CN109912383B - Purification system for recovering dichloromethane from pharmaceutical industry waste liquid - Google Patents
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Abstract
The invention discloses a purification system for recovering dichloromethane from waste liquid in pharmaceutical industry, which comprises a distillation tower, a tubular mixer, an oil-water separation tank and an intermittent extraction rectification tower.
Description
Technical Field
The invention belongs to the field of chemical industry and pharmaceutical industry, and particularly relates to a purification system for recovering dichloromethane from a waste solvent or industrial waste liquid.
Background
Methylene dichloride as a solvent commonly used in the chemical and pharmaceutical fields has the advantages of strong dissolving capacity and low toxicity, but because methylene dichloride has toxicity, the large-amount discharge of methylene dichloride as industrial waste liquid has great influence on environmental protection. The recycling of the dichloromethane is beneficial to environmental protection, and the production cost is saved or new economic value is generated. Therefore, the method is particularly important for the recovery method and the application problem of the dichloromethane, and particularly in the pharmaceutical industrial production, the recovery and the application of the dichloromethane can greatly reduce the cost.
At present, the methylene dichloride is mainly recovered by a dehydration method, so that the moisture content in the methylene dichloride is reduced and other organic components are removed. The existing dehydration methods are various and mainly adopt dehydrating agents, and the commonly used dehydrating agents comprise basic dehydrating agents, acid dehydrating agents and neutral dehydrating agents, wherein the basic dehydrating agents comprise calcium hydride and acid dehydrating agents, and the neutral dehydrating agents comprise molecular sieves; they can reduce the water content in dichloromethane by about 0.5%. However, the operation is troublesome, the problem of recycling and reusing is also involved, and the water content of the recycled dichloromethane is still high, so that the dichloromethane cannot be directly recycled and reused.
CN107986939A discloses a method for recovering dichloromethane in a pyridine hydrochloride B7 working section, which comprises the following steps: a. fully reacting and washing crude dichloromethane and water in a layering tower; b. the upper part of the layering tower is a water phase, the lower part of the layering tower is a dichloromethane phase, dichloromethane is extracted to enter a storage tank to be neutralized, and the alkaline wastewater at the upper layer of the layering tower is discharged to a sewage pool; c. pumping dichloromethane into a neutralization kettle, and adding liquid alkali to neutralize until the pH value is 8; d. stirring and standing for layering, and separating the lower layer of pure dichloromethane to a dichloromethane storage tank for later use. The method is developed from a dichloromethane solvent generated in a pyridine hydrochloride B7 section only, and only aiming at a single material, the recovery process is only one water washing and neutralization process for recovering dichloromethane, but still does not meet the requirement and standard of dichloromethane recovery in complex waste liquid in the pharmaceutical industry.
CN107573211A discloses a recovery process of solvent dichloromethane, which comprises the following steps: (1) pumping dichloromethane into the reaction kettle, stirring for 15min, and measuring the pH value; (2) pumping water, and stirring for 30 min; (3) adjusting pH of the solution to 7-8, stirring for 20min, re-measuring pH, standing for 50min, and layering; (4) transferring the materials in the reaction kettle to a distillation tower, starting steam to heat after the material transfer is finished, and refluxing for 7-8 hours; (5) and after the reflux is finished, discharging and barreling to obtain a dichloromethane product.
CN105085160A discloses a method for recovering dichloromethane in an acesulfame potassium synthesis process, which comprises the steps of carrying out coarse evaporation on a dichloromethane solvent generated by acesulfame potassium synthesis, adding the dichloromethane solvent into a dehydration tower, heating steam to 42 ℃, condensing the mixed steam of dichloromethane and water into a dehydration overflow tank, and allowing dichloromethane with qualified bottom water to enter a semi-finished product tank for a rectification tower; b. the dichloromethane with unqualified water at the bottom of the overflow groove enters the dehydration tower again through reflux, the dichloromethane with high water at the top enters the crude product groove, and the layered water in the crude product groove is discharged at regular intervals; c. the dichloromethane with qualified water content in the semi-finished product tank enters a rectifying tower, the temperature is evaporated to 45 ℃, dichloromethane steam enters a rectifying overflow tank, and dichloromethane containing a large amount of impurities at the bottom is pumped into a residue tank; d. and after the dichloromethane in the rectification overflow groove is detected to be qualified, putting the dichloromethane into a finished product groove for synthetic sulfonation, and re-rectifying the unqualified dichloromethane in a rectification tower.
CN103553868A discloses a method for recovering dichloromethane, which comprises placing dichloromethane into a rectifying tower; secondly, the method comprises the following steps: ethylene glycol was added to the methylene chloride through the addition port of the rectification column, and finally: and separating and purifying the water content of the dichloromethane to be below 0.5% by a rectifying tower. The method is only suitable for rectifying and dehydrating the relatively pure dichloromethane waste liquid with low impurity content.
CN1323994 discloses a method for recovering dichloromethane from a multi-component mixed solution containing dichloromethane, which comprises the following steps: (1) adding an extracting agent A into a mixed solution containing dichloromethane, methanol, pyridine, triethylamine and water at the temperature of 2-10 ℃, wherein the adding amount of the extracting agent A is 0.1-0.3 time of the volume of the mixed solution; extracting under stirring, standing, and separating raffinate phase; (2) carrying out secondary extraction on the raffinate phase obtained in the step (1) by using an extracting agent B according to the condition of the step (1), and separating the raffinate phase; (3) and (3) carrying out normal-pressure batch rectification on the raffinate phase obtained in the step (2): firstly, adopting total reflux operation, wherein the reflux liquid needs to flow through a split-phase dehydrator to remove water and water-soluble impurities, and the total reflux time is 1.5-3.0 hours; then, performing reflux ratio of (6-2): 1, collecting the middle fraction, and stopping collecting the middle fraction when the temperature of the top of the rectifying tower reaches 39.2 ℃; finally, the reflux ratio is 1: 1, collecting dichloromethane, and stopping rectification when the temperature of the top of the rectification tower reaches 42.5 ℃; wherein: the extractant A is 0.05-0.5 wt% inorganic acid water solution, and the extractant B is 0.1-0.3 wt% inorganic salt water solution. In the pharmaceutical industry, the dichloromethane waste liquid is relatively complex in composition, and not only comes from one synthesis section, but also the dichloromethane waste solvent often contains multiple groups of components difficult to separate. The company collects waste solvents from various pharmaceutical enterprises for centralized treatment, the dichloromethane waste liquid is one of the waste liquids frequently collected by the company, and due to the large content and component difference of the dichloromethane solvents generated by different pharmaceutical enterprises and workshops, for example, the recovered solvents for ampicillin synthesis contain dichloromethane, pivalic acid, methanol, water, acetone and the like. For example, the organic solvent contained in the waste dichloromethane solvent of a pharmaceutical factory is methanol, ethanol, acetone, EA, toluene and the like. By adopting the existing process, the azeotropic components with the dichloromethane are difficult to separate, so that the separated dichloromethane is difficult to reach the recycling standard or national standard, and water, methanol, ethanol, acetone, toluene and the like in the dichloromethane cannot be effectively separated. Aiming at the problem that the practical materials of the dichloromethane waste liquid collected by the company are difficult to be effectively separated, a recovery process route and a purification method of the waste dichloromethane are developed according to the components in the dichloromethane waste solvent. The method has wider adaptability, and the recycled dichloromethane reaches the national standard.
Disclosure of Invention
The invention provides a purification system for recovering dichloromethane from pharmaceutical waste solvents according to dichloromethane waste liquid (also called waste solvent) generated in the pharmaceutical industry, the system can recover and purify dichloromethane from pharmaceutical waste liquid with complex components, the recovered dichloromethane reaches the national standard, the dichloromethane is recycled, the extraction solvent adopted in the purification process can be recovered and reused, and the production cost is reduced. Is beneficial to environmental protection and generates economic benefit.
The invention discloses a purification system for recovering dichloromethane from pharmaceutical waste liquid, which comprises a distillation tower, a tubular mixer, an oil-water separation tank and an intermittent extraction rectification tower kettle.
In the purification system of the present invention, the distillation column includes a distillation intermediate tank, the oil-water separation tank includes a water phase intermediate tank and an organic phase intermediate storage tank, the batch extractive distillation column contains a dichloromethane intermediate storage tank and a raffinate intermediate storage tank, the helical blades are twisted at 180 °, and the helical blades in two adjacent mixers have opposite rotation directions and are staggered by 90 °.
In the purification system of the invention, the tubular mixer has a barrel body which is formed by connecting two semicircular ends by flanges, and a gap of the barrel body is bonded and sealed by epoxy resin.
The purification system of the invention further comprises a rectification tower for separating and purifying the extraction solvent for recycling, wherein the rectification tower comprises a front fraction receiving tank, a middle fraction tank and a kettle residue tank.
In one embodiment, the present invention provides a purification system for recovering dichloromethane, the dichloromethane purification scheme comprising: pumping the dichloromethane waste liquid into a distillation tower, regulating the pH value with alkali liquor, heating and distilling, storing the fraction dichloromethane in an intermediate tank, then flowing into or pumping into a tubular mixer, adding alkali liquor through another charging hole of the mixer, uniformly mixing, then entering an oil-water separation tank for standing and separation, storing the separated organic phase in an intermediate storage tank, pumping into an intermittent extraction rectification tower kettle, mixing with an extraction solvent in a rectification tower, heating and refluxing, collecting qualified dichloromethane fractions, and completing dichloromethane recovery and purification. The specific process is shown in figure 1.
The method for recovering dichloromethane by adopting the purification system comprises the following steps:
1) adjusting the pH value of the dichloromethane waste solvent to 7-10 by using acid and/or alkali, and heating, distilling or/and decoloring;
2) adding alkali liquor into the collected fraction dichloromethane, uniformly mixing, and then standing for layering;
3) discarding the upper aqueous phase, taking the lower dichloromethane organic phase, and adding ethylene glycol for extraction and rectification;
4) collecting the fractions at the temperature of 39-42 ℃ to obtain pure dichloromethane, and optionally;
5) further comprises the recovery and reuse of the extractant glycol.
According to the method, the distillation temperature in the step 1) is 39-50 ℃, the alkali liquor in the step 2) is selected from sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate, the pH of the alkali liquor is 7-10, and the dosage of the alkali liquor is 0.1-0.5 times of the mass of a dichloromethane solvent. In the step 3), the volume ratio of the ethylene glycol to the organic phase is 0.1-0.5. The rectification reflux ratio R is 1.5-4.
The recovery and purification method is suitable for recycling the pharmaceutical methylene dichloride solvent. The reclaimed dichloromethane meets the first-class requirement (namely national standard) of the industrial dichloromethane used in GB/T4117 + 2008, the mass fraction of the dichloromethane is more than or equal to 99.5 percent, the water content is less than or equal to 0.02 percent, the mass fraction of the acid is less than or equal to 0.0004 percent, and the chroma is less than or equal to 10 percent.
Drawings
FIG. 1 is a schematic flow diagram of a waste dichloromethane recovery and purification system.
Detailed Description
The following examples are intended to further illustrate and understand the spirit of the present invention, but not to limit the scope of the present invention in any way, and any simple changes and modifications made within the spirit of the present invention are within the scope of the present invention.
The system comprises a distillation tower, a distillation middle tank, a tubular mixer, an oil-water separation tank, a water phase middle tank, an organic phase middle storage tank, an intermittent extraction rectification tower kettle, a dichloromethane middle storage tank and a residual liquid middle storage tank, wherein the tubular mixer is provided with a three-section mixer group, a cylinder body of the mixer is formed by connecting two semicircular cylinders by flanges, the gap of the cylinder body is bonded and sealed by epoxy resin, each section of mixer comprises a helical blade, the helical blade rotates under the action of material movement to slow down the flow pressure of the material, the helical blade is twisted by 180 degrees, and the rotating directions of the helical blades in two adjacent sections of mixers are opposite.
The above-mentioned system for recovering and purifying dichloromethane further comprises a rectifying tower for separating and purifying the extraction solvent for recycling, wherein the rectifying tower comprises a front fraction receiving tank, a middle fraction tank and a still tank (see fig. 1).
Example 2 Process flow for recovering waste dichloromethane by recovery and purification system
The process comprises the following steps:
1) pumping barreled dichloromethane waste solvent (or waste liquid) collected from pharmaceutical enterprises into a distillation still (the distillation still is provided with stirring, vacuumizing, nitrogen, alkali liquor dropwise adding, a steam or electric heating temperature control system and the like as required), adjusting the pH in the distillation still to 7-10 by using acid or alkali, then heating the distillation still, controlling the temperature in the distillation still to 39-42 ℃, passing light components through a tower top condenser by heating and evaporation, wherein the condenser is secondary condensation, circulating water and low-temperature water of 7 ℃ are used, condensing top fraction dichloromethane and then entering an intermediate collecting tank (namely a distillation still intermediate tank), and removing hazardous waste from the bottom kettle of the distillation still. The distillation kettle in the step has the main functions of impurity removal, decoloration, high boiling removal and the like.
2) Mixing dichloromethane in a middle tank of a distillation kettle with alkali liquor (aqueous solution of sodium hydroxide or sodium carbonate and the like, wherein the pH value of the alkali liquor is 7-10) according to the weight ratio of 1: 0.1-0.5, and pumping into a pipeline type (also referred to as a 'tubular' mixer) mixer (the pipeline type mixer is generally a three-section group, each section of mixer is provided with a fixed helical blade twisted at 180 degrees, and comprises a left-handed helical blade and a right-handed helical blade, the helical blades in two adjacent sections have opposite rotating directions and are staggered by 90 degrees, the helical blades are conveniently installed, a cylinder body is made into two semicircular shapes, two ends of the cylinder body are connected by flanges, gaps of the cylinder body are bonded by epoxy resin, the sealing requirement of the cylinder body is ensured, the helical blades of the mixer are motionless, only the mixed materials or media move, and fluid generates pressure reduction by passing through the helical blades without external energy sources, wherein the two media are mainly divided by flow, radially mixed and reversely rotated, and continuously and intensively mixed and diffused to achieve the mixing purpose) the pipeline type mixer selects DN 50-DN 100, the length is 1.0-1.5 m, and the flanges are connected, the inlet is provided with a one-way valve. The mixing efficiency of each section of pipeline type mixer is more than 95%.
3) And (3) allowing a dichloromethane solvent passing through the tubular mixer to enter an oil-water separation tank for standing and layering for 4-6 h, wherein the upper layer is a water phase, and the lower layer is a dichloromethane organic phase (the density of dichloromethane is 1.325g/ml at25 ℃), the upper layer of the water phase enters an intermediate storage tank for hazardous waste removal treatment or recycling, and the lower layer of the dichloromethane organic phase flows into an organic phase intermediate tank for later use.
4) The method comprises the following steps of pumping a solvent in an organic phase intermediate tank into an intermittent extraction rectification tower (a continuous extraction rectification mode can be adopted when the treatment capacity is large), adding an extracting agent ethylene glycol from the upper part of the rectification tower, controlling the feeding temperature of the extracting agent to be 37-42 ℃, the adding amount of the ethylene glycol to be 0.1-0.5 times of the mass of a dichloromethane solvent, controlling the top temperature of the extraction tower to be 39-50 ℃, controlling the reflux ratio R to be 1.5-4, controlling the temperature of a tower kettle to be 50-65 ℃ by adopting steam heating, and configuring secondary condensation, namely circulating water condensation and 7-DEG low-temperature water condensation, on the tower top.
5) And (3) heating and pumping total reflux after feeding in the rectifying tower, collecting fractions at 39-42 ℃, and extracting the fractions to a product intermediate tank to obtain purified dichloromethane when the dichloromethane is qualified (reaches the national standard). And the bottom residual liquid enters a bottom residual liquid intermediate storage tank for temporary storage.
6) And after accumulating a certain amount of residual liquid in the middle storage tank, feeding the residual liquid into a tower kettle of a recycling rectification tower, controlling the vacuum degree at the top of the tower at 20-50 KPa, controlling the temperature at the top of a pre-extraction fraction tower at 60-85 ℃, controlling the temperature at the bottom of the tower at 90-100 ℃, controlling the temperature at the top of a middle extraction fraction glycol tower at 82-100 ℃, controlling the temperature at the bottom of the tower at 90-110 ℃ and controlling the reflux ratio at 1-3.
Collecting the front fraction, feeding into a front fraction intermediate tank, collecting the intermediate fraction (ethylene glycol) after the intermediate fraction is qualified, feeding into an ethylene glycol intermediate tank, and recycling in a dichloromethane extraction rectification tower.
Example 3
A waste dichloromethane solvent collected from a pharmaceutical company has a composition (w%) of 70.30% dichloromethane, 6.29% methanol, 6.80% ethanol, 5.50% acetone, 4.54% EA, 3.14% toluene, 1.15% water, and about 2.28% others, and has a pH of 4, and the waste liquid is yellow brown in color.
The recovery and purification process comprises the following steps:
1. pumping the waste liquid into a 5000L distillation kettle (the distillation kettle needs nitrogen replacement for three times), starting stirring for 50 r/min, adding liquid alkali to adjust the pH to 7-8, starting a steam valve to open the distillation kettle, heating condensed water to distill at 45 ℃, wherein the distillation time is 5h, and collecting fractions to flow into an intermediate tank.
2. The dichloromethane and the aqueous solution of sodium hydroxide with pH being 9 in the intermediate tank are pumped into a pipeline mixer (the pipeline mixer is 1m long and 80mm in diameter and adopts two sections of serial connection), then the mixture enters an oil-water separation tank and stands for 4 hours. The bottom organic intermediate phase was placed in an intermediate storage tank.
3. And pumping dichloromethane in the intermediate storage tank into a 5000L rectifying tower kettle, heating, pumping to reflux completely, adding an extracting agent ethylene glycol from the top of the tower, controlling the temperature of the top of the tower to be 40 ℃, controlling the temperature of the bottom of the tower to be 55 ℃, taking a top distillate sample after the temperature and reflux are stable, and extracting dichloromethane at the top of the tower to a product intermediate tank when the content of dichloromethane is more than or equal to 99.5 percent and the water is less than or equal to 0.02 percent, wherein the reflux ratio R is 4. And if the dichloromethane distilled from the tower top is unqualified in sampling analysis, continuing to perform total reflux for 2h, and then sampling and analyzing. And (4) extracting until the product is qualified (reaches the national standard).
4. And pumping the bottom extractant and other kettle bottom residual liquid into a residual liquid intermediate tank, and after a certain amount of the residual liquid intermediate tank reaches a certain amount, feeding the residual liquid into a tower kettle of a recycling tower to recycle the ethylene glycol. And controlling the vacuum degree at the top of the tower at 30KPa, the temperature at the top of the tower for collecting the front fraction at 70 ℃, the temperature at the bottom of the tower at 95 ℃, the temperature at the top of the tower for collecting the middle fraction ethylene glycol at 90 ℃, the temperature at the bottom of the tower at 100 ℃ and the reflux ratio R at 1.5. Collecting the front fraction, introducing into a front fraction intermediate tank, introducing the qualified intermediate fraction (ethylene glycol is greater than or equal to 99%) into an ethylene glycol intermediate tank, and recovering in a dichloromethane extractive distillation column.
The yield of dichloromethane and ethylene glycol in the process is 78% and 89%.
Example 4
A waste dichloromethane solvent collected from a pharmaceutical company has a composition (w%) of 70.30% dichloromethane, 6.29% methanol, 6.80% ethanol, 5.50% acetone, 4.54% EA, 3.14% toluene, 1.15% water, and about 2.28% others, and has a pH of 4, and the waste liquid is yellow brown in color.
The recovery and purification process comprises the following steps:
1. pumping the waste liquid into a 5000L distillation kettle (the distillation kettle needs nitrogen replacement for three times), starting stirring for 50 r/min, adding liquid alkali to adjust the pH value to 8-10, starting a steam valve to open the distillation kettle, heating condensed water to distill at 45 ℃, wherein the distilling time is 5h, and collecting fractions to flow into an intermediate tank.
2. Respectively pumping dichloromethane in an intermediate tank and a sodium hydroxide aqueous solution (the mass ratio is 1: 0.1-0.3) with the pH value of 9-10 into a pipeline type mixer (the length of the pipeline type mixer is 1m, two sections with the diameter of 80mm are connected in series), then feeding the pipeline type mixer into an oil-water separation tank, and standing for 4 hours. The bottom organic intermediate phase was placed in an intermediate storage tank.
3. And pumping dichloromethane in the intermediate storage tank into a 5000L rectifying tower kettle, heating, pumping to reflux completely, adding an extracting agent ethylene glycol from the top of the tower, controlling the temperature of the top of the tower to be 40 ℃, controlling the temperature of the bottom of the tower to be 55 ℃, taking a top distillate sample after the temperature and reflux are stable, and extracting dichloromethane at the top of the tower to a product intermediate tank when the content of dichloromethane is more than or equal to 99.3 percent and the water is less than or equal to 0.02 percent, wherein the reflux ratio R is 1.5. And if the dichloromethane distilled from the tower top is unqualified in sampling analysis, continuing to perform total reflux for 2h, and then sampling and analyzing. And (4) extracting until the product is qualified (reaches the national standard).
4. And pumping the bottom extractant and other kettle bottom residual liquid into a residual liquid intermediate tank, and after a certain amount of the residual liquid intermediate tank reaches a certain amount, feeding the residual liquid into a tower kettle of a recycling tower to recycle the ethylene glycol. And controlling the vacuum degree at the top of the tower at 30KPa, the temperature at the top of the front fraction tower at 70 ℃, the temperature at the bottom of the tower at 95 ℃, the temperature at the top of the middle fraction ethylene glycol tower at 90 ℃, the temperature at the bottom of the tower at 100 ℃ and the reflux ratio R to 3. Collecting the front fraction, introducing into a front fraction intermediate tank, introducing the qualified intermediate fraction (ethylene glycol is greater than or equal to 99%) into an ethylene glycol intermediate tank, and recovering in a dichloromethane extractive distillation column.
The yield of dichloromethane and ethylene glycol in the process is 76.6% and 90.2%.
Comparative example 1
The solvent of waste methylene chloride of example 2 was recovered by the recovery method of CN105085160A and the recovery and purification methods of CN103553868A and CN1323994, and the contents of the recovered methylene chloride were 90.3% (water content: 2.1%), 87.2% (water content: 0.50%) and 95.8% (water content: 1.05%), respectively.
The experimental results of the comparative example show that the prior art is really difficult to effectively separate, purify and recycle the complex pharmaceutical waste dichloromethane.
Claims (6)
1. A purification system for recovering dichloromethane from pharmaceutical industry waste liquid, the system comprises a distillation tower, a tubular mixer, an oil-water separation tank and a batch extractive distillation tower, the tubular mixer is provided with three-section mixer groups, each mixer group comprises a helical blade, the helical blade rotates under the movement of materials to slow the flowing pressure of the materials, the distillation tower comprises a distillation middle tank, the oil-water separation tank comprises an aqueous phase middle tank and an organic phase middle storage tank, the batch extractive distillation tower comprises a dichloromethane middle storage tank and a raffinate middle storage tank, and the purification system, a dichloromethane purification flow path comprises: pumping the dichloromethane waste liquid into a distillation tower, adjusting the pH value with alkali liquor, heating and distilling, storing the fraction dichloromethane in an intermediate tank, then flowing into or pumping into a tubular mixer, adding alkali liquor through another charging hole of the mixer, uniformly mixing, then entering an oil-water separation tank for standing and separation, storing the separated organic phase in an intermediate storage tank, pumping into an intermittent extraction rectification tower, mixing with an extraction solvent in the rectification tower, heating and refluxing, collecting qualified dichloromethane fractions, and completing dichloromethane recovery and purification.
2. The purification system as recited in claim 1 wherein said helical blades are twisted by 180 ° and the helical blades in adjacent mixers rotate in opposite directions.
3. The purification system of claim 2, wherein the helical blades of adjacent mixers are 90 ° offset.
4. The purification system as claimed in claim 1, wherein the mixer has a cylindrical body formed by two semicircular cylindrical bodies connected at both ends by flanges, and the gap between the cylindrical bodies is sealed by bonding with epoxy resin.
5. The purification system as claimed in claim 1, further comprising separating and purifying the extraction solvent by using a rectifying tower for recycling.
6. The purification system as recited in claim 5 wherein said rectification column comprises a front end receiver tank, a middle distillate tank and a bottoms tank.
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| CN114057541B (en) * | 2021-12-09 | 2023-08-15 | 河南省化工研究所有限责任公司 | Refining recovery method for dehydrating waste dichloromethane through supergravity coupling membrane |
| CN114538554A (en) * | 2022-01-20 | 2022-05-27 | 赵崇毅 | Extraction device, extraction plant set and extraction method for hydrometallurgy or oil-water separation |
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