.
2. carrying the preparation method of iron silica gel arsenic-removing adsorption agent according to claim 1, it is characterised in that: polar organic solvent is
Alcohols or ketone.
3. carrying the preparation method of iron silica gel arsenic-removing adsorption agent according to claim 1, it is characterised in that: step (1) hydrochloric acid
Concentration is 5.5 ~ 6.5 mol/L, and the volume ratio of silica gel and hydrochloric acid is 1:(5 ~ 8).
4. carrying the preparation method of iron silica gel arsenic-removing adsorption agent according to claim 1, it is characterised in that: step (1) silica gel is
Column layer chromatography silicone rubber, partial size are 60 ~ 100 mesh.
5. carrying the preparation method of iron silica gel arsenic-removing adsorption agent according to claim 1, it is characterised in that: step (2) molysite is
Iron chloride or ferric nitrate, silane coupling agent are the organo silane coupling agent of oxygen-containing group, molysite in Fe- organic solvent mixed liquor A
Concentration is 0.1 ~ 0.5g/mL, and silane coupling agent dosage is the volume 0.1% ~ 2% of Fe- organic solvent mixed liquor A.
6. carrying the preparation method of iron silica gel arsenic-removing adsorption agent according to claim 5, it is characterised in that: the organosilicon of oxygen-containing group
Alkane coupling agent is gamma-aminopropyl-triethoxy-silane, γ-glycidyl ether oxygen propyl trimethoxy silicane or γ-metering system
Acryloxypropylethoxysilane trimethoxy silane.
7. carrying the preparation method of iron silica gel arsenic-removing adsorption agent according to claim 1, it is characterised in that: activation in step (3)
The mass ratio of iron ion is 100:(0.5 ~ 2 in silica gel and Fe- organic solvent mixed liquid B).
8. load iron silica gel arsenic removal prepared by any one of claim 1 ~ 7 preparation method for carrying iron silica gel arsenic-removing adsorption agent is inhaled
The attached dose of application in absorption arsenic removal.
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| CN112891811B (en) * | 2021-01-18 | 2022-03-25 | 昆明理工大学 | Method for removing arsenic in contaminated acid by using silica gel reinforced zinc slag |
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Application publication date: 20190219 |