CN215179084U

CN215179084U - Pretreatment device for cation analysis of pre-decarbonization liquid

Info

Publication number: CN215179084U
Application number: CN202121262591.1U
Authority: CN
Inventors: 赵晶晶; 周庆英; 韩宇澄; 甘云青; 贾瑞博
Original assignee: China BlueChemical Ltd; CNOOC Fudao Ltd
Current assignee: China BlueChemical Ltd; CNOOC Fudao Ltd
Priority date: 2021-06-07
Filing date: 2021-06-07
Publication date: 2021-12-14
Anticipated expiration: 2031-06-07

Abstract

The utility model discloses a pretreatment device for analyzing cations in a pre-decarbonization liquid, which comprises a stirrer, a glass tube, a volumetric flask and an ultrasonic heating water bath kettle; the stirrer comprises a stirring rod, and a plurality of stirring blades are arranged on the stirring rod; the stirring rod is a plastic rod; the glass tube is filled with cationic resin, and the stirring rod extends into the glass tube from the stirrer; the volumetric flask is provided withThe bottom of the glass tube is connected with the volumetric flask through a liquid outlet tube; the volumetric flask is arranged in the ultrasonic heating water bath kettle. The utility model adopts the stirrer to intervene the reaction of the resin and the decarbonization liquid, namely, a large amount of CO is avoided because the reaction speed is too fast₂The water solution is carried out by the escaping and CO generated in the reaction process₂Can be discharged in time, and reduce HCO influencing accuracy₃ ^‑Generating ions; simple structure, convenient use, high accuracy and precision.

Description

Pretreatment device for cation analysis of pre-decarbonization liquid

Technical Field

The utility model belongs to the analysis and detection field, concretely relates to decarbonization liquid cation analysis preprocessing device in advance.

Background

The petrochemical industry commonly uses N-Methyldiethanolamine (MDEA) aqueous solution to purify refinery gas and natural gas, ionic amine salt is inevitably generated in the recycling process, and the salts are still combined with amine to present a stable structure in the rich solution regeneration process, so the salts are called as heat stable salts. The heat stable amine salt loses the ability of combining with hydrogen sulfide or carbon dioxide due to the 'constraint' of amine molecules, so that the effective amine concentration of a desulfurizer is reduced, the viscosity is increased, foaming is realized, foam is difficult to eliminate, a desulfurization solution carries hydrocarbon, and a refined product carries amine; heat stable salts can also cause stress corrosion cracking of amine purification units. Therefore, it is necessary to measure the total amount of heat-stable salts, and the results are important for smooth operation of the desulfurization apparatus, safe operation of the equipment, improvement of product quality, and reduction of production cost.

Assay center determination of thermally stable salts Using an H-type cation exchange resin column to associate the cation of the thermally stable salt with H in the resin⁺By exchange, the anions of the various thermostable salts being converted into the correspondingAnd (4) acid. And then carrying out acid-base neutralization titration, and titrating the acid solution by using a standard alkali solution, thereby calculating the corresponding thermal stable salt content. And whether the pretreatment process of the pre-decarbonization liquid is complete or not and no side reaction occurs directly relate to the accuracy and precision of the analysis method. However, no report about a pretreatment device for cation analysis of the pre-decarbonization liquid is found at present.

SUMMERY OF THE UTILITY MODEL

The utility model aims at providing a simple structure, convenient to use, degree of accuracy and high decarbonization liquid cation analysis preprocessing device in advance to current technique is not enough, and the device has accelerated the reaction rate of decarbonization liquid in advance with resin, makes the CO who generates₂Can eliminate in time to avoid HCO generation₃ ^-Removing CO dissolved in the filtrate by ultrasonic heating water bath₂Gas, improve the accuracy of analysis.

In order to realize the purpose, the technical scheme of the utility model is that: provided is a pretreatment device for cation analysis of a preliminary decarbonization liquid, comprising:

a stirrer; the stirrer comprises a stirring rod, and a plurality of stirring blades are arranged on the stirring rod; the stirring rod is a plastic rod, so that cations are prevented from being brought into the metal stirring rod;

a glass tube; the glass tube is filled with cationic resin, and the stirring rod extends into the glass tube from the stirrer;

a volumetric flask; the volumetric flask is arranged below the glass tube, and the bottom of the glass tube is connected with the volumetric flask through a liquid outlet tube;

ultrasonically heating a water bath; the volumetric flask is arranged in the ultrasonic heating water bath kettle.

Further, stirring vane distribute in the upper portion, middle part and the lower part of puddler, and do not contact the glass pipe avoids stirring vane and glass pipe to bump.

The glass tube further comprises glass wool, wherein the glass wool is arranged at the inner bottom of the glass tube and is thin and uniform; not only can play the effect of preventing that the mouth of a river is stopped up to the resin granule, can also make smooth the passing through drain pipe of water, and prevent that cation resin and other impurity from getting into in the volumetric flask.

Further, still include the iron stand platform, the agitator is fixed on the iron stand platform.

Furthermore, a piston type valve is arranged on the liquid outlet pipe, and the effects of opening and closing and adjusting the flow can be achieved.

Furthermore, the water adding amount of the ultrasonic heating water bath kettle is more than or equal to one third of the height of the volumetric flask and less than or equal to one half of the height of the volumetric flask; not only can play the role of ultrasonic degassing, but also can not lead the volumetric flask to float due to the buoyancy of water in the ultrasonic process.

Furthermore, the cation resin is activated by hydrochloric acid and is washed by a large amount of high-purity water, and no ion peak appears after the finally washed water enters ion chromatographic analysis; and anions brought in by water are prevented from exchanging with the resin to influence the accuracy of an analysis result.

Further, the volume of the glass tube is 50-75 mL, and the diameter of the glass tube is larger than 2cm and smaller than 3 cm; in order to prevent the addition of too much cationic resin and the addition of a large amount of water during the rinsing process exceeding the volume of the volumetric flask.

Furthermore, the amount of the sample is 0.1-0.13 g per ml of the cationic resin. The amount of the sample is generally not more than 4g, when the amount of the cationic resin is 30 mL.

Compared with the prior art, the utility model discloses decarbonization liquid cation analysis preprocessing device has following beneficial effect in advance:

(1) the utility model adopts the stirrer to intervene the reaction of the resin and the decarbonization liquid, namely, a large amount of CO is avoided because the reaction speed is too fast₂The water solution is carried out by the escaping and CO generated in the reaction process₂Can be discharged in time, and reduce HCO influencing accuracy₃ ^-And (4) generating ions.

(2) The utility model adopts the ultrasonic heating water bath kettle to remove CO in the volumetric flask₂Avoiding CO in the titration process₂The interference of (2).

(3) The utility model discloses simple structure, convenient to use, degree of accuracy and precision are higher.

Drawings

FIG. 1 is a schematic view of a pretreatment apparatus for cation analysis of a pre-decarbonization liquid according to the present invention;

in the figure: 1. a stirrer; 2. a stirring rod; 3. a glass tube; 4. a cationic resin; 5. glass wool; 6. a piston valve; 7. a volumetric flask; 8. ultrasonically heating a water bath; 9. iron stand.

Detailed Description

The following detailed description is provided for the embodiments of the present invention, and the present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.

As shown in fig. 1, the utility model discloses decarbonization liquid cation analysis preprocessing device in advance, including iron stand platform 9, agitator 1, puddler 2, glass pipe 3, glass cotton 5, volumetric flask 7 and ultrasonic heating water bath 8.

The stirrer 1 is fixed on an iron support 9, the stirring rod 2 is provided with three stirring blades from top to bottom, the three stirring blades are respectively positioned at the upper part, the middle part and the lower part, and the blades of the stirring rod do not rub the periphery and the bottom of the glass tube; the stirring rod is a plastic rod; the stirring rod 2 extends into a glass tube 3 containing a cationic resin 4. Glass cotton 5 is put at the interior bottom of glass pipe 3, and glass pipe 3 bottoms are passed through the drain pipe and are connected with volumetric flask 7, and inside the drain pipe stretched into volumetric flask 7, set up piston valve 6 on the drain pipe, can play the switch and adjust the effect of play liquid flow size. The volumetric flask 7 is arranged in the ultrasonic heating water bath 8, and the volume of the volumetric flask 7 is different according to different sampling quantities.

The utility model discloses decarbonization liquid cation analysis preprocessing device's theory of operation as follows:

starting the stirrer 1, adjusting the stirring speed to 1-3 r/s, transferring a certain amount of pre-decarbonization liquid into a glass tube 3, and filling the glass tube with a cationic resin 4 which is subjected to hydrochloric acid activation treatment and then is soaked in desalted water; fully exchanging cations in the pre-decarbonization liquid with cation resin to generate H under the stirring of the stirrer 1⁺CO produced₂Under the action of stirringForming a small bubble to escape from the upper part of the glass tube 3, and stopping the stirrer 1 after full reaction; opening a piston type valve 6 on a liquid outlet pipe at the bottom of the glass tube 3, and discharging water in the glass tube 3 into a volumetric flask 7 from the liquid outlet pipe; then adding desalted water from the top of the glass tube 3, starting the stirrer 1, stirring for 1 minute, then discharging the water in the glass tube 3 into the volumetric flask 7 from the liquid outlet pipe, repeating the operation for three times, washing the stirring rod 2 with the desalted water, discharging all the washed water into the volumetric flask 7, opening the ultrasonic heating water bath pot 8, setting the water bath temperature to 80 ℃, taking out the volumetric flask 7 from the water bath pot after ultrasonic treatment for 15 minutes, and fixing the volume.

The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, therefore, the present invention is not limited by the appended claims.

Claims

1. A pretreatment device for cation analysis of a pre-decarbonization liquid is characterized by comprising:

a stirrer; the stirrer comprises a stirring rod, and a plurality of stirring blades are arranged on the stirring rod; the stirring rod is a plastic rod;

2. The pretreatment device for cation analysis of a predebonated fluid according to claim 1, wherein: the stirring blades are distributed on the upper part, the middle part and the lower part of the stirring rod and do not contact the glass tube.

3. The pretreatment device for cation analysis of a predebonated fluid according to claim 1, wherein: the glass tube is characterized by further comprising glass wool, wherein the glass wool is arranged at the inner bottom of the glass tube.

4. The pretreatment device for cation analysis of a predebonated fluid according to claim 1, wherein: still include the iron stand platform, the agitator is fixed on the iron stand platform.

5. The pretreatment device for cation analysis of a predebonated fluid according to claim 1, wherein: and a piston type valve is arranged on the liquid outlet pipe.

6. The pretreatment device for cation analysis of a predebonated fluid according to claim 1, wherein: the water adding amount of the ultrasonic heating water bath kettle is more than or equal to one third of the height of the volumetric flask and less than or equal to one half of the height of the volumetric flask.

7. The pretreatment device for cation analysis of a predebonated fluid according to claim 1, wherein: the cation resin is activated by hydrochloric acid and washed by high-purity water.

8. The pretreatment device for cation analysis of the preliminary decarbonization liquid according to any one of claims 1 to 7, characterized in that: the volume of the glass tube is 50-75 mL, and the diameter of the glass tube is larger than 2cm and smaller than 3 cm.

9. The pretreatment device for cation analysis of a predebonated fluid according to claim 8, wherein: adding a sample amount of 0.1-0.13 g per ml of cationic resin.