CN107281894B - Full-temperature-range pressure swing adsorption method for vinyl chloride dehydration - Google Patents
Full-temperature-range pressure swing adsorption method for vinyl chloride dehydration Download PDFInfo
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- CN107281894B CN107281894B CN201610198565.4A CN201610198565A CN107281894B CN 107281894 B CN107281894 B CN 107281894B CN 201610198565 A CN201610198565 A CN 201610198565A CN 107281894 B CN107281894 B CN 107281894B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/047—Pressure swing adsorption
- B01D53/0476—Vacuum pressure swing adsorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/26—Drying gases or vapours
- B01D53/261—Drying gases or vapours by adsorption
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- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
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Abstract
the invention discloses a full temperature range pressure swing adsorption method for vinyl chloride dehydration, which relates to the technical field of vinyl chloride dehydration treatment and comprises a pretreatment process, an adsorption concentration process and a recycling process; the pretreatment process adopts one-time solid adsorption, oil stain, heavy molecular gas, a small amount of water and the like in the raw material gas are adsorbed by an adsorbent, the purer chloroethylene subjected to pretreatment and impurity removal is sent to an adsorption concentration process, the adsorption pressure is 0.5-2.5 Mpa, the operation temperature is 60-150 ℃, pure chloroethylene is output from the top of an adsorption tower, the water which is not adsorbed is pumped out and desorbed by a vacuum pump, the vacuum degree in a chloroethylene dehydration tower is kept at-0.088 Mpa to-0.094 Mpa, the pumped low-concentration chloroethylene gas is cooled to a low-concentration chloroethylene solution and then stored, the low-concentration chloroethylene solution and the low-concentration chloroethylene gas are subjected to heat exchange, and the medium-temperature chloroethylene solution is obtained and sent to a rectifying tower for rectification by a circulating liquid pump for recycling.
Description
Technical Field
the invention relates to the technical field of vinyl chloride dehydration, in particular to a full-temperature-range pressure swing adsorption method for vinyl chloride dehydration.
Background
Chloroethylene is colorless gas at normal temperature and normal pressure, is industrially transported in a liquid state, is not allowed to be directly contacted with a human body, and belongs to an OSHA controlled substance. Vinyl chloride is an important organic chemical product and is also a raw material for producing polyvinyl chloride (PVC). In the production process of vinyl chloride monomer, water is inevitably taken into the system. The existence of water can cause the hydrolysis reaction of the chloroethylene peroxide to generate hydrogen chloride (which is changed into hydrochloric acid, formic acid, formaldehyde and other acidic substances when meeting water, steel equipment is corroded, and the generated iron ions directly influence the quality of the PVC resin. The presence of iron ions in turn promotes the reaction of oxygen in the system with the vinyl chloride monomer to form peroxides. The latter can not only repeatedly hydrolyze, but also initiate the polymerization of vinyl chloride monomer to generate PVC with low polymerization degree, so that the rectification system is self-polymerization blocked, and the normal production is seriously influenced. Therefore, the effective dehydration of the vinyl chloride is very important for improving the quality of the polyvinyl chloride, preventing the equipment from being blocked and preventing the equipment from being excessively corroded.
at present, there are 2 international common methods for dehydration of vinyl chloride: the dehydration of a solid caustic dryer and the temperature swing adsorption dehydration (TSA) process, although the dehydration effect of the solid caustic dehydration device is good, the later operation cost is very high because a large amount of alkali liquor is uninterruptedly circulated; for example: with a 10 ten thousand tons/year polyvinyl chloride device, 100 tons of solid caustic soda are consumed every year, a large amount of alkaline water is discharged, and meanwhile, the polymerization quality of monomers is reduced and the production quality is influenced because fine NaOH powder is entrained in vinyl chloride; when the temperature swing adsorption dehydration (TSA) device is used for hot blowing dehydration of the water absorbed by the drying tower by using the dry gas chloroethylene gas, the operation cost is very high due to the need of consuming heat energy such as steam and a large amount of regenerated gas; the continuous and periodic temperature change can shorten the service life of the adsorbent, affect the safe and stable operation of the temperature swing adsorption dehydration device, and affect the quality of products during the maintenance and shutdown of the device.
disclosure of Invention
Full Temperature Range Pressure Swing Adsorption (FTrPSA) is a Pressure Swing Adsorption-based method for separating and purifying various gases by using the differences of Adsorption and separation coefficients and physicochemical properties of different material components under different pressures and temperatures and by adopting medium-high Temperature operation or low-Temperature operation which is easy to adsorb and sacrifices little Adsorption effect.
The invention provides a full-temperature-range pressure swing adsorption method for vinyl chloride dehydration, which improves the quality of vinyl chloride monomers, prevents pipeline equipment from being corroded due to the monomer water content, and solves the problems of high energy consumption, high cost, short service life of the device and the like in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
a full temperature range pressure swing adsorption method for vinyl chloride dehydration comprises the following steps:
(1) A pretreatment process;
adopting one-time solid adsorption, feeding chloroethylene raw material gas from a chloroethylene rectifying tower from the bottom of the tower, wherein the mass concentration of chloroethylene is 90-99%, adjusting the temperature to 60-150 ℃, adjusting the pressure to 0.5-2.5 MPa, absorbing oil stain, heavy molecular gas, a small amount of water and the like in the raw material gas by an adsorbent, and discharging relatively pure chloroethylene subjected to adsorption and impurity removal from the top of the adsorption tower to enter the next process;
(2) A dehydration step;
a. introducing chloroethylene raw gas to the bottom of one or more adsorption towers in an adsorption concentration system for adsorption by adopting an adsorption concentration process, wherein the adsorption pressure is 0.5-0.6 Mpag, and the operation temperature is 60-150 ℃; a plurality of adsorption towers are alternately and circularly operated to ensure that gas continuously enters;
b. Outputting pure vinyl chloride from the top of the adsorption tower, equalizing the pressure of a vinyl chloride dehydration tower and a middle tank after adsorption is finished, and allowing low-concentration vinyl chloride gas in the vinyl chloride dehydration tower to flow into the middle tank;
c. evacuating by a vacuumizing device after the dehydration tower is equalized; keeping the vacuum degree in the chloroethylene dehydration tower at-0.088 Mpa to-0.094 Mpa, completing the regeneration of the adsorption bed layer, cooling the low-concentration chloroethylene gas pumped out in the vacuumizing process to a low-concentration chloroethylene solution, and then sending the solution into a middle tank for storage;
(3) A recycling process;
The process comprises 1 heat exchanger, 1 medium temperature chloroethylene liquid recovery tank and 1 or more circulating pumps, wherein the low concentration chloroethylene solution stored in the intermediate tank exchanges heat with the low concentration chloroethylene gas to obtain the medium temperature chloroethylene solution, and the obtained medium temperature chloroethylene solution is sent to a rectifying tower for rectification by a circulating liquid pump for cyclic recovery and utilization.
furthermore, the disposable solid adsorption is carried out in an adsorption device comprising at least two adsorption towers, wherein one adsorption tower is always used for adsorption, and the other adsorption towers are shifted out for off-line regeneration or replacement of a new adsorbent;
further, the disposable solid adsorption is carried out in a filter adsorption device, and the filler in the filter is activated carbon or similar solid adsorbent;
furthermore, the adsorption concentration system consists of N adsorption towers, wherein N is a natural number more than 1; wherein 1-N-1 adsorption towers are in adsorption state, and the rest adsorption towers are in regeneration state.
furthermore, the filling material in the adsorption tower is one or more of active carbon, active alumina and molecular sieve.
further, the vacuum pumping device is a vacuum pump.
the traditional pressure swing adsorption is usually carried out at normal temperature, and some gases can be well adsorbed but are difficult to desorb, and even bed layers can be damaged; and FTrPSA solves most regeneration problems of difficult adsorption and easy adsorption of impurities, and can be coupled with other separation methods to realize the effects of saving energy, reducing consumption, prolonging the service life of an adsorption bed layer and the like.
Compared with the prior art, the invention has the beneficial effects that:
(1) because the principle is pressure swing adsorption and desorption is carried out in a pressure reduction mode, a large amount of regenerated gas and heat sources are not needed, and the energy consumption and the cost of the device in operation are greatly reduced; the problems of high energy consumption, high cost, short service life of the device and the like in the prior art are solved;
(2) The low-concentration chloroethylene gas is recycled, the chloroethylene solution is utilized to the maximum extent, the yield of the anhydrous chloroethylene is improved, the resources are saved, and the cost is low;
(3) The cooled low-concentration chloroethylene solution and the low-concentration chloroethylene gas are adopted for heat exchange and temperature reduction, so that the energy of the low-concentration chloroethylene solution is reasonably utilized, and the energy consumption is low;
(4) the low-concentration chloroethylene solution is subjected to step-by-step steam treatment, less low-concentration chloroethylene gas is extracted in the vacuumizing step, the heat exchange cost is reduced, the vacuumizing efficiency is improved, and the energy consumption is reduced;
(5) The intermediate temperature chloroethylene solution in the intermediate tank is adopted to carry out heat exchange on the anhydrous chloroethylene gas, so that the anhydrous chloroethylene gas can be cooled into a liquid finished product, the temperature of the liquid chloroethylene solution can be increased, the liquid chloroethylene solution does not need to be heated during rectification, and the full utilization of heat energy is realized;
(6) the service life of the device is long; because the principle is pressure swing adsorption, the periodic temperature change of heating and cooling is avoided, the long service life of the adsorbent is ensured, and the service life of the device is prolonged to more than 10 years; thereby solving the problems of short service life of the device and the like in the prior art;
(7) The adsorbent is regenerated only by adopting a vacuumizing mode without flushing, so that the residual water content of the adsorbent is reduced by 40-70% compared with the level which can be achieved by the traditional process, a better regeneration effect is achieved, compared with the traditional process, a large amount of flushing gas is saved, the yield of the anhydrous chloroethylene is greatly improved, and the yield of the anhydrous chloroethylene can reach 75-80%;
(8) the regeneration time is saved, and the production efficiency is improved; the invention omits the hot blowing step of heating and the cold blowing step of cooling to the adsorption temperature in the regeneration of the traditional technology, thereby saving the regeneration time and improving the production efficiency.
drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
in order to make those skilled in the art better understand the present invention, the technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the drawings in the embodiments of the present invention.
Example 1
as shown in fig. 1, a full temperature range pressure swing adsorption method for vinyl chloride dehydration comprises the following steps:
(1) A pretreatment process;
Adopting one-time solid adsorption, performing the adsorption in an adsorption device comprising at least two adsorption towers, wherein one adsorption tower is always used for adsorption, and the other adsorption towers are transferred out for off-line regeneration or replacement of a new adsorbent; feeding chloroethylene raw material gas from a chloroethylene rectifying tower from the bottom of the tower, wherein the mass concentration of chloroethylene is 90-99%, adjusting the temperature to 60-80 ℃, adjusting the pressure to 0.5-1.0 MPa, discharging the purer chloroethylene subjected to adsorption and impurity removal from the top of an adsorption tower, and feeding the purer chloroethylene into the next process, wherein oil stains, heavy molecular gas, a small amount of water and the like in the raw material gas are adsorbed by an adsorbent;
(2) A dehydration step;
a. An adsorption concentration process is adopted, and the system consists of 2 adsorption towers, 1 intermediate tank, 1 heat exchanger and a vacuum pump; wherein, 1 adsorption tower is in an adsorption state, the other 1 adsorption tower is in a regeneration state, and the filling material in the adsorption tower is one or more of active carbon, active alumina and molecular sieve; introducing chloroethylene gas into the bottom of 1 adsorption tower to be adsorbed, wherein the adsorption pressure is 0.5-1.0 Mpag, and the operation temperature is 60-80 ℃; the two adsorption towers are alternately and circularly operated to ensure that gas continuously enters;
b. the chloroethylene dehydration tower and the intermediate tank are subjected to pressure equalization through a communicated pipeline and a program control valve; opening valves on the chloroethylene dehydration tower and the intermediate tank, and because the pressure in the chloroethylene dehydration tower is greater than the pressure in the intermediate tank, chloroethylene solution steam in the chloroethylene dehydration tower can automatically flow into the intermediate tank, so that the pressure balance between the chloroethylene dehydration tower and the interior of the intermediate tank is realized;
c. evacuating by a vacuumizing device after the dehydration tower is equalized; keeping the vacuum degree in the chloroethylene dehydration tower at-0.088 Mpa to-0.090 Mpa, completing the regeneration of the molecular sieve, cooling the low-concentration chloroethylene gas pumped out in the vacuumizing process to a low-concentration chloroethylene solution, and then sending the solution to a middle tank for storage;
(3) A recycling process;
the process comprises 1 heat exchanger, 1 medium temperature chloroethylene liquid recovery tank and 1 or more circulating pumps, wherein the low concentration chloroethylene solution stored in the intermediate tank exchanges heat with the low concentration chloroethylene gas to obtain the medium temperature chloroethylene solution, and the obtained medium temperature chloroethylene solution is sent to a rectifying tower for rectification by a circulating liquid pump for cyclic recovery and utilization.
In the embodiment, the vinyl chloride dehydration tower and the intermediate tank are equalized by a pipeline and a program control valve which are communicated; open the valve on chloroethylene dehydration tower and the intermediate tank, because the pressure in the chloroethylene dehydration tower is greater than the pressure in the intermediate tank, chloroethylene solution steam in the chloroethylene dehydration tower can flow into the intermediate tank automatically, realizes that chloroethylene dehydration tower and the inside pressure of intermediate tank are balanced.
the pressure equalizing function of the chloroethylene dehydrating tower and the intermediate tank mainly aims to enable low-concentration chloroethylene steam in the chloroethylene dehydrating tower to automatically enter the intermediate tank, and the mode can enable the subsequent vacuumizing step to extract less low-concentration chloroethylene gas, so that the efficiency of the vacuumizing step is improved; in addition, because the low-concentration chloroethylene gas extracted in the vacuumizing step is less, the heat exchange medium for cooling the low-concentration chloroethylene gas is less, and the resource is saved.
In the embodiment, the adsorbent is subjected to evacuation regeneration under the condition that the vacuum degree in the chloroethylene dehydration tower is-0.088 Mpa to-0.090 Mpa, and after the adsorption concentration process is carried out, the residual water content of the adsorbent is reduced by 40% -50% compared with that of the traditional process under the same regeneration time.
example 2
as shown in fig. 1, a full temperature range pressure swing adsorption method for vinyl chloride dehydration comprises the following steps:
(1) A pretreatment process;
The method adopts disposable solid adsorption and is carried out in a filter adsorption device, and the filler in the filter is activated carbon or similar solid adsorbent; feeding chloroethylene raw material gas from a chloroethylene rectifying tower from the bottom of the tower, wherein the mass concentration of chloroethylene is 90-99%, adjusting the temperature to 120-150 ℃, adjusting the pressure to 1.0-1.8 MPa, discharging the purer chloroethylene subjected to adsorption and impurity removal from the top of an adsorption tower, and feeding the purer chloroethylene into the next process, wherein oil stains, heavy molecular gas, a small amount of water and the like in the raw material gas are adsorbed by an adsorbent;
(2) a dehydration step;
a. an adsorption concentration process is adopted, and the adsorption concentration process consists of 2 adsorption towers, 1 intermediate tank, 1 heat exchanger and a vacuum pump; wherein, 1 adsorption tower is in an adsorption state, the other 1 adsorption tower is in a regeneration state, and the filling material in the adsorption tower is one or more of active carbon, active alumina and molecular sieve; introducing chloroethylene gas into the bottom of 1 adsorption tower to be adsorbed, wherein the adsorption pressure is 1.0-1.8 Mpag, and the operation temperature is 120-150 ℃; the two adsorption towers are alternately and circularly operated to ensure that gas continuously enters;
b. The chloroethylene dehydration tower and the intermediate tank are subjected to pressure equalization through a communicated pipeline and a program control valve; opening valves on the chloroethylene dehydration tower and the intermediate tank, and because the pressure in the chloroethylene dehydration tower is greater than the pressure in the intermediate tank, chloroethylene solution steam in the chloroethylene dehydration tower can automatically flow into the intermediate tank, so that the pressure balance between the chloroethylene dehydration tower and the interior of the intermediate tank is realized;
c. Evacuating by a vacuumizing device after the dehydration tower is equalized; keeping the vacuum degree in the chloroethylene dehydration tower at-0.090 Mpa to-0.092 Mpa, completing the regeneration of the molecular sieve, cooling the low-concentration chloroethylene gas pumped out in the vacuumizing process to a low-concentration chloroethylene solution, and then sending the solution to a middle tank for storage;
(3) a recycling process;
the process comprises 1 heat exchanger, 1 medium temperature chloroethylene liquid recovery tank and 1 or more circulating pumps, wherein the low concentration chloroethylene solution stored in the intermediate tank exchanges heat with the low concentration chloroethylene gas to obtain the medium temperature chloroethylene solution, and the obtained medium temperature chloroethylene solution is sent to a rectifying tower for rectification by a circulating liquid pump for cyclic recovery and utilization.
in the embodiment, the adsorbent is subjected to evacuation regeneration under the condition that the vacuum degree in the vinyl chloride dehydration tower is-0.090 Mpa to-0.092 Mpa, and the residual water content of the adsorbent is reduced by 50-60% compared with that of the traditional process under the same regeneration time.
Example 3
As shown in fig. 1, a full temperature range pressure swing adsorption method for vinyl chloride dehydration comprises the following steps:
the pretreatment process adopts one-time solid adsorption, oil stain, heavy molecular gas, a small amount of water and the like in the raw material gas are adsorbed by an adsorbent, and the relatively pure chloroethylene subjected to adsorption and impurity removal is discharged from the top of an adsorption tower and enters an adsorption and concentration process; the adsorption concentration process is characterized in that chloroethylene gas is introduced to the bottoms of 1 adsorption tower to be adsorbed, the adsorption pressure is 1.8-2.5 Mpag, and the operation temperature is 80-110 ℃; 2, alternately and circularly operating the adsorption towers to ensure that gas continuously enters; evacuating by a vacuumizing device after the dehydration tower is equalized; keeping the vacuum degree in the chloroethylene dehydration tower at-0.092 Mpa to-0.094 Mpa, completing the regeneration of the molecular sieve, cooling the low-concentration chloroethylene gas pumped out in the vacuumizing process to a low-concentration chloroethylene solution, and then sending the solution to a middle tank for storage; in the recycling process, the low-concentration vinyl chloride solution stored in the intermediate tank exchanges heat with the low-concentration vinyl chloride gas to obtain the medium-temperature vinyl chloride solution, and the obtained medium-temperature vinyl chloride solution is sent to a rectifying tower for rectification through a circulating liquid pump for recycling.
In the embodiment, the adsorbent is evacuated and regenerated under the condition that the vacuum degree in the vinyl chloride dehydration tower is-0.092 Mpa to-0.094 Mpa, the adsorbent can obtain a good regeneration effect without heating or flushing, and the residual water content of the adsorbent is reduced by 60-70% compared with that of the traditional process under the same regeneration time.
the vacuum degree in the vinyl chloride dehydration tower is set to be-0.088 Mpa to-0.094 Mpa, so that the balance between the cost and the benefit can be obtained. Theoretically, the pressure relative to vacuum is-0.1 Mpa, corresponding to an absolute pressure of 0, which is practically impossible to achieve. To maintain the vacuum degree higher than-0.094 MPa, parts with more precise size and excellent material performance are needed, so that the production cost is greatly increased, and the cost is greatly increased more than the increase of the vacuum degree index and the cost reduced by the increase of the yield of the anhydrous chloroethylene. When the complete regeneration of the adsorbent can be realized by vacuumizing under the conditions of-0.088 Mpa to-0.094 Mpa, the vacuum degree does not need to be further improved.
It should be apparent that the above-described embodiments are only some, but not all, of the embodiments of the present invention. All other embodiments and structural changes that can be made by those skilled in the art without inventive effort based on the embodiments described in the present invention or based on the teaching of the present invention, all technical solutions that are the same or similar to the present invention, are within the scope of the present invention.
Claims (6)
1. a full-temperature-range pressure swing adsorption method for vinyl chloride dehydration is characterized by comprising the following steps.
(1) a pretreatment process;
Adopting one-time solid adsorption, feeding chloroethylene raw material gas from a chloroethylene rectifying tower from the bottom of the tower, adjusting the mass concentration of chloroethylene to 90-99%, adjusting the temperature to 60-150 ℃, adjusting the pressure to 0.5-2.5 MPa, adsorbing oil stain, heavy molecular gas and a small amount of water in the raw material gas by an adsorbent, and discharging relatively pure chloroethylene subjected to adsorption and impurity removal from the top of the adsorption tower to enter the next process;
(2) A dehydration step;
a. introducing chloroethylene raw gas to the bottom of one or more pressure swing adsorption towers in a full-temperature-range pressure swing adsorption system for adsorption by adopting an adsorption concentration process, wherein the adsorption pressure is 0.5-2.5 Mpag, and the operation temperature is 60-150 ℃; a plurality of adsorption towers are alternately and circularly operated to ensure that gas continuously enters;
b. Outputting pure vinyl chloride from the top of the adsorption tower, equalizing the pressure of a vinyl chloride dehydration tower and a middle tank after adsorption is finished, and allowing low-concentration vinyl chloride gas in the vinyl chloride dehydration tower to flow into the middle tank;
c. Evacuating by a vacuumizing device after the dehydration tower is equalized; keeping the vacuum degree in the chloroethylene dehydration tower at-0.088 Mpa to-0.094 Mpa, completing the regeneration of the adsorption bed layer, cooling the low-concentration chloroethylene gas pumped out in the vacuumizing process to a low-concentration chloroethylene solution, and then sending the solution into a middle tank for storage;
(3) A recycling process;
the process comprises 1 heat exchanger, 1 medium temperature chloroethylene liquid recovery tank and 1 or more circulating pumps, wherein the low concentration chloroethylene solution stored in the intermediate tank exchanges heat with the low concentration chloroethylene gas to obtain the medium temperature chloroethylene solution, and the obtained medium temperature chloroethylene solution is sent to a rectifying tower for rectification by the circulating liquid pump for cyclic recovery and utilization.
2. The full temperature swing adsorption process of vinyl chloride dehydration of claim 1, wherein said full temperature swing adsorption system consists of N pressure swing adsorption columns, N being a natural number greater than 1; wherein 1-N-1 pressure swing adsorption towers are in an adsorption state, and the rest pressure swing adsorption towers are in a regeneration state.
3. the full-temperature-range pressure swing adsorption process of vinyl chloride dehydration of claim 1 or 2, wherein the packing material in said pressure swing adsorption column is one or more of activated carbon, activated alumina, molecular sieve.
4. the full temperature swing adsorption process for vinyl chloride dehydration of claim 1 wherein said evacuating means is a vacuum pump.
5. The full temperature range pressure swing adsorption process of claim 1, wherein the process is carried out in an adsorption unit comprising at least two adsorption columns, one adsorption column being in adsorption operation, the remaining adsorption columns being taken off-line for regeneration or replacement of new adsorbent.
6. The full temperature range pressure swing adsorption process of vinyl chloride dehydration of claim 1, carried out in a filter adsorption unit, the filler in the filter being activated carbon.
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