CN106243041A - The purification process of 4 amino-antipyrines - Google Patents
The purification process of 4 amino-antipyrines Download PDFInfo
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- CN106243041A CN106243041A CN201610549430.8A CN201610549430A CN106243041A CN 106243041 A CN106243041 A CN 106243041A CN 201610549430 A CN201610549430 A CN 201610549430A CN 106243041 A CN106243041 A CN 106243041A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D231/00—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings
- C07D231/02—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings
- C07D231/10—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D231/14—Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D231/44—Oxygen and nitrogen or sulfur and nitrogen atoms
- C07D231/46—Oxygen atom in position 3 or 5 and nitrogen atom in position 4
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Abstract
The invention discloses the purification process of a kind of 4 amino-antipyrines, it is to be joined by bleaching earth in 4 amino-antipyrine solution, stirs, and stands, and separates, and collects filtrate, obtains 4 amino-antipyrine solution after purification；The concentration of 4 amino-antipyrine solution is 1～5wt%；The weight ratio of 4 amino-antipyrines in bleaching earth and 4 amino-antipyrine solution is 1: 1～8: 1.The present invention use bleaching earth purification 4 amino-antipyrine have with high temperature sintering after the suitable effect of florisil silica, and the price that the price of 4 yuan/25kg of bleaching earth is compared to 150 yuan/250g of florisil silica greatly reduces purification cost.
Description
Technical field
The invention belongs to material technical field of purification, be specifically related to the purification process of a kind of 4-AA.
Background technology
4-AA is the important intermediate producing the medicine such as dipyrone, aminophenazone, is also for measuring phenol
The developer of the materials such as class, alcohols, amine, owing to 4-AA is the most oxidized and produces impurity, the most in use
Typically require purification.
At present, the method being suitable to 4-AA purification mainly has following several:
(1) benzene washes method；The advantage of the method is that purification effect is preferable；Shortcoming is then that operation is complicated, the longest, and benzene has
Poison is bigger to human injury.
(2) ethanol embathes method；The advantage of the method is simple to operate, and toxicity is less；Shortcoming is then that purification effect is the best.
(3) florisil silica method of purification: the advantage of the method is simple to operate, and purification effect is preferable；Shortcoming is then valency
Lattice are of a relatively high, cause purification relatively costly；And typically require through high temperature sintering before using.
Summary of the invention
It is an object of the invention to solve the problems referred to above, it is provided that one is simple to operate, purification effect preferable and purification cost
The purification process of relatively low 4-AA.
The technical scheme realizing the object of the invention is: the purification process of a kind of 4-AA, and it is by bleaching earth
Join in 4-AA solution, stir, stand, separate, collect filtrate, obtain 4-amino peace after purification and replace
Ratio woods solution.
The concentration of above-mentioned 4-AA solution is 1～5wt%, preferably 2wt%.
Above-mentioned bleaching earth is 1: 1～8 with the weight ratio of the 4-AA in above-mentioned 4-AA solution:
1；Preferably 4: 1～6: 1.
The good effect that the present invention has: the present invention be finally found that by great many of experiments, uses bleaching earth purification 4-amino
Phenazone have with high temperature sintering after the suitable effect of florisil silica, and the price of 4 yuan/25kg of bleaching earth is compared to not
In sieve, the price of 150 yuan/250g of tripoli greatly reduces purification cost.
Detailed description of the invention
(example)
Weigh the 4-AA of 2g, with water dissolution, then add water and be settled to 100mL, preserve as in refrigerator.
(embodiment 1)
The purification process of the 4-AA of the present embodiment is as follows:
10g bleaching earth is added in the 4-AA solution that 100mL concentration is 2wt% of example 1, after stirring, quiet
Put, be then centrifuged for separating, yield filtrate, obtain 4-AA solution after purification.
According to People's Republic of China (PRC) state environment protecting standard HJ503-2009 " the mensuration 4-amino of water quality volatile phenol
Phenazone spectrophotography " in 18.4 method measure before purification after the blank absorbency of 4-AA solution
Value, respectively 0.161 and 0.049.
(comparative example 1～comparative example 4)
The purification process of each comparative example is substantially the same manner as Example 1, and difference is shown in Table 1.
Table 1
| Embodiment 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| Purified reagent | Bleaching earth | Florisil silica | Kieselguhr | Organobentonite | Activated carbon |
| Blank absorbency after purification | 0.049 | 0.074 | 0.142 | 0.145 | 0.122 |
As can be seen from Table 1: use the purification effect of bleaching earth to be substantially better than the purified reagent such as activated carbon.
(comparative example 5～comparative example 6)
The purification process of each comparative example is substantially the same manner as Example 1, and difference is shown in Table 2.
Table 2
| Embodiment 1 | Comparative example 1 | Comparative example 5 | Comparative example 6 | |
| Purified reagent | Bleaching earth | Florisil silica | Bleaching earth after high temperature sintering | Florisil silica after high temperature sintering |
| Blank absorbency after purification | 0.049 | 0.074 | 0.088 | 0.053 |
Wherein, high temperature sintering temperature is 600 DEG C, and the time is 4h.
As can be seen from Table 2: in the case of consumption is identical, the Fu Luoli after the purification effect of bleaching earth and high temperature sintering
Tripoli is substantially similar, and is better than the florisil silica of non-high temperature sintering, and the bleaching earth purification effect after high temperature sintering is on the contrary
Decline.
(embodiment 2～embodiment 6)
The purification process of each embodiment is substantially the same manner as Example 1, and difference is shown in Table 3.
Table 3
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Bleaching earth consumption | 10g | 12g | 16g | 8g | 5g | 2g |
| Blank absorbency after purification | 0.049 | 0.047 | 0.047 | 0.055 | 0.078 | 0.103 |
(application examples)
Embodiment 1～embodiment 6 4-AA solution after purification are protected according to People's Republic of China's National Environmental
The method protecting in standard HJ503-2009 " the mensuration 4-AA spectrophotography of water quality volatile phenol " 18.3 is answered
Use the detection of aldehydes matter, its graticule absorbance and sensitivity △ A in standard substance (10 μ g) and be shown in Table 4.
Table 4
| Blank absorbency after purification | Graticule absorbance | Sensitivity △ A | |
| Embodiment 1 | 0.049 | 0.462 | 0.413 |
| Embodiment 2 | 0.047 | 0.456 | 0.409 |
| Embodiment 3 | 0.047 | 0.449 | 0.402 |
| Embodiment 4 | 0.055 | 0.480 | 0.425 |
| Embodiment 5 | 0.078 | 0.515 | 0.437 |
| Embodiment 6 | 0.103 | 0.553 | 0.450 |
As can be seen from Table 4: along with the increase of bleaching earth consumption, purification effect is also become better and better, but simultaneously, sensitivity is also
Decreasing, therefore, the consumption with bleaching earth employing 8～12g is optimal.
Claims (5)
1. the purification process of a 4-AA, it is characterised in that: it be bleaching earth is joined 4-amino peace for than
In woods solution, stir, stand, separate, collect filtrate, obtain 4-AA solution after purification.
The purification process of 4-AA the most according to claim 1, it is characterised in that: described 4-amino peace for than
The concentration of woods solution is 1～5wt%.
The purification process of 4-AA the most according to claim 2, it is characterised in that: described 4-amino peace for than
The concentration of woods solution is 2wt%.
4. according to the purification process of the 4-AA one of claims 1 to 3 Suo Shu, it is characterised in that: described bleaching
Native and the 4-AA in described 4-AA solution weight ratio is 1: 1～8: 1.
The purification process of 4-AA the most according to claim 4, it is characterised in that: described bleaching earth is with described
The weight ratio of the 4-AA in 4-AA solution is 4: 1～6: 1.
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| CN201610549430.8A CN106243041B (en) | 2016-07-13 | 2016-07-13 | Purification method of 4-aminoantipyrine |
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| CN201610549430.8A CN106243041B (en) | 2016-07-13 | 2016-07-13 | Purification method of 4-aminoantipyrine |
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| CN106243041B CN106243041B (en) | 2020-12-08 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019196993A (en) * | 2018-05-10 | 2019-11-14 | 東洋紡株式会社 | Method for quantifying 4-hydroxyantipyrin, method for producing biological component measurement kit, and biological component measurement kit |
| JP2019195300A (en) * | 2018-05-10 | 2019-11-14 | 東洋紡株式会社 | Biogenic substance measurement kit and method in which measurement sensitivity is improved |
| JP2019196331A (en) * | 2018-05-10 | 2019-11-14 | 東洋紡株式会社 | Production method of purified 4-amino antipyrine, and produced 4-amino antipyrine |
| CN113200917A (en) * | 2021-05-21 | 2021-08-03 | 河北冀衡药业股份有限公司 | Purification method of 4-aminoantipyrine |
| JP7484998B2 (en) | 2022-11-25 | 2024-05-16 | 東洋紡株式会社 | Biological component measurement kit and biological component measurement method with improved measurement sensitivity |
-
2016
- 2016-07-13 CN CN201610549430.8A patent/CN106243041B/en active Active
Non-Patent Citations (4)
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| 尹继宇: "挥发酚测定中4-氨基安替比林提纯方法的比较", 《环境监测管理与技术》 * |
| 朱艳敏: "活性炭对4-氨基安替比林提纯作用的评定—针对水质监测中对挥发酚的监测分析", 《长春师范学院学报（自然科学版）》 * |
| 谢莲英等: "4-氨基安替比林各种提纯方法的比较", 《干旱环境监测》 * |
| 陈立新: "4-氨基安替比林提纯方法的比较", 《干旱环境监测》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019196993A (en) * | 2018-05-10 | 2019-11-14 | 東洋紡株式会社 | Method for quantifying 4-hydroxyantipyrin, method for producing biological component measurement kit, and biological component measurement kit |
| JP2019195300A (en) * | 2018-05-10 | 2019-11-14 | 東洋紡株式会社 | Biogenic substance measurement kit and method in which measurement sensitivity is improved |
| JP2019196331A (en) * | 2018-05-10 | 2019-11-14 | 東洋紡株式会社 | Production method of purified 4-amino antipyrine, and produced 4-amino antipyrine |
| JP7206631B2 (en) | 2018-05-10 | 2023-01-18 | 東洋紡株式会社 | Method for quantifying 4-hydroxyantipyrine, method for producing biological component measurement kit, and biological component measurement kit |
| JP7210899B2 (en) | 2018-05-10 | 2023-01-24 | 東洋紡株式会社 | Method for producing purified 4-aminoantipyrine and produced 4-aminoantipyrine |
| CN113200917A (en) * | 2021-05-21 | 2021-08-03 | 河北冀衡药业股份有限公司 | Purification method of 4-aminoantipyrine |
| JP7484998B2 (en) | 2022-11-25 | 2024-05-16 | 東洋紡株式会社 | Biological component measurement kit and biological component measurement method with improved measurement sensitivity |
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| CN106243041B (en) | 2020-12-08 |
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