CN107537452A - A kind of ion exchange resin preparation method for Treating Municipal Sewage - Google Patents
A kind of ion exchange resin preparation method for Treating Municipal Sewage Download PDFInfo
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- CN107537452A CN107537452A CN201710793740.9A CN201710793740A CN107537452A CN 107537452 A CN107537452 A CN 107537452A CN 201710793740 A CN201710793740 A CN 201710793740A CN 107537452 A CN107537452 A CN 107537452A
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- prefabricated material
- ion exchange
- exchange resin
- municipal sewage
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Abstract
The invention discloses a kind of ion exchange resin preparation method for Treating Municipal Sewage, comprise the following steps:Macropore chloromethylated polystyrene resin is sent into the piperazine aqueous solution and is swelled, adds 2 aminoethyle alcohols, is heated up, is stirred, cooling, washing obtains the first prefabricated material;Chitosan, propionic acid are well mixed, water is added and stirs, polyethylene glycol is added, heating stirring, heating, adds locust bean gum, the first prefabricated material, calcining coconut shell flour stirring, filter, washing, be dried to obtain the second prefabricated material;In ice-water bath, thionyl chloride is added dropwise into the second prefabricated material, adjusts temperature, is incubated, cools, washs, filtering, is sent into N, is swelled in N dimethylformamides, adds trimethylamine and reacts to obtain the ion exchange resin for Treating Municipal Sewage.
Description
Technical field
The present invention relates to ion-exchange resin technique field, more particularly to a kind of ion exchange for Treating Municipal Sewage
Process for preparing resins.
Background technology
Water is Source of life, is the most valuable resource of nature.Protection, utilization and the processing of water resource are in the world today
One of most popular topic.Therefore, the research work in the world about water quality and water technology have developed rapidly, from Industry Waste
The significant problem that the pollution of water and sanitary wastewater and country face.China is one of country that water resource lacks in the world, water
The exploitation of matter and water technology has very big development, very big contribution is made that to environmental protection, water saving shield water, using ion
Exchanger resin increasingly becomes main flow for handling sewage.
In recent years, the rate of economic development in China city is relatively fast, in city produce and live caused by sewage quantity
Also gradually increasing, current ion exchange resin adsorption capacity does not reach demand increasingly, in view of the above-mentioned problems, improving resin
Adsorption capacity, improve municipal sewage treatment efficiency, it would be highly desirable to solve.
The content of the invention
Based on technical problem existing for background technology, the present invention proposes a kind of ion exchange for Treating Municipal Sewage
Process for preparing resins, the gained ion exchange resin rate of adsorption is fast, and selectivity is high, is firmly combined between carrier, can after absorption
Elution is complete, and easily desorbs, regenerates, and can realize repeatedly, recycle.
A kind of ion exchange resin preparation method for Treating Municipal Sewage proposed by the present invention, comprises the following steps:
It S1, will be swelled in the macropore chloromethylated polystyrene resin feeding piperazine aqueous solution, add 2 hydroxy ethylamine, rise
Temperature, stir, cooling, washing obtains the first prefabricated material;
S2, chitosan, propionic acid be well mixed, add water and stir, added polyethylene glycol, heating stirring, heating, add
Enter locust bean gum, the first prefabricated material, calcining coconut shell flour stirring, filter, washing, be dried to obtain the second prefabricated material;
S3, in ice-water bath, be added dropwise thionyl chloride into the second prefabricated material, adjust temperature, be incubated, cool, washing, mistake
Filter, it is sent into DMF and is swelled, adds trimethylamine and react to obtain the amberlite for Treating Municipal Sewage
Fat.
Preferably, in S1, it is in the 34-38wt% piperazine aqueous solution that macropore chloromethylated polystyrene resin is sent into concentration
3-6h is swelled, adds 2 hydroxy ethylamine, is warming up to 60-80 DEG C, stirs 10-16h, cooling, washing obtains the first prefabricated material.
Preferably, in S1, it is dense that 50-60 part macropore chloromethylated polystyrenes resin is sent into 150-180 parts by weight
Spend to be swelled 3-6h in the 34-38wt% piperazine aqueous solution, add 1-2 part 2 hydroxy ethylamines, be warming up to 60-80 DEG C, stir 10-
16h, cooling, washing obtain the first prefabricated material.
Preferably, in S2, chitosan, propionic acid are well mixed, water is added and stirs, add polyethylene glycol, be warming up to
92-98 DEG C of stirring 4-6h, is warming up to 105-112 DEG C, adds locust bean gum, the first prefabricated material, calcining coconut shell flour stirring 40-
100min, mixing speed 640-700r/min, filter, washing, be dried to obtain the second prefabricated material.
Preferably, in S2,5-10 parts chitosan, 1-2 part propionic acid are well mixed by weight, 20-40 part water is added and stirs
Mix uniformly, add 50-80 part polyethylene glycol, be warming up to 92-98 DEG C of stirring 4-6h, be warming up to 105-112 DEG C, add 10-16 parts
Locust bean gum, the first prefabricated material of 20-40 parts, the calcining coconut shell flour stirring of 1-6 parts 40-100min, mixing speed 640-700r/
Min, filter, washing, be dried to obtain the second prefabricated material.
Preferably, in S3, in ice-water bath, thionyl chloride is added dropwise into the second prefabricated material, adjusts the temperature to 80-90 DEG C,
2-4h is incubated, is cooled, is washed, filtering, is sent into DMF and is swelled 4-8h, trimethylamine reaction 5-10h is added, obtains
To the ion exchange resin for Treating Municipal Sewage.
Preferably, in S3, in ice-water bath, 3-5 part protochlorides are added dropwise by weight into the second prefabricated material of 60-80 parts
Sulfone, 80-90 DEG C is adjusted the temperature to, be incubated 2-4h, cooled, washed, filtering, is sent into 150-240 part DMFs
4-8h is swelled, 4-10 parts trimethylamine reaction 5-10h is added, obtains the ion exchange resin for Treating Municipal Sewage.
The present invention has bigger serface and high porosity, the Sewage Environment of complexity can be dealt with, suitable for sewage disposal.This
Invention is dissolved chitosan in propionic acid, the three-dimensional net structure formed with polyethylene glycol due to hydrogen bond action, not only lubricity
It is good, and preparation process it is green, it is pollution-free, without discharge, can effectively promote between locust bean gum and the first prefabricated material, calcining coconut shell flour
Scattered, mutual combination degree is high, and soft plasticity is good, and water-retaining property is strong, and shrinkage factor is small, and specific surface area is high, and absorption is lived
Property it is high, make that gained resin specific surface area is high, and uniform pore diameter is suitable, significantly improves exchange capacity, to heavy metal ions in sewage
Adsorption activity it is high, it is environment-friendly.
The gained ion exchange resin rate of adsorption of the invention is fast, and selectivity is high, is firmly combined between carrier, can after absorption
Elution is complete, and easily desorbs, regenerates, and can realize repeatedly, recycle;Performance survey is carried out to gained ion exchange resin
It is fixed:Its full exchange capacity is 3.05-3.14mmol/g, and adsorption capacity reduced by only 1.22-1.85% after regenerating ten times, after processing
Water can reach drinking water standard (GB5749-2011).
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of ion exchange resin preparation method for Treating Municipal Sewage, comprise the following steps:
It S1, will be swelled in the macropore chloromethylated polystyrene resin feeding piperazine aqueous solution, add 2 hydroxy ethylamine, rise
Temperature, stir, cooling, washing obtains the first prefabricated material;
S2, chitosan, propionic acid be well mixed, add water and stir, added polyethylene glycol, heating stirring, heating, add
Enter locust bean gum, the first prefabricated material, calcining coconut shell flour stirring, filter, washing, be dried to obtain the second prefabricated material;
S3, in ice-water bath, be added dropwise thionyl chloride into the second prefabricated material, adjust temperature, be incubated, cool, washing, mistake
Filter, it is sent into DMF and is swelled, adds trimethylamine and react to obtain the amberlite for Treating Municipal Sewage
Fat.
Embodiment 2
A kind of ion exchange resin preparation method for Treating Municipal Sewage, comprise the following steps:
S1,50 parts of macropore chloromethylated polystyrene resins are sent into 180 parts of concentration by weight is 34wt% piperazine water
6h is swelled in solution, adds 1 part of 2 hydroxy ethylamine, is warming up to 80 DEG C, stirs 10h, cooling, washing obtains the first prefabricated material;
S2,10 parts of chitosans, 1 part of propionic acid are well mixed by weight, add 40 parts of water and stir, added 50 parts and gather
Ethylene glycol, 98 DEG C of stirring 4h are warming up to, are warming up to 112 DEG C, add 10 parts of locust bean gums, 40 part of first prefabricated material, 1 part of calcining coconut palm
Shell powder stirs 100min, mixing speed 640r/min, filters, and washing, is dried to obtain the second prefabricated material;
S3, in ice-water bath, by weight into 80 part of second prefabricated material be added dropwise 3 parts of thionyl chlorides, adjust the temperature to 90
DEG C, 2h is incubated, is cooled, is washed, filtering, is sent into 240 parts of DMFs and is swelled 4h, adds 10 parts of trimethylamine reactions
5h, obtain the ion exchange resin for Treating Municipal Sewage.
Embodiment 3
A kind of ion exchange resin preparation method for Treating Municipal Sewage, comprise the following steps:
S1,60 parts of macropore chloromethylated polystyrene resins are sent into 150 parts of concentration by weight is 38wt% piperazine water
3h is swelled in solution, adds 2 parts of 2 hydroxy ethylamines, is warming up to 60 DEG C, stirs 16h, cooling, washing obtains the first prefabricated material;
S2,5 parts of chitosans, 2 parts of propionic acid are well mixed by weight, add 20 parts of water and stir, added 80 parts and gather
Ethylene glycol, 92 DEG C of stirring 6h are warming up to, are warming up to 105 DEG C, add 16 parts of locust bean gums, 20 part of first prefabricated material, 6 parts of calcining coconut palms
Shell powder stirs 40min, mixing speed 700r/min, filters, and washing, is dried to obtain the second prefabricated material;
S3, in ice-water bath, by weight into 60 part of second prefabricated material be added dropwise 5 parts of thionyl chlorides, adjust the temperature to 80
DEG C, 4h is incubated, is cooled, is washed, filtering, is sent into 150 parts of DMFs and is swelled 8h, adds 4 parts of trimethylamine reactions
10h, obtain the ion exchange resin for Treating Municipal Sewage.
Embodiment 4
A kind of ion exchange resin preparation method for Treating Municipal Sewage, comprise the following steps:
S1,52 parts of macropore chloromethylated polystyrene resins are sent into 170 parts of concentration by weight is 35wt% piperazine water
5h is swelled in solution, adds 1.2 parts of 2 hydroxy ethylamines, is warming up to 75 DEG C, stirs 12h, cooling, washing obtains the first prefabricated material;
S2,8 parts of chitosans, 1.2 parts of propionic acid are well mixed by weight, add 35 parts of water and stir, add 60 parts
Polyethylene glycol, be warming up to 96 DEG C of stirring 4.5h, be warming up to 110 DEG C, add 12 parts of locust bean gums, 35 part of first prefabricated material, 2 parts forge
Coconut shell flour stirring 80min, mixing speed 660r/min are burnt, filters, washing, is dried to obtain the second prefabricated material;
S3, in ice-water bath, by weight into 75 part of second prefabricated material be added dropwise 3.5 parts of thionyl chlorides, adjust the temperature to
88 DEG C, 2.5h is incubated, is cooled, is washed, filtering, is sent into 220 parts of DMFs and is swelled 5h, adds 8 parts of trimethylamines
6h is reacted, obtains the ion exchange resin for Treating Municipal Sewage.
Embodiment 5
A kind of ion exchange resin preparation method for Treating Municipal Sewage, comprise the following steps:
S1,58 parts of macropore chloromethylated polystyrene resins are sent into 160 parts of concentration by weight is 37wt% piperazine water
4h is swelled in solution, adds 1.8 parts of 2 hydroxy ethylamines, is warming up to 65 DEG C, stirs 14h, cooling, washing obtains the first prefabricated material;
S2,6 parts of chitosans, 1.8 parts of propionic acid are well mixed by weight, add 25 parts of water and stir, add 70 parts
Polyethylene glycol, be warming up to 94 DEG C of stirring 5.5h, be warming up to 106 DEG C, add 14 parts of locust bean gums, 25 part of first prefabricated material, 4 parts forge
Coconut shell flour stirring 60min, mixing speed 680r/min are burnt, filters, washing, is dried to obtain the second prefabricated material;
S3, in ice-water bath, by weight into 65 part of second prefabricated material be added dropwise 4.5 parts of thionyl chlorides, adjust the temperature to
82 DEG C, 3.5h is incubated, is cooled, is washed, filtering, is sent into 160 parts of DMFs and is swelled 7h, adds 6 parts of trimethylamines
8h is reacted, obtains the ion exchange resin for Treating Municipal Sewage.
Embodiment 6
A kind of ion exchange resin preparation method for Treating Municipal Sewage, comprise the following steps:
S1,55 parts of macropore chloromethylated polystyrene resins are sent into 165 parts of concentration by weight is 36wt% piperazine water
4.5h is swelled in solution, adds 1.5 parts of 2 hydroxy ethylamines, is warming up to 70 DEG C, stirs 13h, cooling, it is prefabricated that washing obtains first
Material;
S2,7 parts of chitosans, 1.5 parts of propionic acid are well mixed by weight, add 30 parts of water and stir, add 65 parts
Polyethylene glycol, 95 DEG C of stirring 5h are warming up to, are warming up to 108 DEG C, add 13 parts of locust bean gums, 30 part of first prefabricated material, 3 parts of calcinings
Coconut shell flour stirs 70min, mixing speed 670r/min, filters, and washing, is dried to obtain the second prefabricated material;
S3, in ice-water bath, by weight into 70 part of second prefabricated material be added dropwise 4 parts of thionyl chlorides, adjust the temperature to 85
DEG C, 3h is incubated, is cooled, is washed, filtering, is sent into 200 parts of DMFs and is swelled 6h, adds 7 parts of trimethylamine reactions
7h, obtain the ion exchange resin for Treating Municipal Sewage.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (7)
1. a kind of ion exchange resin preparation method for Treating Municipal Sewage, it is characterised in that comprise the following steps:
It S1, will be swelled in the macropore chloromethylated polystyrene resin feeding piperazine aqueous solution, add 2 hydroxy ethylamine, heating, stir
Mix, cool, washing obtains the first prefabricated material;
S2, chitosan, propionic acid be well mixed, add water and stir, added polyethylene glycol, heating stirring, heating, add thorn
Locust bean gum, the first prefabricated material, calcining coconut shell flour stirring, filter, washing, are dried to obtain the second prefabricated material;
S3, in ice-water bath, be added dropwise thionyl chloride into the second prefabricated material, adjust temperature, be incubated, cool, wash, filtering, send
Enter in DMF and be swelled, add trimethylamine and react to obtain the ion exchange resin for Treating Municipal Sewage.
2. it is used for the ion exchange resin preparation method of Treating Municipal Sewage according to claim 1, it is characterised in that S1
In, it is that 3-6h is swelled in the 34-38wt% piperazine aqueous solution that macropore chloromethylated polystyrene resin is sent into concentration, adds 2- hydroxyls
Base ethamine, 60-80 DEG C is warming up to, stirs 10-16h, cooling, washing obtains the first prefabricated material.
3. the ion exchange resin preparation method according to claim 1 or claim 2 for Treating Municipal Sewage, it is characterised in that
It is 34-38wt% piperazines by weight by 50-60 part macropore chloromethylated polystyrenes resin feeding 150-180 parts concentration in S1
3-6h is swelled in the piperazine aqueous solution, adds 1-2 part 2 hydroxy ethylamines, is warming up to 60-80 DEG C, stirs 10-16h, cooling, washing obtains
First prefabricated material.
4. it is used for the ion exchange resin preparation method of Treating Municipal Sewage, its feature according to claim any one of 1-3
It is, in S2, chitosan, propionic acid is well mixed, adds water and stir, add polyethylene glycol, be warming up to 92-98 DEG C of stirring
4-6h, 105-112 DEG C is warming up to, adds locust bean gum, the first prefabricated material, calcining coconut shell flour stirring 40-100min, mixing speed
For 640-700r/min, filter, washing, be dried to obtain the second prefabricated material.
5. it is used for the ion exchange resin preparation method of Treating Municipal Sewage, its feature according to claim any one of 1-4
It is, in S2, is by weight well mixed 5-10 parts chitosan, 1-2 part propionic acid, adds 20-40 part water and stir, add
50-80 part polyethylene glycol, 92-98 DEG C of stirring 4-6h is warming up to, 105-112 DEG C is warming up to, adds 10-16 parts locust bean gum, 20-
40 part of first prefabricated material, 1-6 parts calcining coconut shell flour stirring 40-100min, mixing speed 640-700r/min, are filtered, washing,
It is dried to obtain the second prefabricated material.
6. it is used for the ion exchange resin preparation method of Treating Municipal Sewage, its feature according to claim any one of 1-5
It is, in S3, in ice-water bath, thionyl chloride is added dropwise into the second prefabricated material, adjust the temperature to 80-90 DEG C, is incubated 2-4h, drop
Temperature, wash, filtering, be sent into DMF and be swelled 4-8h, add trimethylamine reaction 5-10h, obtain being used to handle
The ion exchange resin of municipal sewage.
7. it is used for the ion exchange resin preparation method of Treating Municipal Sewage, its feature according to claim any one of 1-6
It is, in S3, in ice-water bath, 3-5 part thionyl chlorides is added dropwise by weight into the second prefabricated material of 60-80 parts, adjust temperature
To 80-90 DEG C, 2-4h is incubated, is cooled, is washed, filtering, is sent into 150-240 part DMFs and is swelled 4-8h, add
Enter 4-10 parts trimethylamine reaction 5-10h, obtain the ion exchange resin for Treating Municipal Sewage.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111269340A (en) * | 2020-03-31 | 2020-06-12 | 台州学院 | Chelate resin with 1-methanesulfonyl piperazine as ligand and preparation method and application thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102189008A (en) * | 2011-04-11 | 2011-09-21 | 常州大学 | Novel strongly and weakly alkaline anion exchange resin and preparation method thereof |
CN102212155A (en) * | 2011-04-29 | 2011-10-12 | 南开大学 | High-temperature-resistant guanidine-based strong-basic anion exchange resin for strong base and synthesis method thereof |
CN106745633A (en) * | 2016-12-27 | 2017-05-31 | 郑州源冉生物技术有限公司 | A kind of heavy metal-polluted water treatment agent and preparation method thereof |
-
2017
- 2017-09-06 CN CN201710793740.9A patent/CN107537452A/en not_active Withdrawn
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102189008A (en) * | 2011-04-11 | 2011-09-21 | 常州大学 | Novel strongly and weakly alkaline anion exchange resin and preparation method thereof |
CN102212155A (en) * | 2011-04-29 | 2011-10-12 | 南开大学 | High-temperature-resistant guanidine-based strong-basic anion exchange resin for strong base and synthesis method thereof |
CN106745633A (en) * | 2016-12-27 | 2017-05-31 | 郑州源冉生物技术有限公司 | A kind of heavy metal-polluted water treatment agent and preparation method thereof |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111269340A (en) * | 2020-03-31 | 2020-06-12 | 台州学院 | Chelate resin with 1-methanesulfonyl piperazine as ligand and preparation method and application thereof |
CN111269340B (en) * | 2020-03-31 | 2020-12-29 | 台州学院 | Chelate resin with 1-methanesulfonyl piperazine as ligand and preparation method and application thereof |
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