CN212450707U - Recycling device of high-purity graphite impregnation waste acid liquid - Google Patents
Recycling device of high-purity graphite impregnation waste acid liquid Download PDFInfo
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- CN212450707U CN212450707U CN202020355644.3U CN202020355644U CN212450707U CN 212450707 U CN212450707 U CN 212450707U CN 202020355644 U CN202020355644 U CN 202020355644U CN 212450707 U CN212450707 U CN 212450707U
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Abstract
The utility model provides a recycling device of high-purity graphite dipping waste acid liquid, which comprises a graphite dipping waste acid storage tank, an evaporator, a condenser, a recycling acid storage tank and a vacuum system which are connected in sequence; the evaporator is connected with a steam circulating heater and is used for circularly heating the evaporator; the condenser is made of PTFE impregnated graphite, and the evaporator is of a steel lining PTFE structure. The condenser and the evaporator are arranged, so that the condenser is ensured not to be corroded in the mixed acid environment; and simultaneously the utility model discloses still set up circulation heater in the evaporimeter outside, for the evaporation is mixed sour and is provided required heat energy, makes the utility model discloses well evaporation recovery spent acid can successfully be implemented, and, the utility model provides a recycle device is more than 98% to the rate of recovery of high-purity graphite flooding spent acid liquid.
Description
Technical Field
The utility model discloses graphite treatment technical field especially relates to a recycle device of high-purity graphite flooding pickle.
Background
The graphite ore existing in the nature is basically symbiotic with natural feldspar ore, silicate and other ores, although the graphite ore is purified by adopting a flotation technology, the graphite ore with the purity of about 95 percent can be finally obtained, and the requirements of downstream enterprises cannot be met.
The existing processes for preparing high-purity graphite include hydrofluoric acid method, sodium hydroxide method, high-temperature method and the like. However, hydrofluoric acid has the advantages of low production cost, low energy consumption, stable production and the like, and is adopted by many graphite purification enterprises.
The purification process of the hydrofluoric acid from the graphite adopts mixed acid of hydrofluoric acid, nitric acid and hydrochloric acid with certain concentration to react with the graphite raw material at a certain temperature, so that metal ions, silicate and other impurities in the graphite raw material react to convert the solid matter insoluble in water into chloride, fluoride and nitrate which can be dissolved in water, and then the metal salts are separated from the graphite through a solid-liquid separation technology to obtain the high-purity graphite.
However, at present, there is no ideal process for the waste acid solution (waste acid from impregnation) generated by treating graphite by hydrofluoric acid method, and the waste acid solution is usually diluted by water and then neutralized by lime milk and discharged. The treatment process not only generates a large amount of solid waste, but also the concentration of the fluorine ions in the neutralized water body far exceeds the national discharge standard. Therefore, the existence and the development of the graphite hydrofluoric acid purification process are seriously restricted.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a recycle device of high-purity graphite flooding pickle liquor, the utility model provides a recycle device can retrieve almost all fluoride ion, chloride ion and nitrate ion in the flooding waste acid, obtains mixing acid with the recovery of graphite flooding acid nearly the same concentration, can normally be used for the graphite purification after the ratio of properly adjusting various sour, does not have any harmful effects to the graphite purification.
The utility model provides a recycling device of high-purity graphite dipping waste acid liquid, which is characterized by comprising a graphite dipping waste acid storage tank, an evaporator, a condenser, a recycling acid storage tank and a vacuum system which are connected in sequence;
the evaporator is connected with a steam circulating heater and is used for continuously heating the evaporator;
the condenser is a tetrafluoro impregnated graphite condenser, and the evaporator is of a steel lining polytetrafluoroethylene structure.
Preferably, the vacuum system comprises a circulating water pool, a circulating water pump and a water jet vacuum pump which are connected in sequence;
the water jet vacuum pump is communicated with the recovered acid storage tank.
Preferably, the condenser is provided with a cooling water inlet and a cooling water outlet.
Preferably, the condenser is a block-hole tetrafluoro-impregnated graphite heat exchanger.
Preferably, the thickness of the polytetrafluoroethylene lining is 3-40 mm.
The utility model provides a recycling device of high-purity graphite dipping waste acid liquid, which comprises a graphite dipping waste acid storage tank, an evaporator, a condenser, a recycling acid storage tank and a vacuum system which are connected in sequence; the evaporator is connected with a steam circulating heater and is used for circularly heating the evaporator; the condenser is made of PTFE impregnated graphite, and the evaporator is of a steel lining PTFE structure. The condenser and the evaporator are arranged, so that the condenser is ensured not to be corroded in the mixed acid environment; and simultaneously the utility model discloses still set up circulation heater in the evaporimeter outside, for the evaporation is mixed sour and is provided required heat energy, makes the utility model discloses well evaporation recovery spent acid can successfully be implemented, and, the utility model provides a recycle device is more than 98% to the rate of recovery of high-purity graphite flooding spent acid liquid.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a recycling device of the middle and high purity graphite dipping waste acid liquid of the utility model;
wherein, 1 is a graphite dipping waste acid storage tank, 2 is a steam circulation heater, 3 is an evaporator, 4 is a condenser, 5 is a recovered acid storage tank, 6 is a circulating water tank, 7 is a circulating water pump, and 8 is a water jet vacuum pump.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
The utility model provides a recycling device of high-purity graphite dipping waste acid liquid, which comprises a graphite dipping waste acid storage tank, an evaporator, a condenser, a recycling acid storage tank and a vacuum system which are connected in sequence;
the evaporator is connected with a steam circulating heater and is used for circularly heating the evaporator;
the condenser and the steam circulating heater are made of tetrafluoro impregnated graphite materials, and the evaporator is of a steel lining polytetrafluoroethylene structure.
The utility model discloses well high-purity graphite flooding spent acid liquid's recycle device refers to fig. 1 the utility model discloses in, graphite flooding spent acid storage tank is used for holding the graphite flooding spent acid of collecting, the utility model discloses it is right the size of graphite flooding spent acid storage tank does not have special requirement the utility model discloses in, the material of graphite flooding spent acid storage tank is preferred to be engineering plastics.
The utility model discloses in, the evaporimeter is provided with the feed inlet, and the top is provided with the export, the feed inlet with the export of graphite flooding spent acid storage tank is linked together through the pipeline, the export at top with the top entry of condenser is linked together for the mixed acid gas of output hydrochloric acid, hydrofluoric acid and nitric acid.
The utility model discloses in, the evaporimeter is steel inside lining polytetrafluoroethylene structure, can guarantee that the evaporimeter is not corroded under the environment of mixed acid.
And a steam circulating heater is arranged outside the evaporator, and the heat energy required by evaporating the mixed acid is continuously provided for the evaporating process. To the utility model relates to a latent heat of the spent acid that the graphite pickling produced is less than the required heat energy of mixed acid of evaporation far away, must constantly heat in the recovery process, could reach the rate of recovery more than 98%.
The utility model discloses in, the import of condenser with the top export of evaporimeter is linked together, and the bottom export is linked together with the import of retrieving sour storage tank, the condenser still is provided with cooling water import and cooling water export, and the acid mixing gas of evaporimeter output is the mixed acid liquid by the cooling water cooling in the condenser, gets into from the condenser and retrieves sour storage tank.
The utility model discloses in, the condenser is tetrafluoro impregnated graphite material, can guarantee that the condenser is inside not corroded under the environment of mixed acid.
The utility model discloses in, the recovery acid storage tank is used for storing the mixed acid that the evaporation was retrieved and is obtained, the recovery acid storage tank is linked together with vacuum system.
The utility model discloses in, vacuum system includes circulating water pond, circulating water pump and water shot vacuum pump, the water shot vacuum pump with it is linked together to retrieve the sour storage tank.
The utility model also provides a recycle technology of high-purity graphite flooding pickle liquor, including following step:
the recycling device is used, sulfuric acid with the concentration of 20-80% is added into the evaporator, and a vacuum system is started to ensure that the vacuum degree in the evaporator is more than or equal to 680 mmHg;
and then starting heating steam of the evaporator and cooling water of the condenser, introducing graphite dipping waste acid into the evaporator, wherein the evaporation temperature in the evaporator is 60-100 ℃, and obtaining recovered acid in a recovered acid storage tank.
The process is preferably implemented according to the following steps;
firstly, a certain amount of sulfuric acid with proper concentration is added into an evaporator, then a vacuum system consisting of a circulating water tank, a circulating water pump and a water jet vacuum pump is started, after the vacuum degree of an evaporation recovery system obtains a process requirement value, cooling water of a condenser and heating steam of a heater are started, the flow of waste acid in a graphite impregnated waste acid storage tank entering the evaporator is controlled, and pure recovered acid can be obtained at the moment. The recovered acid is added with nitric acid, hydrochloric acid and hydrofluoric acid in a proper amount, and the concentration of the recovered acid is adjusted to reach the technological requirement value, so that the recovered acid can be used for graphite impregnation and purification again.
The utility model discloses the preferred flooding spent acid that produces in the high-purity graphite production process and graphite cleaning wastewater carry out the reposition of redundant personnel and handle, collect the back to the flooding waste liquid of wherein high concentration, carry out recovery processing alone. The utility model discloses the high-purity graphite waste acid that uses indicates is the high concentration impregnation waste liquid of independent recovery processing.
In the present invention, the concentration of the sulfuric acid is preferably 20 to 80%, more preferably 30 to 70%, most preferably 40 to 60%, and specifically, in the embodiment of the present invention, it may be 30%, 45% or 50%. The concentration of sulfuric acid in the evaporator directly affects the recovery rate of the recovered graphite impregnation waste liquid and the evaporation recovery rate of the system. Because the solubility of 1, fluoride ions, chloride ions and nitrate ions in the liquid is related to the concentration of hydrogen ions in the liquid, the higher the concentration of the hydrogen ions is, the higher the probability of the hydrogen ions being converted into corresponding acid molecules is, namely, the ions can be more easily converted into acid molecules to escape from the liquid into gas and be condensed into pure recovered acid; the concentration of the sulfuric acid in the evaporator also affects the temperature of the sulfuric acid circulating liquid, and the higher the concentration of the sulfuric acid is, the higher the evaporation temperature is, and the lower the evaporation speed is. Therefore, the recovery rate of the graphite impregnation waste acid can be ensured by controlling the proper concentration of the sulfuric acid, and the recovery efficiency of the system can also be ensured.
The utility model provides a system's vacuum directly influences system's stability. Because the mixed acid of nitric acid, hydrochloric acid and hydrofluoric acid has very strong corrosivity, at present, no metal or alloy can not be corroded, nonmetal, glass and other materials can be corroded quickly, only a part of artificially synthesized organic polymer materials can be adopted, and the high temperature resistance of the organic polymer materials is not ideal. Therefore, the evaporation temperature must be controlled to be less than or equal to 100 ℃, specifically, in the embodiment of the present invention, 60 ℃, 70 ℃ or 80 ℃; the vaporization temperature of a liquid is a function of the pressure of its environment, and therefore the vacuum of the system must be tightly controlled to ensure that the vaporization temperature is below the safe temperature that the equipment materials can withstand. The utility model discloses require the vacuum degree of system to be not less than 680mmHg post, it is specific, in the embodiment of the utility model, can be 700mmHg posts or 730mmHg posts.
The utility model provides a recycling device of high-purity graphite dipping waste acid liquid, which comprises a graphite dipping waste acid storage tank, an evaporator, a condenser, a recycling acid storage tank and a vacuum system which are connected in sequence; the evaporator is connected with a steam circulating heater and is used for circularly heating the evaporator; the condenser is made of PTFE impregnated graphite, and the evaporator adopts a steel lining PTFE structure. The condenser is not corroded in the mixed acid environment; simultaneously the utility model discloses still set up steam circulation heater in the evaporimeter outside, for the evaporimeter lasts the spent acid evaporation that provides the graphite pickling production and mix the required heat energy of sour, make the utility model discloses well evaporation recovery spent acid can successfully be implemented, and, the utility model provides a recycle device is more than 98% to the rate of recovery of high-purity graphite pickle.
The following examples are all carried out using the apparatus of FIG. 1
Example 1
Firstly, adding 50% sulfuric acid into an evaporator, then starting a vacuum system consisting of a circulating water pool, a circulating water pump and a water jet vacuum pump to ensure that the vacuum degree of the evaporation recovery system reaches 730mmHg, then starting cooling water of a condenser and heating steam of a heater to ensure that the evaporation temperature in the evaporator is 70 ℃, and controlling the flow of waste acid in a graphite impregnation waste acid storage tank into the evaporator, thereby obtaining pure graphite impregnation recovered acid. The recovery rate was 98%.
The recovered acid is added with nitric acid, hydrochloric acid and hydrofluoric acid in a proper amount, and the concentration of the recovered acid is adjusted to reach the process requirement value, so that the recovered acid can be used for graphite impregnation and purification again.
Example 2
Firstly, adding 45% sulfuric acid into an evaporator, then starting a vacuum system consisting of a circulating water tank, a circulating water pump and a water jet vacuum pump to ensure that the vacuum degree of the evaporation recovery system reaches 700mmHg, then starting cooling water of a condenser and heating steam of a heater to ensure that the evaporation temperature in the evaporator is 80 ℃, and controlling the flow of waste acid in a graphite impregnation waste acid storage tank into the evaporator, thereby obtaining pure graphite impregnation recovered acid. The recovery rate was 95%.
The recovered acid is added with nitric acid, hydrochloric acid and hydrofluoric acid in a proper amount, and the concentration of the recovered acid is adjusted to reach the process requirement value, so that the recovered acid can be used for graphite impregnation and purification again.
Example 3
Firstly, adding sulfuric acid with the concentration of 30% into an evaporator, then starting a vacuum system consisting of a circulating water tank, a circulating water pump and a water jet vacuum pump to ensure that the vacuum degree of the evaporation recovery system reaches 730mmHg, then starting cooling water of a condenser and heating steam of a heater to ensure that the evaporation temperature in the evaporator is 60 ℃, and controlling the flow of waste acid in a graphite impregnation waste acid storage tank into the evaporator, thereby obtaining pure graphite impregnation recovered acid. The recovery was 92%.
The recovered acid is added with nitric acid, hydrochloric acid and hydrofluoric acid in a proper amount, and the concentration of the recovered acid is adjusted to reach the process requirement value, so that the recovered acid can be used for graphite impregnation and purification again.
Claims (5)
1. A device for recycling high-purity graphite impregnation waste acid liquid is characterized by comprising a graphite impregnation waste acid storage tank, an evaporator, a condenser, a recovered acid storage tank and a vacuum system which are sequentially connected;
the evaporator is connected with a steam circulating heater and is used for continuously heating the evaporator;
the condenser is a tetrafluoro impregnated graphite condenser, the steam circulating heater is a tetrafluoro impregnated graphite steam circulating heater, and the evaporator is of a steel lining polytetrafluoroethylene structure.
2. The recycling device according to claim 1, wherein the vacuum system comprises a circulating water tank, a circulating water pump and a water jet vacuum pump which are connected in sequence;
the water jet vacuum pump is communicated with the recovered acid storage tank.
3. The recycling apparatus according to claim 1, wherein the condenser is provided with a cooling water inlet and a cooling water outlet.
4. The recycling apparatus according to claim 1, wherein the condenser is a block-hole tetrafluoro-impregnated graphite heat exchanger.
5. The recycling device according to claim 1, wherein the polytetrafluoroethylene lining has a thickness of 3 to 40 mm.
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| CN202020355644.3U CN212450707U (en) | 2020-03-19 | 2020-03-19 | Recycling device of high-purity graphite impregnation waste acid liquid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072233A (en) * | 2021-04-12 | 2021-07-06 | 大同氢都驰拓新能源有限公司 | Treatment method for treating acid wastewater for graphite purification |
| CN113479852A (en) * | 2021-08-10 | 2021-10-08 | 黑龙江普莱德新材料科技有限公司 | Waste acid liquid recycling and regenerating system and method |
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2020
- 2020-03-19 CN CN202020355644.3U patent/CN212450707U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072233A (en) * | 2021-04-12 | 2021-07-06 | 大同氢都驰拓新能源有限公司 | Treatment method for treating acid wastewater for graphite purification |
| CN113072233B (en) * | 2021-04-12 | 2023-03-17 | 大同氢都驰拓新能源有限公司 | Treatment method for treating acidic wastewater generated in graphite purification |
| CN113479852A (en) * | 2021-08-10 | 2021-10-08 | 黑龙江普莱德新材料科技有限公司 | Waste acid liquid recycling and regenerating system and method |
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