CN109536740B - Method for preparing cesium sulfate from salt-containing wastewater - Google Patents
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Abstract
The invention relates to the field of high-value products recovered from industrial wastes, in particular to a method for preparing cesium sulfate from salt-containing wastewater204And kerosene, mixing t-BAMBP, P204Mixing with kerosene to prepare an extracting agent, detecting the ion concentration of a feed liquid, taking salt-containing wastewater to adjust the pH value, carrying out multi-stage countercurrent extraction on the feed liquid by using a post-extracting agent to prepare a loaded organic phase, carrying out circulating countercurrent washing on the loaded organic phase by using a washing liquid, preparing a back-extracting agent, carrying out back-extraction, and finally evaporating to prepare cesium sulfate. Realizes the separation and extraction of cesium in the salt-containing wastewater, provides a method based on t-BAMBP and P under the alkaline condition by utilizing the alkalescence of the salt-containing wastewater204And (4) synergistically extracting cesium in the saline wastewater.
Description
Technical Field
The invention relates to the field of high-value products recovered from industrial wastes, in particular to a method for preparing cesium sulfate from salt-containing wastewater.
Background
Rubidium and cesium are used as important scarce alkali metal resources and widely used in the fields of industrial catalysis, medicine, special glass and the like, the existing method for separating rubidium and cesium mostly adopts distributed precipitation, fractional crystallization, ion exchange and solvent extraction, and solvent extraction is often adopted for obtaining high-quality rubidium and cesium.
In the field of comprehensive recovery of solid hazardous wastes and the process of washing high-chlorine-content materials, rubidium and cesium elements are contained in the produced salt-containing wastewater, in the process of washing the chlorine-containing materials, in order to improve the chlorine washing effect, alkaline auxiliary materials such as caustic soda flakes and soda ash are added, the pH value of the salt-containing wastewater is larger than 9, and in order to reduce the subsequent treatment capacity of the salt-containing wastewater, after multiple cycles, the salt content of the wastewater is higher, meanwhile, rubidium and cesium are also enriched to a higher level, and the high recovery value is achieved.
The performance of BAMBP is optimal in a system for separating rubidium and cesium by using a solvent extraction method, while BAMBP cannot be produced in batches at home and is high in price, so that the cost for separating rubidium and cesium is high, and the recovery rate cannot reach a high level.
The invention patent with the publication number of CN107254589A discloses a method for separating and extracting rubidium and cesium in salt lake brine by a t-BAMBP extraction method, which is intended to recover rubidium and cesium in acidic brine by the extraction method, but is not suitable for alkaline saline wastewater, and meanwhile, cesium in a loaded organic phase enters washing liquid by washing with high acid in a washing section, so that rubidium, cesium and potassium cannot be separated in the washing liquid at the same time, and cesium cannot be enriched and purified, and the method is not suitable for industrial production.
Disclosure of Invention
The invention provides a method for separating and extracting cesium element from salt-containing wastewater based on t-BAMBP and P under alkaline conditions by utilizing alkalescence of the salt-containing wastewater204A method for synergistically extracting cesium in salt-containing wastewater.
The invention solves the technical problem and adopts the technical scheme that the method for preparing cesium sulfate from salt-containing wastewater comprises the following steps:
firstly, preparing an extracting agent, taking t-BAMBP and P204And kerosene, mixing t-BAMBP, P204Mixing with kerosene to obtain an extracting agent;
secondly, detecting the ion concentration of the feed liquid, and detecting Cs in the saline wastewater by an atomic absorption spectrometry+、Rb+、K+And Na+Concentration;
thirdly, taking the salt-containing wastewater to adjust the pH value, and adjusting the pH value of the salt-containing wastewater by using an alkaline substance to prepare a feed liquid;
fourthly, performing multi-stage countercurrent extraction on the feed liquid by using the post-extractant to prepare a loaded organic phase;
fifthly, carrying out circulating countercurrent washing on the loaded organic phase through a washing liquid to prepare a washed loaded organic phase;
sixthly, preparing a stripping agent, and preparing the stripping agent containing sulfuric acid by using water and sulfuric acid;
seventhly, performing back extraction, namely performing back extraction on the washed loaded organic phase prepared in the fifth step by using the back extractant prepared in the sixth step to prepare a cesium sulfate solution;
and step eight, evaporating, namely evaporating the cesium sulfate solution prepared in the step seven to prepare cesium sulfate.
Further, in the first step, t-BAMBP accounts for 15-20 parts by weight, and P2045 parts of kerosene and 75-80 parts of kerosene.
Further, second step, Cs+The concentration is 0.1-1.2 g/L, Rb+The concentration is 0.2-1.2 g/L, K+The concentration of Na is 25-45 g/L+The concentration is 30-80 g/L.
And further, in the third step, the alkaline substances are sodium carbonate, sodium hydroxide and liquid alkali, the pH is adjusted to be more than 13, and the adding mode comprises the steps of dissolving the sodium carbonate or the sodium hydroxide and then adding the sodium carbonate or the sodium hydroxide in a liquid form, or directly reinforcing the solid in a reaction tank to uniformly mix the salt-containing wastewater and the alkali.
And furthermore, in the fourth step, compared with the step (O: A), the ratio of (O: A) is 1-5: 1, stirring is self-suction stirring in the extraction process, the linear speed of stirring is 5-8 m/s, the extraction stage number is 3-5 stages of extraction, countercurrent extraction is performed, and the pH of the extracted raffinate is controlled to be more than 8.
Optionally, in the fifth step, the ratio of the washing section (O: A) to the washing section (O: A) is 2-4: 1, the water washing liquid is industrial production water, two-stage countercurrent washing is carried out, the water is discharged when the potassium content in the washing liquid reaches 50g/L, new water washing liquid is added, and the pH value of the washing water is larger than 9 after circulation.
Optionally, in the sixth step, sulfuric acid with a concentration of 98% is added to industrial process water to prepare a product containing SO2 2->20g/L。
And further, in the seventh step, 2-4 stages of countercurrent extraction are used for back extraction, the ratio (O: A) is 3-8: 1, the solution after back extraction contains 20g/L sulfuric acid, concentrated sulfuric acid is slowly added in the back extraction process to supplement free acid, and when the concentration of the cesium in the solution is more than 60g/L, cesium sulfate is prepared.
And further, in the eighth step, carrying out evaporation concentration on the cesium sulfate solution, wherein the temperature of the solution is 90-120 ℃ in the evaporation process, a large amount of crystals are separated out, filtering to obtain cesium sulfate crystals, and drying to obtain cesium sulfate products.
The beneficial effects of the invention at least comprise one of the following;
1. in an alkaline washing solution, rubidium and cesium and other cations are separated to the maximum extent in the extraction process by controlling the pH value of the solution, the extraction rate of cesium is more than 95%, and when the cesium is washed by industrial production water, partial residual alkali is brought into an organic phase, rubidium, potassium and the like are effectively separated again, and the quality of a subsequent cesium sulfate product is guaranteed.
2. The method solves the problem that the cost for separating rubidium and cesium is high due to the fact that BAMBP cannot be produced in batches at home and is high in price although the performance of BAMBP is optimal in the existing system for separating rubidium and cesium by using a solvent extraction method.
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FIG. 1 is a schematic diagram of a process for preparing cesium sulfate from saline wastewater;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly apparent, the present invention is further described in detail below with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the scope of the invention.
Example 1
As shown in fig. 1, a method for preparing cesium sulfate from salt-containing wastewater comprises the following steps:
firstly, preparing an extracting agent, taking t-BAMBP and P204And kerosene, mixing t-BAMBP, P204Mixing with kerosene to obtain an extracting agent;
secondly, detecting the ion concentration of the feed liquid, and detecting Cs in the saline wastewater by an atomic absorption spectrometry+、Rb+、K+And Na+Concentration;
thirdly, taking the salt-containing wastewater to adjust the pH value, and adjusting the pH value of the salt-containing wastewater by using an alkaline substance to prepare a feed liquid;
fourthly, performing multi-stage countercurrent extraction on the feed liquid by using the post-extractant to prepare a loaded organic phase;
fifthly, carrying out circulating countercurrent washing on the loaded organic phase through a washing liquid to prepare a washed loaded organic phase;
sixthly, preparing a stripping agent, and preparing the stripping agent containing sulfuric acid by using water and sulfuric acid;
seventhly, performing back extraction, namely performing back extraction on the washed loaded organic phase prepared in the fifth step by using the back extractant prepared in the sixth step to prepare a cesium sulfate solution;
and step eight, evaporating, namely evaporating the cesium sulfate solution prepared in the step seven to prepare cesium sulfate.
During use, rubidium and cesium and other cations are separated to the maximum extent in the extraction process by controlling the pH value of the solution in an alkaline washing solution, the extraction rate of cesium is more than 95%, and when the solution is washed by industrial production water, partial residual alkali is brought into an organic phase, rubidium, potassium and the like are effectively separated again, and the quality of a subsequent cesium sulfate product is guaranteed. The method solves the problem that the cost for separating rubidium and cesium is high due to the fact that BAMBP cannot be produced in batches at home and is high in price although the performance of BAMBP is optimal in the existing system for separating rubidium and cesium by using a solvent extraction method.
Example 2
A method for preparing cesium sulfate from salt-containing wastewater comprises the following steps:
firstly, preparing an extracting agent, taking t-BAMBP and P204And kerosene, mixing t-BAMBP, P204Mixing with kerosene to obtain 15 portions of t-BAMBP and P2045 parts and 75 parts of kerosene;
secondly, detecting the ion concentration of the feed liquid, and detecting Cs in the saline wastewater by an atomic absorption spectrometry+、Rb+、K+And Na+Concentration, Cs+The concentration is 0.1g/L, Rb+The concentration is 0.2g/L, K+The concentration is 25g/L, Na+The concentration is 30 g/L;
thirdly, taking the salt-containing wastewater to adjust the PH value, and adjusting the PH value of the salt-containing wastewater by using alkaline substances to prepare feed liquid, wherein the alkaline substances are sodium carbonate, sodium hydroxide and caustic soda liquid, and the pH value is adjusted to be more than 13, and the adding mode comprises the steps of dissolving the sodium carbonate or the sodium hydroxide and then adding the sodium carbonate or the sodium hydroxide in a liquid form to uniformly mix the salt-containing wastewater and the caustic soda;
fourthly, performing multi-stage countercurrent extraction on the feed liquid by using the post-extraction agent to prepare a loaded organic phase, wherein the ratio (O: A) is 1:1, the stirring is self-suction stirring in the extraction process, the linear speed of the stirring is 5m/s, the extraction stage number is 3-stage extraction, the countercurrent extraction is performed, and the pH of the extracted raffinate is controlled to be more than 8;
fifthly, carrying out circulating countercurrent washing on the loaded organic phase through a washing liquid to prepare a washed loaded organic phase, wherein the washing section phase ratio (O: A) is 2:1, the washing liquid is industrial production water, carrying out two-stage countercurrent washing, discharging when potassium in the washing liquid reaches 50g/L, adding new washing liquid, and the pH of the washing water after circulation is more than 9;
sixthly, preparing a stripping agent, preparing the stripping agent containing the sulfuric acid by using water and the sulfuric acid, adding the sulfuric acid with the concentration of 98 percent into industrial production water, and preparing the stripping agent containing the SO2 2-A stripping agent of more than 20 g/L;
seventhly, performing back extraction, namely performing back extraction on the washed loaded organic phase prepared in the fifth step by using the back extractant prepared in the sixth step to prepare a cesium sulfate solution, wherein the back extraction adopts 2-level countercurrent extraction, the solution after back extraction contains 20g/L sulfuric acid compared with (O: A) of 3:1, concentrated sulfuric acid is slowly added to supplement free acid in the back extraction process, and when the concentration of the cesium solution is more than 60g/L, the cesium sulfate is prepared;
and eighthly, evaporating, namely evaporating the cesium sulfate solution prepared in the seventh step to prepare cesium sulfate, wherein the cesium sulfate solution is evaporated and concentrated, the temperature of the solution is 90 ℃ in the evaporation process, a large amount of crystals are separated out, filtering is carried out to obtain cesium sulfate crystals, and the cesium sulfate products are obtained after drying.
During use, rubidium and cesium and other cations are separated to the maximum extent in the extraction process by controlling the pH value of the solution in an alkaline washing solution, the extraction rate of cesium is more than 95%, and when the solution is washed by industrial production water, partial residual alkali is brought into an organic phase, rubidium, potassium and the like are effectively separated again, and the quality of a subsequent cesium sulfate product is guaranteed. The method solves the problem that the cost for separating rubidium and cesium is high due to the fact that BAMBP cannot be produced in batches at home and is high in price although the performance of BAMBP is optimal in the existing system for separating rubidium and cesium by using a solvent extraction method.
Example 3
A method for preparing cesium sulfate from salt-containing wastewater comprises the following steps:
firstly, preparing an extracting agent, taking t-BAMBP and P204And kerosene, mixing t-BAMBP, P204Mixing with kerosene to obtain 20 parts by weight of t-BAMBP, and P2045 parts and 80 parts of kerosene;
secondly, detecting the ion concentration of the feed liquid, and detecting Cs in the saline wastewater by an atomic absorption spectrometry+、Rb+、K+、Na+Concentration, Cs+The concentration is 1.2g/L, Rb+The concentration is 1.2g/L, K+The concentration is 45g/L, Na+The concentration is 80 g/L;
thirdly, taking the salt-containing wastewater to adjust the PH value, and adjusting the PH value of the salt-containing wastewater by using alkaline substances to prepare feed liquid, wherein the alkaline substances are sodium carbonate, sodium hydroxide and caustic soda liquid, and the pH value is adjusted to be more than 13, and the adding mode comprises the steps of dissolving the sodium carbonate or the sodium hydroxide and then adding the sodium carbonate or the sodium hydroxide in a liquid form to uniformly mix the salt-containing wastewater and the caustic soda;
fourthly, performing multi-stage countercurrent extraction on the feed liquid by using the post-extraction agent to prepare a loaded organic phase, wherein the ratio (O: A) is 5:1, the stirring is self-suction stirring in the extraction process, the linear speed of the stirring is 8m/s, the extraction stage number is 5-stage extraction, the countercurrent extraction is performed, and the pH of the extracted raffinate is controlled to be more than 8;
fifthly, carrying out circulating countercurrent washing on the loaded organic phase through a washing liquid to prepare a washed loaded organic phase, wherein the washing section phase ratio (O: A) is 4:1, the washing liquid is industrial production water, carrying out two-stage countercurrent washing, discharging when potassium in the washing liquid reaches 50g/L, adding new washing liquid, and the pH of the washing water after circulation is more than 9;
sixthly, preparing a stripping agent, preparing the stripping agent containing the sulfuric acid by using water and the sulfuric acid, adding the sulfuric acid with the concentration of 98 percent into industrial production water, and preparing the stripping agent containing the SO2 2-A stripping agent of more than 20 g/L;
seventhly, performing back extraction, namely performing back extraction on the washed loaded organic phase prepared in the fifth step by using the back extractant prepared in the sixth step to prepare a cesium sulfate solution, wherein the back extraction adopts 4-level countercurrent extraction, the ratio of (O: A) to (O: A) is 8:1, the back extraction solution contains 20g/L sulfuric acid, concentrated sulfuric acid is slowly added to supplement free acid in the back extraction process, and when the concentration of the cesium solution is more than 60g/L, the cesium sulfate is prepared;
and eighthly, evaporating, namely evaporating the cesium sulfate solution prepared in the seventh step to prepare cesium sulfate, wherein the cesium sulfate solution is evaporated and concentrated, the temperature of the solution is 120 ℃ in the evaporation process, a large amount of crystals are separated out, filtering is carried out to obtain cesium sulfate crystals, and the cesium sulfate products are obtained after drying.
During use, rubidium and cesium and other cations are separated to the maximum extent in the extraction process by controlling the pH value of the solution in an alkaline washing solution, the extraction rate of cesium is more than 95%, and when the solution is washed by industrial production water, partial residual alkali is brought into an organic phase, rubidium, potassium and the like are effectively separated again, and the quality of a subsequent cesium sulfate product is guaranteed. The method solves the problem that the cost for separating rubidium and cesium is high due to the fact that BAMBP cannot be produced in batches at home and is high in price although the performance of BAMBP is optimal in the existing system for separating rubidium and cesium by using a solvent extraction method.
Example 4
Preparing organic phase according to the proportion of the steps, taking the salt-containing wastewater and detecting Cs in the salt-containing wastewater+、Rb+、K+、Na+And (3) adding alkali into the salt-containing wastewater to enable the pH value to be more than 13 to obtain a feed liquid, and performing 5-stage countercurrent extraction on the prepared organic phase and the feed liquid at a ratio (O: A) of 5:1, wherein stirring in the extraction process is self-suction stirring, and the stirring linear speed is 5 m/s. The control ratio of the production water for the washing section (O: A) is 4: 1. Carrying out two-stage countercurrent washing on the loaded organic phase, controlling the pH to be more than 9 when the potassium content of the washed liquid is less than 50g/l, continuously using the washed liquid as washing water, discharging the washed liquid when the potassium content is more than 50g/l, carrying out 2-stage countercurrent back extraction on the organic phase by using water containing 20g/l of sulfuric acid, controlling the phase ratio (O: A) to be 3:1, controlling the content of the back-extracted liquid containing 20g/l of sulfuric acid in the back extraction process, slowly adding concentrated sulfuric acid to supplement free acid in the back extraction process, recycling the obtained product, and when the cesium concentration of the solution is more than 60g/l, evaporating the prepared cesium sulfate solution at the temperature of 110 DEG CAnd obtaining the cesium sulfate product.
Specific data are shown in the following table:
example 5
Preparing organic phase according to the proportion of the steps, taking the salt-containing wastewater and detecting Cs in the salt-containing wastewater+、Rb+、K+、Na+And (3) adding alkali into the salt-containing wastewater to enable the pH value to be more than 13 to obtain a feed liquid, wherein the ratio of the prepared organic phase to the feed liquid (O: A) is 3:1, 4-stage countercurrent extraction is carried out, the stirring in the extraction process is self-suction stirring, and the linear speed of the stirring is 8 m/s. The control ratio of the production water for the washing section (O: A) is 3: 1. And (2) carrying out two-stage countercurrent washing on the loaded organic phase, controlling the pH to be more than 9 when the potassium content of the washed liquid is less than 50g/l, continuously using the washed liquid as washing water, discharging the washed liquid when the potassium content is more than 50g/l, carrying out 3-stage countercurrent back extraction on the organic phase by using water containing 20g/l of sulfuric acid, controlling the ratio (O: A) to be 5:1, controlling the content of the back-extracted liquid containing 20g/l of sulfuric acid in the back extraction process, slowly adding concentrated sulfuric acid to supplement free acid in the back extraction process, recycling the obtained cesium sulfate solution, and evaporating the prepared cesium sulfate solution at the temperature of 90 ℃ when the cesium concentration of the solution is more than 60g/l to obtain a cesium sulfate product.
Specific data are shown in the following table:
example 6
Preparing an organic phase according to the proportion in the step 1, taking the salt-containing wastewater and detecting Cs in the salt-containing wastewater+、Rb+、K+、Na+Concentration, adding alkali into the salt-containing wastewater to make the pH value be greater than 13 to obtain feed liquid, making the prepared organic phase and feed liquid have a phase ratio (O: A) of 2:1, making 3-stage countercurrent extraction, extractingIn the process, the stirring is self-suction stirring, and the linear speed of the stirring is 7 m/s. The control ratio of the production water for the washing section (O: A) is 2: 1. And (2) carrying out two-stage countercurrent washing on the loaded organic phase, controlling the pH to be more than 9 when the potassium content of the washed liquid is less than 50g/l, continuously using the washed liquid as washing water, discharging the washed liquid when the potassium content is more than 50g/l, carrying out 4-stage countercurrent back extraction on the organic phase by using water containing 20g/l of sulfuric acid, controlling the ratio (O: A) to be 8:1, controlling the content of the back-extracted liquid containing 20g/l of sulfuric acid in the back extraction process, slowly adding concentrated sulfuric acid to supplement free acid in the back extraction process, recycling the obtained cesium sulfate solution, and evaporating the prepared cesium sulfate solution at the temperature of 120 ℃ when the cesium concentration of the solution is more than 60g/l to obtain a cesium sulfate product. Specific data are shown in the following table:
Claims (6)
1. a method for preparing cesium sulfate from salt-containing wastewater is characterized by comprising the following steps: the method comprises the following steps:
firstly, preparing an extracting agent, taking t-BAMBP and P204And kerosene, mixing t-BAMBP, P204Mixing with kerosene to obtain an extracting agent;
secondly, detecting the ion concentration of the feed liquid, and detecting Cs in the saline wastewater by an atomic absorption spectrometry+、Rb+、K+And Na+Concentration;
thirdly, taking the salt-containing wastewater to adjust the pH value, and adjusting the pH value of the salt-containing wastewater by using an alkaline substance to prepare a feed liquid;
and fourthly, performing multi-stage countercurrent extraction on the feed liquid by using the extractant to prepare a loaded organic phase, wherein compared with the weight ratio of O: a is 1-5: 1, stirring in the extraction process is self-suction stirring, the linear speed of stirring is 5-8 m/s, the extraction stage number is 3-5 stages of extraction, countercurrent extraction is performed, and the pH of the extracted raffinate is controlled to be more than 8;
and fifthly, carrying out circulating countercurrent washing on the loaded organic phase through a washing liquid to prepare a washed loaded organic phase, wherein the washing section is compared with the ratio of O: a is 2-4: 1, the washing liquid is industrial production water, two-stage countercurrent washing is carried out, when the potassium in the washing liquid reaches 50g/L, the washing liquid is discharged, new washing liquid is added, and the pH value of the washing water after circulation is more than 9;
sixthly, preparing a stripping agent, and preparing the stripping agent containing sulfuric acid by using water and sulfuric acid;
and seventhly, performing back extraction, namely performing back extraction on the washed loaded organic phase prepared in the fifth step by using the back extractant prepared in the sixth step to prepare a cesium sulfate solution, wherein the back extraction adopts 2-4 levels of countercurrent extraction, and compared with O: a is 3-8: 1, the solution after back extraction contains 20g/L sulfuric acid, concentrated sulfuric acid is slowly added in the back extraction process to supplement free acid, and when the cesium concentration of the solution is more than 60g/L, a cesium sulfate solution is prepared;
and step eight, evaporating, namely evaporating the cesium sulfate solution prepared in the step seven to prepare cesium sulfate.
2. The method for preparing cesium sulfate in saline wastewater according to claim 1, characterized by comprising the following steps: in the first step, t-BAMBP accounts for 15-20 parts by weight, and P2045 parts of kerosene and 75-80 parts of kerosene.
3. The method for preparing cesium sulfate in saline wastewater according to claim 2, characterized by comprising the following steps: the second step, Cs+The concentration is 0.1-1.2 g/L, Rb+The concentration is 0.2-1.2 g/L, K+The concentration of Na is 25-45 g/L+The concentration is 30-80 g/L.
4. The method for preparing cesium sulfate in saline wastewater according to claim 3, characterized by comprising the following steps: and thirdly, the alkaline substances are sodium carbonate and sodium hydroxide, the pH value is adjusted to be more than 13, the sodium carbonate or the sodium hydroxide is added in a liquid form after being dissolved, or the solid is directly reinforced in a reaction tank, so that the salt-containing wastewater and the alkali are uniformly mixed.
5. The method for preparing cesium sulfate in saline wastewater according to claim 4, wherein said method comprises the following steps: in the sixth step, sulfuric acid with the concentration of 98 percent is added into industrial production water to prepare the product containing SO4 2->20g/L。
6. The method for preparing cesium sulfate in saline wastewater according to claim 5, characterized by comprising the following steps: and step eight, carrying out evaporation concentration on the cesium sulfate solution, wherein the temperature of the solution is 90-120 ℃ in the evaporation process, filtering to obtain cesium sulfate crystals after a large amount of crystals are separated out, and drying to obtain cesium sulfate products.
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CN107254589A (en) * | 2017-07-06 | 2017-10-17 | 河北工程大学 | A kind of rubidium caesium in t BAMBP extractions separation and Extraction salt lake bittern |
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Denomination of invention: A method for preparing Caesium sulfate from salty wastewater Effective date of registration: 20230625 Granted publication date: 20210727 Pledgee: Gejiu Sub branch of Agricultural Bank of China Co.,Ltd. Pledgor: GREENNOVO ENVIRONMENTAL TECHNOLOGY CO.,LTD. Registration number: Y2023530000042 |