CN214299942U - Baffle plate rectifying equipment for propynol and butynediol aqueous solution system - Google Patents
Baffle plate rectifying equipment for propynol and butynediol aqueous solution system Download PDFInfo
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Abstract
The utility model relates to a baffle rectification device of a propiolic alcohol and butynediol aqueous solution system, which comprises a baffle rectification tower, a preheater, a reboiler, a condenser, a reflux tank, a reflux pump, a side-collecting pump and a tower bottom pump; the feed inlet of baffle rectifying column is connected with the pre-heater, the liquid phase mouth at the bottom of the tower of baffle rectifying column is connected with the reboiler, the gaseous phase space at the bottom of baffle rectifying column tower is returned to the gaseous phase of evaporation, the liquid phase mouth at the bottom of the tower of baffle rectifying column is connected with the bottom of the tower pump simultaneously, baffle rectifying column top of the tower gaseous phase mouth is connected with the condenser, condenser liquid phase mouth is connected with the reflux drum, reflux drum liquid phase mouth is connected with the backwash pump, simultaneously the reflux pump export is connected to baffle rectifying column top reflux mouth and outward conveying pipeline, the side draw export of baffle rectifying column is connected with the side draw pump. The liquid feeding of the feeding pre-separation section and the liquid extraction of the product extraction section are comprehensively considered, and the liquid phase loads of the feeding pre-separation section and the product extraction section are controlled, so that the gas phase loads of the feeding pre-separation section and the product extraction section are controlled.
Description
Technical Field
The utility model relates to a baffle rectification equipment of propiolic alcohol, butynediol aqueous solution system uses baffle rectification technology and equipment, realizes the separation of propiolic alcohol, butynediol and water, is applied to the rectification separation of propiolic alcohol, butynediol aqueous solution.
Background
Formaldehyde and acetylene are used as raw materials, water is used as a solvent, and under the action of a catalyst, certain temperature and pressure are reached to react to generate propiolic alcohol and butynediol. By controlling the reaction conditions, the ratio of the reaction selectivity between propargyl alcohol and butynediol can be controlled to be 4 to 0.25. The non-condensable gas dissolved in the reaction product is removed by decompression, the solid catalyst is removed by filtration, the remaining main component is about 90 percent of water, and the other components are the mixed product of propiolic alcohol and butynediol.
The conventional separation flow comprises the following steps: firstly separating out the concentrated butynediol water solution, then separating out the concentrated propynediol water solution, and recycling the separated waste water. The process of concentrating butynediol and propargyl alcohol consumes a large amount of heat due to the large enthalpy of water.
On the basis of a conventional separation process, the multi-effect evaporation and multi-effect rectification process is combined, so that the energy consumption can be obviously reduced, but the problems of large initial investment, large occupied area, unstable concentrations and separation effects of a propargyl alcohol aqueous solution and a butynediol aqueous solution, unstable COD value of wastewater and the like still exist.
The following studies have proposed new process schemes:
CN102728090A, Wake-Yong et al, proposes a fractionating apparatus and method for separating propargyl alcohol, which is applied in the field of chemical separation, and comprises a double-wall tower, a rectifying tower stripping section, a rectifying tower rectifying section, a rectifying tower condenser, a vacuum evaporator, a rectifying tower tail cooler, a reflux tank, a heater, a vacuum evaporator cooler, etc. The double-wall tower is composed of a stripping section, the top of the double-wall tower is provided with an alkali liquor feed port, the rectifying tower is composed of a rectifying tower stripping section and a rectifying tower rectifying section, and a mixture feed port and a demister are arranged between the rectifying tower stripping section and the rectifying tower rectifying section. The double-walled tower is coupled with the rectifying tower, the double-walled tower and the rectifying tower are respectively connected with a heater, the rectifying tower is connected with a rectifying tower condenser, the rectifying tower condenser is connected with a rectifying tower tail cooler and a reflux tank, and the reflux tank is connected with the top of the rectifying tower through a first pipeline and is connected with a propiolic alcohol extraction pipeline. The utility model discloses a well material of separating is propiolic alcohol, butynediol aqueous solution simultaneously, though cancelled concentrated process, has realized concentration and propiolic alcohol concentration integration to the flow of using double-walled tower has been proposed for the first time, but the verbose complicacy of this flow, double-walled tower is not equivalent to complete thermal coupling, and the automation degree of difficulty of operation is great, and energy-conserving effect is very limited.
In CN104387236A, Wujia et al propose a method for the triple-production continuous production of propiolic alcohol, 1, 4-butynediol and urotropine, and belong to the technical field of chemical industry. The utility model discloses use formalin (10% -37% wt) and acetylene to synthesize propiolic alcohol as the raw materials, coproduction 1, 4-butynediol and urotropine, reaction temperature is 80-120 ℃, and pressure is 1.0-2.5Mpa, can obtain propiolic alcohol, butynediol aqueous solution and urotropine aqueous solution that the purity is more than 99.5%, and the conversion rate of whole technology formaldehyde can reach 100%, has the advantage of safety ring protects. The process for separating the reaction product is not described in depth in the patent, the separation process is more conventional, but the propargyl alcohol is further concentrated in a rectification mode after the butynediol is concentrated in an evaporation mode, and no technical innovation for saving energy and investment is provided.
Disclosure of Invention
The utility model aims at providing a baffle rectification equipment is applied to the rectification separation of propiolic alcohol, butynediol aqueous solution. The utility model provides an equipment has both cancelled concentrated process, has integrated the concentration of butynediol and propiolic alcohol concentration, again based on the principle of baffle rectification, realizes complete thermal coupling through single baffle rectifying column, has shortened the flow, has simplified equipment, has saved the investment, has practiced thrift the energy consumption, reduces investment cost and running cost to the ideal scope simultaneously, can also guarantee complete automation mechanized operation.
The technical scheme of the utility model as follows:
a baffle plate rectifying device of a propiolic alcohol and butynediol aqueous solution system comprises a baffle plate rectifying tower, a preheater, a reboiler, a condenser, a reflux tank, a reflux pump, a side extraction pump and a tower bottom pump; the feed inlet of baffle rectifying column is connected with the pre-heater, the liquid phase mouth at the bottom of the tower of baffle rectifying column is connected with the reboiler, the gaseous phase space at the bottom of baffle rectifying column tower is returned to the gaseous phase of evaporation, the liquid phase mouth at the bottom of the tower of baffle rectifying column is connected with the bottom of the tower pump simultaneously, baffle rectifying column top of the tower gaseous phase mouth is connected with the condenser, condenser liquid phase mouth is connected with the reflux drum, reflux drum liquid phase mouth is connected with the backwash pump, simultaneously the reflux pump export is connected to baffle rectifying column top reflux mouth and outward conveying pipeline, the side draw export of baffle rectifying column is connected with the side draw pump.
The baffle plate rectifying tower is a baffle plate tower, a vertical baffle plate is arranged in the tower, the tower body is divided into a public rectifying section, a public stripping section, a feeding pre-separation section and a product extraction section, and a filler or a tower plate is arranged in the tower.
The utility model discloses a propiolic alcohol, baffle rectification technology of butynediol aqueous solution system, the raw materials that comes from the reaction unit is after desorption gaseous phase and solid phase, propiolic alcohol, water, the mixed material of butynediol gets into the baffle rectifying column through the preheater, set up a reboiler that uses the heat medium at the bottom of the tower, gaseous phase after the reboiler vaporization gets into the condenser from the top of the tower, the material condenses to get into the reflux drum behind the liquid phase, the tail gas discharge to the tail gas system of reflux drum, the liquid phase material of reflux drum is after the backwash pump pressure boost, the part is extracted as propiolic alcohol solution product, the part is carried to the top of the tower and is refluxed; the side-mining material of the clapboard rectifying tower is pressurized by a side-mining pump and is discharged after exchanging heat with the feeding material; and (3) boosting the butynediol solution at the bottom of the tower by a tower bottom pump, and then extracting.
The feeding flow rate of the mixed material is 2-40 t/h, wherein the water content is 70-95%, the propiolic alcohol content is 1-15%, the feeding temperature is 20-60 ℃, and the feeding pressure is 0-1.0 Mpag.
The operation pressure of the clapboard rectifying tower is-0.09 Mpag to 0.2Mpag, the temperature of the top of the tower is 25 ℃ to 140 ℃, and the temperature of the bottom of the tower is 35 ℃ to 150 ℃.
After rectification and separation, the concentration of the propargyl alcohol extracted from the top of the tower is 10-50%, the concentration of the butynediol extracted from the bottom of the tower is 10-80%, the content of the propargyl alcohol in the industrial water extracted from the side line is 0-1%, and the content of the butynediol is 0-1%.
The reboiler adopts steam or conduction oil as a heat source, and the condenser adopts circulating water or 7-degree water as a cold source.
The utility model is applied to the equipment for rectifying and separating the water solution of propiolic alcohol and butynediol, the feed inlet of the clapboard rectifying tower is connected with the preheater, and the heat exchange between the feed and the side-draw material can be realized; the tower bottom liquid phase port of the clapboard rectifying tower is connected with the reboiler, so that the tower bottom liquid phase can be continuously vaporized through the reboiler, and the vaporized gas phase returns to the tower bottom gas phase space of the clapboard rectifying tower; the tower bottom liquid phase port of the clapboard rectifying tower is simultaneously connected with the tower bottom pump, so that the tower bottom materials can be conveyed outwards after being pressurized by the tower bottom pump; the gas phase port at the top of the separation plate rectifying tower is connected with a condenser, and the liquid phase port of the condenser is connected with a reflux tank, so that the gas phase at the top of the tower can be condensed into a liquid phase by the condenser and then automatically flows into the reflux tank; the liquid phase port of the reflux tank is connected with a reflux pump, and the outlet of the reflux pump is connected with the reflux port at the top of the clapboard rectifying tower and an outward delivery pipeline, so that the pump reflux and pump extraction of condensed materials can be realized; the side-draw outlet of the clapboard rectifying tower is connected with a side-draw pump, so that the pressurized delivery of side-draw materials can be realized.
Adopt the utility model discloses a propiolic alcohol, baffle rectification technology and equipment of butynediol aqueous solution system, use baffle rectification technology and equipment, baffle upper portion sets up liquid collector, the liquid that will publicly rectify the section decline is collected the back, through outside governing valve group control feeding preseparation section liquid feed volume, through liquid collector overflow control product extraction section liquid feed volume, the liquid extraction of the liquid feeding of the preseparation section of giving comprehensive consideration to the feeding and product extraction section, the liquid phase load of control feeding preseparation section and product extraction section, thereby the gas phase load of control feeding preseparation section and product extraction section. The separation of the propiolic alcohol, the butynediol and the water is realized, and the material loss is less; compared with the conventional process, the method saves the energy consumption by 20-30%. Less equipment and investment.
Drawings
FIG. 1 is a schematic diagram of a baffle distillation device of a propynol and butynediol aqueous solution system.
Detailed Description
Device connections are shown in fig. 1: the device is formed by connecting a clapboard rectifying tower (1), a preheater (2), a reboiler (3), a condenser (4), a reflux tank (5), a reflux pump (6), a side-extracting pump (7) and a tower bottom pump (8). The feed inlet of the clapboard rectifying tower (1) is connected with the preheater (2), so that the heat exchange between the feed and the side-draw material can be realized; the tower bottom liquid phase port of the clapboard rectifying tower (1) is connected with the reboiler (3), so that the tower bottom liquid phase is continuously vaporized by the reboiler (3), and the vaporized gas phase returns to the tower bottom gas phase space of the clapboard rectifying tower (1); the tower bottom liquid phase port of the clapboard rectifying tower (1) is simultaneously connected with the tower bottom pump (8), so that the tower bottom materials can be conveyed outwards after being pressurized by the tower bottom pump (8); a gas phase port at the top of the partition plate rectifying tower (1) is connected with a condenser (4), a liquid phase port of the condenser (4) is connected with a reflux tank (5), so that the gas phase at the top of the tower can be condensed into a liquid phase by the condenser (4) and then automatically flows into the reflux tank (5); a liquid phase port of the reflux tank (5) is connected with a reflux pump (6), and an outlet of the reflux pump (6) is connected to a reflux port at the top of the clapboard rectifying tower (1) and an outward delivery pipeline, so that pump reflux and pump extraction of condensed materials can be realized; the side-draw outlet of the clapboard rectifying tower (1) is connected with a side-draw pump (7), so that the pressurized delivery of side-draw materials can be realized.
The feeding flow rate of the reaction product is 2-40 t/h, wherein the water content is 70-95%, the propiolic alcohol content is 1-15%, the feeding temperature is 20-60 ℃, and the feeding pressure is 0-1.0 Mpag.
The baffle plate rectifying tower (2) is a baffle plate tower, a vertical baffle plate is arranged in the tower, the tower body is divided into a public rectifying section, a public stripping section, a feeding pre-separation section and a product extraction section, packing or tower plates are arranged in the tower, a propargyl alcohol solution is extracted from the top of the tower, a butynediol solution is extracted from the bottom of the tower, and industrial water is extracted from the lateral line. The operating pressure of the clapboard rectifying tower (2) is-0.09-0.2 Mpag, the temperature at the top of the tower is 25-140 ℃, the temperature at the bottom of the tower is 35-150 ℃, under the operating condition, steam or heat conducting oil is adopted as a heat source in the reboiler (3), and circulating water or 7-degree water is adopted as a cold source in the condenser (4).
After rectification separation, the concentration of the propargyl alcohol extracted from the top of the tower is 10-50%, the concentration of the butynediol extracted from the bottom of the tower is 10-80%, the content of the propargyl alcohol in the industrial water extracted from the side line is 0-1%, and the content of the butynediol is 0-1%.
Specific application examples are as follows:
example 1:
the feeding flow is 2t/h, the selectivity proportion of the reaction of the propiolic alcohol and the butynediol is 0.99, the water content is 89.3 percent, the feeding temperature is 35 ℃, and the pressure of the fed material reaches 0.2Mpag after the pressure of the fed material is increased by a pump.
2t/h of feed is heated to 50 ℃ after passing through a preheater (2) and is sent to the middle part of a clapboard rectifying tower (1), 6 m-mesh corrugated structured packing is filled at the upper part in the tower to be used as a public rectifying section, 5 layers of sieve plate tower trays are installed at the lower part to be used as a public stripping section, the middle part is divided by a clapboard with the height of 13.5m, 10 m-mesh corrugated structured packing is filled at the feed side for feed pre-separation, and 8 m-mesh corrugated structured packing is filled at the extraction side for product purification side extraction. The diameter of the clapboard rectifying tower (1) is 1000 mm. The operating pressure was controlled at-0.03 Mpag, the overhead temperature was 82.8 ℃ and the bottoms temperature was 92.3 ℃.
The gas phase at the top of the tower enters a condenser (4), circulating water is used as a cold source, the gas phase at the top of the tower is condensed into liquid and then enters a reflux tank (5), after the liquid is pressurized by a reflux pump (6), part of reflux is extracted, and the reflux quantity is stabilized at 2.5 t/h.
The reboiler (3) is heated by 0.2Mpag saturated steam, and the average steam addition amount is 2.2t/h in normal operation.
The extraction amount at the top of the tower is 840kg/h, wherein the content of the propiolic alcohol is 10 percent; the side line extraction amount is 948.62kg/h, and the side line extraction amount is cooled to 45 ℃ after heat exchange by the preheater (2), wherein the water content is 100%; the bottom yield was 211.38kg/h, with a butynediol content of 61.5%.
Example 2:
the feed flow is 4t/h, the selectivity ratio of the reaction of the propiolic alcohol and the butynediol is 0.67, the water content is 90.46 percent, the feed temperature is 35 ℃, and the pressure of the feed reaches 0.2Mpag after the feed is pumped and pressurized.
4t/h of feed is heated to 50 ℃ after passing through a preheater (2) and is sent into the middle part of a clapboard rectifying tower (1), 6 m-mesh corrugated structured packing is filled at the upper part in the tower to be used as a public rectifying section, 5 layers of sieve plate tower trays are installed at the lower part to be used as a public stripping section, the middle part is divided by a clapboard with the height of 13.5m, 10 m-mesh corrugated structured packing is filled at the feeding side for feeding pre-separation, and 8 m-mesh corrugated structured packing is filled at the extraction side for product purification side extraction. The diameter of the baffle rectifying tower (1) is 1400 mm. The operating pressure was controlled at-0.03 Mpag, the overhead temperature was 82.8 ℃ and the bottoms temperature was 92.3 ℃.
The gas phase at the top of the tower enters a condenser (4), circulating water is used as a cold source, the gas phase at the top of the tower is condensed into liquid and then enters a reflux tank (5), after the liquid is pressurized by a reflux pump (6), part of reflux is extracted, and the reflux amount is stabilized at 4.9 t/h.
The reboiler (3) is heated by 0.2Mpag saturated steam, and the average steam addition amount is 4.3t/h in normal operation.
The overhead output is 302.87kg/h, wherein the content of the propiolic alcohol is 38.3 percent; the side line extraction amount is 3265.26kg/h, and the side line extraction amount is cooled to 45 ℃ after heat exchange by the preheater (2), wherein the water content is 100%; the bottom yield was 431.87kg/h, with a butynediol content of 61.5%.
Example 3:
the feed flow is 6t/h, the selectivity ratio of the reaction of the propiolic alcohol and the butynediol is 1.54, the water content is 70 percent, the feed temperature is 20 ℃, and the pressure of the feed reaches 1.0Mpag after the feed is pumped and pressurized.
Feeding at a rate of 6t/h, heating to 42 ℃ after passing through a preheater (2), feeding into the middle part of a clapboard rectifying tower (1), filling 8m of scattered pall ring packing in the upper part of the tower as a common rectifying section, filling 2m of scattered pall ring packing in the lower part of the tower as a common stripping section, dividing the middle part by a clapboard with the height of 15m, filling 12m of scattered pall ring packing in a feeding side for feeding pre-separation, and filling 10m of scattered pall ring packing in a sampling side for product purification side mining. The diameter of the baffle plate rectifying tower (1) is 1600 mm. The operating pressure was controlled at 0.2Mpag, the head temperature was 140 ℃ and the bottom temperature was 150 ℃.
The gas phase at the top of the tower enters a condenser (4), circulating water is used as a cold source, the gas phase at the top of the tower is condensed into liquid and then enters a reflux tank (5), after the liquid is pressurized by a reflux pump (6), part of reflux is extracted, and the reflux amount is stabilized at 7.5 t/h.
The reboiler (3) is heated by 0.5Mpag saturated steam, and the average steam addition amount is 6.5t/h in normal operation.
The extraction amount at the top of the tower is 1800kg/h, wherein the content of the propiolic alcohol is 50 percent; the side extraction amount is 3075kg/h, and the mixture is cooled to 45 ℃ after heat exchange by the preheater (2), wherein the content of the propiolic alcohol is 0.02 percent, and the content of the water is 99.98 percent; the bottom yield is 1125kg/h, wherein the butynediol content is 80%.
Example 4:
the feed flow was 13.5t/h, the selectivity ratio of the reaction of propargyl alcohol with butynediol was 0.5, the water content therein was 90.59%, the feed temperature was 50 ℃ and the pressure of the feed after pumping was 0.1 Mpag.
13.5t/h of feed is heated to 62 ℃ after passing through a preheater (2) and then is sent to the middle part of a clapboard rectifying tower (1), 36 layers of floating valve trays are installed at the upper part in the tower to be used as a public rectifying section, 5 layers of sieve tray trays are installed at the lower part in the tower to be used as a public stripping section, the middle part is divided by a clapboard with the height of 30m, 60 layers of floating valve trays are installed at the feed side for feed pre-separation, and 56 layers of floating valve trays are installed at the extraction side for product purification side extraction. The diameter of the baffle plate rectifying tower (1) is 2800 mm. The operating pressure was controlled at-0.06 Mpag, the overhead temperature was 66.7 ℃ and the bottoms temperature was 78.3 ℃.
The gas phase at the top of the tower enters a condenser (4), water with the temperature of 7 ℃ is used as a cold source, the gas phase at the top of the tower is condensed into liquid and then enters a reflux tank (5), after the liquid is pressurized by a reflux pump (6), part of reflux is extracted, and the reflux quantity is stabilized at 16.9 t/h.
The reboiler (3) adopts low temperature conduction oil for heating, and the average heating power is 8540kw during normal operation.
The overhead output is 840.57kg/h, wherein the content of the propiolic alcohol is 37.1 percent; the side extraction amount is 10944.76kg/h, and the side extraction amount is cooled to 55 ℃ after heat exchange by the preheater (2), wherein the water content is 99.99 percent, and the butynediol content is 0.01 percent; the bottom yield is 1714.67kg/h, wherein the butynediol content is 55.9%.
Example 5:
the feed flow is 40t/h, the selectivity ratio of the reaction of the propiolic alcohol and the butynediol is 0.38, the water content is 95 percent, the feed temperature is 60 ℃, and the pressure of the feed reaches 0Mpag after the feed is pumped and pressurized.
40t/h of feed is heated to 72 ℃ after passing through a preheater (2) and then is sent to the middle part of a clapboard rectifying tower (1), 36 layers of floating valve trays are installed at the upper part in the tower to be used as a public rectifying section, 5 layers of sieve plate trays are installed at the lower part in the tower to be used as a public stripping section, the middle part is divided by a clapboard with the height of 30m, 60 layers of floating valve trays are installed at the feed side for feed pre-separation, and 56 layers of floating valve trays are installed at the extraction side for product purification side extraction. The diameter of the clapboard rectifying tower (1) is 4800 mm. The operating pressure was controlled at-0.09 Mpag, the overhead temperature was 25 ℃ and the bottoms temperature was 35 ℃.
The gas phase at the top of the tower enters a condenser (4), water with the temperature of 7 ℃ is used as a cold source, the gas phase at the top of the tower is condensed into liquid and then enters a reflux tank (5), after the liquid is pressurized by a reflux pump (6), part of reflux is extracted, and the reflux quantity is stabilized at 50.1 t/h.
The reboiler (3) adopts low temperature conduction oil for heating, and the average heating power is 25304kw during normal operation.
The overhead output is 1078.17kg/h, wherein the content of the propiolic alcohol is 37.1 percent; the side extraction amount is 22921.83kg/h, and the side extraction amount is cooled to 55 ℃ after heat exchange by the preheater (2), wherein the water content is 99.99 percent, and the butynediol content is 0.01 percent; the bottom yield is 16000kg/h, wherein the butynediol content is 10 percent.
The utility model provides a mixed alcohol aqueous solution system's baffle rectification equipment has been described through the embodiment, and relevant technical personnel obviously can not deviate from the utility model discloses a content, spirit and within range change or suitable change and combination to the equipment herein, realize the technique of the utility model. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (2)
1. A baffle plate rectifying device of a propynol and butynediol aqueous solution system is characterized by comprising a baffle plate rectifying tower, a preheater, a reboiler, a condenser, a reflux tank, a reflux pump, a side-collecting pump and a tower bottom pump; the feed inlet of baffle rectifying column is connected with the pre-heater, the liquid phase mouth at the bottom of the tower of baffle rectifying column is connected with the reboiler, the gaseous phase space at the bottom of baffle rectifying column tower is returned to the gaseous phase of evaporation, the liquid phase mouth at the bottom of the tower of baffle rectifying column is connected with the bottom of the tower pump simultaneously, baffle rectifying column top of the tower gaseous phase mouth is connected with the condenser, condenser liquid phase mouth is connected with the reflux drum, reflux drum liquid phase mouth is connected with the backwash pump, simultaneously the reflux pump export is connected to baffle rectifying column top reflux mouth and outward conveying pipeline, the side draw export of baffle rectifying column is connected with the side draw pump.
2. The apparatus as claimed in claim 1, wherein the dividing plate rectifying column is a dividing plate column, a vertical dividing plate is arranged in the column to divide the column body into a common rectifying section, a common stripping section, a feed pre-separating section and a product extracting section, and packing or column plates are arranged in the column.
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