CN217828930U - Crude monomer rectification energy-saving device - Google Patents
Crude monomer rectification energy-saving device Download PDFInfo
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- CN217828930U CN217828930U CN202221714362.3U CN202221714362U CN217828930U CN 217828930 U CN217828930 U CN 217828930U CN 202221714362 U CN202221714362 U CN 202221714362U CN 217828930 U CN217828930 U CN 217828930U
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Abstract
The utility model relates to a crude monomer rectifying device, crude monomer enters a rectifying tower I, high boiling gas phase material removed from the top of the rectifying tower I firstly enters a rectifying tower four-tower kettle reboiler as a heat source, residual gas phase material enters a rectifying tower three-tower kettle reboiler as a heat source, the residual gas phase material is condensed by the reboiler and then is fed as a rectifying tower two, and crude high boiling is extracted from tower kettles; a methyl trichlorosilane product is extracted from the top of the rectifying tower III; all gas phase materials at the top of the tower enter a reboiler at a second tower kettle of the rectifying tower to be used as a heat source, and a part of the gas phase materials is condensed by the reboiler to be used as tower reflux to return to the top of a third tower of the rectifying tower; the tower bottom is taken as the feed of a third rectifying tower and a fourth rectifying tower. The gas phase material at the top of the first tower of the rectifying tower is preferentially used as a heat source of a reboiler at the four towers of the rectifying tower, the rest is used as a heat source of a reboiler at the three towers of the rectifying tower, and then the gas phase material at the top of the three towers of the rectifying tower is completely used as a heat source of a reboiler at the two towers of the rectifying tower, so that the steam consumption is reduced by at least 30% and the circulating water consumption is reduced by 30% in a same ratio.
Description
Technical Field
The utility model relates to a thick monomer rectification economizer belongs to organosilicon production technical field.
Background
The methyl chlorosilane mixed monomer comprises dimethyl dichlorosilane (dimethyl for short), methyl trichlorosilane (methyl for short), trimethyl monochlorosilane (trimethyl for short), methyl dichlorosilane (methyl for short contains hydrogen), high boiling point substances and low boiling point substances. As is well known, the synthesis of methyl chlorosilane monomers at home and abroad generally adopts a direct method synthesis process, silicon powder and chloromethane are used as raw materials, a methyl chlorosilane mixed monomer is directly synthesized under the action of a copper catalyst system, the methyl chlorosilane mixed monomer is rectified and separated to obtain a main target product dimethyl, and byproducts, namely methyl, methyl contain hydrogen, trimethyl, high-boiling residues and low-boiling residues. Dimethyl is hydrolyzed and cracked to produce various organosilicon intermediates, namely oligomeric methyl siloxane or alkoxy silane, and the oligomeric methyl siloxane or alkoxy silane is further processed into various organosilicon downstream products.
The purity requirement of dimethyl as a raw material is quite high when silicone oil and silicone rubber are prepared, and particularly, the purity of the dimethyl as a key raw material is required to reach more than 99.95 percent when high-temperature vulcanized silicone rubber is prepared. However, the crude monomer components are complex, the boiling point difference is small, and the dimethyl product rectified by the domestic organic silicon manufacturers at present has low purity and large energy consumption compared with the foreign advanced level, so that the market competitiveness of the product is low. The energy consumption for separating the methyl chlorosilane mixed monomer accounts for more than 80 percent of the whole organic silicon device, so that the related technical research on the separation and purification process of the methyl chlorosilane mixed monomer is necessary, and the energy consumption is reduced as much as possible under the condition of ensuring the product quality.
At present, the domestic technology mainly provides variable-pressure thermal coupling rectification of an upper tower and a lower tower, double-effect rectification thermal coupling of a binary tower in parallel connection, and variable-pressure thermal coupling rectification of the upper tower and the binary tower, the utilization rate of the thermal coupling is not high, the comprehensive consideration of the thermal coupling for a three-tower system of the upper tower, the lower tower and the binary tower is not involved, and the energy consumption is still high.
Disclosure of Invention
The utility model provides a thick monomer rectification economizer solves prior art and hardly carries, overcomes the great, higher problem of energy consumption of steam and circulating water quantity in the monomer separation.
The technical terms used in the utility model explain:
coarse high-boiling residues: a component having a boiling point of greater than 70.2 ℃ at atmospheric pressure.
Low-boiling-point substances: components with boiling point less than 40.4 ℃ under normal pressure.
Crude monomer: the methyl chlorosilane mixed monomer comprises, by mass, 6-9% of monomethyl trichlorosilane, 82-87% of dimethyl dichlorosilane, 2.8-3.7% of trimethyl monochlorosilane, 1.3-2% of monomethyl dichlorosilane and 0.05-1% of silicon tetrachloride, and also comprises other mixtures which are difficult to detect.
The utility model discloses technical scheme as follows:
a crude monomer rectification energy-saving device is characterized in that a crude monomer feeding pipe is connected with a first rectification tower;
the top of the rectifying tower is respectively connected with a rectifying tower four-tower kettle reboiler arranged at the four bottoms of the rectifying tower and a rectifying tower three-tower kettle reboiler arranged at the three bottoms of the rectifying tower through a gas phase pipeline;
a rectifying tower three-tower kettle reboiler and a rectifying tower four-tower kettle reboiler are converged through a gas phase pipeline and then connected with a rectifying tower two;
the bottom of the second rectifying tower is respectively connected with a third rectifying tower and a fourth rectifying tower through liquid phase pipelines.
The gas phase pipelines of the rectifying tower three-tower kettle reboiler and the rectifying tower four-tower kettle reboiler are respectively provided with a rectifying tower three-coupling reflux pump and a rectifying tower four-coupling reflux pump before being converged.
The bottom of the second rectifying tower is also provided with a reboiler of the second rectifying tower kettle, and the top of the third rectifying tower is connected with the reboiler of the second rectifying tower kettle arranged at the bottom of the second rectifying tower through a gas phase pipeline.
One path of the reboiler at the second tower kettle of the rectifying tower is connected with the third rectifying tower through a reflux pump of the third rectifying tower, and the other path is connected with the first discharge pipe (namely a methyl trichlorosilane product discharge pipe).
The top of the second rectifying tower is connected with a second condenser of the rectifying tower, the second condenser of the rectifying tower is connected with a second reflux tank of the rectifying tower, the second reflux tank of the rectifying tower is connected with the second rectifying tower through one path of a second reflux pump of the rectifying tower, and the other path of the second reflux tank is connected with a third discharge pipe (namely a discharge pipe of a component with a lower boiling point than the monomethyl trichlorosilane).
And the bottom of the rectifying tower III is also provided with a rectifying tower III steam reboiler, and the bottom of the rectifying tower III is connected to a discharging pipe II (namely a dimethyl dichlorosilane discharging pipe).
The top of the rectifying tower IV is connected with a rectifying tower IV condenser, the rectifying tower IV condenser is connected with a rectifying tower IV reflux groove, the rectifying tower IV reflux groove is connected with the rectifying tower IV through a rectifying tower IV reflux pump, and one way is connected with a discharging pipe IV (namely a methyl trichlorosilane discharging pipe).
The four bottoms of the rectifying tower are connected to a fifth discharge pipe (namely a dimethyldichlorosilane discharge pipe).
The rectifying tower four-tower kettle reboiler is connected with the upper part of the rectifying tower I through a rectifying tower four-coupling reflux pump, and the rectifying tower three-tower kettle reboiler is also connected with the upper part of the rectifying tower I through a rectifying tower three-coupling reflux pump.
One bottom of the rectifying tower is connected to the coarse high-boiling-point substance discharging pipe.
The device of the utility model is simple in structure, control condition rigorous, have good application prospect and using value, compare its good effect with prior art and lie in: in the conventional process, the reboilers of the rectifying tower I, the rectifying tower II, the rectifying tower III and the rectifying tower IV are heated by adopting steam, and the tower top is condensed by adopting circulating water.
Adopt the utility model discloses an among the technology that the device went on, make full use of material component and characteristic adopt the triple effect rectification technology, be rectifying column three with rectifying column four with the three split of rectifying column among the conventional technology, once the split can apply to rectifying column two with the unnecessary heat of rectifying column one, the maximize utilizes the system heat.
Simultaneously, the first rectifying tower and the third rectifying tower are pressurized to operate, so that the temperature of the top of the first rectifying tower and the temperature of the third rectifying tower are increased; because heat transfer basic conditions need to be met, the temperature of the gas phase at the top of the first rectifying tower is higher than the temperature of the kettles of the third rectifying tower and the fourth rectifying tower, and the temperature of the gas phase at the top of the third rectifying tower is higher than the temperature of the kettle of the second rectifying tower, so that the first rectifying tower and the third rectifying tower need to be pressurized, and the temperature of the tops of the first rectifying tower and the third rectifying tower is increased.
Because the third rectifying tower is provided with a steam reboiler used as heat compensation of an external system, firstly, the gas phase material at the top of the first rectifying tower is preferentially used as a heat source of the thermally coupled reboiler at the four towers of the first rectifying tower, the rest is used as a heat source of the reboiler at the three towers of the third rectifying tower, and then, all the gas phase material at the top of the third rectifying tower is used as a heat source of the reboiler at the bottom of the second rectifying tower, so that the latent heat of the gas phase steam material at the top of the first rectifying tower and the top of the third rectifying tower is reasonably utilized, the system heat can be utilized to the maximum, the steam consumption of the second rectifying tower, the third rectifying tower and the fourth rectifying tower is reduced, the circulating water consumption of the first rectifying tower and the third rectifying tower is reduced, and the steam consumption is reduced by at least 30% and the circulating water consumption is reduced by 30% in the same ratio.
Drawings
FIG. 1 is a structural diagram of a crude monomer rectification energy-saving device of the utility model, wherein 1 is a first rectification tower; 2, a second rectifying tower; 3, a third rectifying tower; 4, a rectifying tower IV; 5, a reboiler of the rectifying tower; 6, a reboiler of a rectifying tower and a three-tower kettle; 7, a rectifying tower triple steam reboiler; 8, a reboiler at a second tower kettle of the rectifying tower; 9, a second rectifying tower condenser; 10, a rectifying tower four-tower kettle reboiler; 11, a rectifying tower four condenser; 12, a rectifying tower is coupled with a reflux pump; 13 a rectifying tower three reflux pump; 14, a second kettle liquid pump of the rectifying tower; 15 a second reflux pump of the rectifying tower; 16, coupling a reflux pump with a rectifying tower IV; 17 a rectifying tower four reflux pump; 18 a second reflux groove of the rectifying tower; 19 a rectifying tower four reflux groove; 20 a crude monomer feed pipe; 21 a coarse high-boiling-point substance discharge pipe; 22, discharging a pipe I; 23 discharging a pipe II; a third discharge pipe 24; 25, a fourth methyl trichlorosilane discharge pipe; and 26, discharging a pipe V.
FIG. 2 is a structural diagram of a crude monomer rectification device in the conventional process, wherein 1' a first rectification tower; 2' rectifying tower II; a 3' rectifying tower III; 4' rectifying tower-steam reboiler; a second steam reboiler of the 5' rectifying tower; 6' rectifying tower triple steam reboiler; 7' a rectifying tower-condenser; 8' second condenser of rectifying tower; 9' rectifying tower III condenser; 10' a reflux groove of the rectifying tower; 11' a second reflux groove of the rectifying tower; 12' rectifying tower three reflux tanks; 13' a reflux pump of the rectifying tower; 14' a second reflux pump of the rectifying tower; 15' three feed pumps of the rectifying tower; 16' rectifying tower three reflux pumps; 17' crude monomer feed; 18' coarse high-boiling residue discharge pipe; 19' discharging pipe I; 20' discharging pipe II; 21' discharge pipe III; 22' dimethyl dichlorosilane discharging pipe; 23' a methyltrichlorosilane discharge pipe.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and examples, but the following examples are only preferred embodiments of the present invention, and not all of them. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative work belong to the protection scope of the present invention.
Example 1
A crude monomer rectification energy-saving device is characterized in that a crude monomer feeding pipe is connected with a rectification tower I1;
the top of the rectifying tower I1 is respectively connected with a rectifying tower four-tower kettle reboiler 10 arranged at the bottom of the rectifying tower four 4 and a rectifying tower three-tower kettle reboiler 6 arranged at the bottom of the rectifying tower three 3 through a gas phase pipeline;
a rectifying tower three-tower kettle reboiler 6 and a rectifying tower four-tower kettle reboiler 10 are converged through a gas phase pipeline and then are connected with a rectifying tower two 2;
the bottom of the second rectifying tower 2 is respectively connected with a third rectifying tower 3 and a fourth rectifying tower 4 through liquid phase pipelines.
The gas phase pipelines of the rectifying tower three-tower kettle reboiler 6 and the rectifying tower four-tower kettle reboiler 10 are respectively provided with a rectifying tower three-coupling reflux pump 12 and a rectifying tower four-coupling reflux pump 16 before being converged.
The bottom of the second rectifying tower 2 is also provided with a second rectifying tower kettle reboiler 8, and the top of the third rectifying tower 3 is connected with the second rectifying tower kettle reboiler 8 arranged at the bottom of the second rectifying tower 2 through a gas phase pipeline.
One path of the reboiler 8 of the second tower kettle of the rectifying tower is connected with a third rectifying tower 3 through a third reflux pump 13 of the rectifying tower, and the other path is connected with a first discharging pipe 22.
The top of the second rectifying tower 2 is connected with a second rectifying tower condenser 9, the second rectifying tower condenser 9 is connected with a second rectifying tower reflux groove 18, one path of the second rectifying tower reflux groove 18 is connected with the second rectifying tower 2 through a second rectifying tower reflux pump 15, and the other path is connected with a third discharge pipe 24.
The bottom of the rectifying tower III 3 is also provided with a rectifying tower III steam reboiler 7, and the bottom of the rectifying tower III 3 is connected to the discharging pipe II 23.
The top of the rectifying tower IV 4 is connected with a rectifying tower IV condenser 11, the rectifying tower IV condenser 11 is connected with a rectifying tower IV reflux groove 19, the rectifying tower IV reflux groove 19 is connected with the rectifying tower IV 4 through one path of a rectifying tower IV reflux pump 17, and the other path is connected with a discharge pipe IV 25.
The bottom of the rectifying tower four 4 is connected to a discharge pipe five 26.
The rectifying tower four-tower kettle reboiler 10 is connected with the upper part of the rectifying tower I1 through a rectifying tower four-coupling reflux pump 16, and the rectifying tower three-tower kettle reboiler 6 is further connected with the upper part of the rectifying tower I1 through a rectifying tower three-coupling reflux pump 12.
The bottom of the rectifying tower I1 is connected to a crude high-boiling residue discharge pipe 21.
Example 2
The equipment connection structure of the conventional process is as follows:
the lower part of the first rectifying tower 1 'is provided with a first rectifying tower steam reboiler 4', the top of the first rectifying tower 1 'is connected with a first rectifying tower condenser 7', the top of the first rectifying tower condenser 7 'is connected with a first rectifying tower reflux groove 10' through a gas phase pipeline, the first rectifying tower reflux groove 10 'is connected with a rectifying tower reflux pump 13', one path of the rectifying tower reflux pump 13 'is connected to the upper part of the first rectifying tower 1', the other path of the rectifying tower reflux pump is connected with a second rectifying tower 2 'through a first discharging pipe 19', and the first rectifying tower 1 'kettle is connected with a coarse high-boiling substance discharging pipe 18';
the lower part of the second rectifying tower 2' is provided with a second rectifying tower steam reboiler 5', the top of the second rectifying tower 2' is connected with a second rectifying tower condenser 8', the top of the first rectifying tower condenser 8' is connected with a second rectifying tower reflux groove 11' through a gas phase pipeline, the second rectifying tower reflux groove 11' is connected with a second rectifying tower reflux pump 14', one path of the second rectifying tower reflux pump 14' is connected to the upper part of the second rectifying tower 2', and the other path of the second rectifying tower reflux pump is connected to a third discharging pipe 21';
the bottom of the second rectifying tower is connected with the middle of a third rectifying tower 3 'through a second discharging pipe 20', the lower part of the third rectifying tower 3 'is provided with a third rectifying tower steam reboiler 6', the top of the third rectifying tower 3 'is connected with a third rectifying tower condenser 9' through a gas phase pipeline, the third rectifying tower condenser 9 'is connected with a third rectifying tower reflux groove 12', one path of the third rectifying tower reflux groove 12 'is connected to the upper part of the third rectifying tower 3' through a third rectifying tower reflux pump 16', one path of the third rectifying tower reflux groove is connected to a methyltrichlorosilane discharging pipe 23', and the bottom of the third rectifying tower 3 'is connected to a dimethyldichlorosilane discharging pipe 22'.
Example 3
The energy-saving process for rectifying the crude monomer, which is performed by adopting the embodiment 1, is as follows:
the crude organosilicon monomer is a mixture consisting of methyl chlorosilane, and comprises the main components and the mass fractions of monomethyl trichlorosilane (6-9%), dimethyl dichlorosilane (82-87%), trimethyl monochlorosilane (2.8-3.7%), methyl dichlorosilane (1.3-2%) and silicon tetrachloride (0.05-1%).
(1) The method comprises the following steps of (1) enabling an organic silicon crude monomer to enter a rectifying tower I1 at a flow rate of 25.5t/h, enabling a high-boiling gas-phase material removed from the top of the rectifying tower I1 to firstly enter a rectifying tower IV reboiler 10 as a heat source of a rectifying tower IV with a volume fraction of 35% as a priority, enabling a remaining 65% of gas-phase material to enter a rectifying tower IV reboiler 6 as a heat source, condensing by the reboiler, converging the 85% of gas-phase material with the volume fraction through a rectifying tower III-coupled reflux pump 14 and a rectifying tower IV-coupled reflux pump 16 respectively, enabling the 85% of gas-phase material with the volume fraction to return to the top of the rectifying tower I1 as tower reflux, enabling the 15% of gas-phase material with the volume fraction to be fed into a rectifying tower II 2, and extracting crude high-boiling 21 from a tower kettle; the temperature of the top of the rectifying tower 1 is controlled at 135 ℃, and the pressure of the top of the rectifying tower is controlled at 0.45MPa.
(2) Condensing gas phase at the top of the fourth 4 tower top of the rectifying tower into a fourth reflux groove 19 of the rectifying tower through a fourth condenser 11 of the rectifying tower, conveying 99% of the material in the fourth reflux groove 19 of the rectifying tower through a fourth reflux pump 17 of the rectifying tower as tower reflux to return to the top of the fourth 4 tower of the rectifying tower, extracting a trichlorosilane product 25 with 1% volume fraction, and extracting a dimethyldichlorosilane product 26 from a tower kettle; the temperature of the four 4 tower kettles of the rectifying tower is controlled at 90 ℃, and the pressure of the tower kettles is controlled at 0.07MPa.
(3) The third 3 tower bottom of the rectifying tower adopts a second reboiler, a rectifying tower triple steam reboiler 7 as a supplementary heat source, all gas phase materials at the tower top enter a second tower bottom reboiler 8 of the rectifying tower as a heat source, after the gas phase materials are condensed by the second tower bottom thermal coupling reboiler 8 of the rectifying tower, 99% volume fraction materials are returned to the third 3 tower top of the rectifying tower as tower reflux through a third reflux pump 13 of the rectifying tower, 1% volume fraction materials are extracted as a methyltrichlorosilane product 22, and a dimethyldichlorosilane product 23 is extracted at the tower bottom; the temperature at the top of the third rectifying tower 3 is controlled at 107 ℃, the pressure at the top of the third rectifying tower is controlled at 0.2MPa, and if the temperature at the top of the third rectifying tower 3 can be controlled at 107 ℃ and the pressure at the top of the third rectifying tower is controlled at 0.2MPa as the heat source of the third rectifying tower in the steps, a third steam reboiler 7 of a second reboiler rectifying tower is not needed as a supplementary heat source.
(4) The gas phase at the top of the second rectifying tower 2 is condensed by a second rectifying tower condenser 9 and enters a second rectifying tower reflux groove 18, the material in the second rectifying tower reflux groove 18 is conveyed by a second rectifying tower reflux pump 15 to be 98% volume fraction material as tower reflux and returns to the top of the second rectifying tower 2, the other part of the extracted component 24 with the boiling point lower than that of the methyl trichlorosilane enters a subsequent rectifying tower for separation, the material extracted from the second rectifying tower 2 tower kettle is conveyed by a second rectifying tower kettle liquid pump 14 to be a third rectifying tower 3, and the rest 40% volume fraction material is obtained to be fed as a fourth rectifying tower 4; the temperature of the second 2 tower bottom of the rectification tower is controlled at 90 ℃, and the pressure of the tower bottom is controlled at 0.07MPa.
The energy-saving process (conventional process) for rectifying the crude monomer carried out in example 2 is as follows:
the method comprises the following steps of (1) enabling an organic silicon crude monomer to enter a first rectifying tower 1' at a flow rate of 25.5t/h, enabling a high-boiling gas-phase material removed from the top of the first rectifying tower 1' to enter a reflux groove 10' of the rectifying tower through a first rectifying tower condenser 7', enabling a material in the reflux groove 10' of the rectifying tower to be conveyed by a reflux pump 13' of the rectifying tower in a volume fraction of 85% to return to the top of the first rectifying tower 1' as tower reflux, enabling a gas-phase material in a volume fraction of 15% to be fed as a second rectifying tower 2', and extracting crude high-boiling 18' from a tower kettle; the temperature of the top of the first 1' rectifying tower is controlled at 135 ℃, and the pressure of the top of the rectifying tower is controlled at 0.45MPa.
The gas phase material at the top of the second rectifying tower 2' is condensed by a second rectifying tower condenser 8' and enters a second rectifying tower reflux groove 11', the material in the second rectifying tower reflux groove 11' is conveyed by a second rectifying tower reflux pump 14' to form 98% volume fraction material which is returned to the top of the second rectifying tower 2' as tower reflux, the other part of the material is extracted to form a component 21' with a boiling point lower than that of the methyl trichlorosilane and enters a subsequent rectifying tower for separation, and the material extracted from the bottom of the tower is conveyed by a third rectifying tower feed pump 15' to form third rectifying tower 3' feed; the temperature of the second 2' tower kettle of the rectifying tower is controlled at 90 ℃, and the pressure of the tower kettle is controlled at 0.07MPa.
The gas phase material at the top of the rectifying tower III 3 'is condensed by a rectifying tower III condenser 9' and enters a rectifying tower III reflux groove 12', the material in the rectifying tower III reflux groove 12' is conveyed by a rectifying tower III reflux pump 16 'to be taken as the material with 99% volume fraction to return to the top of the rectifying tower III 3' as the tower reflux, the material with 1% volume fraction, namely a trichlorosilane product 23', and a dimethyldichlorosilane product 22' is extracted at the bottom of the rectifying tower; the top temperature of the third 3' of the rectifying tower is controlled at 107 ℃, and the top pressure is controlled at 0.2MPa.
Under the same throughput and product quality circumstances, conventional device with the utility model discloses an energy consumption contrast data of technology that the device goes on as follows:
the purity of the obtained product, namely the methyl trichlorosilane, can reach 99.7 percent or more under the process conditions of the conventional technical means, and the purity of the dimethyl dichlorosilane can reach 99.98 percent or more.
The steps and the process conditions are the same as those of the embodiment 1, the top of the rectifying tower I1 is controlled to remove less than 35 percent or more than 45 percent of high-boiling gas phase material, the high-boiling gas phase material is firstly fed into a reboiler 10 at the four-tower kettle of the rectifying tower to be used as a heat source, and the system can not normally operate because the high-boiling gas phase material is less than 35 percent or more than 45 percent and the heat received by the reboiler 10 is too low or too high.
It can be seen through the comparison of the above data that the system of the utility model is adopted under the condition of the same treatment capacity and product quality, the heat consumption is only 64.49% of the conventional process, the condenser load is 61.84% of the conventional process, and the energy consumption and the consumption of the circulating water are greatly reduced.
Example 4
The organosilicon crude monomer is a mixture composed of methyl chlorosilane, and comprises the main components and mass fractions of (6% -9%) methyl trichlorosilane, (82% -87%) dimethyl dichlorosilane, (2.8% -3.7%) trimethyl monochlorosilane, (1.3% -2%) methyl dichlorosilane and (0.05% -1%) silicon tetrachloride.
The energy-saving process (conventional process) for rectifying the crude monomer carried out in example 2 is as follows:
feeding organosilicon crude monomers into a first rectifying tower 1' at a flow rate of 25.5t/h, condensing high-boiling gas-phase materials removed from the top of the first rectifying tower 1' through a first rectifying tower condenser 7' and feeding the high-boiling gas-phase materials into a reflux groove 10' of the rectifying tower, conveying the materials in the reflux groove 10' of the rectifying tower through a reflux pump 13' of the rectifying tower to return to the top of the first rectifying tower 1' as tower reflux, feeding 12% of gas-phase materials as a second rectifying tower 2' and extracting crude high-boiling 18' from a tower kettle; the top temperature of the first 1' of the rectifying tower is controlled at 132 ℃, and the top pressure is controlled at 0.42MPa.
The gas phase material at the top of the second 2' rectifying tower is condensed by a second condenser 8' of the rectifying tower and enters a second reflux groove 11' of the rectifying tower, the material in the second reflux groove 11' of the rectifying tower is conveyed by a second reflux pump 14' of the rectifying tower to be 99% volume fraction material as tower reflux and returns to the top of the second 2' rectifying tower, the other part of the material, 1%, of which the component 21' with the boiling point lower than that of the methyltrichlorosilane is extracted, enters a subsequent rectifying tower for separation, and the material extracted at the bottom of the tower is conveyed by a third feed pump 15' of the rectifying tower to be fed as a third 3' of the rectifying tower; the temperature of the second 2' tower kettle of the rectifying tower is controlled at 90 ℃, and the pressure of the tower kettle is controlled at 0.08MPa.
The gas phase material at the top of the rectifying tower III 3 'is condensed by a rectifying tower III condenser 9' and enters a rectifying tower III reflux groove 12', the material in the rectifying tower III reflux groove 12' is conveyed by a rectifying tower III reflux pump 16 'to be taken as the material with 98.5% volume fraction to return to the top of the rectifying tower III 3' as tower reflux, and the material with 1.5% volume fraction, namely a trichlorosilane product 23', and a dimethyldichlorosilane product 22' is extracted at the bottom of the rectifying tower; the tower top temperature of the third 3' of the rectifying tower is controlled at 109 ℃, and the tower top pressure is controlled at 0.21MPa.
The energy-saving process for rectifying the crude monomer, which is performed by adopting the embodiment 1, is as follows:
(1) The method comprises the following steps of (1) enabling an organic silicon crude monomer to enter a rectifying tower I1 at a flow rate of 25.5t/h, enabling a high-boiling gas-phase material removed from the top of the rectifying tower I1 to firstly enter a rectifying tower IV reboiler 10 as a heat source of a rectifying tower IV with a volume fraction of 42%, enabling the remaining 58% of the gas-phase material to enter a rectifying tower III reboiler 6 as a heat source, condensing the gas-phase material by the reboiler, converging the gas-phase material by a rectifying tower III-coupled reflux pump 14 and a rectifying tower IV-coupled reflux pump 16 respectively, enabling the gas-phase material with a volume fraction of 88% to return to the top of the rectifying tower I1 as tower reflux, enabling the gas-phase material with a volume fraction of 12% to be fed into a rectifying tower II 2, and enabling the tower kettle to obtain crude high-boiling 21; the temperature of the top of the rectifying tower I1 is controlled at 132 ℃, and the pressure of the top of the rectifying tower I1 is controlled at 0.42MPa.
(2) Condensing gas phase at the top of the fourth 4 tower top of the rectifying tower by a fourth condenser 11 of the rectifying tower to enter a fourth reflux groove 19 of the rectifying tower, conveying 99 percent of material in the fourth reflux groove 19 of the rectifying tower by a fourth reflux pump 17 of the rectifying tower to return to the top of the fourth 4 tower as tower reflux, extracting a trichlorosilane product 25 with 1 percent volume fraction, and extracting a dimethyldichlorosilane product 26 at the tower bottom; the temperature of the four 4 tower bottom of the rectifying tower is controlled at 92 ℃, and the pressure of the tower bottom is controlled at 0.09MPa.
(3) A rectifying tower III 3 tower kettle adopts a second reboiler, a rectifying tower triple steam reboiler 7 as a supplementary heat source, all gas phase materials at the tower top enter a rectifying tower II tower kettle reboiler 8 as a heat source, after the gas phase materials are condensed by the rectifying tower II tower kettle thermal coupling reboiler 8, 98.5% volume fraction materials are extracted by a rectifying tower III reflux pump 13 and return to the tower top of the rectifying tower III 3 as tower reflux, 1.5% volume fraction monomethyl trichlorosilane products 22 are extracted at the other part, and dimethyl dichlorosilane products 23 are extracted at the tower kettle; the top temperature of the third rectifying tower 3 is controlled at 109 ℃, the top pressure is controlled at 0.21MPa, and if the top temperature of the third rectifying tower 3 can be controlled at 107 ℃ and the top pressure is controlled at 0.2MPa as the heat source of the third rectifying tower in the steps, a second reboiler, a third steam reboiler 7 of the rectifying tower is not needed as a supplementary heat source.
(4) The gas phase at the top of the second rectifying tower 2 is condensed by a second rectifying tower condenser 9 and enters a second rectifying tower reflux groove 18, the material in the second rectifying tower reflux groove 18 is conveyed by a second rectifying tower reflux pump 15 to be 99% in volume fraction as tower reflux and returns to the top of the second rectifying tower 2, the other part is extracted to be 1%, namely, a component 24 with low boiling point of the methyltrichlorosilane enters a subsequent rectifying tower for separation, the material extracted from the second rectifying tower 2 at the bottom of the second rectifying tower is conveyed by a second rectifying tower bottom liquid pump 14 to be used as a third rectifying tower 3, and the material obtained from the rest 32% in volume fraction is used as fourth rectifying tower 4 for feeding; the temperature of the second 2 tower bottom of the rectifying tower is controlled at 90 ℃, and the pressure of the tower bottom is controlled at 0.08MPa.
In the other experimental process of the present application, the gas-phase material in step (1) does not preferentially enter the fourth rectifying tower, but first enters the third rectifying tower, for example, 42% of the gas-phase material in volume fraction enters the reboiler 6 of the third rectifying tower as a heat source, and then 58% of the gas-phase material in volume fraction enters the reboiler 10 of the fourth rectifying tower as a heat source. Other process conditions are the same as above, and this example is 4-1.
In another experimental process of the present application, in the step (1), the gas-phase material does not preferentially enter the rectifying tower four, but first enters the rectifying tower three, for example, 60% of the gas-phase material with volume fraction enters the rectifying tower three-tower kettle reboiler 6 as a heat source, and then 40% of the gas-phase material with volume fraction enters the rectifying tower four-tower kettle reboiler 10 as a heat source of the rectifying tower four. Under the same throughput and product quality circumstances, conventional device with the utility model discloses the energy consumption contrast data of the technology that the device goes on as follows:
Claims (10)
1. a crude monomer rectification energy-saving device is characterized in that a crude monomer feed pipe is connected with a first rectifying tower (1);
the top of the rectifying tower I (1) is respectively connected with a rectifying tower four-tower kettle reboiler (10) arranged at the bottom of the rectifying tower four (4) and a rectifying tower three-tower kettle reboiler (6) arranged at the bottom of the rectifying tower three (3) through a gas phase pipeline;
a rectifying tower three-tower kettle reboiler (6) and a rectifying tower four-tower kettle reboiler (10) are converged through a gas phase pipeline and then are connected with a rectifying tower two (2);
the bottom of the second rectifying tower (2) is respectively connected with a third rectifying tower (3) and a fourth rectifying tower (4) through liquid phase pipelines.
2. The energy-saving device for crude monomer rectification according to claim 1, wherein the gas phase pipelines of the rectifying tower three-tower kettle reboiler (6) and the rectifying tower four-tower kettle reboiler (10) are respectively provided with a rectifying tower three-coupling reflux pump (12) and a rectifying tower four-coupling reflux pump (16) before being merged.
3. The energy-saving device for crude monomer rectification according to claim 2, wherein a reboiler (8) of the second rectifying tower kettle is arranged at the bottom of the second rectifying tower (2), and the top of the third rectifying tower (3) is connected with the reboiler (8) of the second rectifying tower kettle arranged at the bottom of the second rectifying tower (2) through a gas phase pipeline.
4. The energy-saving device for crude monomer rectification according to claim 3, wherein the reboiler (8) at the second tower bottom of the rectification tower is connected with the third rectification tower (3) through the third reflux pump (13) of the rectification tower, and one way is connected with the first discharge pipe (22).
5. The energy-saving crude monomer rectification device according to claim 4, wherein the top of the second rectification tower (2) is connected with a second condenser (9) of the second rectification tower, the second condenser (9) of the second rectification tower is connected with a second reflux groove (18) of the second rectification tower, one path of the second reflux groove (18) of the second rectification tower is connected with the second rectification tower (2) through a second reflux pump (15) of the second rectification tower, and the other path is connected with a third discharge pipe (24).
6. The energy-saving device for crude monomer rectification according to claim 4, wherein a rectifying tower triple steam reboiler (7) is further arranged at the bottom of the rectifying tower III (3), and the bottom of the rectifying tower III (3) is connected to the discharging pipe II (23).
7. The energy-saving crude monomer rectification device according to claim 1, wherein the top of the rectifying tower four (4) is connected with a rectifying tower four condenser (11), the rectifying tower four condenser (11) is connected with a rectifying tower four reflux groove (19), and the rectifying tower four reflux groove (19) is connected with the rectifying tower four (4) through a rectifying tower four reflux pump (17) in one way and is connected with a discharge pipe four (25) in the other way.
8. Crude monomer rectification energy saving device according to claim 7, characterized in that the rectification column four (4) is connected at the bottom to the discharge pipe five (26).
9. The energy-saving crude monomer rectification device according to claim 8, wherein the rectification tower four-tower kettle reboiler (10) is connected with the upper part of the rectification tower I (1) through the rectification tower four-coupling reflux pump (16), and the rectification tower three-tower kettle reboiler (6) is further connected with the upper part of the rectification tower I (1) through the rectification tower three-coupling reflux pump (12).
10. The crude monomer rectification energy-saving device according to claim 9, characterized in that the bottom of the rectification column one (1) is connected to the crude high boiler discharging pipe (21).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115197265A (en) * | 2022-07-05 | 2022-10-18 | 湖北兴瑞硅材料有限公司 | Energy-saving method for rectifying crude monomer |
| CN115228118A (en) * | 2022-07-05 | 2022-10-25 | 湖北兴瑞硅材料有限公司 | Energy-saving method and device for rectifying crude monomer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115197265A (en) * | 2022-07-05 | 2022-10-18 | 湖北兴瑞硅材料有限公司 | Energy-saving method for rectifying crude monomer |
| CN115228118A (en) * | 2022-07-05 | 2022-10-25 | 湖北兴瑞硅材料有限公司 | Energy-saving method and device for rectifying crude monomer |
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