CN114735724B - Method for recycling low-water-content sodium bromide from wastewater - Google Patents
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- CN114735724B CN114735724B CN202210338124.5A CN202210338124A CN114735724B CN 114735724 B CN114735724 B CN 114735724B CN 202210338124 A CN202210338124 A CN 202210338124A CN 114735724 B CN114735724 B CN 114735724B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/10—Bromides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention discloses a method for recycling sodium bromide with low water content from waste water, which comprises the steps of removing sodium carbonate in waste water containing sodium carbonate and sodium bromide by adding acid, evaporating and concentrating the waste water after removing the sodium carbonate, crystallizing while the waste water is hot, and drying to obtain sodium bromide with low water content. The invention provides a solution to the problem of high water content of sodium bromide recovered from wastewater for the first time, and the method has the advantages of simple operation, low treatment cost, good treatment effect, and high purity and low water content of the finally obtained sodium bromide, thereby providing guidance and reference for the problem of high water content of sodium bromide.
Description
Technical Field
The invention relates to a method for recycling sodium bromide from wastewater, in particular to a method for recycling sodium bromide with low water content from wastewater, and belongs to the technical field of wastewater treatment.
Background
Sodium bromide plays an important role in pharmaceutical and chemical production, and sodium bromide is used as a tranquilizer, hypnotic agent and other medicaments in the pharmaceutical industry, and is widely used for preparing bromine and the like in the industry, so that sodium bromide wastewater is generated in various industries. The sodium bromide wastewater contains different components, some are wastewater containing sodium bromide only, some are wastewater containing sodium bromide mixed with other salts, some are wastewater containing sodium bromide and other organic components, and the like, and the wastewater treatment methods of different components are different. Theoretically, sodium bromide is concentrated and crystallized at a temperature lower than 50 ℃ to form crystal water, and concentrated and crystallized at a temperature higher than 50 ℃ to obtain anhydrous sodium bromide, so that a common mode for recovering sodium bromide from sodium bromide wastewater is a thermal concentration and crystallization method. However, in the actual treatment process, it was found that when wastewater containing sodium carbonate, sodium bromide and other components is treated, the sodium bromide obtained by thermal concentration crystallization has the problems of high moisture content and difficult drying out of the water, and even if the drying temperature is raised to 110 ℃, the water is difficult to be distilled out or dried out. The sodium bromide recovered from the wastewater has higher water content, which not only affects the purity and quality of sodium bromide, but also is easy to agglomerate and affects the use. Thus, reducing the moisture content of the recovered sodium bromide is an urgent problem to be solved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for reducing the water content of sodium bromide recovered from wastewater, which is simple to operate, has low water content of sodium bromide separated from wastewater containing sodium carbonate and sodium bromide, improves the purity and quality of sodium bromide, and provides a good thought for the treatment of wastewater containing sodium carbonate and sodium bromide.
In the experimental process, it was found that sodium bromide obtained by thermal concentration crystallization from waste water containing sodium carbonate and sodium bromide has a high water content, and even if dried at high temperature, it is difficult to achieve a low water content. Finally, through a great deal of research and experiments, the main reason for the problem is that when sodium carbonate and sodium bromide are simultaneously contained in the wastewater, three substances of sodium carbonate, sodium bromide and water react to form an xNa 2CO3-yNaBr-zH2 O hydrate system, and the hydrate system is stable, so that more water is taken out from the sodium bromide recovered by a thermal concentration crystallization mode, and the water is difficult to dry and remove, and even if the drying temperature is increased to 110 ℃, the water is difficult to evaporate or bake. Based on the discovery, the method provided by the invention is used for removing sodium carbonate in the wastewater in a targeted manner, and then reheating, concentrating and crystallizing to recover sodium bromide, so that the problem of high sodium bromide water content caused by sodium carbonate is solved, the purity and quality of sodium bromide are improved, and the economical efficiency is improved.
The specific technical scheme of the invention is as follows:
a method for recovering sodium bromide having a low water content from wastewater, the method comprising the steps of:
(1) Taking waste water containing sodium carbonate and sodium bromide, and adding acid to remove sodium carbonate in the waste water;
(2) Evaporating and concentrating the wastewater after removing sodium carbonate, and performing hot filtration after concentrating to obtain sodium bromide wet material;
(3) And drying the wet sodium bromide material to obtain the sodium bromide with low water content.
Furthermore, the wastewater contains sodium carbonate and sodium bromide, and the wastewater can be from the industries of medicine, chemical industry and the like. The salt in the wastewater is mainly sodium carbonate and sodium bromide, wherein the sodium bromide content is 10-90wt%, preferably 10-30wt%. The sodium carbonate content is 20wt% or less, the sodium carbonate content is not 0, and preferably, the sodium carbonate content is 1 to 20wt%.
Further, in the step (1), the acid for removing sodium carbonate may be various acids which do not affect crystallization or purity of sodium bromide, for example, aqueous hydrochloric acid, aqueous sulfuric acid, aqueous nitric acid, etc., preferably aqueous sulfuric acid. The concentration of each acid can be adjusted at will, for example, the concentration of the sulfuric acid aqueous solution can be in the range of 5-98wt%, and the removal effect is not affected. The sulfuric acid and other acids are added into the wastewater to convert sodium carbonate in the wastewater into sodium sulfate and other acid sodium salts, so that xNa 2CO3-yNaBr-zH2 O hydrate in the wastewater is destroyed, and the subsequent recovery of sodium bromide and the removal of water in the sodium bromide are facilitated.
Further, in the step (1), the acid such as sulfuric acid is slowly added to the wastewater under stirring, and for example, dropwise addition, batch addition or continuous slow addition may be adopted. Preferably, the adding speed of the acid is controlled so as to ensure that the temperature of the wastewater does not rise rapidly in the whole adding process, thereby avoiding the safety problem caused by boiling and splashing of the wastewater due to temperature surge. Preferably, the temperature of the wastewater is controlled to be kept within a range of 70 ℃ or lower under the intervention of an external cold source such as cooling water in the whole adding process.
Preferably, in step (1), if the acid added dropwise is a dilute acid, such as dilute sulfuric acid, the addition rate is controlled to keep the wastewater temperature during the whole addition at 50 ℃ and below, and if the acid added dropwise is a higher concentration, such as concentrated sulfuric acid, the addition rate is controlled to keep the wastewater temperature during the whole addition at 70 ℃ and below.
Further, in the step (1), after the acid is added, the reaction is continued for 10-20 min at a constant temperature.
Further, in the step (1), the molar ratio of hydrogen in the acid to carbonate in the sodium carbonate is 1.8-2.2:1, preferably 2:1, to ensure that sodium carbonate is just removed, e.g. the molar ratio of sulfuric acid to sodium carbonate is 0.9-1.1:1, preferably 1:1, when the acid is sulfuric acid; when the acid is hydrochloric acid, the mol ratio of hydrochloric acid to sodium carbonate is 1.8-2.2:1, preferably 2:1. The waste water contains no inorganic salts other than sodium carbonate, which can react with acid.
Further, in the step (1), when the acid reacts with sodium carbonate to form sodium acid salt, carbon dioxide and water, for example, when the acid is sulfuric acid, the sulfuric acid reacts with sodium carbonate to form sodium sulfate, carbon dioxide and water, when the sodium carbonate content in the wastewater is less than or equal to 1wt%, the formed sodium acid salt content is relatively low and cannot be precipitated with sodium bromide in the later crystallization process, so when the sodium carbonate content in the wastewater is less than or equal to 1wt%, the wastewater after removing sodium carbonate is directly subjected to thermal concentration crystallization to recover sodium bromide, but when the sodium carbonate content in the wastewater is more than or equal to 1wt% and less than or equal to 20wt%, the formed sodium acid salt content is increased and can be precipitated together with sodium bromide to affect the purity of sodium bromide, and therefore when the sodium carbonate content in the wastewater is more than or equal to 1wt% and less than or equal to 20wt%, the sodium acid salt content after removing sodium carbonate is firstly removed, the sodium acid salt which affects the purity is removed, and then the sodium bromide is recovered by thermal concentration crystallization.
In a specific embodiment of the invention, the acid is sulfuric acid, when the content of sodium carbonate in the wastewater is less than or equal to 1wt%, the formed sodium sulfate is also relatively low, and sodium bromide is not precipitated along with the sodium bromide in the later crystallization process, so when the content of sodium carbonate in the wastewater is less than or equal to 1wt%, the wastewater after removing sodium carbonate is directly subjected to thermal concentration crystallization to recover sodium bromide, the thermal concentration crystallization refers to the steps of carrying out reduced pressure evaporation concentration on the wastewater at 80-90 ℃ and concentrating to 30% of the original volume, and a large amount of crystals are precipitated at the moment, and filtering while the wastewater is hot. And (3) when the vacuum evaporation concentration is carried out, controlling the vacuum degree to be 0.06-0.07 mpa. However, when the content of sodium carbonate in the wastewater is more than 1wt% and less than or equal to 20wt%, the formed sodium sulfate is increased and possibly separated out together with sodium bromide to affect the purity of the sodium bromide, so when the content of sodium carbonate in the wastewater is more than 1wt% and less than or equal to 20wt%, the wastewater after removing the sodium carbonate is cooled to 0 ℃ for crystallization, sodium sulfate is separated, then the sodium bromide is recovered by reheating concentration crystallization, and the thermal concentration crystallization mode is consistent with the above.
Further, in the step (3), the obtained sodium bromide wet material is dried for 1h at the temperature of 80-90 ℃ to obtain a sodium bromide product. The purity of the recovered sodium bromide is high and is more than 98.9%, the water content is low and is less than or equal to 1.1wt%.
The invention researches the problem of high water content of sodium bromide recovered from wastewater containing sodium carbonate and sodium bromide, and discovers that under the condition that sodium carbonate and sodium bromide are contained in the wastewater, stable xNa 2CO3-yNaBr-zH2 O hydrate is formed, so that the water content of the sodium bromide is higher. The invention has the following beneficial effects:
1. The sodium carbonate in the wastewater is removed by sulfuric acid and other acids to destroy xNa 2CO3-yNaBr-zH2 O hydrate in the wastewater, the sulfuric acid and other acids and the sodium carbonate are preferably added according to the theoretical molar ratio, no impurity is introduced, no secondary pollution is generated, and the sodium acid salt with excessive content can be removed by means of low-temperature crystallization and the like, so that the purity of sodium bromide is not influenced, and the operation is simple.
2. The invention provides a solution to the problem of high water content of sodium bromide recovered from wastewater for the first time, and the method has the advantages of simple operation, low treatment cost, good treatment effect, and high purity and low water content of the finally obtained sodium bromide, thereby providing guidance and reference for the problem of high water content of sodium bromide.
Detailed Description
The present invention will be described in detail by way of specific examples, but the purpose and purpose of these exemplary embodiments are merely to illustrate the present invention, and are not intended to limit the actual scope of the present invention in any way.
In the examples described below, the moisture content was measured using a moisture meter (karl fischer principle) and the bromide content was measured using an ion chromatograph or titration method.
In the examples described below, the wastewater was from a process synthesis of the company technical project.
In the following examples, the concentrations are mass percent concentrations unless otherwise specified.
Example 1
1. The wastewater was taken, wherein the sodium bromide content was 20wt%, the sodium carbonate content was 0.25wt% and the pH was 7.
2. 200G of the wastewater is taken and placed in a container, 10wt% sulfuric acid solution is added under stirring according to the molar ratio of sodium carbonate to sulfuric acid of 1:1, sulfuric acid is added in a dropwise manner, the dropwise speed is controlled to be 3 seconds/drop, the condition that boiling splashing can not occur due to slow rising of the temperature of the wastewater is controlled, the temperature of the wastewater is maintained within the temperature range of 50 ℃ in the whole dropwise adding process, and the reaction is continued for 10 minutes after the dropwise adding is completed.
3. After the reaction is ended, the treated wastewater is evaporated and concentrated under reduced pressure at 80-90 ℃, the vacuum degree is 0.06-0.07 mpa, the concentration is stopped when the original volume is 30%, then the filtration is carried out while the wastewater is hot, the obtained filter cake is measured to have 96.38% of sodium bromide content and 3.17% of water content, and the filter cake is dried for 1h at 80-90 ℃ to obtain a sodium bromide product. The sodium bromide content in the dried sodium bromide product is 99.5 percent.
Example 2
1. The wastewater was taken, wherein the sodium bromide content was 20wt%, the sodium carbonate content was 0.25wt% and the pH was 7.
2. 200G of the wastewater is taken and placed in a container, 10wt% sulfuric acid solution is added under stirring according to the molar ratio of sodium carbonate to sulfuric acid of 1:0.9, sulfuric acid is added in a dropwise manner, the dropwise speed is controlled to be 3 seconds/drop, the condition that boiling splashing can not occur due to slow rising of the temperature of the wastewater is controlled, the temperature of the wastewater is maintained within the temperature range of 50 ℃ in the whole dropwise adding process, and the reaction is continued for 10 minutes after the dropwise adding is completed.
3. After the reaction is ended, the treated wastewater is evaporated and concentrated under reduced pressure at 80-90 ℃, the vacuum degree is 0.06-0.07 mpa, the concentration is stopped when the original volume is 30%, then the filtration is carried out while the wastewater is hot, the obtained filter cake is measured to have 92.45% of sodium bromide content and 7.46% of water content, and the filter cake is dried for 1h at 80-90 ℃ to obtain a sodium bromide product. The sodium bromide content in the dried sodium bromide product is 99.2 percent according to the measurement.
Example 3
1. The wastewater was taken, wherein the sodium bromide content was 20wt%, the sodium carbonate content was 0.25wt% and the pH was 7.
2. 200G of the wastewater is taken and placed in a container, 30wt% sulfuric acid solution is added under stirring according to the molar ratio of sodium carbonate to sulfuric acid of 1:1, sulfuric acid is added in a dropwise manner, the dropwise speed is controlled to be 3 seconds/drop, the condition that boiling splashing can not occur due to slow rising of the temperature of the wastewater is controlled, the temperature of the wastewater is maintained within the temperature range of 50 ℃ in the whole dropwise adding process, and the reaction is continued for 10 minutes after the dropwise adding is completed.
3. After the reaction is ended, the treated wastewater is evaporated and concentrated under reduced pressure at 80-90 ℃, the vacuum degree is 0.06-0.07 mpa, the concentration is stopped when the original volume is 30%, then the filtration is carried out while the wastewater is hot, the obtained filter cake is subjected to measurement of 96.20% of sodium bromide content and 3.77% of water content, and the filter cake is dried for 1h at 80-90 ℃ to obtain a sodium bromide product. The sodium bromide content in the dried sodium bromide product is 98.9 percent.
Example 4
1. The wastewater was taken, wherein the sodium bromide content was 20wt%, the sodium carbonate content was 0.75wt% and the pH was 7.
2. 200G of the wastewater is taken and placed in a container, 10wt% hydrochloric acid solution is added under stirring according to the molar ratio of sodium carbonate to hydrochloric acid of 1:2, hydrochloric acid is added in a dropwise manner, the dropwise speed is controlled to be 3 seconds/drop, the condition that boiling splashing can not occur due to slow rising of the temperature of the wastewater is controlled, the temperature of the wastewater is maintained within the temperature range of 50 ℃ in the whole dropwise adding process, and the reaction is continued for 10min after the dropwise adding is completed.
3. After the reaction is ended, the treated wastewater is evaporated and concentrated under reduced pressure at 80-90 ℃, the vacuum degree is 0.06-0.07 mpa, the concentration is stopped when the original volume is 30%, then the filtration is carried out while the wastewater is still hot, the obtained filter cake is subjected to determination of 96.88% of sodium bromide content and 2.82% of water content, and the filter cake is dried for 1h at 80-90 ℃ to obtain a sodium bromide product. The sodium bromide content in the dried sodium bromide product is 99.5 percent.
Example 5
1. The wastewater was taken, wherein the sodium bromide content was 20wt%, the sodium carbonate content was 10wt% and the pH was 7.
2. 200G of the wastewater is taken and placed in a container, 10wt% sulfuric acid solution is added under stirring according to the molar ratio of sodium carbonate to sulfuric acid of 1:1, sulfuric acid is added in a dropwise manner, the dropwise speed is controlled to be 3 seconds/drop, the condition that boiling splashing can not occur due to slow rising of the temperature of the wastewater is controlled, the temperature of the wastewater is maintained within the temperature range of 50 ℃ in the whole dropwise adding process, and the reaction is continued for 10min after the dropwise adding is completed.
3. After the reaction is finished, cooling the wastewater to 0 ℃ for crystallization, filtering to remove sodium sulfate after the crystallization is completed, heating the wastewater to 80-90 ℃, performing reduced pressure evaporation concentration under the vacuum degree of 0.06-0.07 mpa, concentrating to 30% of the original volume, stopping, filtering while the wastewater is hot, measuring the sodium bromide content of the obtained filter cake to 96.25% and the water content of the filter cake to 3.16%, and drying the filter cake at 80-90 ℃ for 1h to obtain a sodium bromide product. The sodium bromide content in the dried sodium bromide product is 99.2 percent according to the measurement.
Comparative example 1
1. The waste water was taken, wherein the content of sodium bromide was 20wt% and the content of sodium carbonate was 0.25wt%.
2. And (3) placing 200g of the wastewater in a container, decompressing, evaporating and concentrating at 80-90 ℃, stopping concentrating until the vacuum degree is 0.06-0.07 mpa and the concentration is 30% of the original volume, filtering while the wastewater is hot, and drying the obtained filter cake at 80-90 ℃ for 1h to obtain a sodium bromide product. The moisture content of the dried sodium bromide product is 20.14 percent.
Claims (11)
1. A method for recovering sodium bromide with low water content from wastewater, which is characterized by comprising the following steps:
(1) Taking waste water containing sodium carbonate and sodium bromide, and adding acid to remove sodium carbonate in the waste water;
(2) Evaporating and concentrating the wastewater after removing sodium carbonate, and performing hot filtration after concentrating to obtain sodium bromide wet material;
(3) Drying the wet sodium bromide material to obtain sodium bromide with low water content;
In the step (2), when the content of sodium carbonate in the wastewater is less than or equal to 1wt%, the wastewater is directly subjected to thermal concentration crystallization after the sodium carbonate is removed, sodium bromide is recovered, and when the content of sodium carbonate in the wastewater is more than or equal to 1wt% and less than or equal to 20wt%, the sodium carbonate is removed, and then the wastewater is subjected to thermal concentration crystallization, so that sodium bromide is recovered;
The water content of the obtained sodium bromide is less than or equal to 1.1wt%.
2. The method according to claim 1, characterized in that: in the step (1), the sodium bromide content in the wastewater is 10-90wt% and the sodium carbonate content is less than or equal to 20wt%.
3. The method according to claim 1, characterized in that: in the step (1), the sodium bromide content in the wastewater is 10-30wt%.
4. The method according to claim 1, characterized in that: in the step (1), sulfuric acid is added to remove sodium carbonate in the wastewater.
5. The method according to claim 4, characterized in that: in the step (1), sulfuric acid is slowly added into the wastewater under stirring to prevent the wastewater from boiling and splashing.
6. The method according to claim 1, 4 or 5, characterized in that: in the step (1), if the dropwise added acid is dilute acid, the adding speed is controlled to keep the temperature of the wastewater in the whole adding process at 50 ℃ and below, and if the dropwise added acid is concentrated acid, the adding speed is controlled to keep the temperature of the wastewater in the whole adding process at 70 ℃ and below.
7. The method according to claim 1, 4 or 5, characterized in that: in the step (1), the molar ratio of the hydrogen ions in the acid to the carbonate in the sodium carbonate is 1.8-2.2:1.
8. The method according to claim 7, characterized in that: in step (1), the molar ratio of hydrogen ions in the acid to carbonate in the sodium carbonate is 2:1.
9. The method according to claim 1, 4 or 5, characterized in that: in the step (1), after the acid is added, the reaction is continued for 10-20 min.
10. The method according to claim 1, 4 or 5, characterized in that: in the step (2), when the content of sodium carbonate in the wastewater is more than 1wt% and less than or equal to 20wt% and the acid is sulfuric acid, the wastewater after removing the sodium carbonate is firstly cooled to 0 ℃ for crystallization, sodium sulfate is separated, and then the sodium bromide is recovered by reheating, concentration and crystallization.
11. The method according to claim 10, characterized by: in the step (2), the steps of thermal concentration crystallization are as follows: and (3) carrying out reduced pressure evaporation concentration on the wastewater at 80-90 ℃, controlling the vacuum degree at 0.06-0.07 mpa, concentrating until the concentration is 30% of the original volume, and then filtering while the wastewater is hot.
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