CN111153925B - Device and method for continuously purifying 2-cyanoethyl trichlorosilane - Google Patents
Device and method for continuously purifying 2-cyanoethyl trichlorosilane Download PDFInfo
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- CN111153925B CN111153925B CN201911404431.3A CN201911404431A CN111153925B CN 111153925 B CN111153925 B CN 111153925B CN 201911404431 A CN201911404431 A CN 201911404431A CN 111153925 B CN111153925 B CN 111153925B
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- C—CHEMISTRY; METALLURGY
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- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/22—Evaporating by bringing a thin layer of the liquid into contact with a heated surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
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Abstract
A device and a method for continuously purifying 2-cyanoethyl trichlorosilane relate to a device and a method for purifying 2-cyanoethyl trichlorosilane, and aim to solve the technical problem of low yield of the existing method for purifying 2-cyanoethyl trichlorosilane. The device comprises a distillation system, a feeding pump and a raw material storage tank which are sequentially connected in five stages; the raw material storage tank is connected with a feed inlet of a wiped film evaporator of the I-stage distillation system through a feed pump. The method comprises the following steps: and (3) sequentially introducing the crude 2-cyanoethyl trichlorosilane into five-stage distillation systems for distillation, gradually raising the temperature of each group of distillation systems, gradually lowering the pressure and temperature, and purifying. The chromatographic purity of the 2-cyanoethyl trichlorosilane refined product obtained by the method can reach 99.98 percent to the maximum, the yield is more than 75 percent, and the method can be used in the field of purification of 2-cyanoethyl trichlorosilane.
Description
Technical Field
The invention relates to a continuous purification method of 2-cyanoethyl trichlorosilane and an industrial continuous purification device, belonging to the field of fine chemical engineering.
Background
2-cyanoethyl trichlorosilane with the structural formula
It is an important raw material for synthesizing 2-cyanoethyl triethoxysilane. The crude product after the synthesis of the 2-cyanoethyl trichlorosilane contains four front fractions of trichlorosilane, silicon tetrachloride, acrylonitrile and propionitrile, so that the crude product needs to be purified. The conventional vacuum distillation and rectification are generally adopted for purifying a crude product, because the 2-cyanoethyl trichlorosilane is very sensitive to temperature, the long-time purification in a high-temperature environment can lead the 2-cyanoethyl trichlorosilane to form a polymer with a higher boiling point, namely high boiling point, so that the yield of the 2-cyanoethyl trichlorosilane is reduced.
Disclosure of Invention
The invention provides a device and a method for continuously purifying 2-cyanoethyl trichlorosilane, aiming at solving the technical problem of low yield of the existing purification method of 2-cyanoethyl trichlorosilane.
The device for continuously purifying the 2-cyanoethyl trichlorosilane comprises a grade I distillation system, a grade II distillation system, a grade III distillation system, a grade IV distillation system, a grade V distillation system, a feeding pump and a raw material storage tank;
the I, II, III and IV grade distillation systems consist of a wiped film evaporator, a condenser, a finished product tank, a receiving tank and a back pressure valve, and the V grade distillation system consists of a wiped film evaporator, a condenser, a finished product tank and a receiving tank;
the upper part of the side wall of the wiped film evaporator in each stage of distillation system is provided with a feed inlet, the top of the wiped film evaporator is provided with a steam outlet, and the steam outlet is connected with a finished product tank through a condenser; a concentrated solution outlet is arranged at the bottom of the wiped film evaporator; the concentrated solution outlet is connected with the receiving tank; the receiving tank is connected with the feed inlet of the next-stage wiped film evaporator through a back pressure valve;
the raw material storage tank is connected with a feed inlet of a wiped film evaporator of the I-stage distillation system through a feed pump.
Furthermore, the inner wall of the wiped film evaporator and the scrapers are made of corrosion-resistant high-strength phenolic glass fiber reinforced plastics, so that the corrosion resistance of the equipment is improved.
The device for continuously purifying the 2-cyanoethyl trichlorosilane also comprises a nitrogen supply system, a vacuum pumping system and a cooling system;
the method for continuously purifying the 2-cyanoethyl trichlorosilane by using the device comprises the following steps:
firstly, introducing nitrogen into a stage I distillation system to ensure that the pressure in the stage I distillation system reaches 240-250 kPa; then pumping the 2-cyanoethyl trichlorosilane crude product in the raw material storage tank into a first-stage wiped film evaporator, and distilling at the temperature of 60-65 ℃ and under the pressure of 240-250 kPa; the distilled gaseous substance enters a grade I condenser through a steam outlet for condensation, and the condensate flows into a grade I finished product tank; obtaining front cut trichlorosilane; the concentrated solution flows into a grade I receiving tank after distillation;
secondly, introducing nitrogen into the II-stage distillation system to enable the pressure in the II-stage distillation system to reach 110-120 kPa; pumping the concentrated solution in the I-stage receiving tank into a II-stage wiped film evaporator by utilizing differential pressure, and distilling at the temperature of 60-65 ℃ and under the pressure of 110-120 kPa; the distilled gaseous substance enters a first-stage condenser through a steam outlet for condensation, and the condensate flows into a second-stage finished product tank; obtaining front fraction silicon tetrachloride; the concentrated solution flows into a II-stage receiving tank after distillation;
keeping the pressure in the III-grade distillation system at normal pressure, pressing the concentrated solution in the II-grade receiving tank into the III-grade wiped film evaporator by utilizing differential pressure, and distilling at the normal pressure at the temperature of 80-85 ℃; the distilled gaseous substance enters a grade III condenser for condensation, and the condensate flows into a grade III finished product tank; obtaining front cut acrylonitrile; the concentrated solution flows into a grade III receiving tank after distillation;
pumping the pressure of an IV-grade distillation system to-0.05 to-0.06 MPa, pressing the concentrated solution in a III-grade receiving tank into an IV-grade wiped film evaporator by using differential pressure, carrying out reduced pressure distillation at the temperature of 80-85 ℃ and the pressure of-0.05 to-0.06 MPa, feeding the distilled gaseous substance into an IV-grade condenser for condensation, and feeding the condensate into an IV-grade finished product tank; obtaining front cut propionitrile; the distilled concentrated solution flows into an IV-grade receiving tank;
fifthly, pumping the pressure of a V-grade distillation system to-0.090-0.1 MPa, pressing the concentrated solution in an IV-grade receiving tank into a V-grade wiped film evaporator by using a pressure difference, carrying out reduced pressure distillation at the temperature of 110-115 ℃ and the pressure of-0.090-0.1 MPa, allowing the distilled gaseous substances to enter a V-grade condenser for condensation, and allowing the condensate to flow into a V-grade finished product tank; obtaining 2-cyanoethyl trichlorosilane; and (4) the distilled concentrated solution flows into a V-level receiving tank to obtain a high-boiling-point substance, so that the purification of the 2-cyanoethyl trichlorosilane is completed.
Furthermore, in the first step, the flow rate of the crude product of 2-cyanoethyltrichlorosilane is 200 to 220 kg/h.
Aiming at the characteristics that 2-cyanoethyl trichlorosilane is very sensitive to temperature and is not suitable for long-time distillation and purification in a high-temperature system, the invention designs a continuous purification device and a continuous purification method, rapidly and respectively purifies four front fractions including trichlorosilane, silicon tetrachloride, acrylonitrile and propionitrile in a crude product of 2-cyanoethyl trichlorosilane, simultaneously reduces the time of 2-cyanoethyl trichlorosilane in a high-temperature period, improves the yield of 2-cyanoethyl trichlorosilane, reduces the yield of high-boiling substances, and simultaneously, after purification, the chromatographic purity of a refined product of 2-cyanoethyl trichlorosilane can reach 99.98 percent to the maximum extent, and the yield is more than 75 percent.
The invention has simple process, the raw material can not be in a high-temperature environment for a long time, the pressure of each section is gradually reduced, the material transfer is easier, the operation is convenient, the high-boiling residue is changed into the silicone resin powder after being processed, the waste utilization is realized, and the economic benefit is improved.
The device and the method are suitable for the field of purification of 2-cyanoethyl trichlorosilane.
Drawings
FIG. 1 is a schematic view of an apparatus for continuously purifying 2-cyanoethyltrichlorosilane; in the figure:
1 is a grade I distillation system, 2 is a grade II distillation system, 3 is a grade III distillation system, 4 is a grade IV distillation system, 5 is a grade V distillation system, 6 is a feeding pump, and 7 is a raw material storage tank;
in the I-stage distillation system, 1-1 is a wiped film evaporator, 1-3 is a condenser, 1-4 is a finished product tank, 1-2 is a receiving tank, and 1-5 is a back pressure valve;
in the II-stage distillation system, 2-1 is a wiped film evaporator, 2-3 is a condenser, 2-4 is a finished product tank, 2-2 is a receiving tank, and 2-5 is a back pressure valve;
in a III-grade distillation system, 3-1 is a wiped film evaporator, 3-3 is a condenser, 3-4 is a finished product tank, 3-2 is a receiving tank, and 3-5 is a back pressure valve;
in the IV-stage distillation system, 4-1 is a wiped film evaporator, 4-3 is a condenser, 4-4 is a finished product tank, 4-2 is a receiving tank, and 4-5 is a back pressure valve;
in a V-level distillation system, 5-1 is a wiped film evaporator, 5-3 is a condenser, 5-4 is a finished product tank, and 5-2 is a receiving tank;
FIG. 2 is a schematic view of a wiped film evaporator configuration; 1-1 is a grade I wiped film evaporator, 1-1-1 is a feed inlet, 1-1-2 is a steam outlet, and 1-1-3 is a concentrated solution outlet;
FIG. 3 is a schematic view of a receiving tank configuration; 1-2 is a I-stage receiving tank, and 1-2-1 is a feeding hole; 1-2-2 is a discharge port, and 1-2-3 is a discharge port.
Detailed Description
The following examples are used to demonstrate the beneficial effects of the present invention:
example 1: (see attached drawings 1-3) the device for continuously purifying 2-cyanoethyltrichlorosilane in the embodiment comprises a grade I distillation system 1, a grade II distillation system 2, a grade III distillation system 3, a grade IV distillation system 4, a grade V distillation system 5, a feeding pump 6, a raw material storage tank 7, a nitrogen supply system, a vacuum pumping system and a cooling system; the I, II, III and IV grade distillation systems consist of a wiped film evaporator, a condenser, a finished product tank, a receiving tank and a back pressure valve, and the V grade distillation system consists of a wiped film evaporator, a condenser, a finished product tank and a receiving tank; the upper part of the side wall of the wiped film evaporator in each stage of distillation system is provided with a feed inlet, the top of the wiped film evaporator is provided with a steam outlet, and the steam outlet is connected with a finished product tank through a condenser; a concentrated solution outlet is arranged at the bottom of the wiped film evaporator; the concentrated solution outlet is connected with the receiving tank; the receiving tank is connected with the feed inlet of the next-stage wiped film evaporator through a back pressure valve; the raw material storage tank 7 is connected with the feed inlet of the wiped film evaporator of the I-stage distillation system through the feed pump 6.
The continuous purification method of 2-cyanoethyltrichlorosilane by using the device in example 1 comprises the following steps:
firstly, closing a stage I back pressure valve 1-5, raising the temperature of a stage I wiped film evaporator 1-1 of a stage I distillation system to 60 ℃, and introducing nitrogen into the stage I distillation system to enable the pressure in the stage I wiped film evaporator 1-1, a stage I receiving tank 1-2, a stage I condenser 1-3 and a stage I finished product tank 1-4 to reach 240 kPa; cooling water is introduced into the I-stage condenser 1-3;
starting a feeding pump 6, pumping 1200L of 2-cyanoethyl trichlorosilane crude product in a raw material storage tank 7 into a first-stage wiped film evaporator 1-1 at a flow rate of 200kg/h, distilling at the temperature of 60 ℃ and under the pressure of 240kPa, feeding distilled gaseous substances into a first-stage condenser 1-3 through a steam outlet for condensation, and feeding condensate into a first-stage finished product tank 1-4; obtaining front cut trichlorosilane; concentrated solution in the I-stage wiped film evaporator 1-1 flows into the I-stage receiving tank 1-2 through a concentrated solution outlet 1-1-3;
secondly, closing a II-stage back pressure valve 2-5, raising the temperature of a II-stage wiped film evaporator 2-1 of a II-stage distillation system to 60 ℃, and introducing nitrogen into the II-stage distillation system to raise the pressure in the II-stage wiped film evaporator 2-1, a II-stage receiving tank 2-2, a II-stage condenser 2-3 and a II-stage finished product tank 2-4 in the II-stage distillation system to 110 kPa; cooling water is introduced into the II-stage condenser 2-3;
opening a back pressure valve 1-5, pressing the concentrated solution in the I-stage receiving tank 1-2 into a II-stage wiped film evaporator 2-1 by utilizing pressure difference, distilling at the temperature of 60 ℃ and the pressure of 110kPa, feeding the distilled gaseous substance into a II-stage condenser 2-3 for condensation, and feeding the condensate into a II-stage finished product tank 2-4; obtaining front fraction silicon tetrachloride; concentrated solution in the II-stage wiped film evaporator 2-1 flows into the II-stage receiving tank 2-2 through a concentrated solution outlet, and after distillation is finished, a back pressure valve 1-5 is closed;
thirdly, closing a grade III back pressure valve 3-5, raising the temperature of a grade III wiped film evaporator 3-1 of a grade III distillation system to 80 ℃, and keeping the pressure in the grade III wiped film evaporator 3-1, a grade III receiving tank 3-2, a grade III condenser 3-3 and a grade III finished product tank 3-4 in the grade III distillation system at normal pressure; introducing cooling water into the III-grade condenser 3-3;
opening a back pressure valve 2-5, pressing the concentrated solution in the II-stage receiving tank 2-2 into a III-stage wiped film evaporator 3-1 by utilizing pressure difference, distilling at the temperature of 80 ℃ under normal pressure, feeding the distilled gaseous substance into a III-stage condenser 3-3 for condensation, and feeding the condensate into a III-stage finished product tank 3-4; obtaining front cut acrylonitrile; the concentrated solution in the III-grade wiped film evaporator 3-1 flows into a III-grade receiving tank 3-2 through a concentrated solution outlet, and after distillation is finished, a back pressure valve 2-5 is closed;
fourthly, closing the IV-stage back pressure valve 4-5, raising the temperature of the IV-stage wiped film evaporator 4-1 of the IV-stage distillation system to 80 ℃, connecting a vacuum system to enable the pressure in the IV-stage wiped film evaporator 4-1, the IV-stage receiving tank 4-2, the IV-stage condenser 4-3 and the IV-stage finished product tank 4-4 in the IV-stage distillation system to be pumped to-0.05 MPa; cooling water is introduced into the IV-stage condenser 4-3;
opening a back pressure valve 3-5, pressing the concentrated solution in the III-grade receiving tank 3-2 into an IV-grade wiped film evaporator 4-1 by utilizing differential pressure, carrying out reduced pressure distillation under the conditions that the temperature is 80 ℃ and the pressure is-0.05 MPa, feeding the distilled gaseous substance into an IV-grade condenser 4-3 for condensation, and feeding the condensate into an IV-grade finished product tank 4-4; obtaining front cut propionitrile; concentrated solution in the IV-stage wiped film evaporator 4-1 flows into an IV-stage receiving tank 4-2 through a concentrated solution outlet, and after distillation is finished, a back pressure valve 3-5 is closed;
fifthly, raising the temperature of a V-grade wiped film evaporator 5-1 of the V-grade distillation system to 110 ℃, connecting a vacuum system to ensure that the pressure in the V-grade wiped film evaporator 5-1, a V-grade receiving tank 5-2, a V-grade condenser 5-3 and a V-grade finished product tank 5-4 in the V-grade distillation system is pumped to-0.0098 MPa; introducing cooling water into the V-stage condenser 5-3;
opening a back pressure valve 4-5, pressing the concentrated solution in the IV-grade receiving tank 4-2 into a V-grade wiped film evaporator 5-1 by utilizing pressure difference, carrying out reduced pressure distillation under the conditions that the temperature is 110 ℃ and the pressure is-0.0098 MPa, feeding the distilled gaseous substances into a V-grade condenser 5-3 for condensation, and feeding the condensate into a V-grade finished product tank 5-4; obtaining 2-cyanoethyl trichlorosilane; the concentrated solution in the V-stage wiped film evaporator 5-1 flows into a V-stage receiving tank 5-2 through a concentrated solution outlet to obtain a high-boiling-point substance; closing the back pressure valve 4-5 after the distillation is finished; the purification of 2-cyanoethyltrichlorosilane is completed.
The yield of 2-cyanoethyl trichlorosilane is 79.58% by calculation, and the chromatographic purity of the purified 2-cyanoethyl trichlorosilane reaches 99.98%.
And (3) comparison test: the 1200L of the crude 2-cyanoethyltrichlorosilane product is injected into a distillation kettle, a stirring motor is started to rotate at the rotating speed of 200r/h, and the temperature of the distillation kettle is raised to 110 ℃. And opening a cooling circulating water system, maintaining the front-distillation condenser at-15 ℃, and opening a low-temperature oil system to maintain the fine condenser at 35 ℃. Opening a vacuum unit, stabilizing the pressure at-0.03 MPa, starting distillation, condensing the front fraction by a condenser, flowing into a front fraction receiving tank, reducing the pressure to-0.05 MPa after 1h, continuing distillation, switching the condenser to a fine product condenser after the distillation of the front fraction is finished, simultaneously continuously reducing the pressure to-0.1 MPa, starting the distillation of the 2-cyanoethyltrichlorosilane fine product, and finishing the distillation of the fine product after about 8h to obtain 2-cyanoethyltrichlorosilane fine product 756L, front fraction 133L and high-boiling-point substance 288L. The distillation yield of the 2-cyanoethyltrichlorosilane is only 63 percent, and the purity is 97.6 percent.
Comparing the results of example 1 and the comparative experiment, it is understood that the continuous purification of 2-cyanoethyltrichlorosilane using the apparatus of the present invention can improve not only the yield of 2-cyanoethyltrichlorosilane but also the purity of 2-cyanoethyltrichlorosilane, using the same crude product.
Example 2: the method for continuously purifying the 2-cyanoethyltrichlorosilane by using the device of the example 1 comprises the following steps:
firstly, closing a stage I back pressure valve 1-5, raising the temperature of a stage I wiped film evaporator 1-1 of a stage I distillation system to 62 ℃, and introducing nitrogen into the stage I distillation system to enable the pressure in the stage I wiped film evaporator 1-1, a stage I receiving tank 1-2, a stage I condenser 1-3 and a stage I finished product tank 1-4 to reach 245 kPa; cooling water is introduced into the I-stage condenser 1-3;
starting a feeding pump 6, pumping 1200L of 2-cyanoethyl trichlorosilane crude product in a raw material storage tank 7 into a first-stage wiped film evaporator 1-1 at a flow rate of 200kg/h, distilling at the temperature of 62 ℃ and under the pressure of 245kPa, feeding distilled gaseous substances into a first-stage condenser 1-3 through a steam outlet for condensation, and feeding condensate into a first-stage finished product tank 1-4; obtaining front cut trichlorosilane; concentrated solution in the I-stage wiped film evaporator 1-1 flows into the I-stage receiving tank 1-2 through a concentrated solution outlet 1-1-3;
secondly, closing a II-stage back pressure valve 2-5, raising the temperature of a II-stage wiped film evaporator 2-1 of a II-stage distillation system to 62 ℃, and introducing nitrogen into the II-stage distillation system to raise the pressure in the II-stage wiped film evaporator 2-1, a II-stage receiving tank 2-2, a II-stage condenser 2-3 and a II-stage finished product tank 2-4 in the II-stage distillation system to 115 kPa; cooling water is introduced into the II-stage condenser 2-3;
opening a back pressure valve 1-5, pressing the concentrated solution in the I-stage receiving tank 1-2 into a II-stage wiped film evaporator 2-1 by utilizing pressure difference, distilling at the temperature of 62 ℃ and the pressure of 115kPa, feeding the distilled gaseous substance into a II-stage condenser 2-3 for condensation, and feeding the condensate into a II-stage finished product tank 2-4; obtaining front fraction silicon tetrachloride; concentrated solution in the II-stage wiped film evaporator 2-1 flows into the II-stage receiving tank 2-2 through a concentrated solution outlet, and after distillation is finished, a back pressure valve 1-5 is closed;
thirdly, closing a grade III back pressure valve 3-5, raising the temperature of a grade III wiped film evaporator 3-1 of a grade III distillation system to 82 ℃, and keeping the pressure in the grade III wiped film evaporator 3-1, a grade III receiving tank 3-2, a grade III condenser 3-3 and a grade III finished product tank 3-4 in the grade III distillation system at normal pressure; introducing cooling water into the III-grade condenser 3-3;
opening a back pressure valve 2-5, pressing the concentrated solution in the II-stage receiving tank 2-2 into a III-stage wiped film evaporator 3-1 by utilizing pressure difference, distilling at the normal pressure at the temperature of 82 ℃, feeding the distilled gaseous substance into a III-stage condenser 3-3 for condensation, and feeding the condensate into a III-stage finished product tank 3-4; obtaining front cut acrylonitrile; the concentrated solution in the III-grade wiped film evaporator 3-1 flows into a III-grade receiving tank 3-2 through a concentrated solution outlet, and after distillation is finished, a back pressure valve 2-5 is closed;
fourthly, closing the IV-stage back pressure valve 4-5, raising the temperature of the IV-stage wiped film evaporator 4-1 of the IV-stage distillation system to 83 ℃, connecting a vacuum system to ensure that the pressure in the IV-stage wiped film evaporator 4-1, the IV-stage receiving tank 4-2, the IV-stage condenser 4-3 and the IV-stage finished product tank 4-4 in the IV-stage distillation system is pumped to-0.055 MPa; cooling water is introduced into the IV-stage condenser 4-3;
opening a back pressure valve 3-5, pressing the concentrated solution in the III-grade receiving tank 3-2 into an IV-grade wiped film evaporator 4-1 by utilizing differential pressure, carrying out reduced pressure distillation under the conditions that the temperature is 83 ℃ and the pressure is-0.05 MPa, feeding the distilled gaseous substance into an IV-grade condenser 4-3 for condensation, and feeding the condensate into an IV-grade finished product tank 4-4; obtaining front cut propionitrile; concentrated solution in the IV-stage wiped film evaporator 4-1 flows into an IV-stage receiving tank 4-2 through a concentrated solution outlet, and after distillation is finished, a back pressure valve 3-5 is closed;
fifthly, raising the temperature of a V-grade wiped film evaporator 5-1 of the V-grade distillation system to 115 ℃, connecting a vacuum system to ensure that the pressure in the V-grade wiped film evaporator 5-1, a V-grade receiving tank 5-2, a V-grade condenser 5-3 and a V-grade finished product tank 5-4 in the V-grade distillation system is pumped to-0.0098 MPa; introducing cooling water into the V-stage condenser 5-3;
opening a back pressure valve 4-5, pressing the concentrated solution in the IV-grade receiving tank 4-2 into a V-grade wiped film evaporator 5-1 by utilizing pressure difference, carrying out reduced pressure distillation under the conditions that the temperature is 115 ℃ and the pressure is-0.0098 MPa, feeding the distilled gaseous substances into a V-grade condenser 5-3 for condensation, and feeding the condensate into a V-grade finished product tank 5-4; obtaining 2-cyanoethyl trichlorosilane; the concentrated solution in the V-stage wiped film evaporator 5-1 flows into a V-stage receiving tank 5-2 through a concentrated solution outlet to obtain a high-boiling-point substance; closing the back pressure valve 4-5 after the distillation is finished; the purification of 2-cyanoethyltrichlorosilane is completed.
The yield of 2-cyanoethyltrichlorosilane is 79.67% by calculation, and the chromatographic purity of the purified 2-cyanoethyltrichlorosilane reaches 99.985%.
Claims (4)
1. A device for continuously purifying 2-cyanoethyl trichlorosilane is characterized by comprising a grade I distillation system (1), a grade II distillation system (2), a grade III distillation system (3), a grade IV distillation system (4), a grade V distillation system (5), a feeding pump (6) and a raw material storage tank (7);
the I, II, III and IV grade distillation systems consist of a wiped film evaporator, a condenser, a finished product tank, a receiving tank and a back pressure valve, and the V grade distillation system consists of a wiped film evaporator, a condenser, a finished product tank and a receiving tank;
the upper part of the side wall of the wiped film evaporator in each stage of distillation system is provided with a feed inlet, the top of the wiped film evaporator is provided with a steam outlet, and the steam outlet is connected with a finished product tank through a condenser; a concentrated solution outlet is arranged at the bottom of the wiped film evaporator; the concentrated solution outlet is connected with the receiving tank; the receiving tank is connected with the feed inlet of the next-stage wiped film evaporator through a back pressure valve;
a raw material storage tank (7) is connected with a feed inlet of a wiped film evaporator of the I-stage distillation system through a feed pump (6);
the apparatus also includes a nitrogen gas supply system, a vacuum system, and a cooling system.
2. The apparatus according to claim 1, wherein the inner wall of the wiped film evaporator and the scraper are made of phenolic glass fiber reinforced plastic.
3. The method for continuously purifying the 2-cyanoethyltrichlorosilane by using the device as claimed in claim 1, wherein the method comprises the following steps:
firstly, introducing nitrogen into a stage I distillation system to ensure that the pressure in the stage I distillation system reaches 240-250 kPa; then pumping the 2-cyanoethyl trichlorosilane crude product in the raw material storage tank into a first-stage wiped film evaporator, and distilling at the temperature of 60-65 ℃ and under the pressure of 240-250 kPa; the distilled gaseous substance enters a grade I condenser through a steam outlet for condensation, and the condensate flows into a grade I finished product tank; obtaining front cut trichlorosilane; the concentrated solution flows into a grade I receiving tank after distillation;
secondly, introducing nitrogen into the II-stage distillation system to enable the pressure in the II-stage distillation system to reach 110-120 kPa; pumping the concentrated solution in the I-stage receiving tank into a II-stage wiped film evaporator by utilizing differential pressure, and distilling at the temperature of 60-65 ℃ and under the pressure of 110-120 kPa; the distilled gaseous substance enters a first-stage condenser through a steam outlet for condensation, and the condensate flows into a second-stage finished product tank; obtaining front fraction silicon tetrachloride; the concentrated solution flows into a II-stage receiving tank after distillation;
keeping the pressure in the III-grade distillation system at normal pressure, pressing the concentrated solution in the II-grade receiving tank into the III-grade wiped film evaporator by utilizing differential pressure, and distilling at the normal pressure at the temperature of 80-85 ℃; the distilled gaseous substance enters a grade III condenser for condensation, and the condensate flows into a grade III finished product tank; obtaining front cut acrylonitrile; the concentrated solution flows into a grade III receiving tank after distillation;
pumping the pressure of an IV-grade distillation system to-0.05 to-0.06 MPa, pressing the concentrated solution in a III-grade receiving tank into an IV-grade wiped film evaporator by using differential pressure, carrying out reduced pressure distillation at the temperature of 80-85 ℃ and the pressure of-0.05 to-0.06 MPa, feeding the distilled gaseous substance into an IV-grade condenser for condensation, and feeding the condensate into an IV-grade finished product tank; obtaining front cut propionitrile; the distilled concentrated solution flows into an IV-grade receiving tank;
fifthly, pumping the pressure of the V-grade distillation system to-0.090 to-0.1 MPa, pressing the concentrated solution in the IV-grade receiving tank into the V-grade wiped film evaporator by utilizing pressure difference, carrying out reduced pressure distillation under the conditions that the temperature is 110 to 115 ℃ and the pressure is-0.090 to-0.1 MPa, feeding the distilled gaseous substances into a V-grade condenser for condensation, and feeding the condensate into a V-grade finished product tank; obtaining 2-cyanoethyl trichlorosilane; and (4) the distilled concentrated solution flows into a V-level receiving tank to obtain a high-boiling-point substance, so that the purification of the 2-cyanoethyl trichlorosilane is completed.
4. The method of claim 3, wherein the flow rate of the crude 2-cyanoethyltrichlorosilane in the first step is 200-220 kg/h.
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| CN1693192A (en) * | 2005-06-16 | 2005-11-09 | 中国有色工程设计研究总院 | Process for pressure purification of silicon trichlorohydrgen and apparatus thereof |
| CN101519206A (en) * | 2009-04-15 | 2009-09-02 | 山东齐泉硅业有限公司 | Process for purifying trichlorosilane and silicon tetrachloride |
| CN102234112A (en) * | 2010-09-30 | 2011-11-09 | 河南尚宇新能源股份有限公司 | Method for rectifying trichlorosilane |
| WO2015012257A1 (en) * | 2013-07-26 | 2015-01-29 | 株式会社 テクノ・バンダリー | Continuous-distillation-type trichlorosilane vaporization supply device and continuous-distillation-type trichlorosilane gas vaporization method |
| CN109482117A (en) * | 2018-11-13 | 2019-03-19 | 江西宏柏新材料股份有限公司 | The device and method of atmospheric distillation reaction production cyanoethyl alkoxy silane |
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| CN1693192A (en) * | 2005-06-16 | 2005-11-09 | 中国有色工程设计研究总院 | Process for pressure purification of silicon trichlorohydrgen and apparatus thereof |
| CN101519206A (en) * | 2009-04-15 | 2009-09-02 | 山东齐泉硅业有限公司 | Process for purifying trichlorosilane and silicon tetrachloride |
| CN102234112A (en) * | 2010-09-30 | 2011-11-09 | 河南尚宇新能源股份有限公司 | Method for rectifying trichlorosilane |
| WO2015012257A1 (en) * | 2013-07-26 | 2015-01-29 | 株式会社 テクノ・バンダリー | Continuous-distillation-type trichlorosilane vaporization supply device and continuous-distillation-type trichlorosilane gas vaporization method |
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