CN110483229B - Vinyl acetylene refining method - Google Patents
Vinyl acetylene refining method Download PDFInfo
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- CN110483229B CN110483229B CN201910815350.6A CN201910815350A CN110483229B CN 110483229 B CN110483229 B CN 110483229B CN 201910815350 A CN201910815350 A CN 201910815350A CN 110483229 B CN110483229 B CN 110483229B
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/11—Purification; Separation; Use of additives by absorption, i.e. purification or separation of gaseous hydrocarbons with the aid of liquids
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Abstract
The invention relates to the field of chemical industry, in particular to a method for refining vinyl acetylene; the method comprises the following steps: step 1: introducing the absorption liquid obtained by the treatment of the degassing tower into an analytical tower from the middle part of the analytical tower; step 2: heating the absorption liquid introduced into the desorption tower, cooling the gas at the top of the desorption tower, and condensing and refluxing part of the gas; and step 3: detecting the temperature of liquid at the fifth tower plate of the desorption tower from the feed inlet from bottom to top, and increasing the condensation reflux at the top of the desorption tower when the temperature is higher than 18-22 ℃ until the temperature is lower than 10-14 ℃; and 4, step 4: removing water in the liquid above the fourth tower plate from the feeding port from bottom to top, and collecting uncondensed gas at the top of the desorption tower. The refining method of the scheme can remove water in the desorption solution while rectifying the vinyl acetylene, and avoid the water from reducing the boiling point of an organic phase, thereby reducing the divinyl acetylene in the product gas.
Description
Technical Field
The invention relates to the field of chemical industry, and particularly relates to a method for refining vinyl acetylene.
Background
Vinyl acetylene is an important eneyne compound and is mainly used for producing chloroprene rubber, adhesive methanol gum and preparing polymers based on divinyl ether and methyl vinyl (methyl) ketone. Acetylene is generally produced by a calcium carbide method in industry, acetylene is dimerized under the catalysis of cuprous chloride and ammonium chloride acid solution to obtain vinyl acetylene, but when the vinyl acetylene is prepared by acetylene dimerization, a lot of byproducts are generated besides the vinyl acetylene, and the obtained reaction gas also comprises divinyl acetylene, hydrochloric acid, acetylene, acetaldehyde, water and the like besides the vinyl acetylene, so that the reaction gas needs to be washed, absorbed and degassed to obtain a xylene solution (absorption liquid) in which the vinyl acetylene, the divinyl acetylene, the acetaldehyde and the like are dissolved, and the absorption liquid is rectified and washed to obtain the qualified vinyl acetylene with higher purity.
The current refining method commonly used in industry is that absorption liquid is heated firstly, the boiling point of vinyl acetylene is 5 ℃, the boiling point is lower, so that the vinyl acetylene forms a large amount of gas and is primarily separated from impurities; and then condensing the evaporated gas, wherein impurities are changed into liquid, and are separated from the vinyl acetylene again, and finally, a high-purity vinyl acetylene finished product is obtained.
The existing device refines vinyl acetylene by rectification, but because the absorption liquid after degassing contains a small amount of water, the water can be more and more along with the rectification, the water can reduce the boiling point of an organic phase, so that the divinyl acetylene is evaporated out along with the vinyl acetylene, and during condensation, the divinyl acetylene can not be completely condensed into a liquid state and is discharged along with the vinyl acetylene, so that the content of the divinyl acetylene in the finally prepared vinyl acetylene gas exceeds the standard, and the quality is unqualified.
Disclosure of Invention
The invention aims to provide a method for refining vinyl acetylene, which separates water in a desorption solution while rectifying.
In order to achieve the purpose, the technical scheme of the invention is as follows: a vinyl acetylene refining method comprises the following steps:
step 1: introducing the absorption liquid obtained by the treatment of the degassing tower into an analytical tower from the middle part of the analytical tower;
step 2: heating the absorption liquid introduced into the desorption tower, cooling the gas at the top of the desorption tower, and condensing and refluxing part of the gas;
and step 3: detecting the temperature of liquid at the fifth tower plate of the desorption tower from the feed inlet from bottom to top, and increasing the condensation reflux at the top of the desorption tower when the temperature is higher than 18-22 ℃ until the temperature is lower than 10-14 ℃;
and 4, step 4: removing water in the liquid above the fourth tower plate from the feeding port from bottom to top, and collecting uncondensed gas at the top of the desorption tower.
The beneficial effects of the scheme are as follows:
1. get rid of the water in the desorption liquid in this scheme, avoid water to reduce the boiling point of organic phase, lead to the divinylacetylene of evaporation to increase, so this scheme can avoid the divinylacetylene increase in the vinylacetylene that obtains at last to improve vinylacetylene's purity.
2. Since the material components on the fifth tower plate comprise xylene, vinyl acetylene, water, divinyl acetylene and the like, wherein the temperature of the fifth tower plate rises rapidly when water is slightly increased, the temperature change at the fifth tower plate is more sensitive, water vapor formed by evaporation when the absorption liquid is heated in the step 2 is condensed under the action of an overhead condenser and is gathered on the fourth tower plate to form a water-rich liquid, and the separation is more convenient.
Further, step 2 is heated at the bottom of the desorption column.
The beneficial effect of this scheme does: the heating location is at the bottom of the desorption column, which allows sufficient time for the vinyl acetylene to be desorbed from the xylene.
Further, step 2 is heated with steam.
The beneficial effect of this scheme does: compared with a heating element, the steam is more fully contacted with the absorption liquid to be heated, and the heating is more uniform. Compared with the heating by hot water, the temperature of the steam is higher, and the heating effect is better.
Further, the absorption liquid obtained from the degassing tower in the step 1 is preheated before being introduced into the desorption tower, and is introduced into the desorption tower after the temperature of the absorption liquid is higher than 70-75 ℃.
The beneficial effect of this scheme does: the absorption liquid can reach the boiling point of the vinyl acetylene more quickly after being preheated, so that the vinyl acetylene forms gas, and the refining efficiency is improved.
Further, in step 4, before removing water from the liquid above the fourth tray, the liquid above the fourth tray is first led out of the desorption column, and the liquid from which water has been removed is led into the desorption column.
The beneficial effect of this scheme does: the water enrichment area is arranged above the fourth tower plate, the water content is highest, the liquid is extracted for separation, the separated water amount is the largest, and the separation effect is the best.
Further, the liquid after removing water was introduced below the fourth tray.
The beneficial effect of this scheme does: and (3) refluxing the organic phase liquid to the lower part of the fourth tower plate, so that the organic phase after water separation is prevented from being mixed with water again. More importantly, the organic phase is refluxed into the tower by using the potential difference as power without external power.
Further, a dispersion tray was disposed below the fourth tray, and the liquid phase after water removal was directly led to the dispersion tray.
The beneficial effect of this scheme does: after the liquid is led out, the liquid is kept stand to divide water, the organic phase liquid without water enters the desorption tower again and is dispersed by the dispersion plate, so that the organic phase is uniformly distributed in the desorption tower and is uniformly mixed with other desorption liquid, and the condition that the concentration at a certain position is obviously uneven can not occur in the desorption tower.
Further, in the step 4, after the liquid above the fourth tower plate is led out, the fourth tower plate is firstly kept stand until the water and the organic phase are separated, and then the water is removed.
The beneficial effect of this scheme does: the liquid led out from the desorption tower is in a flowing state, clear limits are difficult to appear between water and the organic phase, and the water can be gathered under the organic phase by standing, so that the separation is convenient.
Further, step 2 uses brine with temperature lower than the boiling point of vinyl acetylene to cool the gas.
The beneficial effect of this scheme does: compared with water, the saline water has better heat conductivity and better cooling effect on the top of the desorption tower.
Further, the temperature of the brine in step 2 is equal to or lower than-15 ℃.
The beneficial effect of this scheme does: the temperature of the brine is lower, and the cooling effect is better.
Drawings
FIG. 1 is an elevational longitudinal sectional view of an embodiment of the invention.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: the tower body 1, a feeding hole 11, a discharging hole 12, a first tower plate 13, a dispersion disc 14, a fourth tower plate 15, a gas channel 151, a support rod 152, an umbrella cover 153, a fifth tower plate 16, a reboiler 2, a tube array 21, a steam inlet 22, a condensed water outlet 23, an interface meter 3, a liquid phase outlet tube 41, a liquid phase inlet tube 42, a water separator 45, a water discharge tube 46, a water discharge valve 47 and a tower top condenser 5.
The embodiment is basically as shown in the attached figure 1:
a vinyl acetylene refining method comprises the following steps:
step 1: preheating the absorption liquid obtained by the treatment of the degassing tower to 70-75 ℃, and introducing the absorption liquid into the desorption tower from the middle part of the desorption tower;
step 2: heating the absorption liquid introduced into the desorption tower at the bottom of the desorption tower by adopting steam, introducing saline water with the temperature of-15 ℃ into a tower top condenser to cool the gas at the top of the tower, and refluxing part of gas into the desorption tower from the lower opening of the condenser after condensing;
and step 3: detecting the temperature of liquid at the fifth tower plate from the bottom to the top of the feeding port of the desorption tower by using a remote thermometer, and increasing the condensation reflux at the top of the desorption tower when the temperature is higher than 18-22 ℃ until the temperature is lower than 10-14 ℃, specifically, increasing the condensate reflux when the temperature is higher than 20 ℃ in the embodiment;
and 4, step 4: guiding the absorption liquid above a fourth tower plate from bottom to top from a feeding port out of the desorption tower, standing until water and the organic phase are separated, removing the water below the absorption liquid, guiding the upper-layer organic phase below the fourth tower plate, and horizontally arranging a dispersion disc below the fourth tower plate to ensure that the flowing direction of the entering organic phase is opposite to the upper surface of the dispersion disc; and finally, collecting the uncondensed gas obtained after the temperature of the condenser 5 is reduced through a pipeline connected to the top of the overhead condenser 5 at the top of the desorption tower.
As shown in fig. 1, the desorption column in the steps 1 to 4 includes a cylindrical column body 1, and a reboiler 2 is communicated with the bottom of the column body 1; at least six tower plates are fixed in the tower body 1 from bottom to top, the height between the adjacent tower plates is not less than 330mm, a feed inlet 11 is formed in the middle of the tower body 1, a discharge outlet 12 is formed in the top of the tower body 1, the number of the tower plates above the feed inlet 11 is more than or equal to five, the reboiler 2 is communicated with the tower body 1 below the feed inlet 11 through a pipeline, a liquid phase outlet pipe 41 is arranged above a fourth tower plate 15 from bottom to top, a normally open valve is arranged on the liquid phase outlet pipe 41, and the liquid phase outlet pipe is communicated with a water separator 45; a liquid phase inlet pipe 42 communicated with the water separator 45 is arranged below the fourth tower plate 15, and a normally open valve is also arranged between the liquid phase inlet pipe 42 and the water separator 45; a dispersion plate 14 fixed on the inner wall of the tower body 1 is arranged below the fourth tower plate 15, the top surface of the dispersion plate 14 is an arc-shaped surface, and one end of the liquid phase inlet pipe 42 far away from the water separator 45 is opposite to the arc-shaped surface.
The concrete connection relationship of the analytic tower is as follows: the top of the tower body 1 is connected with a tower top condenser 5 through a pipeline, the refined gas is discharged from a discharge port 12 and enters the tower top condenser 5, part of the gas is condensed into liquid, and the liquid flows back into the tower body 1 again through the pipeline connected with the lower port of the tower top condenser 5. The uncondensed gas is collected by a pipe connected to the top of the condenser 5 and sent to the next step.
The number of the tower plates of the desorption tower adopted in the embodiment is more than five (the partial tower plates below the feed inlet 11 are not shown), wherein the number of the tower plates above the feed inlet 11 is five, the inner wall of the tower body 1 is welded with a tower ring, the tower plates are fixed on the tower ring through bolts, the five tower plates are all welded on the inner wall of the tower body 1, and the height between the adjacent tower plates is 330 mm. From down supreme fourth column plate 15 transversely seals tower body 1 space, and above-mentioned fourth column plate 15 middle part is vertical to be equipped with gas passage 151, and gas passage 151 lower extreme runs through fourth column plate 15 and with fourth column plate 15 weld forming. A plurality of support rods 152 are vertically welded at the upper end of the gas channel 151, and umbrella covers 153 are welded at the tops of the support rods 152; the liquid phase outlet pipe 41 is communicated with the tower body 1 and is lower than the top end of the gas channel 151. The bottom of the water separator 45 is provided with a drain pipe 46, and the drain pipe 46 is provided with a drain valve 47. The side wall of the water separator 45 is clamped and communicated with the interface meter 3, so that the distribution conditions of water and the organic phase in the water separator 45 can be conveniently observed, when the water in the water separator 45 is too little, the drainage valve 47 is timely closed, and the organic phase is prevented from leaking from the drainage pipe 46 to cause loss and pollution.
Reboiler 2 is shell and tube heater, and reboiler 2 includes shell, two heads, two tube sheets and is located a plurality of shell and tube nest 21 of shell, and the head welds both ends about the shell respectively, and two tube sheets transversely weld respectively on the inner wall at both ends about the shell, and both ends weld respectively on two tube sheets about tube nest 21, all are equipped with the through-hole with shell and tube nest 21 intercommunication on two tube sheets. Tube nest 21 forms the tube side with the head, the shell lateral wall is equipped with steam inlet 22 and congeals water outlet 23, steam inlet 22 is located the shell upper end, it is located the shell lower extreme to congeal water outlet 23, steam inlet 22 with congeal water outlet 23 and can communicate with external steam generator and steam collection device respectively through the pipeline, the tube side lower extreme that is located the shell below passes through pipeline and tower body bottom intercommunication, the tube side top that is located the shell top is through another pipeline and tower body 1 intercommunication below the feed inlet.
The absorption liquid in the step 1 enters the tower body 1 from the feed inlet 11 and then flows downwards into the tubes 21 in the reboiler 2, the absorption liquid is heated by steam in the shell of the reboiler 2, a large amount of vinyl acetylene, acetylene and the like in the absorption liquid are evaporated to form gas, and the density of the heated absorption liquid at the tower bottom is continuously reduced, so that a density difference is formed. Due to the density difference caused by heating, the absorption liquid circularly flows at the reboiler 2 and the bottom of the tower, and is uniformly heated. The gas evaporated by heating upwards enters the tower body 1 and is positioned above the feeding hole 11, the channel 151 moves to the upper part of the tower body 1 and is in reverse contact with the liquid condensed and refluxed on the tower top on the tower plate, and the rectification is continuously carried out. The rectified gas mainly contains vinyl acetylene and acetaldehyde, the gas is conveyed to the tower top and discharged from a discharge port 12, enters a tower top condenser 5, part of the gas is condensed by the tower top condenser 5, flows back into the tower body 1 through a pipeline at the lower opening of the condenser 5 as reflux, and flows downwards along the tower plate to perform reverse contact with ascending gas for rectification. Qualified vinyl acetylene gas (containing acetaldehyde) is discharged from a pipeline at the top of the overhead condenser 5 and enters the next working procedure.
Along with the rectification, a rich water liquid is formed on the fourth tower plate 15, and the rich water liquid automatically flows into the water separator 45 through the liquid phase outlet pipe 41 under the action of the potential difference. Because of the density difference, the water and the organic phase are layered, because the density of the water is higher than that of the organic phase, the water is positioned below the organic phase, the water and the organic phase in the water separator 45 are continuously increased along with the refining, and when the liquid level reaches a certain height, the organic phase flows back into the tower body 1 from the liquid phase inlet pipe 42 due to the difference of the phase. The interface condition in the water separator 45 is observed through the interface meter 3, the interface can not be higher than the liquid phase inlet pipe 42, otherwise, water enters the tower again, and the rectification is influenced. When the interface is close to the liquid phase, the liquid phase is discharged into the pipe 42, the water in the lower layer of the water separator 45 needs to be discharged, the water discharge valve 47 is opened, the water in the lower layer is discharged from the water discharge pipe 46, and the water discharge valve 47 is closed after the water is completely discharged.
The organic phase entering the tower body 1 from the liquid phase inlet pipe 42 is downward contacted with the top surface of the dispersion plate 14, flows towards the edge of the dispersion plate 14 along the arc surface under the limiting action of the top surface of the dispersion plate 14, the gas below the dispersion plate 14 flows upward from the gap between the dispersion plate 14 and the tower body 1 and is contacted with the liquid on the dispersion plate 14, and the organic phase is uniformly mixed with the analytic liquid after being dispersed and distributed.
The beneficial effect of adopting above-mentioned analytic tower lies in:
1. when the organic phase flows along the arc surface to the edge of the dispersion plate 14, the flow direction of the organic phase is inclined downward and is in counter contact with the flow direction of the gas flowing upward. And (4) distributing the organic phase after water diversion by using a dispersion disc to promote the organic phase to be uniformly mixed with the analysis liquid.
2. The top surface of dispersing tray 14 is an arc surface, and the organic phase entering from liquid phase inlet pipe 42 contacts dispersing tray 14 without splashing upward and splashes above fifth tower plate 16.
3. The liquid drops flowing down from the upper tower plate fall on the umbrella cover 153, and the liquid which is not divided can not flow to the lower tower plate from the gas channel 151, so that the water dividing effect is ensured, and the refining of the vinyl acetylene is facilitated.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make various changes and modifications without departing from the concept of the present invention, and these should be construed as the scope of protection of the present invention, which will not affect the effect of the implementation of the present invention and the utility of the patent. The techniques, shapes, and structural parts, which are omitted from the description of the present invention, are all known techniques.
Claims (10)
1. A method for refining vinyl acetylene is characterized in that: the method comprises the following steps:
step 1: introducing the absorption liquid obtained by the treatment of the degassing tower into an analytical tower from the middle part of the analytical tower;
step 2: heating the absorption liquid introduced into the desorption tower, cooling the gas at the top of the desorption tower, and condensing and refluxing part of the gas;
and step 3: detecting the temperature of liquid at the fifth tower plate of the desorption tower from the feed inlet from bottom to top, and increasing the condensation reflux at the top of the desorption tower when the temperature is higher than 18-22 ℃ until the temperature is lower than 10-14 ℃;
and 4, step 4: removing water in the liquid above the fourth tower plate from the feeding port from bottom to top, and collecting uncondensed gas at the top of the desorption tower.
2. The vinyl acetylene purification process according to claim 1, characterized in that: and 2, heating at the bottom of the desorption tower.
3. The vinyl acetylene purification process according to claim 2, characterized in that: and step 2, heating by adopting steam.
4. The vinyl acetylene purification process according to claim 2, characterized in that: preheating the absorption liquid obtained from the degassing tower in the step 1 before introducing the absorption liquid into an analytical tower, and introducing the absorption liquid into the analytical tower after the temperature of the absorption liquid is higher than 70-75 ℃.
5. The vinyl acetylene purification process according to claim 1, characterized in that: in the step 4, before removing water from the liquid above the fourth tray, the liquid above the fourth tray is led out of the desorption tower, and the liquid after removing water is led into the desorption tower.
6. The vinyl acetylene purification process according to claim 5, characterized in that: the liquid after water removal is directed below the fourth tray.
7. The vinyl acetylene purification process according to claim 6, characterized in that: a dispersion tray is arranged below the fourth tower plate, and the liquid after water removal is directly guided to the dispersion tray.
8. The vinyl acetylene purification process according to claim 5, characterized in that: and 4, after the liquid above the fourth tower plate is led out, standing until the water and the organic phase are separated, and then removing the water.
9. The vinyl acetylene purification process according to claim 1, characterized in that: and 2, cooling the gas by adopting brine with the temperature lower than the boiling point of the vinyl acetylene.
10. The vinyl acetylene purification process according to claim 9, characterized in that: the temperature of the brine in step 2 is equal to or lower than-15 ℃.
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| CN201910815350.6A CN110483229B (en) | 2019-08-30 | 2019-08-30 | Vinyl acetylene refining method |
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