CN215691759U - System for hydrochloric acid removes free chlorine in succession - Google Patents
System for hydrochloric acid removes free chlorine in succession Download PDFInfo
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- CN215691759U CN215691759U CN202122215818.3U CN202122215818U CN215691759U CN 215691759 U CN215691759 U CN 215691759U CN 202122215818 U CN202122215818 U CN 202122215818U CN 215691759 U CN215691759 U CN 215691759U
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Abstract
The utility model discloses a system for continuously removing free chlorine by hydrochloric acid, which comprises: the rectifying device comprises a rectifier with a heat exchange structure, a liquid phase outlet of the rectifier is communicated with a dilute hydrochloric acid conveying pipeline, and a gas phase outlet of the rectifier is communicated with the dechlorination device through the conveying pipeline; the lower interface of the dechlorination device is communicated with the gas phase outlet of the rectifier, the upper interface of the dechlorination device is communicated with the lower interface of the rectifying tower, a copper absorption layer is arranged in the dechlorination device and is positioned between the upper interface and the lower interface of the dechlorination device, and gas-phase hydrochloric acid can pass through the copper absorption layer and reach the rectifying tower; the device comprises a rectifying tower and a condensing tower, wherein an upper connector of the rectifying tower is communicated with the condensing tower through a conveying pipeline. The method reduces the free chlorine in the hydrochloric acid by using the copper absorption layer, does not need to analyze the content of the free chlorine in the hydrochloric acid, has extremely low use cost, can realize continuous dechlorination operation of the hydrochloric acid, and has simple process and high dechlorination efficiency.
Description
Technical Field
The utility model relates to the technical field of hydrochloric acid purification, in particular to a system for continuously removing free chlorine from hydrochloric acid.
Background
The industrial synthesis of hydrochloric acid is carried out by synthesizing hydrogen chloride from hydrogen and chlorine generated by electrolysis by combustion, and absorbing hydrogen chloride with water to obtain the final product. In the process of purifying industrial synthetic hydrochloric acid to obtain reagent-grade hydrochloric acid, free chlorine in the reagent-grade hydrochloric acid is difficult to remove, so that a special chlorine removal procedure needs to be designed for the free chlorine. For the removal of free chlorine, a common process is to add reducing agents such as hydrazine hydrate and the like into hydrochloric acid, although the chlorine removal effect is good, the defect is obvious, the reducing agents such as hydrazine hydrate and the like are all liquid, before chlorine removal, the concentration of the free chlorine in the hydrochloric acid needs to be detected and analyzed, the addition amount is calculated according to the amount, the treatment process is complicated, if the addition amount of the reducing agents is too much, an oxidizing agent needs to be added for secondary treatment, and the treatment cost is too high.
Chinese patent CN103879964A discloses a continuous production method of high purity hydrochloric acid, in which a reducing substance capable of reducing free chlorine into chloride ions is added to industrial grade hydrochloric acid in a dechlorination step; stannous chloride, ferrous sulfate, oxalic acid and sodium sulfite, the adding amount is 0.01-1% of the weight of the industrial grade hydrochloric acid, then the high-purity hydrochloric acid is obtained by rectification, and the content of free chlorine can be reduced to be below 300ppb by adding the reducing substances. Similarly, these reducing agents still need to detect and analyze the content of free chlorine in hydrochloric acid before chlorine removal, and then calculate the addition amount according to the amount, which is cumbersome to process and too high in processing cost.
Chinese patent CN111960384A discloses a method for removing free chlorine in hydrochloric acid, which also adds a certain mass of hydrazine solution to hydrochloric acid to reduce and remove chlorine, and simultaneously adds hydrogen peroxide solution to oxidize and remove hydrazine.
SUMMERY OF THE UTILITY MODEL
The utility model aims to: aiming at the existing problems, the utility model provides a system for continuously removing free chlorine from hydrochloric acid, which reduces the free chlorine in the hydrochloric acid by using a copper absorption layer, does not need to analyze the content of the free chlorine in the hydrochloric acid, does not need to use an oxidizing agent to remove redundant reducing agent, has extremely low consumption and extremely low use cost, can realize continuous chlorine removal operation of the hydrochloric acid, has simple process and high chlorine removal efficiency, and overcomes the defects of the existing chlorine removal technology.
The technical scheme adopted by the utility model is as follows: a system for continuously removing free chlorine by hydrochloric acid is characterized by comprising:
the rectifying device is used for rectifying the industrial grade hydrochloric acid for the first time and comprises a rectifier with a heat exchange structure, a liquid phase outlet of the rectifier is communicated with a dilute hydrochloric acid conveying pipeline, and a gas phase outlet of the rectifier is communicated with the dechlorination device through the conveying pipeline;
the dechlorination device is used for removing free chlorine in the gas-phase hydrochloric acid, a lower interface of the dechlorination device is communicated with a gas-phase outlet of the rectifying tower, an upper interface of the dechlorination device is communicated with a lower interface of the rectifying tower, a copper absorption layer is arranged in the dechlorination device and is positioned between the upper interface and the lower interface of the dechlorination device, and the gas-phase hydrochloric acid can pass through the copper absorption layer and reach the rectifying tower;
the rectifying tower and the condensing tower are respectively used for carrying out secondary rectification and condensation after the secondary rectification on the gas-phase hydrochloric acid after dechlorination, and an upper interface of the rectifying tower is communicated with the condensing tower through a conveying pipeline.
In the system, free chlorine is removed mainly through a copper absorption layer, copper and the free chlorine react to generate copper chloride, the boiling point of the copper chloride is 993 ℃, the copper chloride cannot be rectified when hydrochloric acid is rectified, the copper and the hydrochloric acid basically do not react (the reducibility of the copper is less than [ H ]), the copper absorption layer basically consumes when the copper absorption layer absorbs the free chlorine, the consumption is very low, the free chlorine in the hydrochloric acid can be finally reduced to be less than 0.5ppm, the concentration of the industrial hydrochloric acid can be directly and continuously produced to reach reagent-grade hydrochloric acid, the technical process is simple, the chlorine removal efficiency is high, and the defects of the existing chlorine removal technology are overcome.
Furthermore, a liquid phase outlet of the rectifying device is communicated with a dilute hydrochloric acid conveying pipeline, and a raw material inlet of the rectifying device is communicated with a hydrochloric acid raw material conveying pipeline.
In the utility model, a liquid phase outlet of the rectifying tower is communicated with a raw material inlet of the rectifying device through a pipeline. And during secondary rectification, the liquid hydrochloric acid obtained by secondary rectification is used as the hydrochloric acid raw material of primary rectification for return use. Even if the liquid hydrochloric acid after secondary rectification contains a certain amount of copper chloride, the copper chloride is not enriched in the high-purity hydrochloric acid after rectification but remains in the dilute hydrochloric acid due to the high boiling point of the copper chloride when the copper chloride is recycled, so that the liquid hydrochloric acid after secondary rectification can be effectively recovered.
In the utility model, the dechlorination device is provided with a pure water interface which is positioned at the upper part of the copper absorption layer and is communicated with the copper absorption layer. When the contact surface of the copper absorption layer and hydrochloric acid is shielded by impurities such as copper chloride and the like to influence the contact of copper and free chlorine, the impurities on the surface of the copper absorption layer are removed in a pure water leaching mode, and then the copper absorption layer can be reused.
Furthermore, the copper absorption layer is formed by filling electrolytic red copper or copper scraps, the porosity of the copper absorption layer is 30-40%, the pore size is 1-6 mm, and preferably the porosity is 30%, and the pore size is 3 mm.
In the utility model, the rectifying device is formed by connecting a plurality of rectifying devices in series to form a plurality of heating sections. The industrial-grade hydrochloric acid is heated by rectification in a multi-section heating mode, gas-phase hydrochloric acid generated by multi-section heating is collected uniformly, and finally obtained dilute hydrochloric acid is discharged and treated additionally.
Preferably, the rectification apparatus is formed by 5 rectifiers connected in series.
In summary, due to the adoption of the technical scheme, the utility model has the beneficial effects that: the method reduces the free chlorine in the hydrochloric acid by using the copper absorption layer, does not need to analyze the content of the free chlorine in the hydrochloric acid, does not need to use an oxidant to remove redundant reducing agent, has low consumption and low use cost, can realize continuous dechlorination operation of the hydrochloric acid, can finally reduce the content of the free chlorine in the hydrochloric acid to be less than 0.5ppm, has simple process and high dechlorination efficiency, and overcomes the defects of the existing dechlorination technology.
Drawings
FIG. 1 is a schematic structural diagram of a system for continuously removing free chlorine by hydrochloric acid according to the present invention;
FIG. 2 is a schematic view of a rectification apparatus according to the present invention;
FIG. 3 is a schematic view of a chlorine removal installation according to the present invention;
FIG. 4 is a schematic structural view of another chlorine removal device of the present invention.
The labels in the figure are: 1 is a rectifying device, 101 is a rectifier, 2 is a conveying pipeline, 3 is a dechlorination device, 301 is a lower connector, 302 is an upper connector, 303 is a copper absorption layer, 304 is a pure water connector, 4 is a rectifying tower, and 5 is a condensing tower.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the utility model and are not intended to limit the utility model.
As shown in fig. 1-3, a system for continuously removing free chlorine with hydrochloric acid comprises:
the device comprises a rectifying device 1, a heat source collecting device and a heat source collecting device, wherein the rectifying device 1 is used for rectifying industrial-grade hydrochloric acid for the first time to obtain liquid dilute hydrochloric acid and gas-phase hydrochloric acid after rectification, a liquid-phase outlet of the rectifying device 1 is communicated with a dilute hydrochloric acid conveying pipeline (not marked), a raw material inlet of the rectifying device 1 is communicated with a hydrochloric acid raw material conveying pipeline (not marked), the rectifying device 1 comprises a rectifier 101 with a heat exchange structure, the rectifier 101 can adopt the existing structure without special requirements, a gas-phase outlet of the rectifier 101 is communicated with a chlorine removal device 3 through a conveying pipeline 2, and a steam inlet and a steam outlet (not marked) of the rectifier 101 are respectively communicated with a steam conveying pipeline (not shown) to realize the conveying of the heat source of the rectifier 101;
the chlorine removal device 3 is used for removing free chlorine in gas-phase hydrochloric acid, a lower interface 301 of the chlorine removal device 3 is communicated with a gas-phase outlet of the rectifier 101, an upper interface 302 of the chlorine removal device 3 is communicated with a lower interface of the rectifying tower 4, a copper absorption layer 303 is arranged in the chlorine removal device 3, the copper absorption layer 303 is positioned between the upper interface 302 and the lower interface 301 of the chlorine removal device 3, and the gas-phase hydrochloric acid can pass through the copper absorption layer 303 and reach the rectifying tower 4;
the rectifying tower 4 and the condensing tower 5 are respectively used for carrying out secondary rectification on the gas-phase hydrochloric acid subjected to chlorine removal and condensation after the secondary rectification, and an upper interface of the rectifying tower 4 is communicated with the condensing tower 5 through the conveying pipeline 2.
The dechlorination process of the system comprises the following steps:
s1, carrying out primary rectification on the raw material of 31-33 wt% industrial grade hydrochloric acid by a rectification device 1 at the rectification temperature of 90-110 ℃ to obtain gas-phase hydrochloric acid and liquid-phase dilute hydrochloric acid after the primary rectification;
s2, before the gas-phase hydrochloric acid enters the dechlorination device 3, controlling the temperature of the gas-phase hydrochloric acid within the range of 90-110 ℃, controlling the flow rate at 100L/h, and after the gas-phase hydrochloric acid enters the dechlorination device 3, enabling the gas-phase hydrochloric acid to pass through the copper absorption layer 303 for 5-10S to obtain the dechlorinated gas-phase hydrochloric acid;
s3, conveying the dechlorinated gas-phase hydrochloric acid to a rectifying tower 4 for secondary rectification, wherein the temperature of the secondary rectification is controlled at 110 ℃ below 100 ℃ to obtain the gas-phase hydrochloric acid after the secondary rectification;
and S4, introducing the gas-phase hydrochloric acid subjected to secondary rectification into a condensing tower 5 for condensation, and finally discharging the gas-phase hydrochloric acid from a liquid-phase outlet of the condensing tower 5 to obtain the reagent-grade hydrochloric acid with high purity and low free chlorine.
In the above system, as a preferred embodiment, during a single rectification, the industrial-grade hydrochloric acid is heated and rectified by a multi-stage heating manner, as shown in fig. 2, the rectification apparatus 1 is formed by connecting 5 rectifiers 101 in series, a liquid phase outlet of a rectifier 101 is connected to a raw material inlet of the next rectifier 101, gas-phase hydrochloric acid generated by multi-stage heating is collected uniformly, and finally obtained diluted hydrochloric acid is discharged and treated separately.
Further, for the chlorine removal device 3, the copper absorbing layer 303 is preferably formed by filling red copper or copper scraps, and has a porosity of 30 to 40%, a pore size of 1 to 6mm, more preferably a porosity of 30%, and a pore size of 3 mm. Meanwhile, in order to enable the copper absorption layer 303 to be continuously used and improve the utilization rate of the copper absorption layer, the chlorine removal device 3 is further provided with a pure water interface 304, as shown in fig. 4, the pure water interface 304 is used for connecting a pure water conveying pipeline (not shown), and the pure water interface 304 is positioned on the upper part of the copper absorption layer 303 and is connected with the copper absorption layer 303. When the contact surface of the copper absorption layer 303 and hydrochloric acid is shielded by impurities such as copper chloride and the like to influence the contact of copper and free chlorine, the impurities on the surface of the copper absorption layer 303 are removed in a pure water leaching mode, and then the copper absorption layer can be reused.
Further, during secondary rectification, the liquid hydrochloric acid obtained by the secondary rectification is used as the hydrochloric acid raw material of the primary rectification for return use. Even if the liquid hydrochloric acid after secondary rectification contains a certain amount of copper chloride, the copper chloride is not enriched in the high-purity hydrochloric acid after rectification but remains in the dilute hydrochloric acid due to the high boiling point of the copper chloride when the copper chloride is recycled, so that the liquid hydrochloric acid after secondary rectification can be effectively recovered.
According to the system for continuously removing the free chlorine by hydrochloric acid, the free chlorine in the hydrochloric acid is reduced by using the copper absorption layer, the content of the free chlorine in the hydrochloric acid does not need to be analyzed, an oxidant does not need to be used for removing redundant reducing agent, the consumption is low, the use cost is low, the continuous chlorine removing operation of the hydrochloric acid can be realized, the free chlorine in the hydrochloric acid can be finally reduced to be below 0.5ppm, the technical process is simple, the chlorine removing efficiency is high, and the defects of the existing chlorine removing technology are overcome.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the utility model, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. A system for continuously removing free chlorine by hydrochloric acid is characterized by comprising:
the rectifying device is used for rectifying the industrial grade hydrochloric acid for the first time and comprises a rectifier with a heat exchange structure, a liquid phase outlet of the rectifier is communicated with a dilute hydrochloric acid conveying pipeline, and a gas phase outlet of the rectifier is communicated with the dechlorination device through the conveying pipeline;
the dechlorination device is used for removing free chlorine in the gas-phase hydrochloric acid, a lower interface of the dechlorination device is communicated with a gas-phase outlet of the rectifying tower, an upper interface of the dechlorination device is communicated with a lower interface of the rectifying tower, a copper absorption layer is arranged in the dechlorination device and is positioned between the upper interface and the lower interface of the dechlorination device, and the gas-phase hydrochloric acid can pass through the copper absorption layer and reach the rectifying tower;
the rectifying tower and the condensing tower are respectively used for carrying out secondary rectification and condensation after the secondary rectification on the gas-phase hydrochloric acid after dechlorination, and an upper interface of the rectifying tower is communicated with the condensing tower through a conveying pipeline.
2. The system for continuously removing free chlorine by hydrochloric acid as claimed in claim 1, wherein the liquid phase outlet of the rectifying device is communicated with a dilute hydrochloric acid conveying pipeline, and the raw material inlet of the rectifying device is communicated with a hydrochloric acid raw material conveying pipeline.
3. The system for continuously removing the free chlorine by the hydrochloric acid as claimed in claim 2, wherein the liquid phase outlet of the rectifying tower is communicated with the raw material inlet of the rectifying device through a pipeline.
4. The system for continuously removing free chlorine with hydrochloric acid as claimed in claim 1, wherein the chlorine removing device is provided with a pure water port, and the pure water port is positioned at the upper part of the copper absorption layer and is communicated with the copper absorption layer.
5. The system for continuously removing free chlorine by hydrochloric acid as claimed in claim 1, wherein the copper absorption layer is formed by filling electrolytic red copper or copper scraps, and has a porosity of 30-40% and a pore size of 1-6 mm.
6. The system for continuously removing free chlorine from hydrochloric acid as claimed in any one of claims 1 to 5, wherein said rectifying means is formed by a plurality of rectifiers connected in series to form a plurality of heating sections.
7. The system for continuously removing free chlorine from hydrochloric acid as claimed in claim 6, wherein said rectifying means is formed by 5 rectifying devices connected in series.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202122215818.3U CN215691759U (en) | 2021-09-14 | 2021-09-14 | System for hydrochloric acid removes free chlorine in succession |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122215818.3U CN215691759U (en) | 2021-09-14 | 2021-09-14 | System for hydrochloric acid removes free chlorine in succession |
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| CN215691759U true CN215691759U (en) | 2022-02-01 |
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| CN202122215818.3U Active CN215691759U (en) | 2021-09-14 | 2021-09-14 | System for hydrochloric acid removes free chlorine in succession |
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