CN217828931U - Coarse monomer separation device - Google Patents
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- CN217828931U CN217828931U CN202221714393.9U CN202221714393U CN217828931U CN 217828931 U CN217828931 U CN 217828931U CN 202221714393 U CN202221714393 U CN 202221714393U CN 217828931 U CN217828931 U CN 217828931U
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Abstract
The invention relates to a crude monomer separation device, which is characterized in that crude monomers enter a first rectifying tower, high-boiling gas-phase materials removed from the top of the first rectifying tower enter a reboiler at the bottom of a third rectifying tower to be used as a heat source, and the rest gas-phase materials enter a reboiler at the bottom of a second rectifying tower to be used as a heat source; a steam reboiler is adopted as a supplementary heat source in the second tower kettle of the rectifying tower, and the tower kettle is used as the feeding materials of a third rectifying tower and a fourth rectifying tower; and the gas phase material at the third tower top of the rectifying tower completely enters a thermal coupling reboiler at the fourth tower bottom of the rectifying tower to be used as a heat source, and a part of the gas phase material is condensed by the thermal coupling reboiler to be used as tower reflux to return to the third tower top of the rectifying tower. The invention fully adopts the thermal coupling rectification technology, preferentially takes the gas phase material at the top of the first rectifying tower as the heat source of the thermal coupling reboiler at the three towers of the rectifying tower, takes the rest as the heat source of the thermal coupling reboiler at the two towers of the rectifying tower, and takes all the gas phase material at the top of the third rectifying tower as the heat source of the thermal coupling reboiler at the four towers of the rectifying tower, thereby reducing the steam consumption by 40 percent and the circulating water consumption by 40 percent in a same ratio.
Description
Technical Field
The utility model relates to a thick monomer separator 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 at present, silicon powder and chloromethane are used as raw materials to directly synthesize a methyl chlorosilane mixed monomer 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 containing hydrogen, trimethyl, high-boiling-point substances and low-boiling-point substances. And hydrolyzing and cracking dimethyl to produce various organosilicon intermediates, namely oligomeric methyl siloxane or alkoxy silane, and further processing the oligomeric methyl siloxane or alkoxy silane 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 the pressure swing thermal coupling rectification of the high-removing tower and the low-removing tower, the dual-effect rectification thermal coupling of the dual-element tower in parallel connection, and the pressure swing thermal coupling rectification of the high-removing tower and the dual-element tower, the utilization rate of the thermal coupling is not high, the comprehensive consideration of the thermal coupling to the three-tower system of the high-removing tower, the low-removing tower and the dual-element tower is not involved, and the energy consumption is still high.
Disclosure of Invention
The utility model provides a thick monomer separator solves prior art difficulty and 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 having a boiling point at atmospheric pressure greater than 66.4 ℃.
Crude monomer: the main components of the methyl chlorosilane mixed monomer are monomethyl trichlorosilane, dimethyl dichlorosilane, trimethyl monochlorosilane, monomethyl dichlorosilane, silicon tetrachloride and the like; the utility model discloses technical concept as follows: feeding the crude monomer into a first rectifying tower, removing high-boiling gas-phase materials at the top of the first rectifying tower, preferentially feeding the high-boiling gas-phase materials into a reboiler at a third tower kettle of the rectifying tower as a heat source, feeding the rest gas-phase materials into a reboiler at a second tower kettle of the rectifying tower as a heat source, condensing the rest gas-phase materials by the reboiler, returning a part of the condensed gas-phase materials to the top of the first rectifying tower as tower reflux, feeding the other part of the condensed gas-phase materials into a second rectifying tower, and extracting coarse high-boiling materials from the tower kettle; a steam reboiler is adopted as a supplementary heat source in the second tower kettle of the rectifying tower, components with a boiling point lower than that of the monomethyl trichlorosilane are extracted from the tower top and enter a subsequent rectifying tower for separation, and the components extracted from the tower kettle are used as feed of a third rectifying tower and a fourth rectifying tower; all gas phase materials at the top of the third tower of the rectifying tower enter a reboiler at the bottom of the fourth tower of the rectifying tower to be used as a heat source, a part of the gas phase materials is condensed by the reboiler to be used as tower reflux and returned to the top of the third tower of the rectifying tower, the other part of the gas phase materials is used as a methyl trichlorosilane product to be extracted, and a dimethyl dichlorosilane product is extracted from the tower bottom; and a methyl trichlorosilane product is extracted from the top of the rectifying tower IV, and a dimethyl dichlorosilane product is extracted from the bottom of the rectifying tower IV. The specific scheme is as follows:
a crude monomer separation device is characterized in that a crude monomer feed pipe is connected with a first rectifying tower; the first rectifying tower is respectively connected with a reboiler of a second rectifying tower kettle arranged at the bottom of the second rectifying tower and a reboiler of a third rectifying tower kettle arranged at the bottom of the rectifying tower;
a reboiler at the bottom of the second rectifying tower is connected with the second rectifying tower through a second rectifying tower coupling reflux pump;
a reboiler of a third tower kettle of the rectifying tower is connected with a second rectifying tower through a third coupling reflux pump of the rectifying tower;
the bottom of the second rectifying tower is connected with a second rectifying tower kettle liquid pump, and the second rectifying tower kettle liquid pump is respectively connected with a third rectifying tower and a fourth rectifying tower.
And a second rectifying tower steam reboiler is arranged at the bottom of the second rectifying tower, the top of the second rectifying tower is connected with a second rectifying tower condenser, the second rectifying tower condenser is connected with a second rectifying tower reflux groove, the second rectifying tower reflux groove is connected with the second rectifying tower through one way of a second rectifying tower reflux pump, and the other way of the second rectifying tower reflux groove is connected with the first rectifying tower discharge pipe.
The rectifying tower three-top part is connected with a rectifying tower four-tower kettle reboiler arranged at the rectifying tower four-bottom part, the rectifying tower four-tower kettle reboiler is connected with a rectifying tower three-reflux pump, the rectifying tower three-reflux pump is connected with the rectifying tower three-upper part all the way, the rectifying tower three-reflux pump is connected to a discharging pipe two, and the rectifying tower three-bottom part is connected with a discharging pipe three.
The top of the rectifying tower is connected with the rectifying tower four condenser, the rectifying tower four condenser is connected with the rectifying tower four reflux groove, the rectifying tower four reflux groove is connected with the rectifying tower four through the rectifying tower four reflux pump, the rectifying tower four reflux groove is connected with the rectifying tower four, the rectifying tower four reflux groove is connected with the discharging pipe four, the rectifying tower four bottom is connected with the discharging pipe five.
A reboiler at the bottom of the second rectifying tower is connected with the first rectifying tower through a second rectifying tower coupling reflux pump;
a reboiler of a rectifying tower three-tower kettle is connected with a rectifying tower I through a rectifying tower three-coupling reflux pump;
the rectifying tower is connected with a coarse high-boiling-point substance discharging pipe;
the bottom of the rectifying tower is also provided with a reboiler of the rectifying tower.
The utility model discloses simple structure, control condition are rigorous, have good application prospect and using value, compare its good effect with prior art and lie in: in the conventional process, reboilers of a rectifying tower I, a rectifying tower II, a rectifying tower III and a rectifying tower IV (in the embodiment, I, II and III) are heated by adopting steam, and circulating water is adopted for condensation at the tower top. By adopting the device of the utility model to fully utilize the components and the characteristics of the materials and adopting the triple-effect rectification technology,
the heat transfer basic condition is required to be met, the heat transfer condition is required to be that a temperature difference exists between two objects, the gas phase temperature at the top of the first rectifying tower is required to be higher than the tower kettle temperatures of the second rectifying tower and the third rectifying tower, and the heat of the first rectifying tower can be effectively transferred to the second rectifying tower and the third rectifying tower; in order to meet the most reasonable design conditions of the second rectifying tower and the third rectifying tower, the heat exchange area and the heat transfer coefficient parameters of the second rectifying tower and the third rectifying tower are determined according to the design, and the gas phase temperature at the top of the first rectifying tower is 20-65 ℃ higher than the temperature at the bottom of the second rectifying tower and the third rectifying tower.
The heat transfer basic condition is required to be met, the condition for heat transfer must be that a temperature difference exists between two objects, the gas phase temperature at the top of the third rectifying tower is required to be higher than the tower kettle temperature of the fourth rectifying tower, the heat of the third rectifying tower can be effectively transferred to the fourth rectifying tower, and in order to meet the most reasonable design condition of the fourth rectifying tower reboiler, the heat exchange area and the heat transfer coefficient parameters of the fourth rectifying tower reboiler are determined according to the design, and the gas phase temperature at the top of the third rectifying tower is 5-40 ℃ higher than the tower kettle temperature of the fourth rectifying tower.
Compared with the prior art, the device of the utility model has the good effects that: 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.
The utility model discloses make full use of material component and characteristic adopt the triple effect rectification technology, and the rectifying column three splits in the conventional art is rectifying column three and rectifying column four, and a split can apply to rectifying column two 2, the maximize utilizes the system heat with the unnecessary heat of rectifying column one 1.
Simultaneously, the first rectifying tower and the third rectifying tower are pressurized to increase the temperature of the first rectifying tower and the third rectifying tower; as 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 temperatures of the tower kettles of the third rectifying tower and the second rectifying tower, and the temperature of the gas phase at the top of the third rectifying tower is higher than the temperature of the tower kettle of the fourth rectifying tower, so that the first rectifying tower and the third rectifying tower need to be pressurized, and the temperature of the top of the first rectifying tower and the temperature of the third rectifying tower are increased.
Because the second rectifying tower is provided with the steam reboiler 6 to compensate heat 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 a thermally coupled reboiler at the three towers of the first rectifying tower, the rest of the gas-phase material at the top of the second rectifying tower is used as a heat source of the reboiler at the two towers of the second rectifying tower, and then, the gas-phase material at the top of the third rectifying tower is completely used as a heat source of a reboiler at the four towers of the fourth 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 maximally utilized, 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 by at least 40% in proportion, and the circulating water consumption is reduced by 40%.
Drawings
FIG. 1 is a schematic diagram of a crude monomer coupling method of the present invention, wherein 1 is a first rectifying 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 at a second tower kettle of the rectifying tower; 7, a second steam reboiler of the rectifying tower; 8, a second condenser of the rectifying tower; 9, a rectifying tower three-tower kettle reboiler; 10 rectifying tower four-tower kettle reboiler; 11, a rectifying tower four condenser; 12 a second reflux groove of the rectifying tower; 13 a rectifying tower four reflux groove; 14, coupling a reflux pump with the second rectifying tower; 15 a second reflux pump of the rectifying tower; 16 a second-kettle liquid pump of the rectifying tower; 17, a rectifying tower is coupled with a reflux pump; 18 rectification column three reflux pumps; 19 a rectifying tower four reflux pump; 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 discharging a pipe IV; and 26, discharging a pipe V. FIG. 2 is a structural diagram of a crude monomer rectification method of a 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' a second condenser of the 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' rectifying tower three feed pumps; 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' discharging 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 separation device, a crude monomer feed pipe 20 is connected with a rectifying tower I1; the rectifying tower I1 is respectively connected with a rectifying tower II kettle reboiler 6 arranged at the bottom of the rectifying tower II 2 and a rectifying tower III kettle reboiler 9 arranged at the bottom of the rectifying tower 3;
a second rectifying tower kettle reboiler 6 is converged with a third rectifying tower kettle reboiler 9 through a second rectifying tower coupling reflux pump 14 and a third rectifying tower coupling reflux pump 17 and then is connected with a second rectifying tower 2;
the bottom of the second rectifying tower 2 is connected with a second rectifying tower liquid tank pump 16, and the second rectifying tower liquid tank pump 16 is respectively connected with a third rectifying tower 3 and a fourth rectifying tower 4.
And a second rectifying tower steam reboiler 7 is arranged at the bottom of the second rectifying tower 2.
The top of the second rectifying tower 2 is connected with a second condenser 8 of the rectifying tower, the second condenser 8 of the rectifying tower is connected with a second reflux groove 12 of the rectifying tower, one path of the second reflux groove 12 of the rectifying tower is connected with the second rectifying tower 2 through a second reflux pump 15 of the rectifying tower, and the other path is connected with a first discharge pipe 22.
The top of the rectifying tower III 3 is connected with a rectifying tower four-tower kettle reboiler 10 arranged at the bottom of the rectifying tower IV 4.
The rectifying tower four-tower kettle reboiler 10 is connected with a rectifying tower three reflux pump 18, one path of the rectifying tower three reflux pump 18 is connected with the upper part of a rectifying tower three 3, and the other path is connected with a discharge pipe two 23.
The bottom of the rectifying tower III 3 is connected with a discharge pipe III 24.
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 13, the rectifying tower four reflux groove 13 is connected with the rectifying tower four 4 through a rectifying tower four reflux pump 19, one path is connected to a discharging pipe four 25, and the bottom of the rectifying tower four 4 is connected to a discharging pipe five 26.
And a reboiler 6 at the second tower bottom of the rectifying tower is connected with the first rectifying tower 1 through a second coupling reflux pump 14 of the rectifying tower.
A rectifying tower three-tower kettle reboiler 9 is connected with the rectifying tower I1 through a rectifying tower three-coupling reflux pump 17; the rectification column one 1 is connected to a crude high boiler outlet pipe 21.
The bottom of the rectifying tower I1 is also provided with a reboiler 5 of the rectifying tower.
The material stream qualification parameter ranges are as follows:
dimethyl dichlorosilane: 20-50%, trimethylchlorosilane: 0.01-0.1%, high boiling point substance: 50 to 80 percent.
A stream 22 is extracted from the top of the second rectifying tower:
monomethyltrichlorosilane: 0.1-8%, trimethylchlorosilane: 40-60%, monomethyldichlorosilane: 30-50%, dimethylchlorosilane 5-10%, silicon tetrachloride: 0-0.55%, low boiling substance: 3 to 10 percent.
And a stream 23 is extracted from the top of the rectifying tower at the third tower:
monomethyltrichlorosilane: 99.7-100%, dimethyldichlorosilane: 0.05-1%, trimethylchlorosilane: 0.01-0.5%, silicon tetrachloride: 0.01 to 0.3 percent.
And (3) producing a stream 24 at the bottom of the three towers of the rectifying tower:
dimethyl dichlorosilane: 99.98-100%, monomethyltrichlorosilane: 0.005-0.02%, high boiling substance: 0.04-0.2 percent.
A four-tower top produced stream 25 of the rectifying tower:
mono-methyltrichlorosilane: 99.7-100%, dimethyldichlorosilane: 0.05-1%, trimethylchlorosilane: 0.01-0.5%, silicon tetrachloride: 0.01 to 0.3 percent.
And (3) producing a stream 26 at the bottom of the four towers of the rectifying tower:
dimethyl dichlorosilane: 99.98-100%, monomethyltrichlorosilane: 0.005-0.02%, high boiling substance: 0.04-0.2 percent.
Example 2
The equipment connecting 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', one 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
In this embodiment, the crude organosilicon monomer is a mixture of methylchlorosilanes, and the major components and mass fractions thereof are monomethyltrichlorosilane (8.6%), dimethyldichlorosilane (85%), trimethylmonochlorosilane (3.8%), monomethyldichlorosilane (1.6%), and silicon tetrachloride (1%). The pressure is 0.7MPa and the temperature is 42 ℃.
The conventional process was carried out using the apparatus connection structure of example 2 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 be 85 volume percent as tower reflux and returning the materials to the top of the first rectifying tower 1', feeding 15 volume percent 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 135 ℃, and the top pressure 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.
Condensing the gas phase material at the top of the rectifying tower III 3 'by a rectifying tower III condenser 9' to enter a rectifying tower III reflux groove 12', conveying the material in the rectifying tower III reflux groove 12' by a rectifying tower III reflux pump 16 'to return the material with 99% volume fraction to the top of the rectifying tower III 3' as tower reflux, and collecting the material with 1% volume fraction, namely a trichlorosilane product 23', and collecting a dimethyldichlorosilane product 22' at the bottom of the rectifying tower; the tower top temperature of the third 3' of the rectifying tower is controlled at 107 ℃, and the tower top pressure is controlled at 0.2MPa.
The energy-saving process for rectifying the crude monomer by using the embodiment 1 is as follows:
(1) Feeding organosilicon crude monomers into a rectifying tower I1 at a flow rate of 25.5t/h, preferentially feeding high-boiling gas-phase materials removed from the tower top of the rectifying tower I1 into a rectifying tower third-tower kettle reboiler 9 by 35% volume fraction as a heat source, feeding the rest 65% volume fraction gas-phase materials into a rectifying tower second-tower kettle reboiler 6 as a heat source, condensing by a thermal coupling reboiler, respectively feeding 85% volume fraction materials serving as tower reflux back to the tower top of the rectifying tower I1 through a rectifying tower third-coupling reflux pump 17 and a rectifying tower second-coupling reflux pump 14, feeding 15% volume fraction materials serving as a rectifying tower second 2, and extracting crude high-boiling 21 from the 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) The second 2 tower bottom of the rectifying tower adopts a second reboiler, a second steam reboiler 7 of the rectifying tower is used as a supplementary heat source, the gas phase at the top of the rectifying tower is condensed by a second condenser 8 of the rectifying tower and enters a second reflux groove 12 of the rectifying tower, the materials in the second reflux groove 12 of the rectifying tower are conveyed by a second reflux pump 15 of the rectifying tower to 98% in volume fraction as the materials which are refluxed to the top of the second 2 rectifying tower, 2% of the components 22 with the boiling point lower than that of the methyl trichlorosilane are extracted and enter a subsequent rectifying tower for separation, 60% of the materials with the volume fraction are conveyed by a second kettle liquid pump 16 of the rectifying tower to enter a third 3 rectifying tower, and the rest 40% of the materials with the volume fraction are fed as a fourth 4 rectifying tower; the temperature of the second 2 rectifying tower kettle is controlled at 87 ℃, and the pressure of the tower kettle is controlled at 0.06MPa.
(3) All gas phase materials at the top of the third 3 rectifying tower enter a reboiler 10 of a fourth tower kettle of the rectifying tower as a heat source, after being condensed by the reboiler 10 of the fourth tower kettle of the rectifying tower, 99 percent of materials with volume fraction are extracted by a third reflux pump 18 of the rectifying tower and return to the top of the third 3 rectifying tower as tower reflux, 1 percent of materials with volume fraction are extracted as a methyl trichlorosilane product 23, and a dimethyl dichlorosilane product 24 is extracted at the bottom of the rectifying tower; the top temperature of the third rectifying tower 3 is controlled at 107 ℃, and the top pressure is controlled at 0.2MPa.
(4) The gas phase at the top of the fourth 4 tower top of the rectifying tower is condensed by a fourth condenser 11 of the rectifying tower and enters a fourth reflux groove 13 of the rectifying tower, the material in the fourth reflux groove 13 of the rectifying tower is conveyed by a fourth reflux pump 19 of the rectifying tower to be 98.5 percent of material in volume fraction as tower reflux and returns to the top of the fourth 4 tower, the other part of the material adopts a mono-trichlorosilane product 25 with 1.5 percent of material in volume fraction, and the dimethyl dichlorosilane product 26 is extracted from the 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.
The step (1) refers to the split flow condition that the high-boiling gas phase material is removed from the top of the rectifying tower 1, and the high-boiling gas phase material preferentially enters a rectifying tower three-tower kettle reboiler 9 as a heat source, and the gas phase material enters a rectifying tower two-tower kettle reboiler 6 as a heat source for feeding.
The second column of step (1) refers to the split flow condition of the material returned to the top of the first rectifying tower 1 as tower reflux and fed as the second rectifying tower 2 through the third rectifying tower coupled reflux pump 17 and the second rectifying tower coupled reflux pump 14.
The step (2) refers to the split flow condition that the distillation product from the second 2 tower bottom of the rectifying tower is conveyed to the third 3 rectifying tower through the second 16 tower bottom liquid pump and is used as the feeding material of the fourth 4 rectifying tower.
Under the same throughput and the product quality condition, conventional device with adopt the utility model discloses an energy consumption contrast data of device as follows:
the process conditions of the method and the process conditions of the conventional technical means can ensure that the purity of the obtained product, namely the methyl trichlorosilane, reaches 99.7 percent or more, and the purity of the dimethyl dichlorosilane reaches 99.98 percent or more.
It can be seen through the comparison of above data, adopt the utility model discloses a device, under the condition of same treatment capacity and product quality, the heat consumption only is 55.43% of conventional technology, and the condenser load is 50.92% of conventional technology, has reduced by a wide margin the energy and the quantity of circulating water.
Example 4
Taking the components of the organosilicon monomers in example 3 as raw materials for separation, feeding organosilicon crude monomers into a first rectifying tower 1 at a flow rate of 25.5t/h, removing high-boiling gas-phase materials at the top of the first rectifying tower 1, feeding 65% of gas-phase materials with volume fraction into a reboiler 6 at the bottom of a second rectifying tower as a heat source, feeding the rest 35% of gas-phase materials with volume fraction into a reboiler 9 at the bottom of a third rectifying tower as a heat source after being used as the heat source of the second rectifying tower, condensing by a thermal coupling reboiler, feeding 85% of materials with volume fraction as tower reflux back to the top of the first rectifying tower 1 by a third rectifying tower coupling reflux pump 17 and a second rectifying tower coupling reflux pump 14 respectively, feeding 15% of materials with volume fraction into a second rectifying tower 2, and extracting crude high-boiling 21 at the bottom of the first rectifying tower; the temperature of the top of the rectifying tower I1 is controlled at 135 ℃, and the pressure of the top of the rectifying tower I1 is controlled at 0.45MPa.
Compared with the example 3, the above steps are only the start-up steps of the rectification system are changed, the distribution parameters of the material streams are not changed, and the realized process effect is consistent with the example 3.
Or the high-boiling gas phase material removed from the top of the rectifying tower I1 firstly enters a reboiler 6 of a second tower kettle of the rectifying tower in 35 volume percent as a heat source, and after being used as the heat source of the second rectifying tower, the rest 65 volume percent enters a reboiler 9 of a third tower kettle of the rectifying tower as a heat source, after being condensed by a thermal coupling reboiler, the material in 85 volume percent is returned to the top of the rectifying tower I1 as tower reflux through a third coupling reflux pump 17 of the rectifying tower and a second coupling reflux pump 14 of the rectifying tower respectively, the material in 15 volume percent is fed into a second rectifying tower 2, and the coarse high-boiling 21 is extracted from the 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.
Compared with the embodiment 3, the starting steps and the material stream distribution parameters of the rectification system are changed, the distribution parameters of the material stream exceed the process range, and the realized process effect is that the rectification system cannot be normally started to operate.
Example 5
The general process for the rectification of crude monomer carried out using example 2 is as follows:
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 20.5t/h, enabling a high-boiling gas phase material removed from the top of the rectifying tower I1 to enter a reflux tank 10 of the rectifying tower through a condenser 7 of the rectifying tower I1, enabling the material in the reflux tank 10 of the rectifying tower I1 to return 89% of the material with volume fraction as tower reflux to the top of the rectifying tower I1 through a reflux pump 13 of the rectifying tower I1, enabling the material with 11% of volume fraction to be fed as a rectifying tower II 2, and extracting crude high-boiling 18 from a tower kettle; the top temperature of the rectifying tower 1 is controlled at 132 ℃, and the top pressure is controlled at 0.42MPa.
Gas phase materials at the top of the second rectifying tower 2 enter a second rectifying tower 2 reflux groove 11 after being condensed by a second rectifying tower 2 condenser 8, the materials in the second rectifying tower 2 reflux groove 11 are conveyed by a second rectifying tower 2 reflux pump 14 to be 99% volume fraction materials as tower reflux to return to the top of the second rectifying tower 2, the extracted components 21 with the boiling point lower than that of the methyl trichlorosilane of 1% enter a subsequent rectifying tower for separation, and the extracted components at the bottom of the tower are conveyed by a third rectifying tower feed pump 15 to be used as feed of a third rectifying tower 3; 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.
Condensing the gas-phase material at the top of the third rectifying tower 3 through a third rectifying tower 3 condenser 9, feeding the gas-phase material into a third rectifying tower 3 reflux tank 12, extracting 98.5% of the material in the third rectifying tower 3 reflux tank 12 through a third rectifying tower 3 reflux pump 16, returning the extracted material to the top of the third rectifying tower 3 as tower reflux, extracting a trichlorosilane product 23 from the material with 1.5% of the volume fraction, and extracting a dimethyldichlorosilane product 22 from the tower bottom; the top temperature of the third rectifying tower 3 is controlled at 109 ℃, and the top pressure is controlled at 0.21MPa.
The energy-saving process for rectifying the crude monomer by using the embodiment 1 is as follows:
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 20.5t/h, enabling a high-boiling gas-phase material removed from the top of the rectifying tower I1 to preferentially enter a rectifying tower III kettle reboiler 9 as a heat source in a volume fraction of 44%, enabling the remaining 56% of the gas-phase material in the volume fraction to enter a rectifying tower II kettle reboiler 6 as a heat source, condensing the gas-phase material in the thermal coupling reboiler, enabling 89% of the material in the volume fraction to return to the top of the rectifying tower I1 as tower reflux through a rectifying tower III coupling reflux pump 17 and a rectifying tower II coupling reflux pump 14 respectively, enabling the material in the volume fraction of 11% to be fed into a rectifying tower II 2, and extracting crude high-boiling 21 from the tower kettle; 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.
The second 2 tower bottom of the rectifying tower adopts a second reboiler, a second steam reboiler 7 of the rectifying tower is used as a supplementary heat source, the gas phase at the top of the rectifying tower is condensed by a second condenser 8 of the rectifying tower and enters a second reflux groove 12 of the rectifying tower, the materials in the second reflux groove 12 of the rectifying tower are conveyed by a second reflux pump 15 of the rectifying tower to 99% in volume fraction as tower reflux and return to the top of the second 2 rectifying tower, 1% of the component 22 with the boiling point lower than that of the methyltrichlorosilane is extracted and enters a subsequent rectifying tower for separation, 64% in volume fraction is conveyed by a second kettle liquid pump 16 of the rectifying tower as a third 3 of the rectifying tower, and the rest 36% in volume fraction is fed as a fourth 4 of the rectifying tower; 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.
All gas phase materials at the top of the third 3 rectifying tower enter a reboiler 10 at the four towers of the rectifying tower to be used as a heat source, after the gas phase materials are condensed by the reboiler 10 at the four towers of the rectifying tower, 98.5 percent of materials with volume fraction are extracted by a third reflux pump 18 of the rectifying tower to be used as tower reflux to return to the top of the third 3 rectifying tower, 1.5 percent of materials with volume fraction are extracted as a methyltrichlorosilane product 23, and a dimethyldichlorosilane product 24 is extracted at the bottom of the rectifying tower; the top temperature of the third rectifying tower 3 is controlled at 109 ℃, and the pressure of the bottom of the rectifying tower is controlled at 0.21MPa.
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 13 of the rectifying tower, conveying 99% volume fraction material in the fourth reflux groove 13 of the rectifying tower by a fourth reflux pump 19 of the rectifying tower to return to the top of the fourth 4 tower as tower reflux, extracting 1% volume fraction material-trichlorosilane product 25, and extracting 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 0.08MPa.
Under the same throughput and the product quality condition, conventional device with adopt the utility model discloses a device carries out the energy consumption contrast data of technology as follows:
the purity of the obtained product, namely the methyl trichlorosilane, can reach 99.7 percent and above under the process conditions of the conventional technical means, and the purity of the dimethyl dichlorosilane can reach 99.98 percent and above;
it can be seen through the comparison of above data, adopt the utility model discloses an in the process that the device goes on, under the condition of same handling capacity and product quality, the heat consumption only is 57.25% of conventional technology, and the condenser load is 55.39% of conventional technology, has reduced by a wide margin the ability and has reached the quantity of circulating water.
Claims (10)
1. A crude monomer separation device is characterized in that a crude monomer feeding pipe (20) is connected with a first rectifying tower (1); the first rectifying tower (1) is respectively connected with a second rectifying tower kettle reboiler (6) arranged at the bottom of the second rectifying tower (2) and a third rectifying tower kettle reboiler (9) arranged at the bottom of the third rectifying tower (3);
a reboiler (6) at the second tower kettle of the rectifying tower is converged by a second coupling reflux pump (14) of the rectifying tower and a reboiler (9) at the third tower kettle of the rectifying tower through a third coupling reflux pump (17) of the rectifying tower and then is connected with the second rectifying tower (2);
the bottom of the second rectifying tower (2) is connected with a second rectifying tower liquid pump (16), and the second rectifying tower liquid pump (16) is respectively connected with a third rectifying tower (3) and a fourth rectifying tower (4).
2. The crude monomer separation apparatus according to claim 1, wherein a second distillation column steam reboiler (7) is provided at the bottom of the second distillation column (2).
3. The crude monomer separation device according to claim 2, wherein the top of the second rectifying tower (2) is connected with a second condenser (8) of the rectifying tower, the second condenser (8) of the rectifying tower is connected with a second reflux groove (12) of the rectifying tower, one path of the second reflux groove (12) of the rectifying tower is connected with the second rectifying tower (2) through a second reflux pump (15) of the rectifying tower, and the other path is connected with a first discharge pipe (22).
4. The crude monomer separation apparatus according to claim 2, wherein the top of the rectifying column three (3) is connected with a rectifying column four-kettle reboiler (10) arranged at the bottom of the rectifying column four (4).
5. The crude monomer separation device according to claim 4, wherein the rectifying tower four-kettle reboiler (10) is connected with a rectifying tower three-reflux pump (18), one path of the rectifying tower three-reflux pump (18) is connected with the upper part of the rectifying tower three (3), and the other path is connected with the discharge pipe two (23).
6. The crude monomer separation apparatus according to claim 5, wherein the bottom of rectifying column III (3) is connected to discharge pipe III (24).
7. The crude monomer separation 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 (13), the rectifying tower four reflux groove (13) is connected with the rectifying tower four (4) through a rectifying tower four reflux pump (19) in one way, is connected with a discharging pipe four (25) in one way, and is connected with a discharging pipe five (26) at the bottom of the rectifying tower four (4).
8. The crude monomer separation device according to claim 1, wherein the reboiler (6) of the second distillation column is connected to the first distillation column (1) through a second coupling reflux pump (14).
9. The crude monomer separation device according to claim 1, wherein the rectifying tower triple-kettle reboiler (9) is connected with the rectifying tower I (1) through a rectifying tower triple-coupling reflux pump (17); the first rectifying tower (1) is connected to a coarse high-boiling-point substance discharging pipe (21).
10. The crude monomer separation apparatus according to claim 1, wherein the bottom of the first rectification column (1) is further provided with a reboiler (5) for the rectification column.
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