CN110711559A - Ion adsorbent and preparation method and application thereof - Google Patents
Ion adsorbent and preparation method and application thereof Download PDFInfo
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- CN110711559A CN110711559A CN201810764953.3A CN201810764953A CN110711559A CN 110711559 A CN110711559 A CN 110711559A CN 201810764953 A CN201810764953 A CN 201810764953A CN 110711559 A CN110711559 A CN 110711559A
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 150000002500 ions Chemical class 0.000 claims abstract description 91
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000001179 sorption measurement Methods 0.000 claims abstract description 40
- 235000010443 alginic acid Nutrition 0.000 claims abstract description 33
- 229920000615 alginic acid Polymers 0.000 claims abstract description 33
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 28
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229940072056 alginate Drugs 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims abstract description 26
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 26
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 23
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000007112 amidation reaction Methods 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 11
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 40
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 39
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 22
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 18
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 17
- 239000000661 sodium alginate Substances 0.000 claims description 17
- 235000010413 sodium alginate Nutrition 0.000 claims description 17
- 229940005550 sodium alginate Drugs 0.000 claims description 17
- 230000004913 activation Effects 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 14
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 13
- 230000003213 activating effect Effects 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 229960001126 alginic acid Drugs 0.000 claims description 6
- 239000000783 alginic acid Substances 0.000 claims description 6
- 150000004781 alginic acids Chemical class 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- -1 mercury ions Chemical class 0.000 claims description 5
- 239000000737 potassium alginate Substances 0.000 claims description 5
- 235000010408 potassium alginate Nutrition 0.000 claims description 5
- MZYRDLHIWXQJCQ-YZOKENDUSA-L potassium alginate Chemical compound [K+].[K+].O1[C@@H](C([O-])=O)[C@@H](OC)[C@H](O)[C@H](O)[C@@H]1O[C@@H]1[C@@H](C([O-])=O)O[C@@H](O)[C@@H](O)[C@H]1O MZYRDLHIWXQJCQ-YZOKENDUSA-L 0.000 claims description 5
- 239000001508 potassium citrate Substances 0.000 claims description 5
- 229960002635 potassium citrate Drugs 0.000 claims description 5
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims description 5
- 235000011082 potassium citrates Nutrition 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 230000009435 amidation Effects 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 229910052753 mercury Inorganic materials 0.000 claims description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 2
- 229910001430 chromium ion Inorganic materials 0.000 claims description 2
- 229910001431 copper ion Inorganic materials 0.000 claims description 2
- 230000002862 amidating effect Effects 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 10
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 6
- 238000004064 recycling Methods 0.000 abstract description 6
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000007790 solid phase Substances 0.000 abstract description 2
- 238000001879 gelation Methods 0.000 abstract 1
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 20
- 229910021645 metal ion Inorganic materials 0.000 description 18
- 238000005303 weighing Methods 0.000 description 14
- 238000001914 filtration Methods 0.000 description 13
- LMDZBCPBFSXMTL-UHFFFAOYSA-N 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide Substances CCN=C=NCCCN(C)C LMDZBCPBFSXMTL-UHFFFAOYSA-N 0.000 description 11
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 239000012265 solid product Substances 0.000 description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000011575 calcium Substances 0.000 description 9
- 239000008233 hard water Substances 0.000 description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 5
- 238000009616 inductively coupled plasma Methods 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000000909 electrodialysis Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000003002 pH adjusting agent Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- LIZLHLFVAAOLKE-UHFFFAOYSA-N C(CN)N.ON1C(CCC1=O)=O Chemical compound C(CN)N.ON1C(CCC1=O)=O LIZLHLFVAAOLKE-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000007160 gastrointestinal dysfunction Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- IYKMDRMCUIFHRA-UHFFFAOYSA-H tripotassium;trisodium;2-hydroxypropane-1,2,3-tricarboxylate;hydrate Chemical compound O.[Na+].[Na+].[Na+].[K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O IYKMDRMCUIFHRA-UHFFFAOYSA-H 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
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
- B01J20/22—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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
-
- 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
-
- 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
-
- 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
-
- 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
Abstract
The application discloses an ion adsorbent and a preparation method and application thereof, and belongs to the technical field of solid phase adsorption. The method adopts alginate and citrate as raw materials, the alginate and the citrate are connected through amidation reaction by using ethylenediamine as a connecting agent, then the connecting agent is dripped into an alkaline earth metal ion solution for gelation, and the ion adsorbent is prepared through solid-liquid separation and drying. The ion adsorbent is preferably used for removing calcium ions and/or magnesium ions in a water body. The ion adsorbent provided by the application has the advantages of high adsorption rate, high adsorption rate and large adsorption capacity on various heavy metal ions, particularly calcium ions and magnesium ions, is reproducible through simple treatment, and still keeps stable adsorption performance after repeated recycling; the preparation method of the ion adsorbent provided by the application has the advantages of simple process, few steps, mild conditions and green and cheap raw materials, so that the efficient and environment-friendly ion adsorbent can be prepared at low cost.
Description
Technical Field
The application relates to an ion adsorbent and a preparation method and application thereof, belonging to the technical field of solid phase adsorption.
Background
Due to the influence of geographical factors and human activities, the content of calcium and magnesium salts in the environmental water in most regions of China is too high, and the problem of hard water exists. The use and drinking of hard water can cause a plurality of problems, such as the occurrence of scale plaques on water appliances, the reduction of the washing efficiency of a cleaning agent, rough skin after bath, messy and lusterless hair, the influence on food taste, gastrointestinal dysfunction and the like, wherein the damage to the skin and clothes is particularly obvious. Therefore, the method has important practical significance for removing high-content calcium and magnesium ions in the water body.
The common treatment methods of the water containing calcium and magnesium ions at present comprise: lime soda process, ion exchange process, electrodialysis process, boiling process, adsorption process, etc. The ion exchange method has obvious effect but less water treatment amount; the electrodialysis and lime soda method have low removal efficiency when treating low-concentration hard water and high operation cost; the boiling method is simple and convenient to operate when treating a small amount of hard water, but the process is complicated when treating a large amount of hard water, and the energy consumption is large.
The adsorption method is concerned with because of the advantages of simple and easy operation, recycling, little pollution, high removal efficiency and the like. The core of the adsorption process is a solid adsorbent. At present, a few of reported adsorbents for softening hard water are available, so that the preparation of the calcium and magnesium ion adsorbent which is efficient, environment-friendly, easy to operate and easy to treat has a very wide application prospect.
Disclosure of Invention
According to one aspect of the present application, an ion adsorbent is provided, which has excellent adsorption performance on calcium, magnesium ions and various heavy metal ions, is reproducible, and has stable performance after repeated recycling.
The ion adsorbent is characterized by being obtained by carrying out amidation reaction on ethylenediamine, alginate and citrate.
Preferably, the ion adsorbent can adsorb at least one of lead ions, calcium ions, copper ions, mercury ions, chromium ions, zinc ions, iron ions, and magnesium ions in a solution.
Preferably, the calcium ion concentration in the solution is 10-4mol/L～1.5×10-3And the mol/L is that under the condition that the liquid-solid ratio of the solution to the ion adsorbent is 0.2L/g, the adsorption rate of the ion adsorbent to calcium ions at room temperature is 90-99.9%.
Preferably, the concentration of magnesium ions in the solution is 10-4mol/L～1.5×10-3And the mol/L is that under the condition that the liquid-solid ratio of the solution to the ion adsorbent is 0.2L/g, the adsorption rate of the ion adsorbent to magnesium ions at room temperature is 90-99%.
Preferably, the ion adsorbent is a calcium ion and/or magnesium ion adsorbent.
According to another aspect of the present application, a method for preparing the ion adsorbent is provided, the method has the advantages of simple process, mild conditions, green and cheap raw materials, and the ion adsorbent with high efficiency and environmental protection can be prepared at low cost.
The preparation method of the ion adsorbent is characterized by comprising the step of carrying out amidation reaction on alginate and citrate and ethylenediamine.
In one embodiment, the method of making the ionic adsorbent comprises at least the steps of:
(a) mixing a solution containing alginate, citrate and an activating agent with ethylenediamine for amidation reaction to obtain a solution I;
(b) dripping the solution I into an alkaline earth metal ion solution to obtain a mixture II;
(c) and (3) separating the solid in the obtained mixture II, washing and drying to obtain the ion adsorbent.
Preferably, the alginate in step (a) is selected from at least one of sodium alginate, potassium alginate and alginic acid.
Preferably, the citrate in step (a) is selected from at least one of sodium citrate, potassium citrate, citric acid.
Preferably, the activating agents in step (a) are 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide.
Preferably, the weight ratio of the alginate, the citrate, the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, the N-hydroxysuccinimide and the ethylenediamine in the step (a) is as follows:
alginate, namely citrate, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and ethylenediamine, wherein the weight ratio of the N-hydroxysuccinimide to the ethylenediamine is 0.2-2: 1: 0.22-0.28: 0.13-0.17: 8-10.
More preferably, the alginate is citrate 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and the N-hydroxysuccinimide ethylenediamine is 0.2-2: 1:0.25:0.15: 9.
Further preferred is alginate, citrate, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide, ethylenediamine, 1:1:0.25:0.15: 9.
Preferably, the reaction temperature of the amidation in the step (a) is 0-70 ℃, and the reaction time is more than 1 hour.
More preferably, the reaction temperature of the amidation in the step (a) is 5 to 50 ℃, and the reaction time is 2 to 3 hours.
Preferably, the solution containing alginate, citrate and activator in step (a) is obtained by mixing the solution containing alginate and citrate with activator and activating; wherein the activation is carried out by stirring at 0-70 ℃ for not less than 1 hour.
More preferably, the activation is stirring at 5 to 50 ℃ for 3 to 6 hours.
Preferably, in the step (b), the solution I is dripped into the alkaline earth metal ion solution, and the mixture is stirred for more than 10 minutes at 0-50 ℃ to obtain a mixture II.
More preferably, in the step (b), the solution I is dropped into the alkaline earth metal ion solution, and the mixture is stirred for 10 to 20 minutes at 5 to 30 ℃ to obtain the mixture II.
Preferably, the alkaline earth metal ion solution in step (b) is a calcium ion solution.
Preferably, the drying in step (c) is vacuum freeze drying.
Preferably, the separation in step (c) is performed by means of filtration.
Thus, in a particular embodiment, the process for the preparation of the ionic adsorbent comprises at least the following steps:
(a) weighing alginate and citrate according to the weight ratio, dissolving in water, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide under stirring, and adding ethylenediamine to obtain a solution I;
(b) under the stirring condition, dripping the solution I into the calcium ion solution and continuously stirring to obtain a mixture II;
(c) and (3) washing and freeze-drying the solid obtained after the solid-liquid separation of the mixture II to obtain the ion adsorbent.
Thus, in a more specific embodiment, step (a) comprises: weighing alginate and citrate according to the weight ratio, dissolving in water, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide under stirring, adding ethylenediamine, and reacting at 0-70 ℃ for more than 1 hour to obtain a solution I;
the step (b) includes: and under the stirring condition, dripping the solution I into the calcium ion solution and continuously stirring, wherein the reaction temperature is 0-50 ℃, and the reaction time is more than 10 minutes to obtain a solid-liquid mixture II.
According to a further aspect of the application, there is provided a use of the ion adsorbent, the ion adsorbent prepared according to the method, for removing calcium ions and/or magnesium ions in a body of water.
Preferably, the concentration of calcium ions in the water body is 0.0001-0.01 mol/L; the concentration of magnesium ions in the water body is 0.0001-0.01 mol/L.
The beneficial effects that this application can produce include:
1) the ion adsorbent provided by the application has the advantages of high adsorption rate, high adsorption rate and large adsorption capacity on various heavy metal ions, particularly calcium ions and magnesium ions, is reproducible through simple treatment, and keeps stable adsorption performance after repeated recycling.
2) The preparation method of the ion adsorbent provided by the application has the advantages of simple process, few steps, mild conditions and green and cheap raw materials, so that the efficient and environment-friendly ion adsorbent can be prepared at low cost.
Drawings
Fig. 1 is a photograph of the morphology of the ion adsorbent prepared in example 1 of the present application.
Detailed Description
The application aims to provide a green, efficient and recyclable ion adsorbent, and a preparation method and application thereof.
According to the ion adsorbent, cheap alginate and citrate are used as raw materials, the adsorbent is prepared by connecting ethylenediamine through amidation reaction, and the ion adsorbent with the best performance and shape is obtained by adjusting the concentration of reactants and the raw materials.
In the application, alginate and citrate are used as raw materials, carboxyl groups in the alginate and the citrate are activated through 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, then a connecting agent ethylenediamine is added, amino groups at two ends are subjected to condensation reaction with the alginate and the citrate, the two are connected, then the gel is formed in an alkaline earth metal ion solution, and the ion adsorbent is obtained through freeze-drying. The adsorbent is rich in carboxyl, hydroxyl and amino, wherein lone electron pairs of oxygen atoms can coordinate with vacant electron orbitals such as calcium and magnesium ions, so that the calcium and magnesium ions are enriched in pores on the surface or inside the adsorbent, and the amino also provides the lone electron pairs to coordinate with the calcium and magnesium ions to enhance the adsorption capacity.
The ion adsorbent can be applied to hard water bodies, such as water samples in rivers and lakes, factory wastewater, domestic sewage and the like through experimental inspection.
It should be understood that the ion adsorbent according to the present application can adsorb not only calcium and magnesium ions in a water body at a high level, but also other heavy metal ions such as lead, copper, mercury, chromium, zinc, iron, etc. in a water body, which also has a good adsorption effect, as demonstrated in the examples hereinafter in the present application.
For the purposes of the present invention, in the context of the present application, the term "alginate" also covers alginic acid itself, in addition to salts of alginic acid such as sodium alginate, potassium alginate and the like. Similarly, the term "citrate" encompasses citric acid itself in addition to salts of citric acid such as sodium citrate, potassium citrate, and the like.
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
Unless otherwise specified, the raw materials in the examples of the present application were all purchased commercially.
Unless otherwise specified, the ion adsorption performance in the examples of the present application was measured at room temperature.
The conditions for vacuum freeze-drying employed in this application are as follows: 10-20 pa, -70 ℃ to-60 ℃ for 24-48 h.
The analysis method in the examples of the present application is as follows:
the actual concentration values of the metal ions in the metal ion solution were determined using an inductively coupled plasma atomic emission spectrometer (available from SPECTRO corporation, Germany, model SPECTROROCOSCOS II).
The calculation method in the embodiment of the present application is as follows:
in the examples of the present application, the adsorption rate and adsorption capacity for metal ions were calculated based on the following formulas:
wherein C isoIs the initial concentration (mmol/L) of metal ions, CfIn terms of the concentration (mmol/L) of the metal ion after adsorption, V is the volume (L) of the solution, W is the mass (g) of the adsorbent used, and M is the relative atomic mass (g/mol) of the metal ion.
Example 1
Preparation of ion adsorbent:
(1) weighing 1.0g of sodium alginate and 1.0g of citric acid, dissolving in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 3h under the stirring condition, adding 9.0g of ethylenediamine, and reacting for 2h at 25 ℃ to prepare a solution I;
(2) dripping the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuing stirring for 20 minutes after dripping; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
The photo of the ion adsorbent is shown in FIG. 1.
Example 2
Preparation of ion adsorbent:
(1) weighing 1.0g of potassium alginate and 1.0g of citric acid, dissolving in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 3h under the condition of stirring, then adding 9.0g of ethylenediamine, and reacting for 2h at 25 ℃ to obtain a solution I;
(2) dripping the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuing stirring for 20 minutes after dripping; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
Example 2 differs from example 1 in that: sodium alginate is replaced by potassium alginate.
Example 3
Preparation of ion adsorbent:
(1) weighing 1.0g of alginic acid and 1.0g of citric acid, dissolving in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 3h under the condition of stirring, then adding 9.0g of ethylenediamine, and reacting for 2h at 25 ℃ to obtain a solution I;
(2) dripping the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuing stirring for 20 minutes after dripping; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
Example 3 differs from example 1 in that: replacing sodium alginate with alginic acid.
Example 4
Preparation of ion adsorbent:
(1) weighing 2.0g of sodium alginate and 1.0g of citric acid, dissolving in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 3h under the stirring condition, then adding 9.0g of ethylenediamine, and reacting for 2h at 25 ℃ to prepare a solution I;
(2) dropwise adding the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuously stirring for 20 minutes after dropwise adding; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
Example 4 differs from example 1 in that: the mass of the sodium alginate is changed from 1.0g to 2.0 g.
Example 5
Preparation of ion adsorbent:
(1) weighing 0.2g of sodium alginate and 1.0g of citric acid, dissolving in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 3h under the stirring condition, then adding 9.0g of ethylenediamine, and reacting for 2h at 25 ℃ to prepare a solution I;
(2) dripping the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuing stirring for 20 minutes after dripping; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
Example 5 differs from example 1 in that: the mass of the sodium alginate is changed from 1.0g to 0.2 g.
Example 6
Preparation of ion adsorbent:
(1) weighing 1.0g of sodium alginate and 1.0g of sodium citrate, dissolving the sodium alginate and the sodium citrate in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 3h under the stirring condition, then adding 9.0g of ethylenediamine, and reacting for 2h at the temperature of 25 ℃ to prepare a solution I;
(2) dripping the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuing stirring for 20 minutes after dripping; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
Example 6 differs from example 1 in that: citric acid was replaced with sodium citrate.
Example 7
Preparation of ion adsorbent:
(1) weighing 1.0g of sodium alginate and 1.0g of potassium citrate, dissolving the sodium alginate and the potassium citrate in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 3h under the stirring condition, then adding 9.0g of ethylenediamine, and reacting for 2h at the temperature of 25 ℃ to prepare a solution I;
(2) dripping the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuing stirring for 20 minutes after dripping; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
Example 7 differs from example 1 in that: citric acid was replaced with potassium citrate.
Example 8
Preparation of ion adsorbent:
(1) weighing 1.0g of sodium alginate and 1.0g of citric acid, dissolving in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 6h under the stirring condition, then adding 9.0g of ethylenediamine, and reacting for 2h at 25 ℃ to prepare a solution I;
(2) dripping the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuing stirring for 20 minutes after dripping; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
Example 8 differs from example 1 in that: and (3) replacing the activation time in the step (1) with 6h from 3 h.
Example 9
Preparation of ion adsorbent:
(1) weighing 1.0g of sodium alginate and 1.0g of citric acid, dissolving in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 3h under the stirring condition, then adding 9.0g of ethylenediamine, and reacting for 3h at 25 ℃ to prepare a solution I;
(2) dripping the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuing stirring for 20 minutes after dripping; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
Example 9 differs from example 1 in that: the amidation reaction time in step (1) was changed from 2h to 3 h.
Example 10
Preparation of ion adsorbent:
(1) weighing 1.0g of sodium alginate and 1.0g of citric acid, dissolving in 50mL of water, adding 0.25g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride and 0.15g of 0.15g N-hydroxysuccinimide for activation for 3h under the stirring condition, then adding 9.0g of ethylenediamine, and reacting for 2h at 50 ℃ to prepare a solution I;
(2) dripping the solution I into 0.2mol/L calcium nitrate solution at 25 ℃ under the stirring condition, and continuing stirring for 20 minutes after dripping; filtering, washing the solid product with deionized water, and then carrying out vacuum freeze drying to prepare the ion adsorbent.
Example 10 differs from example 1 in that: the amidation reaction temperature in step (1) was changed from 25 ℃ to 50 ℃.
Example 11
The ion adsorbents prepared in examples 1 to 10 were subjected to adsorption performance tests, and the obtained data are shown in tables 1 and 2:
TABLE 1 Experimental data for adsorption rate, adsorption capacity, and cyclability of the ion adsorbents of examples 1-5
TABLE 2 Experimental data for adsorption rate, adsorption capacity, and cyclability of the ion adsorbents of examples 6-10
Example 12
The experiment simulates a single metal ion environmental water sample, the adsorption performance of the ion adsorbent of example 1 is tested, and the obtained experimental data are shown in table 3:
the specific operation steps of the adsorption experiment are as follows:
(a) preparing each metal ion mother liquor with the concentration of 0.150mol/L, and then respectively diluting the mother liquor to 10-4mol/L、1.5×10-4mol/L、1.5×10-3mol/L、1.0×10-2mol/L、1.5×10-2mol/L；
(b) Measuring the actual concentration value of each prepared metal ion solution by using an inductively coupled plasma atomic emission spectrometer;
(c) respectively weighing 100mg of the ion adsorbent prepared in example 1, placing the ion adsorbent in 20mL of metal ion solution with each concentration prepared in the step (a), magnetically stirring for 3 hours, filtering, and detecting the concentration of the metal ions in the filtrate by using an inductively coupled plasma atomic emission spectrometer;
(d) the adsorption rate and the adsorption capacity of the ion adsorbent to the corresponding metal ions are calculated through the formula.
TABLE 3 adsorption parameters of the ion adsorbent of example 1 for adsorbing a single heavy metal ion water sample
Example 13
An environmental water sample containing metal ions was collected and then subjected to an adsorption performance test using the ion adsorbent of example 1, and the results obtained are shown in table 4:
the adsorption test comprises the following specific steps:
(a) collecting a water sample to be adsorbed: collecting water samples at certain depths (10-40 cm) of three different places in Yangtze river (Anhui Anqing section) by using a collecting bottle, and adjusting the pH value of the collected water samples to obtain water samples to be adsorbed in order to achieve a better adsorption effect;
wherein the adjusted pH is 1.0-8.0, preferably 4.0-7.0; the pH adjuster includes an inorganic acid such as hydrochloric acid, sulfuric acid, nitric acid, carbonic acid, or phosphoric acid, or an inorganic base such as sodium hydroxide, potassium hydroxide, or aqueous ammonia, preferably nitric acid or sodium hydroxide; in step (a) of this example, the adjusted pH was 5.5, and the pH adjusting agents were nitric acid and sodium hydroxide;
(b) measuring the concentration value of each metal ion by using an inductively coupled plasma atomic emission spectrometer;
(c) and (3) weighing 100mg of ion adsorbent, dispersing in 20mL of the water sample to be adsorbed in the step (a), filtering after 6h, and measuring the concentration of each metal ion in the filtrate by using an inductively coupled plasma atomic emission spectrometer, thereby calculating the adsorption rate of the adsorbent to each metal ion.
Table 4 adsorption parameters of the ion adsorbent of example 1 for adsorbing mixed heavy metal ions in an environmental water sample
Example 14
The ionic adsorbent of example 1 was recycled, and the parameters obtained are shown in table 5.
The specific operation of the cycling experiment was as follows: the adsorbent with the metal ions is added into the acid solution, and the metal ions are separated from the adsorbent through the protonation of the acid, so that the aim of recycling the adsorbent is fulfilled.
Wherein the acid is selected from hydrochloric acid, nitric acid, sulfuric acid, acetic acid, oxalic acid or a combination thereof, preferably nitric acid.
TABLE 5 Performance parameters for Recycling of the ion adsorbent of example 1
Examples 15 to 20
The procedure of example 1 was repeated to prepare ion adsorbents of examples 15 to 20 according to the raw material compositions listed in Table 6.
TABLE 6 raw material composition of ion adsorbents of examples 15 to 20
The ion adsorbents prepared in examples 15 to 20 were subjected to the same adsorption performance test as described above, and the results were similar to those of the ion adsorbent of example 1.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. The ion adsorbent is characterized by being obtained by carrying out amidation reaction on ethylenediamine, alginate and citrate.
2. The ion adsorbent of claim 1, wherein the ion adsorbent can adsorb at least one of lead ions, calcium ions, copper ions, mercury ions, chromium ions, zinc ions, iron ions, and magnesium ions in a solution;
preferably, the ion adsorbent is a calcium ion and/or magnesium ion adsorbent.
3. The ion adsorbent according to claim 1, wherein the concentration of calcium ion in the solution is 10-4mol/L～1.5×10-3mol/L, wherein the adsorption rate of the ion adsorbent to calcium ions at room temperature is 90-99.9% under the condition that the liquid-solid ratio of the solution to the ion adsorbent is 0.2L/g;
magnesium ion concentration in solution is 10-4mol/L～1.5×10-3And the mol/L is that under the condition that the liquid-solid ratio of the solution to the ion adsorbent is 0.2L/g, the adsorption rate of the ion adsorbent to magnesium ions at room temperature is 90-99%.
4. A method for preparing the ionic adsorbent of any one of claims 1 to 3, comprising amidating alginate and citrate with ethylenediamine.
5. Method according to claim 4, characterized in that it comprises at least the following steps:
(a) mixing a solution containing alginate, citrate and an activating agent with ethylenediamine for amidation reaction to obtain a solution I;
(b) dripping the solution I into an alkaline earth metal ion solution to obtain a mixture II;
(c) and (3) separating the solid in the obtained mixture II, washing and drying to obtain the ion adsorbent.
6. The method according to claim 5, wherein the alginate in step (a) is selected from at least one of sodium alginate, potassium alginate, alginic acid;
the citrate in the step (a) is at least one of sodium citrate, potassium citrate and citric acid;
the activating agents in step (a) are 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide;
preferably, the weight ratio of the alginate, the citrate, the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, the N-hydroxysuccinimide and the ethylenediamine in the step (a) is as follows:
alginate, namely citrate, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and ethylenediamine, wherein the weight ratio of the N-hydroxysuccinimide to the ethylenediamine is 0.2-2: 1: 0.22-0.28: 0.13-0.17: 8-10.
7. The process according to claim 5, wherein the reaction temperature of the amidation in the step (a) is 0 to 70 ℃, and the reaction time is more than 1 hour;
preferably, the reaction temperature of the amidation in the step (a) is 5-50 ℃, and the reaction time is 2-3 hours;
the solution containing alginate, citrate and an activating agent in the step (a) is obtained by mixing the solution containing alginate and citrate with the activating agent and then activating;
the activation is that the mixture is stirred for not less than 1 hour at the temperature of 0-70 ℃;
preferably, the activation is stirring for 3-6 hours at 5-50 ℃.
8. The method according to claim 5, wherein in the step (b), the solution I is dripped into the alkaline earth metal ion solution, and the mixture is stirred for more than 10 minutes at 0-50 ℃ to obtain a mixture II;
preferably, in the step (b), the solution I is dripped into the alkaline earth metal ion solution, and the mixture is stirred for 10 to 20 minutes at the temperature of 5 to 30 ℃ to obtain a mixture II;
preferably, the alkaline earth metal ion solution in step (b) is a calcium ion solution;
the drying in step (c) is vacuum freeze drying.
9. Use of the ion adsorbent of any one of claims 1 to 3, the ion adsorbent prepared according to the method of any one of claims 4 to 8, for removing calcium ions and/or magnesium ions from a body of water.
10. The use according to claim 9, wherein the concentration of calcium ions in the water body is 0.0001-0.01 mol/L;
the concentration of magnesium ions in the water body is 0.0001-0.01 mol/L.
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