CN107337218B - Method for recovering sodium bromide from bromine-containing wastewater - Google Patents
Method for recovering sodium bromide from bromine-containing wastewater Download PDFInfo
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- CN107337218B CN107337218B CN201710600327.6A CN201710600327A CN107337218B CN 107337218 B CN107337218 B CN 107337218B CN 201710600327 A CN201710600327 A CN 201710600327A CN 107337218 B CN107337218 B CN 107337218B
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- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 title claims abstract description 110
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052794 bromium Inorganic materials 0.000 title claims abstract description 49
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000002351 wastewater Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000706 filtrate Substances 0.000 claims abstract description 39
- 238000001914 filtration Methods 0.000 claims abstract description 35
- 150000003839 salts Chemical class 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000012043 crude product Substances 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 90
- 239000000047 product Substances 0.000 claims description 60
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 48
- 239000010410 layer Substances 0.000 claims description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 26
- 239000012044 organic layer Substances 0.000 claims description 18
- 238000011084 recovery Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 239000000400 angiotensin II type 1 receptor blocker Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000004537 pulping Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- JXLBBMKZXKVUEI-UHFFFAOYSA-N 1,1'-biphenyl;hydrobromide Chemical compound Br.C1=CC=CC=C1C1=CC=CC=C1 JXLBBMKZXKVUEI-UHFFFAOYSA-N 0.000 description 2
- LQPCAPMUDDPGHJ-UHFFFAOYSA-N 5-(bromomethyl)-2-phenylbenzonitrile Chemical group N#CC1=CC(CBr)=CC=C1C1=CC=CC=C1 LQPCAPMUDDPGHJ-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- -1 Bromine ions Chemical class 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 229940071870 hydroiodic acid Drugs 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for recovering sodium bromide from bromine-containing wastewater, which comprises the following steps: adjusting the pH value of bromine-containing wastewater by using acid, adding a solvent for washing, and distilling a water layer to be dry; adding a solvent into the evaporated material, pulping, filtering to remove impurity salts, concentrating and filtering the obtained filtrate to obtain sodium bromide. The method provided by the invention is simple to operate and environment-friendly, and the obtained sodium bromide crude product has the purity of 90%. The method has the advantages of low cost and low equipment requirement, and meanwhile, the method is extremely simple to operate, environment-friendly and suitable for industrial production.
Description
Technical Field
The invention relates to the field of pharmaceutical chemicals, in particular to a method for recovering sodium bromide from bromine-containing wastewater.
Technical Field
The biphenyl bromide is a key intermediate raw material in the preparation of sartans, and has the chemical name of 4-bromomethyl-2-cyano-1,1-biphenyl. The raw material can generate hydrobromic acid or sodium bromide salt in the preparation process of sartans, and the hydrobromic acid or the sodium bromide salt is dissolved in water.
It is common practice to recover bromine from bromine-containing wastewater by a bromine recovery process, which is very common in the bromine production industry. Bromine ions are oxidized into elemental bromine by chlorine or hydrogen peroxide, then bromine in water is separated, some bromine is provided by steam distillation method such as a new bromine extraction technology-steam distillation method (natural gas exploration and development, 6 months 2004) by utilizing the difference of boiling points, bromine is blown out from an aqueous solution by an air blowing method by utilizing the large partial pressure of bromine in air to be easy to enrich, and then the elemental bromine in the blown gas such as CN200710014116.0 and CN200610045061.5 is absorbed by sulfur dioxide and water. Each of these methods has advantages and disadvantages, but all require the use of an oxidizing agent and recovery of elemental bromine. In the recovery process, high requirements are placed on recovery equipment and safe operation, and certain influence is brought to the environment.
Disclosure of Invention
A recovery method for recovering sodium bromide from bromine-containing wastewater is characterized by comprising the following steps:
1) Adjusting the pH value of bromine-containing wastewater by using acid, adding an organic solvent for washing, and distilling a water layer to be dry.
2) Adding a solvent into the material after evaporation to dryness, pulping, filtering to remove mixed salt, concentrating and filtering the obtained filtrate to obtain sodium bromide.
The PH value in the step 1) is 4-10, preferably 6-8.
The acid used in the step 1) is an inorganic acid selected from hydrochloric acid, hydrobromic acid, hydroiodic acid, sulfuric acid and nitric acid; hydrochloric acid is preferred.
The organic solvent used in the step 1) is dichloromethane, ethyl acetate, toluene and xylene, and toluene is preferred.
The solvent used in the step 2) is water, methanol, ethanol or acetone, preferably water, methanol or a mixed solvent of two solvents, and more preferably methanol.
The solvent added in the step 2) is 2-10 times, preferably 3-8 times and more preferably 5-7 times of the evaporated material.
The weight of the concentrated solution in the step 2) is 10-40% of that before concentration, and preferably 20-30%.
The biphenyl bromide is a key intermediate raw material in the preparation of sartans, and has the chemical name of 4-bromomethyl-2-cyano-1,1-biphenyl. The raw material can generate sodium bromide with an acid-binding agent (sodium carbonate, sodium hydroxide or a mixture of the two) in the preparation process of the sartan, and the sodium bromide is dissolved in water to form bromine-containing wastewater.
Recovering sodium bromide from bromine-containing wastewater: firstly, adjusting the pH value of bromine-containing wastewater, washing a water layer by using a solvent, concentrating to be dry, adding the solvent for pulping and filtering, concentrating the obtained filtrate, and filtering to obtain the sodium bromide with higher purity. In detail, see figure 1
The method provided by the invention is used for recovering the sodium bromide in the bromine-containing wastewater, is simple to operate and environment-friendly, and can obtain a crude product of the sodium bromide, wherein the purity of the crude product can reach 90%. The method has the advantages of low cost and low equipment requirement, and meanwhile, the method is extremely simple to operate, environment-friendly and suitable for industrial production.
Drawings
FIG. 1: the invention relates to a process flow chart for recovering sodium bromide from bromine-containing wastewater.
Detailed Description
Example 1:
300ml of bromine-containing wastewater was added to a 1000ml three-necked reaction flask, 2.1g of purified hydrochloric acid was added to adjust the pH to 8, 100ml of toluene was added thereto to wash for 2 times, and after separating the organic layer, the aqueous layer was distilled under reduced pressure at 40 to 50 ℃ until 46.1g was dried. Adding 300g of methanol, controlling the temperature at 25-35 ℃, stirring for 1 hour, and filtering to obtain 18.6g of a wet miscellaneous salt product. The filtrate is distilled under reduced pressure at 40-50 ℃ until 32.5g is dried. Then 40g of methanol is added, the temperature is controlled to be between 25 and 35 ℃, the mixture is stirred for 1 hour and then filtered to obtain 30.3g of wet product, and the dried product is dried to obtain 25.2g of crude sodium bromide, wherein the purity of the sodium bromide is 90.2 percent, and the yield is 94.3 percent.
Example 2:
adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.2g of refined hydrochloric acid to adjust the pH to 7, adding 100ml of toluene to wash for 1 time, separating an organic layer, and then distilling a water layer at 40-50 ℃ under reduced pressure until the water layer is dried to 45.5g. Adding 300g of methanol, controlling the temperature at 25-35 ℃, stirring for 1 hour, and filtering to obtain 19.1g of a wet miscellaneous salt product. The filtrate was distilled under reduced pressure at 40-50 ℃ until dried 33.1g. Then adding 40g of methanol, controlling the temperature to be 25-35 ℃, stirring for 1 hour, filtering to obtain 31.3g of wet product, drying to obtain 25.5g of crude sodium bromide product with the purity of 90.5% and the yield of 95.4%.
Example 3:
adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.3g of refined hydrochloric acid to adjust the pH to 6, adding 100ml of toluene to wash for 1 time, separating an organic layer, and then distilling a water layer at 40-50 ℃ under reduced pressure until the water layer is dried to 46.1g. Adding 300g of methanol, controlling the temperature at 25-35 ℃, stirring for 1 hour, and filtering to obtain 18.9g of a wet miscellaneous salt product. The filtrate is distilled under reduced pressure at 40-50 ℃ until 33.5g is dried. Then 50g of methanol is added, the temperature is controlled to be 25-35 ℃, the mixture is stirred for 1 hour and then filtered to obtain 29.3g of wet product, and the dried product is dried to obtain 23.7g of crude sodium bromide, wherein the purity of the sodium bromide is 87.8 percent, and the yield is 88.7 percent.
Example 4:
adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.2g of refined hydrochloric acid to adjust the pH to 8, adding 100ml of toluene to wash for 1 time, separating an organic layer, and then distilling a water layer at 40-50 ℃ under reduced pressure until the water layer is dried to 46.5g. Adding 300g of methanol, controlling the temperature at 25-35 ℃, stirring for 1 hour, and filtering to obtain 17.4g of a wet miscellaneous salt product. And (3) controlling the temperature of the filtrate at 40-50 ℃, distilling the filtrate under reduced pressure to 73.2g, controlling the temperature at 25-35 ℃, stirring the filtrate for 1 hour, filtering the filtrate to obtain 31.5g of wet product, and drying the wet product to obtain 24.9g of crude sodium bromide product with the purity of 88.9 percent and the yield of 93.2 percent.
Example 5:
300ml of bromine-containing wastewater is added into a 1000ml three-mouth reaction bottle, 2.2g of refined hydrochloric acid is added to adjust the pH to 7, 100ml of toluene is added to wash for 1 time, and after an organic layer is separated, a water layer is distilled under reduced pressure at 40-50 ℃ until the water layer is dried to 45.8g. 245g of methanol is added, the temperature is controlled between 25 ℃ and 35 ℃, the mixture is stirred for 1 hour, and 18.7g of wet miscellaneous salt is obtained by filtration. And (3) controlling the temperature of the filtrate at 40-50 ℃, distilling the filtrate under reduced pressure to 74.5g, controlling the temperature at 25-35 ℃, stirring the filtrate for 1 hour, filtering the filtrate to obtain 31.8g of wet product, and drying the wet product to obtain 25.1g of crude sodium bromide product, wherein the purity of the sodium bromide product is 90.8 percent, and the yield is 93.9 percent.
Example 6:
adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.3g of refined hydrochloric acid to adjust the pH to 6, adding 100ml of toluene to wash for 1 time, separating an organic layer, and then distilling a water layer at 40-50 ℃ under reduced pressure until the water layer is dried to 44.9g. 245g of methanol is added, the mixture is stirred for 1 hour at the temperature of 25 to 35 ℃ and filtered to obtain 19.1g of a wet miscellaneous salt product. And (3) carrying out reduced pressure distillation on the filtrate at the temperature of 40-50 ℃ until the filtrate is dried to 32.5g, then adding 50g of ethanol, stirring at the temperature of 25-35 ℃ for 1 hour, filtering to obtain 34.1g of wet product, and drying to obtain 26.1g of dry product crude sodium bromide, wherein the purity of the sodium bromide is 86.1%, and the yield is 97.5%.
Example 7:
adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.1g of refined hydrochloric acid to adjust the pH to 7, adding 100ml of toluene to wash for 1 time, separating an organic layer, and then distilling a water layer at 40-50 ℃ under reduced pressure until the water layer is dried to 45.8g. 200g of methanol aqueous solution (a mixture of 180g of methanol and 20g of water) was added thereto, and the mixture was stirred at 25 to 35 ℃ for 1 hour, followed by filtration to obtain 19.2g of a wet miscellaneous salt product. The filtrate was distilled under reduced pressure at 40-50 ℃ until dried 33.1g. Then 50g of methanol is added, the temperature is controlled to be 25-35 ℃, the mixture is stirred for 1 hour and then filtered to obtain 32.9g of wet product, and the dry product is dried to obtain 24.2g of crude sodium bromide, wherein the purity of the sodium bromide is 91.7 percent, and the yield is 90.5 percent.
Example 8:
adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.2 refined hydrochloric acid to adjust the pH to 7, adding 100ml of dichloromethane to wash for 1 time, separating an organic layer, and then distilling a water layer at 40-50 ℃ under reduced pressure until the water layer is dried to 45.3g. 245g of methanol is added, the temperature is controlled between 25 ℃ and 35 ℃, the mixture is stirred for 1 hour, and 18.9g of wet miscellaneous salt is obtained by filtration. And (3) controlling the temperature of the filtrate at 40-50 ℃, distilling the filtrate under reduced pressure to 74.2g, controlling the temperature at 25-35 ℃, stirring the filtrate for 1 hour, filtering the filtrate to obtain 33.7g of wet product, and drying the wet product to obtain 25.2g of crude sodium bromide product, wherein the purity of the sodium bromide product is 90.2 percent, and the yield is 94.3 percent.
Example 9:
adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 1.9g of sulfuric acid to adjust the pH to 8, adding 100ml of ethyl acetate to wash for 1 time, separating an organic layer, and then distilling a water layer at 40-50 ℃ under reduced pressure until the water layer is dried to 44.8g. 245g of methanol is added, the temperature is controlled between 25 ℃ and 35 ℃, the mixture is stirred for 1 hour, and the mixture is filtered to obtain 19.2g of wet miscellaneous salt. And (3) controlling the temperature of the filtrate at 40-50 ℃, distilling the filtrate under reduced pressure to 73.2g, controlling the temperature at 25-35 ℃, stirring the filtrate for 1 hour, filtering the filtrate to obtain 32.1g of wet product, and drying the wet product to obtain 24.7g of crude sodium bromide product, wherein the purity of the sodium bromide is 90.8 percent, and the yield is 92.4 percent.
Claims (9)
1. A recovery method for recovering sodium bromide from bromine-containing wastewater generated in a process for preparing sartans, characterized in that the method comprises the following steps: adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.1g of refined hydrochloric acid to adjust the pH to 8, adding 100ml of toluene, washing for 2 times, separating an organic layer, and distilling a water layer at a temperature of 40-50 ℃ under reduced pressure until the water layer is dried to 46.1g; adding 300g of methanol, stirring for 1 hour at the temperature of 25-35 ℃, and filtering to obtain 18.6g of a wet miscellaneous salt product; distilling the filtrate at 40-50 ℃ under reduced pressure until the filtrate is dried to 32.5g; then adding 40g of methanol, controlling the temperature to be 25-35 ℃, stirring for 1 hour, filtering to obtain 30.3g of wet product, and drying to obtain 25.2g of crude sodium bromide product of which the purity is 90.2% and the yield is 94.3%.
2. A recovery method for recovering sodium bromide from bromine-containing wastewater generated in a process for preparing sartans, characterized in that the method comprises the following steps: adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.2g of refined hydrochloric acid to adjust the pH to 7, adding 100ml of toluene, washing for 1 time, separating an organic layer, and distilling a water layer at a temperature of 40-50 ℃ under reduced pressure until the water layer is dried to 45.5g; adding 300g of methanol, stirring for 1 hour at the temperature of 25 to 35 ℃, and filtering to obtain 19.1g of a wet salt product; distilling the filtrate at 40-50 ℃ under reduced pressure until the filtrate is dried to 33.1g; then adding 40g of methanol, controlling the temperature to be 25-35 ℃, stirring for 1 hour, filtering to obtain 31.3g of wet product, and drying to obtain 25.5g of crude sodium bromide product with the purity of 90.5% and the yield of 95.4%.
3. A recovery method for recovering sodium bromide from bromine-containing wastewater generated in a sartan production process, characterized in that the method comprises the steps of: adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.3g of refined hydrochloric acid to adjust the pH to 6, adding 100ml of toluene, washing for 1 time, separating an organic layer, and distilling a water layer at the temperature of 40-50 ℃ under reduced pressure until the water layer is dried to 46.1g; adding 300g of methanol, stirring for 1 hour at the temperature of 25-35 ℃, and filtering to obtain 18.9g of a wet miscellaneous salt product; distilling the filtrate under reduced pressure at 40 to 50 ℃ until the filtrate is dried to 33.5g; then 50g of methanol is added, the mixture is stirred for 1 hour at the temperature of 25 to 35 ℃ and filtered to obtain 29.3g of wet product, and dried to obtain 23.7g of crude sodium bromide product with the purity of 87.8 percent and the yield of 88.7 percent.
4. A recovery method for recovering sodium bromide from bromine-containing wastewater generated in a process for preparing sartans, characterized in that the method comprises the following steps: adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.2g of refined hydrochloric acid to adjust the pH to 8, adding 100ml of toluene, washing for 1 time, separating an organic layer, and distilling a water layer at the temperature of 40-50 ℃ under reduced pressure until the water layer is dried to 46.5g; adding 300g of methanol, stirring for 1 hour at the temperature of 25 to 35 ℃, and filtering to obtain 17.4g of a wet salt product; and (3) distilling the filtrate at the temperature of 40-50 ℃ under reduced pressure to 73.2g, stirring at the temperature of 25-35 ℃ for 1 hour, filtering to obtain 31.5g of wet product, and drying to obtain a dry product 24.9g crude product of sodium bromide, wherein the purity of the sodium bromide is 88.9%, and the yield is 93.2%.
5. A recovery method for recovering sodium bromide from bromine-containing wastewater generated in a process for preparing sartans, characterized in that the method comprises the following steps: adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.2g of refined hydrochloric acid to adjust the pH value to 7, adding 100ml of toluene, washing for 1 time, separating an organic layer, and distilling a water layer at a temperature of 40-50 ℃ under reduced pressure until the water layer is dried to 45.8g; adding 245g of methanol, stirring for 1 hour at the temperature of 25-35 ℃, and filtering to obtain 18.7g of a wet salt product; and (3) distilling the filtrate at the temperature of 40-50 ℃ under reduced pressure to 74.5g, stirring at the temperature of 25-35 ℃ for 1 hour, filtering to obtain 31.8g of wet product, and drying to obtain 25.1g crude sodium bromide product as a dry product, wherein the purity of the sodium bromide is 90.8%, and the yield is 93.9%.
6. A recovery method for recovering sodium bromide from bromine-containing wastewater generated in a process for preparing sartans, characterized in that the method comprises the following steps: adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.3g of refined hydrochloric acid to adjust the pH to 6, adding 100ml of toluene, washing for 1 time, separating an organic layer, and distilling a water layer at a temperature of 40-50 ℃ under reduced pressure until the water layer is dried to 44.9g; adding 245g of methanol, stirring for 1 hour at the temperature of 25-35 ℃, and filtering to obtain 19.1g of a wet salt product; distilling the filtrate under reduced pressure at 40 to 50 ℃ until the filtrate is dried to 32.5g, then adding 50g of ethanol, stirring for 1 hour at 25 to 35 ℃, filtering to obtain 34.1g of wet product, and drying to obtain 26.1g sodium bromide crude product as a dried product, wherein the purity of the sodium bromide is 86.1%, and the yield is 97.5%.
7. A recovery method for recovering sodium bromide from bromine-containing wastewater generated in a process for preparing sartans, characterized in that the method comprises the following steps: adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.1g of refined hydrochloric acid to adjust the pH to 7, adding 100ml of toluene, washing for 1 time, separating an organic layer, and distilling a water layer at the temperature of 40-50 ℃ under reduced pressure until the water layer is dried to 45.8g; adding a methanol water solution consisting of 180g of methanol and 20g of water, controlling the temperature to be 25 to 35 ℃, stirring for 1 hour, and filtering to obtain 19.2g of a mixed salt wet product; distilling the filtrate at 40-50 ℃ under reduced pressure until the filtrate is dried to 33.1g; then 50g of methanol is added, the mixture is stirred for 1 hour at the temperature of 25 to 35 ℃ and then filtered to obtain 32.9g of wet product, and the wet product is dried to obtain 24.2g of crude sodium bromide product, wherein the purity of the sodium bromide product is 91.7 percent, and the yield is 90.5 percent.
8. A recovery method for recovering sodium bromide from bromine-containing wastewater generated in a process for preparing sartans, characterized in that the method comprises the following steps: adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 2.2 refined hydrochloric acid to adjust the pH to 7, adding 100ml of dichloromethane, washing for 1 time, separating an organic layer, and distilling a water layer at a temperature of 40-50 ℃ under reduced pressure until the water layer is dried to 45.3g; adding 245g of methanol, stirring for 1 hour at the temperature of 25-35 ℃, and filtering to obtain 18.9g of a wet miscellaneous salt product; and distilling the filtrate at the temperature of 40-50 ℃ under reduced pressure to 74.2g, stirring at the temperature of 25-35 ℃ for 1 hour, filtering to obtain 33.7g of wet product, and drying to obtain 25.2g of crude sodium bromide product of which the purity is 90.2% and the yield is 94.3%.
9. A recovery method for recovering sodium bromide from bromine-containing wastewater generated in a process for preparing sartans, characterized in that the method comprises the following steps: adding 300ml of bromine-containing wastewater into a 1000ml three-mouth reaction bottle, adding 1.9g of sulfuric acid to adjust the pH to 8, adding 100ml of ethyl acetate to wash for 1 time, separating an organic layer, and distilling a water layer at the temperature of 40-50 ℃ under reduced pressure until the water layer is dried to 44.8g; adding 245g of methanol, stirring for 1 hour at the temperature of 25-35 ℃, and filtering to obtain 19.2g of a wet miscellaneous salt product; distilling the filtrate under reduced pressure at 40-50 ℃ to 73.2g, stirring at 25-35 ℃ for 1 hour, filtering to obtain 32.1g of wet product, and drying to obtain a dry product 24.7g sodium bromide crude product, wherein the purity of the sodium bromide is 90.8%, and the yield is 92.4%.
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