CN106243041B

CN106243041B - Purification method of 4-aminoantipyrine

Info

Publication number: CN106243041B
Application number: CN201610549430.8A
Authority: CN
Inventors: 陈杰; 耿玉明; 柏佳明; 管华玫; 吴雪静; 陈志�
Original assignee: Liyang Center For Diseases Prevention And Control
Current assignee: Liyang Center For Diseases Prevention And Control
Priority date: 2016-07-13
Filing date: 2016-07-13
Publication date: 2020-12-08
Anticipated expiration: 2036-07-13
Also published as: CN106243041A

Abstract

The invention discloses a purification method of 4-aminoantipyrine, which comprises the steps of adding bleaching earth into a 4-aminoantipyrine solution, uniformly stirring, standing, separating, and collecting filtrate to obtain a purified 4-aminoantipyrine solution; the concentration of the 4-aminoantipyrine solution is 1-5 wt%; the weight ratio of the bleaching earth to the 4-aminoantipyrine in the 4-aminoantipyrine solution is 1: 1-8: 1. The method for purifying the 4-aminoantipyrine by adopting the bleaching earth has the effect equivalent to that of Florisil burnt at high temperature, and compared with the price of Florisil of 150 yuan/250 g, the price of bleaching earth of 4 yuan/25 kg greatly reduces the purification cost.

Description

Purification method of 4-aminoantipyrine

Technical Field

The invention belongs to the technical field of substance purification, and particularly relates to a purification method of 4-aminoantipyrine.

Background

4-aminoantipyrine is an important intermediate for producing medicines such as analgin, aminopyrine and the like, is also a color developing agent for measuring substances such as phenols, alcohols, amines and the like, and is easy to be oxidized to generate impurities, so that purification is generally required during use.

At present, the methods suitable for purifying 4-aminoantipyrine mainly comprise the following methods:

(1) benzene washing; the method has the advantages of good purification effect; the disadvantages are complex operation, long time consumption, toxic benzene and great harm to human body.

(2) Ethanol immersion cleaning; the method has the advantages of simple operation and low toxicity; the disadvantage is poor purification.

(3) Florisil purification method: the method has the advantages of simple operation and good purification effect; the disadvantage is that the price is relatively high, resulting in high purification cost; and is usually subjected to high temperature ignition prior to use.

Disclosure of Invention

The invention aims to solve the problems and provides a method for purifying 4-aminoantipyrine, which is simple to operate, good in purification effect and low in purification cost.

The technical scheme for realizing the purpose of the invention is as follows: a method for purifying 4-aminoantipyrine comprises the steps of adding bleaching earth into a 4-aminoantipyrine solution, uniformly stirring, standing, separating, and collecting filtrate to obtain a purified 4-aminoantipyrine solution.

The concentration of the 4-aminoantipyrine solution is 1-5 wt%, preferably 2 wt%.

The weight ratio of the bleaching earth to the 4-aminoantipyrine in the 4-aminoantipyrine solution is 1: 1-8: 1; preferably 4: 1 to 6: 1.

The invention has the following positive effects: according to a large number of experiments, the invention finally discovers that the method for purifying 4-aminoantipyrine by using bleaching earth has the effect equivalent to Florisil burnt at high temperature, and compared with the price of Florisil of 150 yuan/250 g, the price of bleaching earth of 4 yuan/25 kg greatly reduces the purification cost.

Detailed Description

(examples)

Weighing 2g of 4-aminoantipyrine, dissolving the 4-aminoantipyrine in water, adding water to a constant volume of 100mL, and storing the solution in a refrigerator.

(example 1)

The purification method of 4-aminoantipyrine of this example is as follows:

to 100mL of 2wt% 4-aminoantipyrine solution of example 1 was added 10g of bleaching earth, followed by stirring, standing, and then centrifugal separation to obtain a filtrate in yield, thereby obtaining a purified 4-aminoantipyrine solution.

Blank absorbance values of the 4-aminoantipyrine solution before and after purification are respectively 0.161 and 0.049 according to a method of 18.4 in national environmental protection standard HJ503-2009 determination of water quality volatile phenol 4-aminoantipyrine spectrophotometry of the people's republic of China.

(comparative examples 1 to 4)

The comparative purification method was substantially the same as in example 1 except for the differences shown in Table 1.

TABLE 1

	Example 1	Comparative example 1	Comparative example 2	Comparative example 3	Comparative example 4
						Purification reagent	Bleaching earth	Florisil earth	Diatomite	Organic bentonite	Activated carbon
Absorbance of purified blank	0.049	0.074	0.142	0.145	0.122

As can be seen from table 1: the purification effect of bleaching earth adopted is obviously superior to that of purification reagents such as activated carbon and the like.

(comparative examples 5 to 6)

The comparative purification method was substantially the same as in example 1 except for the differences shown in Table 2.

TABLE 2

	Example 1	Comparative example 1	Comparative example 5	Comparative example 6
					Purification reagent	Bleaching earth	Florisil earth	Bleaching earth after high-temperature firing	Florisil after high temperature firing
Absorbance of purified blank	0.049	0.074	0.088	0.053

Wherein the high-temperature burning temperature is 600 ℃, and the time is 4 hours.

As can be seen from table 2: under the condition of the same dosage, the purification effect of the bleaching earth is almost the same as that of Florisil burnt at high temperature and is superior to that of Florisil not burnt at high temperature, and the purification effect of the bleaching earth burnt at high temperature is reduced.

(examples 2 to 6)

The purification process of each example was substantially the same as in example 1 except for the differences shown in Table 3.

TABLE 3

Example 1

Example 2

Example 3

Example 4

Example 5

Example 6

Bleaching clay dosage

10g

12g

16g

8g

5g

2g

Absorbance of purified blank

0.049

0.047

0.055

0.078

0.103

(application example)

The 4-aminoantipyrine solutions purified in examples 1 to 6 were applied to the detection of phenolic substances in the standard (10 μ g) according to the method of 18.3 in the national environmental protection standard of the people's republic of china HJ503-2009 spectrophotometry for determining 4-aminoantipyrine volatile phenol in water, and the absorbance and sensitivity Δ a of the marked line are shown in table 4.

TABLE 4

	Absorbance of purified blank	Absorbance of the marked line	Sensitivity Δ A
				Example 1	0.049	0.462	0.413
Example 2	0.047	0.456	0.409
				Example 3	0.047	0.449	0.402
Example 4	0.055	0.480	0.425
				Example 5	0.078	0.515	0.437
Example 6	0.103	0.553	0.450

As can be seen from table 4: with the increase of the dosage of bleaching earth, the purification effect is better and better, but simultaneously, the sensitivity is reduced, so that the dosage of 8-12 g of bleaching earth is optimal.

Claims

1. A method for purifying 4-aminoantipyrine is characterized in that: adding bleaching earth into a 4-aminoantipyrine solution, uniformly stirring, standing, separating, and collecting filtrate to obtain a purified 4-aminoantipyrine solution;

the weight ratio of the bleaching earth to the 4-aminoantipyrine in the 4-aminoantipyrine solution is 4: 1-6: 1.

2. The method of purifying 4-aminoantipyrine according to claim 1, wherein: the concentration of the 4-aminoantipyrine solution is 1-5 wt%.

3. The method of purifying 4-aminoantipyrine according to claim 2, wherein: the concentration of the 4-aminoantipyrine solution is 2 wt%.