CN112875727A - Method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor - Google Patents
Method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor Download PDFInfo
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- CN112875727A CN112875727A CN202110197532.9A CN202110197532A CN112875727A CN 112875727 A CN112875727 A CN 112875727A CN 202110197532 A CN202110197532 A CN 202110197532A CN 112875727 A CN112875727 A CN 112875727A
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- mother liquor
- chloroacetanilide
- sodium chloride
- sodium carbonate
- recovering
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
- C01D7/26—Purification by precipitation or adsorption
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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
- C01D3/04—Chlorides
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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
- C01D3/16—Purification by precipitation or adsorption
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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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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor, belonging to the technical field of high-salinity wastewater treatment energy conservation. The method comprises 1) slowly adding a dechlorinating agent into the chloroacetanilide mother liquor, stirring and standing; removing available chlorine in the chloroacetanilide mother liquor; 2) passing the mother liquor treated in the step 1) through an activated and filled adsorption resin column; used for removing residual organic matters in the mother liquor; 3) distilling the mother liquor treated in the step 2), concentrating the mother liquor, leading out and filtering while the mother liquor is hot, wherein a filter cake is sodium chloride, cooling and crystallizing the filtrate, and filtering the filter cake to obtain sodium carbonate. The invention removes the effective chlorine and organic matters in the mother liquor, and avoids the problem that distilled water has color. The reduced pressure four-effect evaporator is adopted for reduced pressure distillation, so that a large amount of energy can be saved; the recovered sodium carbonate and sodium chloride have high purity, the purity of the sodium carbonate is more than 95 percent, the purity of the sodium chloride is more than 95 percent, and the method can be applied to other processes in the factory.
Description
Technical Field
The invention belongs to the technical field of high-salinity wastewater treatment and energy conservation, and particularly relates to a method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor.
Background
The chloroacetanilide is an intermediate for preparing doxycycline, and the preparation process comprises the following steps: stirring acetanilide with a certain proportion of water and sodium bicarbonate, then dropwise adding a certain proportion of sodium hypochlorite solution, controlling the temperature to react for a period of time, and then centrifugally filtering and washing, wherein the solution directly filtered by filtering is called mother liquor. The mother liquor contains about 10% of sodium carbonate, 3% -4% of sodium chloride and 0-1% of organic matters, and is typical high-salinity wastewater with the characteristics of high salinity, strong alkalinity and poor biodegradability. The direct discharge of the high-salt-content wastewater can cause the following hazards: the soil structure is damaged, the soil alkalinity is enhanced, the soil quality is hardened and the soil is blocked, so that the physiological activity of the soil is difficult to recover, soil organisms and plants die due to dehydration, the soil ecosystem is disrupted, and the process of the eutrophication of rivers and lakes can be accelerated. In addition, during treatment, a large amount of clear water can be added for dilution after simple neutralization, and then biological treatment is carried out, so that a large amount of water resources are wasted, and a large amount of salt substances are discharged into a sewage treatment system and still pollute the environment, so that the research and development of a method for efficiently treating the high-salt-content wastewater is particularly important.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor, wherein the purity of the separated sodium carbonate is more than 95 percent, and the purity of the sodium chloride is more than 95 percent.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor comprises the following steps:
1) slowly adding a dechlorinating agent into the chloroacetanilide mother liquor, stirring and standing; removing available chlorine in the chloroacetanilide mother liquor;
2) passing the mother liquor treated in the step 1) through an activated and filled adsorption resin column; used for removing residual organic matters in the mother liquor;
3) distilling the mother liquor treated in the step 2), concentrating the mother liquor, leading out and filtering while the mother liquor is hot, wherein a filter cake is sodium chloride, and cooling and crystallizing the filtrate, and filtering to obtain a filter cake which is sodium carbonate.
The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor comprises the step of removing the chlorine by using formic acid.
The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor comprises the step 1), wherein the mass ratio of the chloroacetanilide mother liquor to a dechlorinating agent is 1: 0.003-1: 0.005, and the reaction temperature is 30-50 ℃.
The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor comprises the step 1), wherein the mass ratio of the chloroacetanilide mother liquor to a chlorine removal agent is 1:0.004, and the reaction temperature is 50 ℃.
The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor comprises the step 2), wherein the adsorption resin is any one of HPD-100, HPD-300, D-101 or H103; the adsorption flow rate is 1-4 BV/hr, and the adsorption temperature is 30-50 ℃.
The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor comprises the step 2), wherein the adsorption resin is D-101 type, the adsorption flow rate is 3BV/hr, and the adsorption temperature is 40 ℃.
In the method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor, in the step 3), the distillation equipment is any one of single tank or four-effect evaporation; distilling under normal pressure or reduced pressure, wherein the volume of the concentrated mother liquor is 20-40% of the volume before concentration, and the density of the hot concentrated solution is 1.17-1.25.
In the method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor, in the step 3), the distillation equipment adopts four-effect evaporation, a reduced pressure distillation mode is adopted, the volume of the concentrated mother liquor is 30% of the volume before concentration, and the density of the hot concentrated solution is 1.22.
Has the advantages that: compared with the prior art, the invention has the advantages that:
1) the invention removes the available chlorine and organic matters (acetanilide and chloroacetanilide) in the mother liquor, and avoids the problem that distilled water has color. 2) The reduced pressure four-effect evaporator is adopted for reduced pressure distillation, so that a large amount of energy can be saved; 3) the recovered sodium carbonate and sodium chloride have high purity and can be applied to other processes in the plant.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example 1
A method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor comprises the following steps:
1) 2000g of chloroacetanilide mother liquor (containing sodium carbonate: 9.84%, sodium chloride: 3.5 percent), placing the mixture into a 3L beaker, stirring and heating the mixture to 40 ℃, dropwise adding 6.48g of formic acid, continuously stirring the mixture for 1 hour, and standing the mixture for 0.5 hour;
2) passing the treated mother liquor through activated and filled D-101 resin column at 40 deg.C and flow rate of 3BV/hr, and collecting the passed mother liquor;
3) adding the mother liquor obtained in the step 2) into a 2L three-necked bottle in batches for distillation, and concentrating until the distilled residual liquid is 600mL, wherein the density of the concentrated solution is as follows: 1.19, stopping distilling, filtering while hot to obtain a filter cake of sodium chloride, wherein the damp product weight is as follows: 32.5g, purity: 96.7 percent. Cooling the filtrate to 20 ℃, and filtering to obtain a filter cake which is sodium carbonate, wherein the damp weight is as follows: 125.2g, purity: 95.5 percent.
Example 2
A method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor comprises the following steps:
1) 2000Kg of chloroacetanilide mother liquor (containing sodium carbonate: 10.04%, sodium chloride: 3.6 percent) Put in 3m3Stirring and heating the mixture to 40 ℃ in a reaction tank, dripping 10.8Kg of formic acid, continuously stirring the mixture for 1 hour, and standing the mixture for 0.5 hour;
2) passing the treated mother liquor through activated and filled D-101 resin column at 40 deg.C and flow rate of 4BV/hr, and collecting the passed mother liquor;
3) adding the mother liquor obtained in the step 2) to 4m3Distilling in a reaction pot, and concentrating until the distillation residual liquid has 0.5m3The density of the concentrate is: 1.21, stopping distilling, filtering while hot to obtain a filter cake of sodium chloride, wherein the damp product weight is as follows: 41.1Kg, purity: 95.6 percent. Cooling the filtrate to 20 ℃, and filtering to obtain a filter cake which is sodium carbonate, wherein the damp weight is as follows: 142.5Kg, purity: 95.3 percent.
Example 3
A method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor comprises the following steps:
1) 10000Kg of chloroacetanilide mother liquor (containing sodium carbonate: 10.14%, sodium chloride: 3.1%) of the above-mentioned material, put into a container of 10m3Stirring and heating the mixture to 50 ℃ in a reaction tank, dripping 43.2Kg of formic acid in total, continuously stirring the mixture for 1 hour, and standing the mixture for 0.5 hour;
2) passing the treated mother liquor through activated and filled D-101 resin column at 50 deg.C and flow rate of 4BV/hr, and collecting the passed mother liquor;
3) adding the mother liquor obtained in the step 2) into a four-effect evaporator, and concentrating until 4m of distillation residual liquid is remained3The density of the concentrate is: 1.22, stopping distilling, filtering while hot to obtain a filter cake of sodium chloride, wherein the damp product weight is as follows: 187.3Kg, the purity is: 95.3 percent. Cooling the filtrate to 20 ℃, and filtering to obtain a filter cake which is sodium carbonate, wherein the damp weight is as follows: 678.6Kg, the purity is: 95.1 percent.
Claims (8)
1. A method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor is characterized by comprising the following steps:
1) slowly adding a dechlorinating agent into the chloroacetanilide mother liquor, stirring and standing;
2) passing the mother liquor treated in the step 1) through an activated and filled adsorption resin column;
3) distilling the mother liquor treated in the step 2), concentrating the mother liquor, leading out and filtering while the mother liquor is hot, wherein a filter cake is sodium chloride, and cooling and crystallizing the filtrate, and filtering to obtain a filter cake which is sodium carbonate.
2. The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor according to claim 1, wherein said chlorine scavenger is formic acid.
3. The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor according to claim 1, wherein in the step 1), the mass ratio of the chloroacetanilide mother liquor to the dechlorinating agent is 1: 0.003-1: 0.005, and the reaction temperature is 30-50 ℃.
4. The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor according to claim 1, wherein in step 1), the mass ratio of the chloroacetanilide mother liquor to the chlorine removal agent is 1:0.004, and the reaction temperature is 50 ℃.
5. The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor according to claim 1, wherein the step 2), the adsorption resin is any one of HPD-100, HPD-300, D-101 or H103; the adsorption flow rate is 1-4 BV/hr, and the adsorption temperature is 30-50 ℃.
6. The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor according to claim 1, wherein in the step 2), the adsorption resin is D-101 type, the adsorption flow rate is 3BV/hr, and the adsorption temperature is 40 ℃.
7. The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor according to claim 1, wherein said step 3), the distillation apparatus is any one of single-pot or four-effect evaporation; distilling under normal pressure or reduced pressure, wherein the volume of the concentrated mother liquor is 20-40% of the volume before concentration, and the density of the hot concentrated solution is 1.17-1.25.
8. The method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor according to claim 1, wherein in the step 3), the distillation apparatus is a four-effect evaporation, the volume of the mother liquor after concentration is 30% of the volume before concentration by using reduced pressure distillation, and the density of the hot concentrated liquor is 1.22.
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| CN202110197532.9A CN112875727A (en) | 2021-02-22 | 2021-02-22 | Method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor |
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| CN202110197532.9A CN112875727A (en) | 2021-02-22 | 2021-02-22 | Method for recovering sodium carbonate and sodium chloride from chloroacetanilide mother liquor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387494A (en) * | 2021-06-10 | 2021-09-14 | 深圳星河环境股份有限公司 | Method for removing and refining copper sulfate based on organic matters |
| CN115594605A (en) * | 2022-11-29 | 2023-01-13 | 山东国邦药业有限公司（Cn） | Preparation method of doxycycline intermediate |
Citations (4)
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|---|---|---|---|---|
| CA1147742A (en) * | 1981-03-18 | 1983-06-07 | John P. Chupp | Process for the production of tertiary 2- haloacetamides |
| CN102642815A (en) * | 2012-03-05 | 2012-08-22 | 浙江金科过氧化物股份有限公司 | Circulatory recycling method of sodium percarbonate mother liquor |
| CN103415471A (en) * | 2011-02-22 | 2013-11-27 | 威立雅水处理技术北美公司 | Selective salt recovery from mixed salt brine |
| CN109400495A (en) * | 2018-12-22 | 2019-03-01 | 山东国邦药业股份有限公司 | A kind of preparation method of acetochloroanilide |
-
2021
- 2021-02-22 CN CN202110197532.9A patent/CN112875727A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1147742A (en) * | 1981-03-18 | 1983-06-07 | John P. Chupp | Process for the production of tertiary 2- haloacetamides |
| CN103415471A (en) * | 2011-02-22 | 2013-11-27 | 威立雅水处理技术北美公司 | Selective salt recovery from mixed salt brine |
| CN102642815A (en) * | 2012-03-05 | 2012-08-22 | 浙江金科过氧化物股份有限公司 | Circulatory recycling method of sodium percarbonate mother liquor |
| CN109400495A (en) * | 2018-12-22 | 2019-03-01 | 山东国邦药业股份有限公司 | A kind of preparation method of acetochloroanilide |
Non-Patent Citations (2)
| Title |
|---|
| 张必翔: "《专业学位研究生实验课程 医科篇》", 30 September 2011 * |
| 黄晓东等: "甲酸去除有效氯法改进漂白粉中总钙质量分数的测定", 《高师理科学刊》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113387494A (en) * | 2021-06-10 | 2021-09-14 | 深圳星河环境股份有限公司 | Method for removing and refining copper sulfate based on organic matters |
| CN115594605A (en) * | 2022-11-29 | 2023-01-13 | 山东国邦药业有限公司（Cn） | Preparation method of doxycycline intermediate |
| CN115594605B (en) * | 2022-11-29 | 2023-03-10 | 山东国邦药业有限公司 | Preparation method of doxycycline intermediate |
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