CN211585272U - Intermittent recovery device for dimethylacetamide - Google Patents
Intermittent recovery device for dimethylacetamide Download PDFInfo
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- CN211585272U CN211585272U CN201922140991.4U CN201922140991U CN211585272U CN 211585272 U CN211585272 U CN 211585272U CN 201922140991 U CN201922140991 U CN 201922140991U CN 211585272 U CN211585272 U CN 211585272U
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Abstract
The utility model discloses a dimethylacetamide intermittent recovery device, which comprises an evaporation kettle, a dimethylacetamide recovery tower, a two-phase separator, a condenser, a distillation tank, a product tank and the like, wherein the top of the evaporation kettle is connected with a flange at the bottom of the dimethylacetamide recovery tower, a gas phase discharge port at the top of the dimethylacetamide recovery tower is connected with a heat medium inlet pipeline of the condenser, four pipelines in parallel connection with the outlet of heat medium of the condenser are respectively connected with the top feed inlets of the distillation tank and the product tank, a liquid phase discharge port of the dimethylacetamide recovery tower is connected with a feed inlet pipeline of the two-phase separator, a water phase outlet of the two-phase separator is connected with a feed inlet pipeline of a waste water collection tank, four pipelines in parallel connection with the outlet of oil phase of the two-phase separator are respectively connected with the distillation tank and the feed inlet of the product tank, recovery pipes at the bottoms of the, the device separates to obtain different products, has improved the separation effect, has reduced the waste and the environmental pollution of raw materials.
Description
Technical Field
The utility model belongs to the technical field of the chemical industry preparation, concretely relates to dimethylacetamide intermittent type recovery unit.
Background
Dimethylacetamide (DMAC) is a strong polar aprotic solvent and a chemical raw material, has the characteristics of high thermal stability, low corrosion, low toxicity and the like, is not easy to hydrolyze, and is widely applied to the fields of synthetic materials, medicines, pesticides, chemical fibers, petroleum processing, organic pigments and the like. The waste liquid from the production of dimethylacetamide is directly discharged as industrial waste water, which not only causes waste of raw materials, but also increases the treatment cost and causes certain pollution to the environment, so that many manufacturers choose to purify and recover dimethylacetamide by evaporation, concentration and rectification. However, the distillation equipment occupies a large space and is limited in use, and the traditional evaporation concentration distillation process can only obtain a single dimethylacetamide fraction, and the purity of the fraction is not high, the unit energy consumption is high, and the recovery cost is high, so that the dimethylacetamide recovery loses economic value.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to overcome prior art's not enough, provide a dimethylacetamide intermittent type recovery unit, this utility model realizes that different results are collected simultaneously, improves separation efficiency, reduces the dimethylacetamide loss, realizes its cyclic utilization, reduces environmental pollution.
The utility model discloses a realize through following technical scheme:
a dimethylacetamide intermittent recovery device is characterized in that: the device comprises an evaporation kettle, a dimethylacetamide recovery tower, a two-phase separator, a wastewater collection tank, a condenser, a first distillation tank, a second distillation tank, a third distillation tank and a product tank, wherein the top of the evaporation kettle is connected with the bottom of the dimethylacetamide recovery tower through a flange, a gas phase discharge port at the top of the dimethylacetamide recovery tower is connected with a heat medium inlet pipeline of the condenser, four pipelines are connected in parallel with a heat medium outlet of the condenser, the four pipelines are respectively connected with feed inlets at the tops of the first distillation tank, the second distillation tank, the third distillation tank and the product tank, a liquid phase discharge port at the top of the dimethylacetamide recovery tower is connected with a feed inlet pipeline at the middle part of the side wall of the two-phase separator, a water phase outlet of the two-phase separator is connected with a feed inlet pipeline at the top of the wastewater collection tank, and an oil phase outlet of the two-phase separator is connected with, the four pipelines are respectively connected with top feed inlets of a first distillation tank, a second distillation tank, a third distillation tank and a product tank, outlets at the bottoms of the first distillation tank, the second distillation tank, the third distillation tank and the product tank are respectively connected with a distillation collecting pipe and a solution recycling pipe in parallel, and the solution recycling pipes at the bottoms of the first distillation tank, the second distillation tank, the third distillation tank and the product tank are gathered to a recycling header pipe and return to a feed inlet of the evaporation kettle; a steam heating coil is arranged at the bottom of the evaporation kettle; the condenser heat medium pipeline is also provided with a vacuum pipe, and the vacuum pipe is connected to a vacuum system and a tail gas absorption system; a built-in condenser is arranged at the top of the dimethylacetamide recovery tower, a gas-phase discharge port at the top of the dimethylacetamide recovery tower is arranged at the upper part of the built-in condenser, and a liquid-phase discharge port at the top of the dimethylacetamide recovery tower is arranged at the lower part of the built-in condenser; the two-phase separator is a mobile device.
In the technical scheme, the liquid level meter is arranged outside the evaporation kettle, so that the functions of liquid level measurement, indication and alarm are realized; the top of the evaporation kettle is provided with a thermometer and a pressure gauge, so that the temperature and the pressure can be measured and displayed.
In the technical scheme, a middle-lower thermometer, a middle-lower pressure gauge, a middle-upper thermometer and a middle-upper pressure gauge are respectively arranged at the middle-lower part and the middle-upper part of the dimethylacetamide recovery tower, and the middle-lower thermometer is interlocked with a control valve on a steam feed pipe of a steam heating coil at the bottom of an evaporation kettle.
In the technical scheme, a nitrogen feeding pipe is arranged on a vacuum pipe of the condenser heat medium pipeline; the waste water collecting tank, the first fraction tank, the second fraction tank, the third fraction tank and the product tank are all provided with nitrogen feeding pipes at the tops.
In the technical scheme, the built-in condenser at the top of the dimethylacetamide recovery tower is provided with an inlet pipeline and an outlet pipeline for cooling circulating water.
In the technical scheme, the condenser is a shell-and-tube vacuum condenser, the heat medium inlet and outlet are arranged on the shell pass, and the freezing circulating water inlet and outlet are arranged on the tube pass.
In the above technical scheme, the two-phase separator includes a mixing chamber and a clarifying chamber, the stirring motor is disposed in the mixing chamber, the feed inlet of the two-phase separator is disposed in the mixing chamber, the water phase outlet of the two-phase separator is disposed at the bottom of the clarifying chamber, and the oil phase outlet of the two-phase separator is disposed at the upper portion of the clarifying chamber.
Among the above-mentioned technical scheme, jar, first fraction jar are collected to waste water, second fraction jar, third fraction jar and product jar all are equipped with the manometer at the top, jar, first fraction jar are collected to waste water, and second fraction jar, third fraction jar and product jar all are equipped with the level gauge at the barrel, jar, first fraction jar are collected to waste water, and second fraction jar, third fraction jar and product jar all are equipped with the thermometer in the lower part.
In the technical scheme, the feed pipes of the wastewater collection tank, the first fraction tank, the second fraction tank, the third fraction tank and the product tank are all deep into the bottoms of the corresponding devices.
In the technical scheme, the dimethylacetamide recovery tower is a filler type recovery tower, the filler is stainless steel wire mesh filler, the filler efficiency is high, and the dimethylacetamide recovery tower is corrosion-resistant.
The utility model discloses an advantage and beneficial effect do:
1. the condenser arranged in the dimethylacetamide recovery tower is used for condensing distillate at the top of the tower, excessive pipelines and equipment of an external condenser are omitted for condensing in the tower, and welding spots and flange connection points are reduced, so that vacuum air leakage points are reduced, excessive pipelines and equipment of the external condenser are omitted, pressure drop generated by the external equipment is avoided, and vacuum operation is facilitated.
2. And a two-phase separator is added in front of the liquid phase extraction stream at the top of the tower to enter the fraction tank, and the water phase and the solvent phase are separated by utilizing the high-efficiency separation of the two-phase separator to obtain a high-purity product.
Drawings
FIG. 1 is a schematic view of a device for intermittently recovering dimethylacetamide.
Wherein: 1: evaporation kettle, 2: dimethylacetamide recovery column, 3: two-phase separator, 4: condenser, 5: waste water collection tank, 6: first fraction drum, 7: second distillate pot, 8: third cut tank, 9: a product tank;
for a person skilled in the art, other relevant figures can be obtained from the above figures without inventive effort.
Detailed Description
In order to make the technical field person understand the solution of the present invention better, the technical solution of the present invention is further described below with reference to the specific embodiments.
Example one
A dimethylacetamide intermittent recovery device is characterized in that: the device comprises an evaporation kettle, a dimethylacetamide recovery tower, a two-phase separator, a wastewater collection tank, a condenser, a first distillation tank, a second distillation tank, a third distillation tank and a product tank, wherein the top of the evaporation kettle is connected with the bottom of the dimethylacetamide recovery tower through a flange, a gas phase discharge port at the top of the dimethylacetamide recovery tower is connected with a heat medium inlet pipeline of the condenser, four pipelines are connected in parallel with a heat medium outlet of the condenser, the four pipelines are respectively connected with feed inlets at the tops of the first distillation tank, the second distillation tank, the third distillation tank and the product tank, a liquid phase discharge port at the top of the dimethylacetamide recovery tower is connected with a feed inlet pipeline at the middle part of the side wall of the two-phase separator, a water phase outlet of the two-phase separator is connected with a feed inlet pipeline at the top of the wastewater collection tank, and an oil phase outlet of the two-phase separator is connected with, the four pipelines are respectively connected with top feed inlets of a first distillation tank, a second distillation tank, a third distillation tank and a product tank, outlets at the bottoms of the first distillation tank, the second distillation tank, the third distillation tank and the product tank are respectively connected with a distillation collecting pipe and a solution recycling pipe in parallel, and the solution recycling pipes at the bottoms of the first distillation tank, the second distillation tank, the third distillation tank and the product tank are gathered to a recycling header pipe and return to a feed inlet of the evaporation kettle; a steam heating coil is arranged at the bottom of the evaporation kettle; the condenser heat medium pipeline is also provided with a vacuum pipe, and the vacuum pipe is connected to a vacuum system and a tail gas absorption system; a built-in condenser is arranged at the top of the dimethylacetamide recovery tower, a gas-phase discharge port at the top of the dimethylacetamide recovery tower is arranged at the upper part of the built-in condenser, and a liquid-phase discharge port at the top of the dimethylacetamide recovery tower is arranged at the lower part of the built-in condenser; the two-phase separator is a mobile device.
Example two
A dimethylacetamide intermittent recovery device is characterized in that: the device comprises an evaporation kettle, a dimethylacetamide recovery tower, a two-phase separator, a wastewater collection tank, a condenser, a first distillation tank, a second distillation tank, a third distillation tank and a product tank, wherein the top of the evaporation kettle is connected with the bottom of the dimethylacetamide recovery tower through a flange, a gas phase discharge port at the top of the dimethylacetamide recovery tower is connected with a heat medium inlet pipeline of the condenser, four pipelines are connected in parallel with a heat medium outlet of the condenser, the four pipelines are respectively connected with feed inlets at the tops of the first distillation tank, the second distillation tank, the third distillation tank and the product tank, a liquid phase discharge port at the top of the dimethylacetamide recovery tower is connected with a feed inlet pipeline at the middle part of the side wall of the two-phase separator, a water phase outlet of the two-phase separator is connected with a feed inlet pipeline at the top of the wastewater collection tank, and an oil phase outlet of the two-phase separator is connected with, the four pipelines are respectively connected with top feed inlets of a first distillation tank, a second distillation tank, a third distillation tank and a product tank, outlets at the bottoms of the first distillation tank, the second distillation tank, the third distillation tank and the product tank are respectively connected with a distillation collecting pipe and a solution recycling pipe in parallel, and the solution recycling pipes at the bottoms of the first distillation tank, the second distillation tank, the third distillation tank and the product tank are gathered to a recycling header pipe and return to a feed inlet of the evaporation kettle; a steam heating coil is arranged at the bottom of the evaporation kettle; the condenser heat medium pipeline is also provided with a vacuum pipe, the vacuum pipe is connected to a vacuum system and a tail gas absorption system, the vacuum degree in the evaporation kettle is 10-50 kPa, the vacuum degree in the dimethylacetamide recovery tower is 10-50 kPa, the evaporation temperature in the evaporation kettle is reduced by vacuum operation, the high-temperature pyrolysis of key products in the raw materials is reduced to the greatest extent, and the corrosivity of the raw materials is reduced; a built-in condenser is arranged at the top of the dimethylacetamide recovery tower, a gas-phase discharge port at the top of the dimethylacetamide recovery tower is arranged at the upper part of the built-in condenser, and a liquid-phase discharge port at the top of the dimethylacetamide recovery tower is arranged at the lower part of the built-in condenser; the two-phase separator is a mobile device.
A liquid level meter is arranged outside the evaporation kettle, so that the functions of liquid level measurement, indication and alarm are realized; a temperature meter and a pressure meter are sequentially arranged above the evaporation kettle, so that the measurement and display of temperature and pressure can be realized; the middle-lower part and the middle-upper part of the dimethylacetamide recovery tower are respectively provided with a middle-lower part thermometer, a middle-lower part pressure gauge, a middle-upper part thermometer and a middle-upper part pressure gauge, so that real-time monitoring of temperature and pressure at different positions in the dimethylacetamide recovery tower can be realized, the middle-lower part thermometer is interlocked with a control valve on a steam feed pipe of a steam heating coil at the bottom of an evaporation kettle, and when the temperature of the middle-lower part thermometer exceeds a limited range, the middle-lower part thermometer regulates and controls the control valve on the steam feed pipe of the heating steam coil, so that the gas flow of low-pressure steam is regulated; the built-in condenser at the top of the dimethylacetamide recovery tower is provided with an inlet pipeline and an outlet pipeline for cooling circulating water, so that the built-in condenser maintains a low temperature, and further the steam at the top of the recovery tower is liquefied;
the condenser is a shell-and-tube vacuum condenser, the heat medium inlet and outlet are arranged on the shell pass, and the freezing circulating water inlet and outlet are arranged on the tube pass; a nitrogen feeding pipe is arranged on a vacuum pipe of the condenser heat medium pipeline and used for controlling the stability of the vacuum degree of the system; the top parts of the wastewater collection tank, the first fraction tank, the second fraction tank, the third fraction tank and the product tank are all provided with nitrogen feeding pipes, nitrogen is used as replacement gas and protective gas to remove other gases in the wastewater collection tank, the first fraction tank, the second fraction tank, the third fraction tank and the product tank, so as to prevent other chemical reactions from occurring, and the nitrogen belongs to chemical reactions in a chemical inert gas fraction tank and the product tank, so that the smooth proceeding of the reactions is ensured; the two-phase separator comprises a mixing chamber and a clarifying chamber, the stirring motor is arranged in the mixing chamber, a feed inlet of the two-phase separator is arranged in the mixing chamber, a water phase outlet of the two-phase separator is arranged at the bottom of the clarifying chamber, and an oil phase outlet of the two-phase separator is arranged at the upper part of the clarifying chamber; when the stirring motor is started, the stirring paddle is driven to rotate, so that water-oil two-phase components are efficiently separated, the waste water collection tank, the first distillation tank, the second distillation tank, the third distillation tank and the product tank are respectively provided with a pressure gauge at the top, the waste water collection tank, the first distillation tank, the second distillation tank, the third distillation tank and the product tank are respectively provided with a liquid level meter at the barrel body, the waste water collection tank, the first distillation tank, the second distillation tank, the third distillation tank and the product tank are respectively provided with a temperature gauge at the lower part, and the measurement and display of the temperature and the pressure gauge liquid level in the waste water collection tank, the first distillation tank, the second distillation tank, the third distillation tank and the product tank are respectively realized; the feed pipes of the waste water collecting tank, the first fraction tank, the second fraction tank, the third fraction tank and the product tank are all deep into the bottoms of the corresponding devices so as to prevent static electricity generated by material spraying.
EXAMPLE III
An operation method of the intermittent dimethylacetamide recovery device according to embodiment 1 or 2 includes the following steps: the system is an intermittent rectification process, and firstly, raw materials are added into an evaporation kettle, wherein the raw materials mainly comprise chloroform, dimethylacetamide, water and tar. Heating steam is introduced into a heating coil of the evaporation kettle through a steam inlet pipe to heat the raw material, the raw material components after heating and gasification enter a dimethylacetamide recovery tower to be rectified and separated, the rectified components are at the top of the tower, a part of gas-phase components at the top of the tower are condensed by a condenser arranged in the top of the tower, and are extracted and sent to a two-phase separator, and the rest of the gas-phase components flow back to the tower. The extracted material enters a mixing chamber of a two-phase separator, a stirring motor is started, the stirring motor drives a stirring paddle to rotate to accelerate the separation of water-oil two-phase components, the first-stage fraction mainly contains water and chloroform, after the separation of the two-phase separator, the chloroform enters a first fraction tank through an oil phase outlet at the upper part of a clarification chamber, the water enters a wastewater collection tank through a water phase outlet at the bottom of the clarification chamber, the second-stage fraction mainly contains chloroform, the part of the material is separated from trace water through the two-phase separator and then sent into a second fraction tank, the third-stage fraction is a chloroform and dimethylacetamide mixed fraction, and the part of the material is sent into a third fraction tank after passing through the two-phase separator; and then opening a vacuum system, controlling the vacuum degree of the system to be 10-20 kPa, carrying out reduced pressure rectification to obtain fraction dimethylacetamide of the fourth stage, and conveying the fraction into a product tank after passing through a two-phase separator. And the fractions in each stage which are not condensed at the top of the rectifying tower are condensed by a condenser and then are respectively sent into the collecting tanks corresponding to the fractions in each stage, the fractions are collected by fraction collecting pipes at the bottom outlets of the fraction collecting tanks, and residual solvents in the fraction collecting tanks are gathered to a collecting main pipe through solution recycling pipes at the bottoms of the fraction collecting tanks and then return to a feeding hole of the evaporation kettle. When the materials in the evaporation kettle are too little, the gas-liquid load is lower than the operation elasticity of the rectifying tower, and the normal operation of the rectifying tower is difficult to maintain, stopping introducing steam into the evaporation kettle, instead introducing circulating water for cooling, discharging tar heavy components from the bottom of the evaporation kettle after the cooling is finished, and finishing the batch distillation process.
Spatially relative terms, such as "upper," "lower," "left," "right," and the like, may be used in the embodiments for ease of description to describe one element or feature's relationship to another element or feature as illustrated in the figures. It will be understood that the spatial terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "below" other elements or features would then be oriented "above" the other elements or features. Thus, the exemplary term "lower" can encompass both an upper and a lower orientation. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
Moreover, relational terms such as "first" and "second," and the like, may be used solely to distinguish one element from another element having the same name, without necessarily requiring or implying any actual such relationship or order between such elements.
The invention has been described above by way of example, and it should be noted that any simple variants, modifications or other equivalent substitutions by a person skilled in the art without spending creative effort may fall within the scope of protection of the present invention without departing from the core of the present invention.
Claims (10)
1. A dimethylacetamide intermittent recovery device is characterized in that: the device comprises an evaporation kettle, a dimethylacetamide recovery tower, a two-phase separator, a wastewater collection tank, a condenser, a first distillation tank, a second distillation tank, a third distillation tank and a product tank, wherein the top of the evaporation kettle is connected with the bottom of the dimethylacetamide recovery tower through a flange, a gas phase discharge port at the top of the dimethylacetamide recovery tower is connected with a heat medium inlet pipeline of the condenser, four pipelines are connected in parallel with a heat medium outlet of the condenser, the four pipelines are respectively connected with feed inlets at the tops of the first distillation tank, the second distillation tank, the third distillation tank and the product tank, a liquid phase discharge port at the top of the dimethylacetamide recovery tower is connected with a feed inlet pipeline at the middle part of the side wall of the two-phase separator, a water phase outlet of the two-phase separator is connected with a feed inlet pipeline at the top of the wastewater collection tank, and an oil phase outlet of the two-phase separator is connected with, the four pipelines are respectively connected with top feed inlets of a first distillation tank, a second distillation tank, a third distillation tank and a product tank, outlets at the bottoms of the first distillation tank, the second distillation tank, the third distillation tank and the product tank are respectively connected with a distillation collecting pipe and a solution recycling pipe in parallel, and the solution recycling pipes at the bottoms of the first distillation tank, the second distillation tank, the third distillation tank and the product tank are gathered to a recycling header pipe and return to a feed inlet of the evaporation kettle; a steam heating coil is arranged at the bottom of the evaporation kettle; the condenser heat medium pipeline is also provided with a vacuum pipe, and the vacuum pipe is connected to a vacuum system and a tail gas absorption system; a built-in condenser is arranged at the top of the dimethylacetamide recovery tower, a gas-phase discharge port at the top of the dimethylacetamide recovery tower is arranged at the upper part of the built-in condenser, and a liquid-phase discharge port at the top of the dimethylacetamide recovery tower is arranged at the lower part of the built-in condenser; the two-phase separator is a mobile device.
2. A dimethylacetamide intermittent recovery device according to claim 1, characterized in that: a liquid level meter is arranged outside the evaporation kettle, so that the functions of liquid level measurement, indication and alarm are realized; the top of the evaporation kettle is provided with a thermometer and a pressure gauge, so that the temperature and the pressure can be measured and displayed.
3. A dimethylacetamide intermittent recovery device according to claim 1, characterized in that: the device comprises a dimethyl acetamide recovery tower, a steam feed pipe, a steam heating coil pipe, a control valve, a temperature gauge, a pressure gauge, a middle-lower part thermometer, a middle-upper part pressure gauge and a control valve, wherein the middle-lower part thermometer, the middle-lower part pressure gauge, the middle-upper part thermometer and the middle-upper part pressure gauge are respectively arranged at the middle-lower part and the middle-upper part of the.
4. A dimethylacetamide intermittent recovery device according to claim 1, characterized in that: a nitrogen feeding pipe is arranged on a vacuum pipe of the condenser heat medium pipeline; the waste water collecting tank, the first fraction tank, the second fraction tank, the third fraction tank and the product tank are all provided with nitrogen feeding pipes at the tops.
5. A dimethylacetamide intermittent recovery device according to claim 1, characterized in that: and an inlet pipeline and an outlet pipeline of cooling circulating water are arranged on the built-in condenser at the top of the dimethylacetamide recovery tower.
6. A dimethylacetamide intermittent recovery device according to claim 1, characterized in that: the condenser is a shell-and-tube vacuum condenser, the heat medium inlet and outlet are arranged on the shell pass, and the freezing circulating water inlet and outlet are arranged on the tube pass.
7. A dimethylacetamide intermittent recovery device according to claim 1, characterized in that: the two-phase separator comprises a mixing chamber and a clarifying chamber, a stirring motor is arranged in the mixing chamber, a feed inlet of the two-phase separator is arranged in the mixing chamber, a water phase outlet of the two-phase separator is arranged at the bottom of the clarifying chamber, and an oil phase outlet of the two-phase separator is arranged at the upper part of the clarifying chamber.
8. A dimethylacetamide intermittent recovery device according to claim 1, characterized in that: waste water collection tank, first fraction jar, second fraction jar, third fraction jar and product jar all are equipped with the manometer at the top, waste water collection tank, first fraction jar, second fraction jar, third fraction jar and product jar all are equipped with the level gauge at the barrel, waste water collection tank, first fraction jar, second fraction jar, third fraction jar and product jar all are equipped with the thermometer in the lower part.
9. The intermittent recovering apparatus of dimethylacetamide according to claim 1, characterized in that: the feed pipes of the wastewater collection tank, the first fraction tank, the second fraction tank, the third fraction tank and the product tank are all deep into the bottoms of the corresponding devices.
10. The intermittent recovering apparatus of dimethylacetamide according to claim 1, characterized in that: the dimethylacetamide recovery tower is a filler type recovery tower, the filler is stainless steel wire mesh filler, the filler efficiency is high, and the dimethylacetamide recovery tower is corrosion-resistant.
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