CN219590253U

CN219590253U - Detection system for 4, 6-diaminoresorcinol hydrochloride

Info

Publication number: CN219590253U
Application number: CN202321881408.5U
Authority: CN
Inventors: 王叔超; 王凤德; 田远; 黄聪; 陈浩; 黄朝东
Original assignee: Chengdu Xinchen New Material Technology Co ltd
Current assignee: Chengdu Xinchen New Material Technology Co ltd
Priority date: 2023-07-18
Filing date: 2023-07-18
Publication date: 2023-08-25
Anticipated expiration: 2033-07-18

Abstract

The utility model discloses a detection system for 4, 6-diaminoresorcinol hydrochloride, which belongs to the technical field of high performance liquid chromatography detection and comprises a detector and an auxiliary device, wherein a sample container and a solvent container are vacuumized, air in the sample container and the solvent container is removed, and then nitrogen is filled into the sample container and the solvent container to normal pressure. And (3) filling a sample into a sample container under the condition of keeping low-flow flowing nitrogen, filling a solvent into the solvent container, closing container covers respectively, replacing nitrogen respectively, putting the solvent in the solvent container into the sample container to complete sample dissolution, and then introducing the dissolved sample into a detector to perform high performance liquid chromatography detection to obtain the purity of the sample, so that the oxidation of the sample is effectively avoided, and the accuracy of the high performance liquid chromatography detection of the sample is improved.

Description

Detection system for 4, 6-diaminoresorcinol hydrochloride

Technical Field

The utility model relates to a detection system for 4, 6-diaminoresorcinol hydrochloride, belonging to the technical field of high performance liquid chromatography detection.

Background

Poly (p-Phenylene Benzobisoxazole) (PBO) fiber is an organic synthetic fiber with highest strength and modulus which can be prepared by the current industry, has excellent performance due to a unique rigid structure, and has wide application in a plurality of tip fields. 4, 6-diaminoresorcinol hydrochloride (4, 6-diaminoresorcinol, abbreviated DAR) is a key monomer for synthesizing high performance fiber PBO. The purity determines whether it can meet the polymerization degree requirements for producing high performance PBO fibers. Because the structure of the compound contains two hydroxyl groups and two amino groups, the compound has poor oxidative decomposition property, so that the compound has poor stability, and the solution can undergo chemical reaction to change color and deteriorate after being exposed to air.

The HPLC detection is a conventional detection method for analyzing the purity of chemical samples, and according to the conventional operation mode and flow of dissolving samples, the dissolved 4, 6-diaminoresorcinol hydrochloride sample solution can be oxidized and decomposed in a short time after contacting with air, on one hand, the sample preparation of the sample to be detected is extremely difficult, and on the other hand, the detection result is High Performance Liquid Chromatography (HPLC) data after the sample oxidation, and the purity result of the 4, 6-diaminoresorcinol hydrochloride sample cannot be accurately reacted. Therefore, a detection system of 4, 6-diaminoresorcinol hydrochloride needs to be designed, so that the detection accuracy and efficiency of a key monomer DAR of PBO fibers are improved.

Disclosure of Invention

The utility model aims to solve the problems of low detection accuracy and low efficiency when the existing high performance liquid chromatography is used for detecting 4, 6-diaminoresorcinol hydrochloride, and provides a detection system for the 4, 6-diaminoresorcinol hydrochloride. And (3) filling a sample into a sample container under the condition of keeping low-flow flowing nitrogen, filling a solvent into the solvent container, closing container covers respectively, replacing nitrogen respectively, putting the solvent in the solvent container into the sample container to complete sample dissolution, and then introducing the dissolved sample into a detector to perform high performance liquid chromatography detection to obtain the purity of the sample, so that the oxidation of the sample is effectively avoided, and the accuracy of the high performance liquid chromatography detection of the sample is improved.

The utility model is realized by the following technical scheme:

the detection system for the 4, 6-diaminoresorcinol hydrochloride comprises a detector and an auxiliary device, wherein the detector is used for acquiring a set amount of to-be-detected objects in the auxiliary device and detecting the purity of the to-be-detected objects; the auxiliary device comprises a sample container with an open upper end and a solvent container with an open upper end, wherein container covers are arranged at the upper ends of the sample container and the solvent container, the lower end of the solvent container is connected with the sample container through a first connecting pipe, a first valve is arranged on the first connecting pipe, the lower end of the solvent container is connected with a fourth connecting pipe through a second connecting pipe, a second valve is arranged on the second connecting pipe, the lower end of the sample container is connected with the fourth connecting pipe through a third connecting pipe, a third valve is arranged on the third connecting pipe, a fourth valve is arranged on the fourth connecting pipe, and the fourth valve is respectively connected with a nitrogen inlet pipe and a vacuum pipe.

Preferably, the first valve adopts a ball valve or a stop valve.

Preferably, the second valve and the third valve are needle valves.

Preferably, the fourth valve is a three-way switching valve.

Preferably, a discharging pipe is arranged below the sample container.

Preferably, a discharge valve is arranged on the discharge pipe.

Preferably, the container cover is screwed or snap-fitted or transition-fitted to the peripheral walls of the sample container and the solvent container.

Compared with the prior art, the utility model has the following advantages:

1. the detection system for the 4, 6-diaminoresorcinol hydrochloride provided by the utility model is characterized in that a sample container and a solvent container are vacuumized, air in the sample container and the solvent container is removed, and then nitrogen is flushed into the sample container and the solvent container to normal pressure. And (3) filling a sample (namely 4, 6-diaminoresorcinol hydrochloride) into a sample container under the condition of keeping low-flow flowing nitrogen, filling a solvent (one or more of methanol, ethanol and high-purity water are adopted as the solvent) into a solvent container, closing a container cover respectively, respectively replacing nitrogen, putting the solvent in the solvent container into the sample container to complete sample dissolution, and then introducing the dissolved sample into a detector for high-performance liquid chromatography detection to obtain the purity of the sample, so that the oxidation of the sample is effectively avoided, and the accuracy of the high-performance liquid chromatography detection of the sample is improved.

2. The detection system for the 4, 6-diaminoresorcinol hydrochloride provided by the utility model has the advantages that the auxiliary device is simple in structure and easy to detach and clean.

Drawings

FIG. 1 is a schematic diagram of the structure of the present utility model;

FIG. 2 is a schematic diagram of an auxiliary device according to the present utility model;

wherein: 100. a detector; 200. an auxiliary device; 1. a sample container; 2. a solvent container; 3. a container cover; 4. a first connection pipe; 5. a first valve; 6. a second connection pipe; 7. a second valve; 8. a third connection pipe; 9. a third valve; 10. a fourth connection pipe; 11. a fourth valve; 12. a nitrogen inlet pipe; 13. a vacuum tube; 14. a discharge pipe; 15. and a discharge valve.

Detailed Description

The present utility model will be described in further detail with reference to examples, but embodiments of the present utility model are not limited thereto.

Example 1

As shown in fig. 1 and 2, the present embodiment provides a detection system for 4, 6-diaminoresorcinol hydrochloride, which includes a detector 100 and an auxiliary device 200, wherein the detector 100 is used for obtaining a set amount of an object to be detected in the auxiliary device 200 and detecting the purity of the object to be detected, and the detector 100 adopts a high performance liquid chromatography detector; the auxiliary device 200 comprises a sample container 1 with an opening at the upper end and a solvent container 2 with an opening at the upper end, wherein container covers 3 are arranged at the upper ends of the sample container 1 and the solvent container 2, the lower end of the solvent container 2 is connected with the sample container 1 through a first connecting pipe 4, a first valve 5 is arranged on the first connecting pipe 4, the lower end of the solvent container 2 is connected with a fourth connecting pipe 10 through a second connecting pipe 6, a second valve 7 is arranged on the second connecting pipe 6, the lower end of the sample container 1 is connected with the fourth connecting pipe 10 through a third connecting pipe 8, a third valve 9 is arranged on the third connecting pipe 8, a fourth valve 11 is arranged on the fourth connecting pipe 10, and the fourth valve 11 is respectively connected with a nitrogen inlet pipe 12 and a vacuum pipe 13.

Vacuumizing the sample container 1 and the solvent container 2, removing air in the sample container 1 and the solvent container 2, then flushing nitrogen into the sample container 1 and the solvent container 2, then filling a sample (namely 4, 6-diaminoresorcinol hydrochloride) into the sample container 1, filling a solvent (one or more of methanol, ethanol and high-purity water) into the solvent container, then placing the solvent in the solvent container 2 into the sample container 1, completing sample dissolution, and then introducing the dissolved sample into the detector 100 for high-performance liquid chromatography detection to obtain the purity of the sample, thereby effectively avoiding sample oxidation and improving the accuracy of the high-performance liquid chromatography detection of the sample.

Example 2

The difference between the utility model and the embodiment 1 is that: the first valve 5 adopts a ball valve or a stop valve.

Wherein, the second valve 7 and the third valve 9 are needle valves.

Wherein the fourth valve 11 is a three-way switching valve.

Wherein a discharge pipe 14 is arranged below the sample container 1.

Wherein, the discharging pipe 14 is provided with a discharging valve 15.

Wherein the container cover 3 is in threaded connection with the outer peripheral walls of the sample container 1 and the solvent container 2, either in a snap-fit connection or in a transition fit.

The auxiliary device 200 has a simple structure and is easy to disassemble and clean.

When the system is used, step 1, the first valve 5 and the discharge valve 15 in the detection system are closed, and the sample solvent are respectively emptied and defoamed for pretreatment.

1) The second valve 7 and the third valve 9 are opened, the fourth valve 11 is cut to the vacuum tube 13 to pump negative pressure to minus 0.09MPa, the fourth valve 11 is closed, the fourth valve 11 is slowly cut to the nitrogen inlet tube 12, the nitrogen is supplemented to normal pressure, and the process is repeated once.

2) Closing the second valve 7, opening the third valve 9, cutting the fourth valve 11 to a nitrogen inlet pipe 12, opening the container cover 3 of the sample container 1 under the condition of low-flow flowing nitrogen, adding the sample to be tested (namely 4, 6-diaminoresorcinol hydrochloride) under the condition of flowing nitrogen, then covering the container cover 3, and carrying out negative pressure emptying and nitrogen supplementing normal pressure operation through the fourth valve 11.

3) Closing the third valve 9, opening the second valve 7, cutting the fourth valve 11 to a nitrogen inlet pipe 12, opening the container cover 3 of the solvent container 2 under the condition of low-flow flowing nitrogen, adding a sample solvent (the solvent adopts one or two of methanol, ethanol and high-purity water) under the condition of flowing nitrogen, then covering the container cover 3, and performing negative pressure defoaming emptying and nitrogen supplementing normal pressure operation through the fourth valve 11.

And 2, closing a fourth valve 11 and a discharge valve 15, opening a second valve 7 and a third valve 9, opening a first valve 5 under the condition that the pressure balance state of the sample container 1 and the solvent container 2 is kept, putting the solvent in the solvent container 2 into the sample container 1, completing sample dissolution and sample preparation, and then introducing the dissolved sample to be tested into a detector 100 for high performance liquid chromatography detection to obtain the purity of the sample, so that sample oxidation is effectively avoided, and the accuracy of the high performance liquid chromatography detection of the sample is improved.

The foregoing description is only a preferred embodiment of the present utility model, and is not intended to limit the present utility model in any way, and any simple modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present utility model fall within the scope of the present utility model.

Claims

1. A detection system for 4, 6-diaminoresorcinol hydrochloride, characterized in that: the device comprises a detector (100) and an auxiliary device (200), wherein the detector (100) is used for acquiring a set amount of to-be-detected objects in the auxiliary device (200) and detecting the purity of the to-be-detected objects; auxiliary device (200) are including upper end open-ended sample container (1) and upper end open-ended solvent container (2), sample container (1) and solvent container (2) upper end all set up container lid (3), solvent container (2) lower extreme links to each other with sample container (1) through first connecting pipe (4), be provided with first valve (5) on first connecting pipe (4), solvent container (2) lower extreme links to each other with fourth connecting pipe (10) through second connecting pipe (6), set up second valve (7) on second connecting pipe (6), sample container (1) lower extreme links to each other with fourth connecting pipe (10) through third connecting pipe (8), set up third valve (9) on third connecting pipe (8), be provided with fourth valve (11) on fourth connecting pipe (10), fourth valve (11) link to each other with nitrogen gas inlet tube (12) and vacuum tube (13) respectively.

2. The detection system for 4, 6-diaminoresorcinol hydrochloride of claim 1 wherein: the first valve (5) adopts a ball valve or a stop valve.

3. The detection system for 4, 6-diaminoresorcinol hydrochloride of claim 1 wherein: the second valve (7) and the third valve (9) are needle valves.

4. The detection system for 4, 6-diaminoresorcinol hydrochloride of claim 1 wherein: the fourth valve (11) is a three-way switching valve.

5. The detection system for 4, 6-diaminoresorcinol hydrochloride of claim 1 wherein: a discharging pipe (14) is arranged below the sample container (1).

6. The detection system for 4, 6-diaminoresorcinol hydrochloride of claim 5 wherein: a discharge valve (15) is arranged on the discharge pipe (14).

7. The detection system for 4, 6-diaminoresorcinol hydrochloride of claim 1 wherein: the container cover (3) is in threaded connection with the outer peripheral walls of the sample container (1) and the solvent container (2), or is in snap connection or transition fit.