CN103537268B - A kind of preparation method of adsorption resin with high cyanuric acid adsorption capacity and application thereof - Google Patents
A kind of preparation method of adsorption resin with high cyanuric acid adsorption capacity and application thereof Download PDFInfo
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- CN103537268B CN103537268B CN201310541507.3A CN201310541507A CN103537268B CN 103537268 B CN103537268 B CN 103537268B CN 201310541507 A CN201310541507 A CN 201310541507A CN 103537268 B CN103537268 B CN 103537268B
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Abstract
The invention provides a kind of preparation method cyanuric acid to the macroporous absorbent resin of high-adsorption-capacity.The method adopts chloromethylation macroporous cross-linked polystyrene pearl body while carrying out post-crosslinking reaction, adds the reagent that can associate with cyanuric acid and participates in reacting, produce macroporous absorbent resin cyanuric acid to high-adsorption-capacity.The cyanuric acid adsorption capacity of polymeric adsorbent of the present invention, up to more than 120mg/ml, improves more than 30% compared with the cyanuric acid adsorption capacity of conventional absorbtion resin, and present invention process controls simple, and raw material is easy to get.
Description
Technical field
The invention provides a kind of preparation method cyanuric acid to the macroporous absorbent resin of high-selectivity adsorption capacity.
Background technology
Be inevitably produce a large amount of technique waste waters in the process of raw material production chlorated fulminuric acid compounds with cyanuric acid, not only containing cyanuric acid class material in these waste water, also containing salts such as NaCl, if directly outer row, severe contamination certainly will be caused to environment, therefore must process these waste water further.The method that the process of cyanuric acid waste water is comparatively economic adopts macroporous absorbent resin to carry out adsorption and enrichment to cyanuric acid class material, remove the waste water after cyanuric acid because containing NaCl, directly can repeat to be back to chloric alkali electrolysis raw material, after resin adsorption is saturated, reclaim cyanuric acid with solvent elution again.
Many macroporous absorbent resins can both be used for absorption and the enrichment of cyanuric acid class, but known all macroporous absorbent resins all exist cyanuric acid adsorption capacity shortcoming on the low side, cause the processing cost of cyanuric acid spent acid higher, can not be generally used.
Adsorption resin with high cyanuric acid adsorption capacity prepared by the present invention is a kind of macroporous absorbent resin with the high-specific surface area of the functional group of the cyanuric acid that can associate, and its cyanuric acid adsorption capacity can reach more than 120mg/g.
Summary of the invention
The object of this invention is to provide a kind of macroporous absorbent resin with the high-specific surface area of the functional group of the cyanuric acid that can associate, its cyanuric acid adsorbance can reach more than 120mg/g.
Technical scheme of the present invention is as follows:
A kind of preparation method of adsorption resin with high cyanuric acid adsorption capacity, it is characterized in that: chloromethylation macroporous cross-linked polystyrene pearl body is while carrying out post-crosslinking reaction, add the reagent that can associate with cyanuric acid to participate in reacting, be connected on the phenyl ring of chloromethylation macroporous cross-linked polystyrene, produce macroporous absorbent resin cyanuric acid to high-adsorption-capacity, described post-crosslinking reaction is that the phenyl ring of the vicinity of chloromethylation macroporous cross-linked polystyrene is under solvent swell state, react under catalysis, remove the HCl of a part, by the phenyl ring of two vicinities by methylene (-CH
2-) bridging is connected together.The feature of method described above is: the degree of cross linking of chloromethylation macroporous cross-linked polystyrene pearl body used is 2 ~ 45%, preferably 4 ~ 25%, more preferably 4 ~ 10%.
The feature of method described above is: the chlorinity of chloromethylation macroporous cross-linked polystyrene pearl body is 10% ~ 30%, preferably 13 ~ 30%, more preferably 15 ~ 30%.
The feature of method described above is: the catalyst of post-crosslinking reaction is metal chloride AlCl
3, FeCl
3deng lewis acid.
The feature of method described above is: the reagent that can associate with cyanuric acid added while carrying out post-crosslinking reaction is one or more in cyanuric acid, melamine, uric acid.
The reaction equation that rear reaction that is crosslinked and that introduce cyanuric acid is carried out simultaneously is as follows:
The reaction equation that rear reaction that is crosslinked and that introduce melamine is carried out simultaneously is as follows:
The reaction equation that rear reaction that is crosslinked and that introduce uric acid is carried out simultaneously is as follows:
Detailed description of the invention
Following instance is only further illustrate the present invention, is not restriction the scope of protection of the invention.
Embodiment 1
The degree of cross linking of getting the chloromethylation of triumphant auspicious Chemical Manufacture is the D301 chlorine ball of 7% (chlorinity is 15%) 100g, adding 500ml DMF carries out swelling, add 50g alchlor to make post-crosslinking reaction catalyst, add 20g cyanuric acid and make association reagent, be warming up to 50 DEG C of reactions 10 hours, obtain 115g macroporous absorbent resin A-1.
Embodiment 2
According to the method that embodiment 1 is same, just association reagent is 15g melamine, obtains the macroporous absorbent resin A-2 of 103g.
Embodiment 3
According to the method that embodiment 1 is same, just association reagent is 35g uric acid, obtains 127g macroporous absorbent resin A-3.
Embodiment 4
According to the method that embodiment 1 is same, just chlorine ball to be the degree of cross linking of triumphant auspicious Chemical Manufacture be 10% D201 chlorine ball (chlorinity 25.5%), association reagent is 20g cyanuric acid and 10g uric acid, obtains 129g macroporous absorbent resin A-4.
Embodiment 5
According to the method that embodiment 1 is same, just chlorine ball to be the degree of cross linking of triumphant auspicious Chemical Manufacture be 10% D201 chlorine ball (chlorinity 25.5%), association reagent is 25g cyanuric acid and 15g melamine, obtains 136g macroporous absorbent resin A-5.
Embodiment 6
According to the method that embodiment 1 is same, just chlorine ball to be the degree of cross linking of triumphant auspicious Chemical Manufacture be 10% D201 chlorine ball (chlorinity 25.5%), association reagent is 20g uric acid and 15g melamine, obtains 130g macroporous absorbent resin A-6.
Comparative example 1
D301 chloromethylation chlorine ball 100g does not add any association reagent, directly carries out post-crosslinking reaction according to embodiment 1 method and obtains 98g macroporous absorbent resin (C-1).
Comparative example 2
D201 chloromethylation chlorine ball 100g does not add any association reagent, directly carries out post-crosslinking reaction according to embodiment 1 method and obtains 97g macroporous absorbent resin (C-2).
Cyanuric acid absorption evaluation experiment
Get a glass exchange column, load the above-mentioned resin of treated 100ml, cross post with the air speed of 5/h, detected once every 1 hour, the water 20ml test tube crossed after post meets about 10ml.Post water sample is crossed in the small test tube of dried and clean by pipette, extract.In small test tube, add a phenolphthalein indicator, with the titration of NaOH standard liquid, when solution colour starts to occur blush, stop titration, read the volume of the NaOH standard liquid consumed, the mol number of the NaOH now consumed is the mol number of cyanuric acid.Served as post water sample cyanuric acid concentration when equaling influent density, be inefficacy, the total amount (mg) of the cyanuric acid of resin adsorption is the adsorption capacity (mg/ml) of resin to cyanuric acid divided by the volume (ml) of resin.
The main physical and chemical index of polymeric adsorbent that said method is produced and adsorption test the results are shown in Table 1.
The main physical and chemical index analysis result of table 1 polymeric adsorbent and adsorption test result
As can be seen from Table 1, the polymeric adsorbent that the inventive method is produced and the polymeric adsorbent that known method is produced, its pore structure is not obviously distinguished, but because the inventive method adds the reagent that can associate with cyanuric acid, make the cyanuric acid adsorption capacity of polymeric adsorbent of the present invention up to more than 120mg/ml, improve more than 30% compared with the cyanuric acid adsorption capacity of conventional absorbtion resin, and present invention process controls simple, raw material is easy to get.
Claims (9)
1. the preparation method of an adsorption resin with high cyanuric acid adsorption capacity, it is characterized in that: chloromethylation macroporous cross-linked polystyrene pearl body is while carrying out post-crosslinking reaction, add the reagent that can associate with cyanuric acid to participate in reacting, be connected on the phenyl ring of chloromethylation macroporous cross-linked polystyrene, produce macroporous absorbent resin cyanuric acid to high-adsorption-capacity, described post-crosslinking reaction is that the phenyl ring of the vicinity of chloromethylation macroporous cross-linked polystyrene is under solvent swell state, react under catalysis, remove the HCl of a part, by the phenyl ring of two vicinities by methylene (-CH
2-) bridging is connected together, the described reagent that can associate with cyanuric acid is one or more in cyanuric acid, melamine, uric acid.
2. according to preparation method according to claim 1, it is characterized in that: the degree of cross linking of chloromethylation macroporous cross-linked polystyrene pearl body used is 2 ~ 45%.
3. according to preparation method according to claim 2, it is characterized in that: the degree of cross linking of chloromethylation macroporous cross-linked polystyrene pearl body used is 4 ~ 25%.
4. according to preparation method according to claim 3, it is characterized in that: the degree of cross linking of chloromethylation macroporous cross-linked polystyrene pearl body used is 4 ~ 10%.
5. according to preparation method according to claim 1, it is characterized in that: the chlorinity of chloromethylation macroporous cross-linked polystyrene pearl body is 10% ~ 30%.
6. according to preparation method according to claim 5, it is characterized in that: the chlorinity of chloromethylation macroporous cross-linked polystyrene pearl body is 13 ~ 30%.
7. according to preparation method according to claim 6, it is characterized in that: the chlorinity of chloromethylation macroporous cross-linked polystyrene pearl body is 15 ~ 30%.
8. according to preparation method according to claim 1, it is characterized in that: the catalyst of post-crosslinking reaction is metal chloride AlCl
3, FeCl
3.
9. adsorb a method for Cyanide in Waste Water uric acid and salt thereof with macroporous absorbent resin, it is characterized in that using the macroporous absorbent resin that described in any one of claim 1-8, preparation method obtains.
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| CN108940294A (en) * | 2018-07-19 | 2018-12-07 | 中国日用化学研究院有限公司 | The catalyst and preparation method of cyanuric acid in a kind of Electrocatalysis Degradation swimming-pool water containing chlorine |
Citations (3)
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|---|---|---|---|---|
| CN1394820A (en) * | 2001-11-23 | 2003-02-05 | 广西南宁科林特技术工程有限公司 | Method for treating waste water produced by chloro-isocyanuric acid production |
| CN101987291A (en) * | 2010-11-05 | 2011-03-23 | 山东鲁抗立科药物化学有限公司 | Macropore adsorption resin as well as preparation method and application thereof |
| CN102229710A (en) * | 2011-05-11 | 2011-11-02 | 凯瑞化工股份有限公司 | Method for producing phenol adsorbent resin |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1394820A (en) * | 2001-11-23 | 2003-02-05 | 广西南宁科林特技术工程有限公司 | Method for treating waste water produced by chloro-isocyanuric acid production |
| CN101987291A (en) * | 2010-11-05 | 2011-03-23 | 山东鲁抗立科药物化学有限公司 | Macropore adsorption resin as well as preparation method and application thereof |
| CN102229710A (en) * | 2011-05-11 | 2011-11-02 | 凯瑞化工股份有限公司 | Method for producing phenol adsorbent resin |
Non-Patent Citations (1)
| Title |
|---|
| 3种高比表面积吸附树脂的合成及其对氰尿酸吸附的研究;刘文飞 等;《离子交换与吸附》;20131031;第29卷(第5期);第449页摘要，前言部分和第2.1节，第450页第2.2节，第452页第1段，及第453页第3.3节 * |
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