CN212532800U - Organic waste liquid separation system of ethyl ester toluene that contains a small amount of water - Google Patents
Organic waste liquid separation system of ethyl ester toluene that contains a small amount of water Download PDFInfo
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- CN212532800U CN212532800U CN202021663248.3U CN202021663248U CN212532800U CN 212532800 U CN212532800 U CN 212532800U CN 202021663248 U CN202021663248 U CN 202021663248U CN 212532800 U CN212532800 U CN 212532800U
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Abstract
The utility model relates to an organic waste liquid piece-rate system of ethyl ester toluene that contains a small amount of water belongs to organic solvent waste liquid separation technical field. The system comprises a feed pump, a dehydration tower, a toluene-ethyl ester separation tower and a toluene purification tower which are sequentially communicated; the bottom of the dehydration tower is provided with a first heater; the top of the dehydration tower is sequentially communicated with a first condenser and a first condensate buffer tank, and one side of the bottom of the first condensate buffer tank is provided with a water distribution bag; the water was cut out of the system, and then ethyl ester and toluene were separated according to the difference in boiling point between toluene and ethyl ester. The utility model adopts three-tower rectification, utilizes toluene as entrainer to form a ternary azeotropic system, directly separates water at the tower top, breaks away the influence of toluene-water and ethyl ester-water azeotropy, and realizes the separation of the three.
Description
Technical Field
The utility model relates to a hydrous organic waste liquid separation technical field specifically provides an organic waste liquid piece-rate system of ethyl ester toluene that contains a small amount of water.
Background
With the rapid development of national economy, public concern about resource waste and environmental pollution is increasing. The unjustified use of resources is a major cause of environmental pollution. The pollution is eliminated, and the reasonable utilization of resources and the saving and emission reduction are started, wherein the resource and the renewable utilization of the chemical residual liquid are the main contents. The ideal comprehensive utilization of resources is to eat, dry and squeeze the resources as much as possible. However, under the restriction of domestic technical treatment conditions, in most cases, the main components in the resources are utilized, and the used or difficultly treated parts are discarded as wastes, thereby causing great waste and pollution. Therefore, the main form of resource comprehensive utilization is represented by separation, extraction, purification and regeneration of effective components of residual liquid resources.
Toluene and ethyl ester are important organic solvents widely used in chemical, pharmaceutical, dye and other fields. Toluene is an organic compound of aromatic hydrocarbon, and is in liquid state at room temperature, and has a boiling point of 110.8 deg.C and a density of 0.866g/cm3And is poorly soluble in water. Ethyl ester, i.e. ethyl acetate, is colorless transparent liquid, is easily volatile, has a boiling point of 77 ℃ and a density of 0.902g/cm3Slightly soluble in water.
In the industrial production process, most of organic waste liquid contains water, toluene and water form a binary azeotrope under normal pressure, ethyl ester and water can also form a binary azeotrope, and water can simultaneously form an azeotrope with toluene and ethyl ester, so that the separation is difficult.
In the prior art, on one hand, because the relative volatility of toluene, ethyl ester and water is not greatly different at normal pressure, the purification is difficult by using the conventional common rectification, and the prior art has more column plates, large reflux ratio, large energy consumption and low efficiency and is only suitable for the crude purification of toluene and ethyl ester products; on the other hand, the ketone substance is used as an extracting agent, toluene is separated from a mixed solvent containing toluene, ethyl ester, ethanol and the like through twice extraction and rectification, and the alcohol substance is further used as an extracting agent to separate a mixture of ethyl ester and ethanol; however, two kinds of extraction agents are adopted, so that the process is complicated, the consumed time is long, impurities are easily introduced to influence the product purity, and in addition, the energy consumption of the extraction and rectification tower is high, and the economical efficiency is poor.
The azeotropic distillation refers to that a third component, namely an entrainer or an entrainer, is added into a system with two components of constant boiling liquid or similar volatility to improve the vapor-liquid equilibrium relationship between the components to be separated, the component can form a minimum azeotrope with one or more components in raw material liquid, so that the distillation separation becomes the separation of azeotrope-pure component, and the distillation separation has larger relative volatility, so that the number of plates and reflux ratio required by the separation are reduced, and the energy consumption is correspondingly lower than that of the common distillation. However, for the water-toluene-ethyl ester system, water forms an azeotrope with both toluene and ethyl ester and separation is difficult.
SUMMERY OF THE UTILITY MODEL
In order to solve the problems that in the prior art, ethyl ester, toluene and water cannot be separated by common rectification, an extractant needs to be added in the traditional extractive rectification, the size and energy consumption of equipment are increased, and solvent pollution is easily caused; the utility model provides an organic waste liquid piece-rate system of ethyl ester toluene that contains a small amount of water. The utility model discloses utilize azeotropic distillation principle, select the most suitable azeotropic agent to form minimum azeotrope, the toluene that adopts raw materials self to contain forms ternary azeotropic system for smuggleing secretly the agent, through smuggleing heterogeneous azeotropic distillation flow certainly, directly separates the water at the top of the tower, has broken the influence of toluene-water and ethyl ester-water binary azeotrope, has created the condition for the separation of follow-up toluene-ethyl ester.
In order to solve the technical problem, the utility model provides a technical scheme as follows:
the utility model provides an organic waste liquid piece-rate system of ethyl ester toluene that contains a small amount of water, include: the device comprises a feed pump, a dehydration tower, a toluene-ethyl ester separation tower and a toluene purification tower which are sequentially communicated, wherein organic waste liquid sequentially flows through the dehydration tower, the toluene-ethyl ester separation tower and the toluene purification tower through the feed pump.
Further, a first heater is arranged at the bottom of the dehydration tower, and organic waste liquid at the bottom of the tower flows in the first heater through a pump in a circulating manner to obtain heat so as to enable the heat to be partially gasified and enter the dehydration tower; the top of the dehydration tower is sequentially communicated with a feeding preheater, a first condenser and a first condensate buffer tank, one side of the bottom of the first condensate buffer tank is provided with a water distribution bag protruding downwards, the bottom of the water distribution bag is communicated with a water recovery pipeline device, the water recovery pipeline device is provided with an adjusting valve, and the opening degree of the water distribution bag is adjusted according to the water level height of the water distribution bag; the other side of the bottom of the first condensate buffer tank is provided with a first return pipeline communicated with the top of the dehydrating tower, the first return pipeline is provided with a flow regulating valve, opening degree regulation is carried out according to the liquid level height of the first condensate buffer tank body, the bottom pipeline of the dehydrating tower is communicated with the toluene-ethyl ester separating tower, and organic waste liquid is pumped into the toluene-ethyl ester separating tower from the bottom of the dehydrating tower.
Further, a second heater is arranged at the bottom of the toluene-ethyl ester separation tower, the mixed organic waste liquid at the bottom of the tower circularly flows in the second heater through a pump to obtain heat, so that the heat is partially gasified and enters the toluene-ethyl ester separation tower, the top of the mixed organic waste liquid is sequentially communicated with a second condenser and a second condensate buffer tank, a first three-way pipeline is arranged at the bottom of the second condensate buffer tank, a second return pipeline is arranged on one side of the mixed organic waste liquid, is communicated with the top of the toluene-ethyl ester separation tower and is used for returning ethyl ester containing a small amount of toluene, and a flow regulating valve is arranged on the second return pipeline; the other side is communicated with an ethyl ester recovery device through an ethyl ester recovery pipeline, and the ethyl ester recovery pipeline is provided with an ethyl ester recovery regulating valve. And the opening degree of the flow regulating valve and the opening degree of the ethyl ester recovery regulating valve on the second return pipeline are controlled by the liquid level of the second condensate buffer tank, and the flow of the return pipeline is measured and fed back to the opening degree signal of the ethyl ester recovery regulating valve through cascade control to set a corresponding reflux ratio.
Furthermore, the bottom of the toluene-ethyl ester separation tower is communicated with a toluene purification tower, mixed organic waste liquid at the bottom of the toluene purification tower is pumped into the toluene purification tower, a third heater is arranged at the bottom of the toluene purification tower, and the organic waste liquid at the bottom of the toluene purification tower flows in the third heater in a circulating mode through a pump to obtain heat, so that part of the heat is gasified and enters the toluene purification tower. The top communicates third condenser and third condensate buffer tank in proper order, the bottom of third condensate buffer tank sets up the second tee bend pipeline. One side of the third reflux pipeline is provided with a flow regulating valve, and the third reflux pipeline is communicated with the top of the toluene purification tower and is used for refluxing the toluene condensed in the third buffer tank so as to realize gas-liquid exchange with ascending steam in the toluene purification tower; the other side is communicated with a toluene recovery device through a toluene recovery pipeline, and the toluene recovery pipeline is provided with an adjusting valve. And the opening degree of the regulating valve and the opening degree of the toluene recovery regulating valve on the third return pipeline are controlled by the liquid level of the third condensate buffer tank, and the flow of the return pipeline is measured and fed back to the opening degree signal of the toluene recovery regulating valve through cascade control, so that the corresponding reflux ratio is set.
Preferably, a liquid level controller is further arranged between the feeding pump and the dehydration tower and used for regulating and controlling feeding of the organic waste liquid.
Further, the bottom of the water distributing drum is also connected with a moisture measurement controller; the bottom of the second condensate buffer tank is communicated with a first purity detection device; the bottom of the third condensate buffer tank is communicated with a second purity detection device; temperature monitors are arranged in the dehydration tower, the toluene-ethyl ester separation tower and the toluene purification tower.
Further, in the above-mentioned case,
the bottom of the dehydration tower is communicated with a first lift pump, the liquid level at the bottom of the dehydration tower is measured by a liquid level meter designed at the bottom of the dehydration tower, the opening of a regulating valve of an outlet pipeline of the first lift pump can be regulated according to liquid level feedback, organic waste liquid is pumped into the toluene-ethyl ester separation tower, and meanwhile, the liquid level at the bottom of the dehydration tower is ensured to be stable; the bottom of the toluene-ethyl ester separation tower is communicated with a second lift pump, the liquid level at the bottom of the toluene-ethyl ester separation tower is measured by a liquid level meter designed at the bottom of the toluene-ethyl ester separation tower, the opening degree of an adjusting valve of an outlet pipeline of the second lift pump can be adjusted according to liquid level feedback, organic waste liquid is pumped into the toluene purification tower, and meanwhile, the liquid level at the bottom of the toluene-ethyl ester separation tower is ensured to be stable; the bottom of the toluene purification tower is communicated with the kettle liquid discharge pump, the liquid level at the bottom of the toluene purification tower is measured by the liquid level meter arranged at the bottom of the toluene purification tower, the opening degree of the regulating valve on the pipeline of the kettle liquid discharge pump can be regulated according to liquid level feedback, the stability of the liquid level at the bottom of the toluene purification tower is ensured, and meanwhile, an impurity discharge system is adopted
Compared with the prior art, the utility model discloses following beneficial effect has:
the utility model discloses use three tower rectification, at first the azeotropic composition-water in the ternary azeotrope that distills at the first dehydration column top destroys the azeotropy of toluene-water, ethyl ester-water, then the boiling point difference of rethread, through second toluene-ethyl ester knockout tower top distillate ethyl ester, through third toluene purification tower top distillate toluene at last, azeotropic composition easily retrieves, can regard as the product reuse, the energy consumption is the economy most. The utility model discloses both applicable in the continuity of production, also can be applicable to intermittent type nature production, operation elasticity is big. The equipment is compact, the occupied space is small, and the arrangement on a flat surface is convenient.
Drawings
FIG. 1 is a schematic view of an ethyl ester toluene water separation system in embodiment 1 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
Example 1
The utility model provides an organic waste liquid separation system of ethyl ester toluene that contains a small amount of water, see figure 1, including charge pump 1, dehydration tower 8, toluene-ethyl ester knockout tower 11 and toluene purification tower 20 that communicate in order, organic waste liquid flows through dehydration tower 8, toluene-ethyl ester knockout tower 11 and toluene purification tower 20 through charge pump 1 in proper order;
the bottom of the dehydration tower 8 is provided with a first heater 9, and the mixed organic waste liquid at the bottom of the tower flows in the first heater 9 through a pump in a circulating way to obtain heat so as to enable part of the heat to be gasified and enter the dehydration tower 8; the top of the dehydrating tower 8 is sequentially communicated with a feeding preheater 3, a first condenser 7 and a first condensate buffer tank 4, one side of the bottom of the first condensate buffer tank 4 is provided with a convex water distribution bag 5, and the bottom of the water distribution bag 5 is communicated with a water recovery pipeline device, wherein the water recovery pipeline device is a water recovery tank (not shown) communicated with a pipeline, the pipeline is provided with an adjusting valve 6, and the opening degree is adjusted according to the water level height of the water distribution bag 5; the other side of the bottom of the first condensate buffer tank 4 is provided with a first return pipeline 23 communicated with the top of the dehydrating tower 8, the first return pipeline 23 is also provided with a flow regulating valve (not shown), opening degree regulation can be carried out according to the liquid level height of the tank body, the bottom pipeline of the dehydrating tower 8 is communicated with the toluene-ethyl ester separating tower 11, and organic waste liquid is pumped into the toluene-ethyl ester separating tower 11 from the bottom of the dehydrating tower 8.
A second heater 15 is arranged at the bottom of the toluene-ethyl ester separation tower 11, the mixed organic waste liquid at the bottom of the tower flows in the second heater 15 through a pump in a circulating manner to obtain heat so as to enable the heat to be partially gasified and enter the toluene-ethyl ester separation tower 11, the top of the mixed organic waste liquid is sequentially communicated with a second condenser 12 and a second condensate buffer tank 13, a first three-way pipeline 14 is arranged at the bottom of the second condensate buffer tank 13, a second return pipeline 24 is arranged on one side of the mixed organic waste liquid, is communicated with the top of the toluene-ethyl ester separation tower 11 and is used for returning ethyl ester containing a small amount of toluene, and a flow regulating valve is arranged on the; the other side is communicated with an ethyl ester recovery device (not shown) through an ethyl ester recovery pipeline, and the ethyl ester recovery pipeline is provided with an ethyl ester recovery regulating valve (not shown). The liquid level of the second condensate buffer tank 13 controls the opening degree of a flow regulating valve and an ethyl ester recovery regulating valve on the second return pipeline 24, the flow of the return pipeline is measured through cascade control and fed back to an opening degree signal of the ethyl ester recovery regulating valve, and a corresponding reflux ratio is set.
The bottom of the toluene-ethyl ester separation tower 11 is communicated with a toluene purification tower 20, the mixed organic waste liquid at the bottom of the tower is pumped into the toluene purification tower 20, a third heater 21 is arranged at the bottom of the toluene purification tower 20, and the mixed organic waste liquid at the bottom of the tower circularly flows in the third heater 21 through a pump to obtain heat so as to enable part of the heat to be gasified and enter the toluene purification tower 20. The top of the condenser is communicated with a third condenser 17 and a third condensate buffer tank 18 in sequence, and the bottom of the third condensate buffer tank 18 is provided with a second three-way pipeline 19. One side of the third reflux pipeline 25 is communicated with the top of the toluene purification tower 20 and is used for refluxing the toluene condensed in the third buffer tank 18 so as to realize gas-liquid exchange with ascending steam in the toluene purification tower 20, and the third reflux pipeline 25 is provided with a flow regulating valve; the other side is communicated with a toluene recovery device (not shown) through a toluene recovery pipeline, and the toluene recovery pipeline is provided with an adjusting valve. The opening degree of the regulating valve and the opening degree of the toluene recovery regulating valve on the third return pipeline are controlled through the liquid level of the third condensate buffer tank 18, the flow of the return pipeline is measured through cascade control and fed back to the opening degree signal of the toluene recovery regulating valve, and the corresponding reflux ratio is set.
The utility model discloses use three tower rectification, at first the azeotropic composition-water in the ternary azeotrope that distills off at the first dehydration tower top, ethyl ester is distilled off at rethread second toluene-ethyl ester knockout tower top, and toluene is distilled off through third toluene purification tower top at last, and each component of organic solvent all obtains effective recovery, and the energy consumption utilizes most economically. The utility model discloses both applicable in the continuity of production, also can be applicable to intermittent type nature production, operation elasticity is big. The equipment is compact, the occupied space is small, and the arrangement on a flat surface is convenient.
Preferably, a liquid level controller 2 is arranged between the feeding pump 1 and the dehydrating tower 8 and is used for regulating and controlling feeding of the organic waste liquid.
Further, the bottom of the water diversion package 5 is also connected with a water content measurement controller for measuring the water diversion quantity; the bottom of the second condensate buffer tank 13 is communicated with a first purity detection device for detecting the purity of the ethyl ester; the bottom of the third condensate buffer tank 18 is communicated with a second purity detection device for detecting the purity of the methylbenzene, and the methylbenzene can be recovered after meeting the conditions. Temperature monitors are arranged inside the dehydration tower 8, the toluene-ethyl ester separation tower 11 and the toluene purification tower 20 and used for regulating and controlling the internal temperature of the system.
Further, the bottom of the dehydration tower 8 is communicated with a first lift pump 10, the opening degree of a regulating valve of an outlet pipeline of the first lift pump 10 is regulated by measuring the liquid level at the bottom of the dehydration tower 8, organic waste liquid is pumped into a toluene-ethyl ester separation tower 11, and meanwhile, the liquid level at the bottom of the dehydration tower 8 is ensured to be stable; the bottom of the toluene-ethyl ester separation tower 11 is communicated with a second lift pump 12, the opening degree of a regulating valve of an outlet pipeline of the second lift pump 12 is regulated by measuring the liquid level at the bottom of the toluene-ethyl ester separation tower 11 and feeding back, organic waste liquid is pumped into a toluene purification tower 20, and meanwhile, the liquid level at the bottom of the toluene-ethyl ester separation tower 11 is ensured to be stable; the bottom of the toluene purification tower 20 is communicated with a kettle liquid discharge pump 22, the opening degree of a regulating valve on a pipeline of the kettle liquid discharge pump 22 is regulated by measuring the liquid level at the bottom of the toluene purification tower 20, the liquid level at the bottom of the toluene purification tower 20 is ensured to be stable, and impurities are discharged out of the system.
The utility model pumps the toluene ethyl ester water mixed liquid with the water content of 0.2-15% into the heat exchanger through the feed pump, and then the mixed liquid enters the dehydration tower after preheating and temperature rising, the bottom of the dehydration tower is heated through the first heater, and the temperature in the dehydration tower is controlled to gasify the liquid; the azeotrope composition of ethyl ester-water is% toluene: water% — 87.9: 12.1, boiling point 70.99 ℃, toluene-water azeotrope composition as% toluene: water% 78.8: 21.2, the boiling point is 70.29 ℃, the toluene-water azeotrope reaches the boiling point firstly and carries a small amount of ethyl ester-water to form mixed steam to reach the top of the tower by heating at the bottom of the tower, the heat exchanger releases latent heat of the steam to heat the feed mixed liquid, the mixed steam is completely liquefied by the first condenser to reach the first condensate buffer tank, the bottom of the first condensate buffer tank is provided with a water distributing drum which protrudes downwards, and organic miscibility of the ethyl ester and the toluene and hydrophobic difference of water carried by the azeotrope in the organic waste liquid cause layering of the organic waste liquid-water, and the water enters the water distributing drum due to large water specific gravity, so that the organic waste liquid (the ethyl ester, the toluene or other trace organic impurities) floats on the upper layer. The water in the water dividing bag is directly cut out through a yield test, other substances on the upper layer enter the dehydrating tower again for gas-liquid exchange, and the evaporation capacity/feeding capacity of the top of the dehydrating tower is controlled to be about 1.5-2.5 through flow control. As the water in the water bag is continuously cut off, the water content of the ethyl ester-toluene mixture at the bottom of the tower can gradually decrease to below 1000 ppm. Thereby breaking the azeotropic generation conditions of ethyl ester-water and toluene-water and creating conditions for the subsequent purification of ethyl ester/toluene.
And then, an ethyl ester-toluene mixture containing a small amount of water at the bottom of the dehydration tower enters a toluene-ethyl ester separation tower through a first lift pump, a second heater is arranged at the bottom of the toluene-ethyl ester separation tower, the boiling temperature of ethyl ester is 77 ℃, the boiling temperature of toluene is 110.8 ℃, the temperature of the toluene-ethyl ester separation tower is controlled to be 77-110 ℃ through temperature control, ethyl ester is gasified to carry a small amount of toluene vapor to the top of the toluene-ethyl ester separation tower, the ethyl ester enters a second condensate buffer tank through a second condenser, all the toluene vapor flows back to the tower, so that the liquid drags and pulls down the high-boiling toluene in the rising vapor, the vapor carries a small amount of low-boiling light components in the reflux liquid to continuously rise, and the gas-liquid balance. And a three-way pipeline is arranged at the bottom of the second condensate buffer tank, after the gas-liquid balance is stable, one part of ethyl ester is cut into products, and the other part of ethyl ester is reintroduced into the toluene-ethyl ester separation tower for gas-liquid exchange so as to ensure the purity of the ethyl ester. The reflux ratio of the toluene-ethyl ester separation tower is controlled to be 3-6, the reflux ratio is equal to the reflux tower flow/product extraction amount, the higher the reflux ratio is, the higher the product purity is, when the reflux ratio R exceeds 6, the purity tends to be stable, the energy consumption of a heater is increased, and the economical efficiency of a system is deteriorated.
And finally, pumping toluene liquid containing a small amount of high-boiling organic impurities at the bottom of the toluene-ethyl ester separation tower into a toluene purification tower through a second lift pump, heating the bottom of the toluene purification tower through a third heater, controlling the toluene purification tower at 132 ℃, heating, allowing the toluene vapor to carry a small amount of high-boiling organic impurities to reach the top of the tower, allowing the toluene vapor to enter a third condensate buffer tank through a third condenser, allowing all liquid in the third condensate buffer tank to flow back into the tower, allowing the liquid to drag and pull down the high-boiling organic impurities in the rising vapor, allowing a small amount of low-boiling toluene components in the vapor-carried reflux liquid to continuously rise, and gradually realizing gas-liquid balance. The bottom of a condensate buffer tank of the condenser is provided with a three-way pipeline, one part of condensate is cut into toluene products, the other part of condensate enters a toluene purification tower again through a pipeline for gas-liquid exchange, and liquid at the bottom of the tower is mainly high-boiling-point organic impurities and is pumped out through a kettle liquid discharge pump. The reflux ratio of the toluene purification tower is controlled to be 3-7.
Example 2
The organic waste liquid containing 2 wt% of water, 53.4% of toluene, 44% of ethyl ester and 0.6% of heavy component impurities was separated by using the system for separating ethyl ester toluene organic waste liquid containing a small amount of water in example 1; the method specifically comprises the following steps:
step 1: pumping the organic waste liquid of ethyl toluate water into a dehydrating tower, wherein the tower feeding amount is 1200kg/h, then heating, ensuring that the temperature of the top of the tower is 72 ℃, the temperature of liquid at the bottom of the tower is 84 ℃, and the weight ratio of the evaporation amount at the top of the dehydrating tower to the feeding amount is 1.5-2.5; continuously gasifying liquid in a dehydration tower, evaporating moisture and a small amount of organic matters, preheating organic waste liquid by releasing latent heat of steam from a heat exchanger outside the dehydration tower through a pipeline, condensing the organic waste liquid by a condenser, carrying out phase splitting in a first condensate buffer tank, allowing the moisture to enter a water splitting drum and allowing an organic solvent to float on an upper layer due to a large density difference, discharging the moisture out of a system, wherein the discharge amount of water at the tower top is more than 25.5kg/h, the organic phase is recycled by refluxing, the refluxing amount is 2457.4kg/h, and when the moisture content in the liquid at the tower bottom is detected to be reduced to be below 1000ppm on line through a moisture detector arranged in the dehydration tower, keeping the operation condition stable, and carrying out the next step; the weight ratio of the evaporation capacity at the top of the dehydrating tower to the feeding capacity is 2;
step 2: pumping the liquid at the bottom of the dehydration tower into a toluene-ethyl ester separation tower, heating the liquid at the bottom of the dehydration tower with the tower feeding amount of 1174.5kg/h, controlling the temperature of the top of the toluene-ethyl ester separation tower to be 77 ℃, the temperature of the liquid at the bottom of the toluene-ethyl ester separation tower to be 111 ℃ and the reflux ratio to be 4, gasifying ethyl ester to carry a small amount of toluene vapor to the top of the toluene-ethyl ester separation tower, condensing the liquid outside the toluene-ethyl ester separation tower through a pipeline by a condenser, and then returning the liquid back to the tower; then separating ethyl ester according to the reflux ratio of 4 until the purity of the ethyl ester in the condensate buffer tank is more than 99.5 percent, wherein the discharge amount at the top of the tower is 525.5 kg/h;
and step 3: pumping liquid at the bottom of a toluene-ethyl ester separation tower into a toluene purification tower, heating the liquid with the tower inlet amount of 649kg/h, controlling the temperature of the top of the toluene purification tower to be 110 ℃, the temperature of liquid at the bottom of the toluene purification tower to be 132 ℃, the reflux ratio to be 4, gasifying toluene to carry a small amount of impurity steam to the top of the toluene purification tower, condensing the steam outside the toluene purification tower through a pipeline by a condenser, and then returning the steam back to the tower completely until gas-liquid balance is realized; then, toluene was separated at a reflux ratio of 4 until the toluene purity in the condensate buffer tank became 99.5% or more, and the overhead discharge amount was 641 kg/h. And discharging the impurities in the liquid at the bottom of the tower at 8 kg/h.
Therefore, the utility model adopts the self-entrainment azeotropic distillation process to break the binary azeotropy of toluene-water and ethyl ester-water, the system equipment is compact, the occupied space is small, and the arrangement of the flat surface is convenient. Compared with the extraction and rectification, no other impurities are introduced, so that the purity of the final product is greatly ensured
The foregoing is a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of improvements and decorations can be made without departing from the principle of the present invention, and these improvements and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. A separation system of ethyl ester toluene organic waste liquid containing a small amount of water is characterized by comprising a feed pump, a dehydration tower, a toluene-ethyl ester separation tower and a toluene purification tower which are sequentially communicated;
a first heater is arranged at the bottom of the dehydration tower, and organic waste liquid at the bottom of the tower flows in the first heater through a pump in a circulating manner to obtain heat so as to enable the heat to be partially gasified and enter the dehydration tower; the top of the dehydration tower is sequentially communicated with a feeding preheater, a first condenser and a first condensate buffer tank, one side of the bottom of the first condensate buffer tank is provided with a water diversion bag protruding downwards, and the bottom of the water diversion bag is communicated with a water recovery pipeline device for recovering water; a first return pipeline is arranged on the other side of the bottom of the first condensate buffer tank, communicated with the top of the dehydration tower and used for returning the organic waste liquid; the bottom pipeline of the dehydration tower is communicated with the toluene-ethyl ester separation tower;
the bottom of the toluene-ethyl ester separation tower is provided with a second heater, the mixed organic waste liquid at the bottom of the toluene-ethyl ester separation tower circularly flows in the second heater through a pump to obtain heat, so that part of the mixed organic waste liquid is gasified and enters the toluene-ethyl ester separation tower, the top of the mixed organic waste liquid is sequentially communicated with a second condenser and a second condensate buffer tank, the bottom of the second condensate buffer tank is provided with a first three-way adjusting pipeline, one side of the first three-way adjusting pipeline is provided with a second return pipeline, and the second three-way adjusting pipeline is communicated with the top of the toluene-ethyl ester separation tower and is; the other side is communicated with an ethyl ester recovery device through an ethyl ester recovery pipe;
the bottom of the toluene-ethyl ester separation tower is communicated with a toluene purification tower, organic waste liquid is pumped into the toluene purification tower from the bottom of the toluene-ethyl ester separation tower, a third heater is arranged at the bottom of the toluene purification tower, and mixed organic waste liquid at the bottom of the toluene purification tower flows in the third heater through a pump in a circulating manner to obtain heat so that part of the heat is gasified and enters the toluene purification tower; the top of the third condensate buffer tank is communicated with a third condenser and a third condensate buffer tank in sequence, the bottom of the third condensate buffer tank is provided with a second three-way adjusting pipeline, wherein one side of the third condensate buffer tank is provided with a third return pipeline which is communicated with the top of the toluene purification tower and is used for refluxing the condensed toluene at the top of the tower so as to realize gas-liquid exchange with ascending steam in the tower; the other side is communicated with a toluene recovery device through a toluene recovery pipe.
2. The system for separating the organic waste liquor of ethyl ester with small water content as claimed in claim 1, wherein a liquid level controller is further arranged between the feeding pump and the dehydration tower for controlling the feeding of the organic waste liquor of ethyl ester with water content.
3. The system for separating the ethyl ester toluene organic waste liquid containing a small amount of water according to claim 2, wherein the bottom of the water dividing bag is further connected with a moisture measurement controller; the bottom of the second condensate buffer tank is communicated with a first purity detection device; the bottom of the third condensate buffer tank is communicated with a second purity detection device; temperature monitors are arranged in the dehydration tower, the toluene-ethyl ester separation tower and the toluene purification tower.
4. The system for separating the organic waste liquor of ethyl ester toluene containing a small amount of water according to claim 3, wherein the bottom of the dehydration tower is communicated with a first lift pump, and the organic waste liquor is pumped into the toluene-ethyl ester separation tower; the bottom of the toluene-ethyl ester separation tower is communicated with a second lift pump, and organic waste liquid is pumped into a toluene purification tower; and the bottom of the toluene purification tower is communicated with a kettle liquid discharge pump to discharge impurities out of the system.
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| CN202021663248.3U CN212532800U (en) | 2020-08-11 | 2020-08-11 | Organic waste liquid separation system of ethyl ester toluene that contains a small amount of water |
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| CN202021663248.3U CN212532800U (en) | 2020-08-11 | 2020-08-11 | Organic waste liquid separation system of ethyl ester toluene that contains a small amount of water |
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