CN102702412A - Preparation technology of selective resin for removing trace nitrate ion in water - Google Patents
Preparation technology of selective resin for removing trace nitrate ion in water Download PDFInfo
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Abstract
The invention discloses a preparation technology of selective resin for removing trace nitrate ion in water and belongs to the field of preparation of organic high-molecular compound. The technology comprises the steps of respectively adding a water phase including purified water, a dispersing agent and a auxiliary dispersing agent and an oil phase including styrene, divinylbenzene, porogen and initiator to a polymerization reactor, carrying out suspension polymerization, and preparing the selective resin by chloromethylation and amination, wherein the porogen is mixed porogen prepared from 65-75 parts of toluene or benzene and 60-70 parts of white oil or isobutanol. By adopting the resin prepared from the mixed porogen, a hole structure inside the resin is improved, and the resin not only has proper specific surface area, but also has larger exchange capacity, and can remove the nitrate ion in the water by physical adsorption and chemical exchange methods at the same time, so that the selectivity on the nitrate ion is larger and trace nitrate ion in the water can be effectively removed.
Description
Technical field
The invention belongs to the preparation field of organic high molecular compound, be specifically related to a kind of preparation technology who removes the selective resin of micro-nitrate ion in the water.
Background technology
The Along with people's growth in the living standard, increasingly high to the requirement of safety of drinking water property.When the content of nitrate radical in the tap water is 90～140mg/l, promptly might cause the baby to suffer from methemoglobinemia, make red blood corpuscle not be with oxygen and cause the baby to suffocate.In view of the harm of nitrate radical, it all is that nitrate radical defines the highest concentration that exists in the tap water that the environment protection of various countries is organized.The maximum concentration of nitrate radical must not surpass 10mg/l in the Environmental Protection Agency regulation tap water; The maximum concentration of nitrate radical must not surpass 11.3mg/l in European Union's regulation tap water.
Remove that the method for nitrate ion mainly contains physico-chemical processes, chemical method, biological process and absorption method etc. in the water.Chemical method is the nitrate salt that utilizes in certain reductive agent reductive water; Biological process is to utilize denitrifying bacteria that nitrate salt is degraded to the bioprocess of nitrogen, though this method cost is lower, because of the changeable and difficult realization of waste water composition; Absorption method is the nitrate radical that utilizes in the adsorbents adsorb water, has fast, equipment is simple, reliable, can recycle advantages such as nitrate radical resource simultaneously, but effect is unsatisfactory.
Physico-chemical processes mainly refers to ion exchange method, and ion exchange resin is a kind of reticular polymer polyelectrolyte with active function group, can carry out the reversibility chemisorption with the ion in the water.Resin is different to various ionic exchange capacities, and some ions are easy to absorption, and other ions but are difficult to absorption.In addition, resin is relevant to the concentration of ionic selectivity and solution, cross-linkage of resin etc.
At present, it is relatively ripe that IX is applied to the tap water denitration technology, become one of main means of tap water denitration.But existing ion exchange resin is not ideal to the removal effect of nitrate radical, especially in the water nitrate ion content hour, removal effect is relatively poor.
Summary of the invention
The technical problem that the present invention will solve is: overcome the deficiency of prior art, a kind of preparation technology who removes the selective resin of micro-nitrate ion in the water is provided, but adopt the nitrate ion of trace in the resin effective elimination water of this prepared.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of preparation technology who removes the selective resin of micro-nitrate ion in the water is characterized in that, comprises following process step:
1) polymerization: the oil phase that will comprise the water of pure water, dispersion agent, dispersion aids and comprise vinylbenzene, divinylbenzene, pore-creating agent, initiator adds polymerization reaction kettle respectively; Carry out suspension polymerization; Make the matrix polymer of resin, wherein said water is formed and mass fraction is:
500～600 parts of pure water
3～4 parts of dispersion agents
40～50 parts of dispersion aidss
Described oil phase is formed and mass fraction is:
70～75 parts of vinylbenzene
24～30 parts of divinylbenzenes
125～145 parts of pore-creating agents
0.8～1 part of initiator;
Wherein, described pore-creating agent mixes pore-creating agent by what 65～75 parts toluene or benzene and 60～70 parts white oil or isopropylcarbinol were formed;
2) chloromethylation: 100 parts of matrix polymers that makes in the step 1) and chloromethylation reagent are added in the exsiccant reaction kettle for 400～600 parts, swelling 1～3 hour, then; Add lewis acid catalyst in batches; Be warming up to 35～50 ℃, be incubated 12～28 hours, make the chloromethylation Archon;
3) in 100 parts of adding reaction kettles of the chloromethylation Archon that makes amination: with step 2); Add 100～300 parts of swellings of swelling agent 1～3 hour, and slowly added aminating agent then, be warming up to 50～80 ℃; Be incubated 24～36 hours, make the selective resin that removes micro-nitrate ion in the water.
Preferably, described water also comprises 1～5 part of methylene blue in forming.
Preferably, described dispersion agent is technical gelatine or Z 150PH; Described dispersion aids is one or more in sal epsom, yellow soda ash, Sodium phosphate, dibasic and the tsp; Described initiator is Diisopropyl azodicarboxylate or Lucidol.
Preferably, the chloromethylation reagent step 2) is chloromethyl ether; Described lewis acid catalyst is Zinc Chloride Anhydrous or aluminum trichloride (anhydrous).
Preferably, the swelling agent described in the step 3) is methyl alcohol or ethanol; Described aminating agent is a tripropyl amine.
Preferably, in the step 3), swelling time is 1.5 hours in the reaction kettle, slowly is warming up to 45 ℃, is incubated 20 hours.
Preferably, in the step 3), swelling time is 2 hours in the reaction kettle, slowly is warming up to 65 ℃, is incubated 30 hours.
This invention adopts the mixing pore-creating agent to prepare ion exchange resin; Improved the inner pore structure of resin; Not only have suitable specific surface area, and have bigger exchange capacity, can remove the nitrate ion in the water through physical adsorption and two kinds of methods of chemical exchange simultaneously; Therefore bigger to the selectivity of nitrate ion, but the nitrate ion of trace in the effective elimination water.
Embodiment
Below in conjunction with embodiment, the present invention done further describing:
Embodiment 1
1) polymerization: in 2 liters polymerization reaction kettle, add 600 parts of pure water; Under agitation condition, add 3 parts of gelatin successively, 24 parts of sal epsom, 16 parts of yellow soda ash; Be warming up to 50 ℃ then; Add 3 parts of methylene blues, stop to stir, add by 70 parts of vinylbenzene, 30 parts of divinylbenzenes, 65 parts of toluene, 60 parts of white oils, 0.7 part of oil phase that Lucidol mixes.The capping still is opened and is stirred, and liquid bead degree is transferred to 0.125～0.8mm, is warming up to 79 ℃, is incubated 2 hours, is warming up to 85 ℃, is incubated 4 hours, is warming up to 95 ℃, is incubated 6 hours.Washing, dry, sieve the Archon of 0.315～0.71mm.
2) chloromethylation: 500 parts of 100 parts of the Archons that makes in the step 1) and chloromethyl ethers are joined in 2 liters the reaction kettle, swelling was divided 3 times and is added Zinc Chloride Anhydrous after 1.5 hours, and each 12 parts, each 0.5h at interval.Slowly be warming up to 45 ℃ then, be incubated 20 hours.Be cooled to room temperature, control siccative liquid makes the chloromethylation Archon.
3) in the reaction kettle that 100 parts and 200 parts methyl alcohol inputs of the chloromethylation Archon that makes amination: with step 2) are 2 liters, swelling 2 hours.Slowly add 400 parts of tripropyl amines, be warming up to 65 ℃ then, be incubated 30 hours, be cooled to room temperature, washing makes the selective resin that removes micro-nitrate ion in the water, and its performance index are seen table 1.
Embodiment 2
1) polymerization: in 2 liters polymerization reaction kettle, add 500 parts of pure water; Under agitation condition, add 3.5 parts of Z 150PH successively, 30 parts of Sodium phosphate, dibasics, 15 parts of tsps; Be warming up to 50 ℃ then; Add 2 parts of methylene blues, stop to stir, add by 75 parts of vinylbenzene, 25 parts of divinylbenzenes, 70 parts of toluene, 60 parts of isopropylcarbinols, 0.8 part of oil phase that Diisopropyl azodicarboxylate mixes.The capping still is opened and is stirred, and liquid bead degree is transferred to 0.125～0.8mm, is warming up to 79 ℃, is incubated 2 hours, is warming up to 85 ℃, is incubated 4 hours, is warming up to 95 ℃, is incubated 6 hours.Washing, dry, sieve the Archon of 0.315～0.71mm.
2) chloromethylation: 400 parts of 100 parts of the Archons that makes in the step 1) and chloromethyl ethers are joined in 2 liters the reaction kettle, swelling was divided 3 times and is added Zinc Chloride Anhydrous after 1 hour, and each 12 parts, each 0.5h at interval.Slowly be warming up to 40 ℃ then, be incubated 14 hours.Be cooled to room temperature, control siccative liquid makes the chloromethylation Archon.
3) in the reaction kettle that 100 parts and 100 parts methyl alcohol inputs of the chloromethylation Archon that makes amination: with step 2) are 2 liters, swelling 1 hour.Slowly add 400 parts of tripropyl amines then, be warming up to 55 ℃ then, be incubated 26 hours, be cooled to room temperature, washing makes the selective resin that removes micro-nitrate ion in the water, and the performance index of the selective resin that obtains are seen table 1.
Embodiment 3
1) polymerization: in 2 liters polymerization reaction kettle, add 600 parts of pure water; Under agitation condition, add 4 parts of Z 150PH successively, 30 parts of sal epsom, 20 parts of yellow soda ash; Be warming up to 50 ℃ then; Add 4 parts of methylene blues, stop to stir, add by 75 parts of vinylbenzene, 30 parts of divinylbenzenes, 75 parts of benzene, 70 parts of white oils, 1 part of oil phase that Lucidol mixes.The capping still is opened and is stirred, and liquid bead degree is transferred to 0.125～0.8mm, is warming up to 79 ℃, is incubated 2 hours, is warming up to 85 ℃, is incubated 4 hours, is warming up to 95 ℃, is incubated 6 hours.Washing, dry, sieve the Archon of 0.315～0.71mm.
2) chloromethylation: 600 parts of 100 parts of the Archons that makes in the step 1) and chloromethyl ethers are joined in 2 liters the reaction kettle, swelling was divided 3 times and is added Zinc Chloride Anhydrous after 3 hours, and each 12 parts, each 0.5h at interval.Slowly be warming up to 50 ℃ then, be incubated 28 hours.Be cooled to room temperature, control siccative liquid makes the chloromethylation Archon.
3) in the reaction kettle that 100 parts and 300 parts methyl alcohol inputs of the chloromethylation Archon that makes amination: with step 2) are 2 liters, swelling 3 hours.Slowly add 400 parts of tripropyl amines then, be warming up to 80 ℃ then, be incubated 36 hours, be cooled to room temperature, washing makes the selective resin that removes micro-nitrate ion in the water, and the performance index of the selective resin that obtains are seen table 1.
Embodiment 4
1) polymerization: in 2 liters polymerization reaction kettle, add 550 parts of pure water; Under agitation condition, add 3.5 parts of gelatin successively, 25 parts of Sodium phosphate, dibasics, 20 parts of tsps; Be warming up to 50 ℃ then; Add 3 parts of methylene blues, stop to stir, add by 75 parts of vinylbenzene, 26 parts of divinylbenzenes, 70 parts of benzene, 65 parts of isopropylcarbinols, 1 part of oil phase that Lucidol mixes.The capping still is opened and is stirred, and liquid bead degree is transferred to 0.125～0.8mm, is warming up to 79 ℃, is incubated 2 hours, is warming up to 85 ℃, is incubated 4 hours, is warming up to 95 ℃, is incubated 6 hours.Washing, dry, sieve the Archon of 0.315～0.71mm.
2) chloromethylation: 550 parts of 100 parts of the Archons that makes in the step 1) and chloromethyl ethers are joined in 2 liters the reaction kettle, swelling was divided 3 times and is added Zinc Chloride Anhydrous after 3 hours, and each 12 parts, each 0.5h at interval.Slowly be warming up to 40 ℃ then, be incubated 18 hours.Be cooled to room temperature, control siccative liquid makes the chloromethylation Archon.
3) in the reaction kettle that 100 parts and 300 parts methyl alcohol inputs of the chloromethylation Archon that makes amination: with step 2) are 2 liters, swelling 3 hours.Slowly add 400 parts of tripropyl amines then, be warming up to 70 ℃ then, be incubated 32 hours, be cooled to room temperature, washing makes the selective resin that removes micro-nitrate ion in the water, and the performance index of the selective resin that obtains are seen table 1.
Embodiment 5
1) polymerization: in 2 liters polymerization reaction kettle, add 600 parts of pure water; Under agitation condition, add 4 parts of Z 150PH successively, 25 parts of sal epsom, 15 parts of yellow soda ash; Be warming up to 50 ℃ then; Add 2 parts of methylene blues, stop to stir, add by 70 parts of vinylbenzene, 25 parts of divinylbenzenes, 65 parts of benzene, 60 parts of white oils, 0.8 part of oil phase that Lucidol mixes.The capping still is opened and is stirred, and liquid bead degree is transferred to 0.125～0.8mm, is warming up to 79 ℃, is incubated 2 hours, is warming up to 85 ℃, is incubated 4 hours, is warming up to 95 ℃, is incubated 6 hours.Washing, dry, sieve the Archon of 0.315～0.71mm.
2) chloromethylation: 600 parts of 100 parts of the Archons that makes in the step 1) and chloromethyl ethers are joined in 2 liters the reaction kettle, swelling was divided 3 times and is added Zinc Chloride Anhydrous after 1 hour, and each 12 parts, each 0.5h at interval.Slowly be warming up to 38 ℃ then, be incubated 12 hours.Be cooled to room temperature, control siccative liquid makes the chloromethylation Archon.
3) in the reaction kettle that 100 parts and 200 parts methyl alcohol inputs of the chloromethylation Archon that makes amination: with step 2) are 2 liters, swelling 2 hours.Slowly add 400 parts of tripropyl amines then, be warming up to 50 ℃ then, be incubated 36 hours, be cooled to room temperature, washing makes the selective resin that removes micro-nitrate ion in the water, and the performance index of the selective resin that obtains are seen table 1.
Embodiment 6
1) polymerization: in 2 liters polymerization reaction kettle, add 550 parts of pure water; Under agitation condition, add 3.5 parts of Z 150PH successively, 25 parts of sal epsom, 20 parts of yellow soda ash; Be warming up to 50 ℃ then; Add 4 parts of methylene blues, stop to stir, add by 73 parts of vinylbenzene, 27 parts of divinylbenzenes, 70 parts of benzene, 65 parts of white oils, 0.9 part of oil phase that Lucidol mixes.The capping still is opened and is stirred, and liquid bead degree is transferred to 0.125～0.8mm, is warming up to 79 ℃, is incubated 2 hours, is warming up to 85 ℃, is incubated 4 hours, is warming up to 95 ℃, is incubated 6 hours.Washing, dry, sieve the Archon of 0.315～0.71mm.
2) chloromethylation: 500 parts of 100 parts of the Archons that makes in the step 1) and chloromethyl ethers are joined in 2 liters the reaction kettle, swelling was divided 3 times and is added Zinc Chloride Anhydrous after 2 hours, and each 12 parts, each 0.5h at interval.Slowly be warming up to 45 ℃ then, be incubated 20 hours.Be cooled to room temperature, control siccative liquid makes the chloromethylation Archon.
3) in the reaction kettle that 100 parts and 300 parts methyl alcohol inputs of the chloromethylation Archon that makes amination: with step 2) are 2 liters, swelling 2 hours.Slowly add 400 parts of tripropyl amines then, be warming up to 65 ℃ then, be incubated 30 hours, be cooled to room temperature, washing makes the selective resin that removes micro-nitrate ion in the water, and the performance index of the selective resin that obtains are seen table 1.
Embodiment 7
1) polymerization: in 2 liters polymerization reaction kettle, add 600 parts of pure water; Under agitation condition, add 4 parts of gelatin successively, 25 parts of sal epsom, 15 parts of yellow soda ash; Be warming up to 50 ℃ then; Add 2 parts of methylene blues, stop to stir, add by 75 parts of vinylbenzene, 25 parts of divinylbenzenes, 65 parts of toluene, 60 parts of white oils, 0.85 part of oil phase that Lucidol mixes.The capping still is opened and is stirred, and liquid bead degree is transferred to 0.125～0.8mm, is warming up to 79 ℃, is incubated 2 hours, is warming up to 85 ℃, is incubated 4 hours, is warming up to 95 ℃, is incubated 6 hours.Washing, dry, sieve the Archon of 0.315～0.71mm.
2) chloromethylation: 600 parts of 100 parts of the Archons that makes in the step 1) and chloromethyl ethers are joined in 2 liters the reaction kettle, swelling was divided 3 times and is added Zinc Chloride Anhydrous after 1 hour, and each 12 parts, each 0.5h at interval.Slowly be warming up to 38 ℃ then, be incubated 12 hours.Be cooled to room temperature, control siccative liquid makes the chloromethylation Archon.
3) in the reaction kettle that 100 parts and 300 parts ethanol inputs of the chloromethylation Archon that makes amination: with step 2) are 2 liters, swelling 2 hours.Slowly add 400 parts of tripropyl amines then, be warming up to 65 ℃ then, be incubated 36 hours, be cooled to room temperature, washing makes the selective resin that removes micro-nitrate ion in the water, and the performance index of the selective resin that obtains are seen table 1.
Product of the present invention shows the selectivity experiment of nitrate radical; Product of the present invention has absorption property preferably to nitrate radical; The loading capacity that penetrates to nitrate radical is 74.5mg/ml (influent concentration is 90mg/l, when being 10mg/l to go out water concentration as breakthrough point) to the maximum, compared with similar products; Have the higher penetrating loading capacity, this shows that product of the present invention has micro-nitrate radical in the water to remove performance preferably.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any professional and technical personnel of being familiar with possibly utilize the technology contents of above-mentioned announcement to change to the equivalent embodiment of equivalent variations.But everyly do not break away from technical scheme content of the present invention, to any simple modification, equivalent variations that above embodiment did, still belong to the protection domain of technical scheme of the present invention according to technical spirit of the present invention.
Table 1: the performance index that remove the selective resin of micro-nitrate ion in the water
Annotate: penetrating adsorptive capacity is that influent concentration is 90mg/l, is the loading capacity of 10mg/l during as breakthrough point to go out water concentration.
Claims (7)
1. a preparation technology who removes the selective resin of micro-nitrate ion in the water is characterized in that, comprises following process step:
1) polymerization: the oil phase that will comprise the water of pure water, dispersion agent, dispersion aids and comprise vinylbenzene, divinylbenzene, pore-creating agent, initiator adds polymerization reaction kettle respectively; Carry out suspension polymerization; Make the matrix polymer of resin, wherein said water is formed and mass fraction is:
500～600 parts of pure water
3～4 parts of dispersion agents
40～50 parts of dispersion aidss
Described oil phase is formed and mass fraction is:
70～75 parts of vinylbenzene
24～30 parts of divinylbenzenes
125～145 parts of pore-creating agents
0.8～1 part of initiator;
Wherein, described pore-creating agent mixes pore-creating agent by what 65～75 parts toluene or benzene and 60～70 parts white oil or isopropylcarbinol were formed;
2) chloromethylation: 100 parts of matrix polymers that makes in the step 1) and chloromethylation reagent are added in the exsiccant reaction kettle for 400～600 parts, swelling 1～3 hour, then; Add lewis acid catalyst in batches; Be warming up to 35～50 ℃, be incubated 12～28 hours, make the chloromethylation Archon;
3) in 100 parts of adding reaction kettles of the chloromethylation Archon that makes amination: with step 2); Added 100～300 parts of swellings of swelling agent 1～3 hour; Slowly add aminating agent then, be warming up to 50～80 ℃, be incubated 24～36 hours; Cooling, washing make the selective resin that removes micro-nitrate ion in the water.
2. the preparation technology who removes the selective resin of micro-nitrate ion in the water according to claim 1 is characterized in that: described water also comprises 1～5 part of methylene blue in forming.
3. the preparation technology who removes the selective resin of micro-nitrate ion in the water according to claim 1 and 2 is characterized in that: described dispersion agent is technical gelatine or Z 150PH; Described dispersion aids is one or more in sal epsom, yellow soda ash, Sodium phosphate, dibasic and the tsp; Described initiator is Diisopropyl azodicarboxylate or Lucidol.
4. the preparation technology who removes the selective resin of micro-nitrate ion in the water according to claim 3 is characterized in that: step 2) described in chloromethylation reagent be chloromethyl ether; Described lewis acid catalyst is Zinc Chloride Anhydrous or aluminum trichloride (anhydrous).
5. the preparation technology who removes the selective resin of micro-nitrate ion in the water according to claim 4 is characterized in that: the swelling agent described in the step 3) is methyl alcohol or ethanol; Described aminating agent is a tripropyl amine.
6. the preparation technology who removes the selective resin of micro-nitrate ion in the water according to claim 5 is characterized in that: in the step 3), swelling time is 1.5 hours in the reaction kettle, slowly is warming up to 45 ℃, is incubated 20 hours.
7. the preparation technology who removes the selective resin of micro-nitrate ion in the water according to claim 5 is characterized in that: in the step 3), swelling time is 2 hours in the reaction kettle, slowly is warming up to 65 ℃, is incubated 30 hours.
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| CN103447089A (en) * | 2013-09-18 | 2013-12-18 | 凯瑞化工股份有限公司 | Low-carbon olefine oligomerization catalyst and preparation method thereof |
| CN104959170A (en) * | 2015-06-11 | 2015-10-07 | 东南大学 | Easily regenerable nitrate radical selective ion exchange resin and preparation method thereof |
| CN105273138A (en) * | 2015-11-25 | 2016-01-27 | 蚌埠市天星树脂有限责任公司 | Super-large specific surface area adsorbent resin and preparation method thereof |
| CN110639624A (en) * | 2019-10-11 | 2020-01-03 | 丹东明珠特种树脂有限公司 | Anion and cation exchange resin for purifying caprolactam production wastewater and wastewater purification method |
| CN112742356A (en) * | 2020-12-15 | 2021-05-04 | 蚌埠市天星树脂有限责任公司 | Adsorption resin for treating waste water and gas and preparation method thereof |
| CN113101902A (en) * | 2021-04-13 | 2021-07-13 | 北京赛科康仑环保科技有限公司 | Adsorption material for acidic phosphate extraction system, preparation method and application |
| CN113501901A (en) * | 2021-07-23 | 2021-10-15 | 核工业北京化工冶金研究院 | Preparation method of uranium-adsorbing strongly-basic resin with narrow distribution particle size |
| CN113773420A (en) * | 2021-08-04 | 2021-12-10 | 江苏金杉新材料有限公司 | Preparation method of nitrate radical adsorption resin |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103447089A (en) * | 2013-09-18 | 2013-12-18 | 凯瑞化工股份有限公司 | Low-carbon olefine oligomerization catalyst and preparation method thereof |
| CN104959170A (en) * | 2015-06-11 | 2015-10-07 | 东南大学 | Easily regenerable nitrate radical selective ion exchange resin and preparation method thereof |
| CN105273138A (en) * | 2015-11-25 | 2016-01-27 | 蚌埠市天星树脂有限责任公司 | Super-large specific surface area adsorbent resin and preparation method thereof |
| CN110639624A (en) * | 2019-10-11 | 2020-01-03 | 丹东明珠特种树脂有限公司 | Anion and cation exchange resin for purifying caprolactam production wastewater and wastewater purification method |
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| CN112742356A (en) * | 2020-12-15 | 2021-05-04 | 蚌埠市天星树脂有限责任公司 | Adsorption resin for treating waste water and gas and preparation method thereof |
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| CN113501901A (en) * | 2021-07-23 | 2021-10-15 | 核工业北京化工冶金研究院 | Preparation method of uranium-adsorbing strongly-basic resin with narrow distribution particle size |
| CN113501901B (en) * | 2021-07-23 | 2023-11-28 | 核工业北京化工冶金研究院 | Preparation method of strong alkaline resin with narrow-distribution particle size for adsorbing uranium |
| CN113773420A (en) * | 2021-08-04 | 2021-12-10 | 江苏金杉新材料有限公司 | Preparation method of nitrate radical adsorption resin |
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Application publication date: 20121003 |