CN217535876U - Deep dechlorination system for dimethyl dichlorosilane hydrolysate - Google Patents
Deep dechlorination system for dimethyl dichlorosilane hydrolysate Download PDFInfo
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- CN217535876U CN217535876U CN202221355236.3U CN202221355236U CN217535876U CN 217535876 U CN217535876 U CN 217535876U CN 202221355236 U CN202221355236 U CN 202221355236U CN 217535876 U CN217535876 U CN 217535876U
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Abstract
The utility model discloses a degree of depth dechlorination system of dimethyl dichlorosilane hydrolysate, including hydrolysis unit and degasser, degasser's gas outlet is connected with the absorption tower through the blast pipe, degasser's liquid outlet has one-level washing device through first drain union coupling, second grade washing device and tertiary washing device, be provided with demineralized water import pipe on the tertiary washing device, the liquid outlet of tertiary washing device passes through the liquid inlet intercommunication of first back flow with second grade washing device, the liquid outlet of second grade washing device passes through the liquid inlet intercommunication of second back flow with the absorption tower, the liquid outlet of absorption tower passes through the liquid inlet intercommunication of second back flow with one-level washing device, be provided with the hydrochloric acid on the first washing device and supply the pipe, the liquid outlet of one-level washing device passes through the liquid inlet intercommunication of third back flow with the hydrolysis unit. The device not only can maintain the balance of the whole system and realize high-efficiency dechlorination, but also can realize high-efficiency recycling of the hydrochloric acid.
Description
Technical Field
The utility model relates to a deep-processing technical field of organosilicon by-product, concretely relates to degree of depth dechlorination system of dimethyl dichlorosilane hydrolysate.
Background
The organic silicon products are various in types and complex in production process, and are prepared by starting from raw materials such as silicon powder, chloromethane and the like, synthesizing methyl chlorosilane monomers through catalytic reaction, preparing various types of polymers through a series of chemical reactions such as hydrolysis, cracking, polymerization and the like, and further processing the polymers into different types of products. Methylchlorosilanes are one of the most important, and among them, dimethyldichlorosilane is hydrolyzed to form polymethylsiloxane, which is the most important intermediate in the silicone industry, and various silicone products can be prepared from the polymethylsiloxane. The hydrolysis process of methyl chlorosilane is the most important link in the production process of the organosilicon industry, and cyclic siloxane and linear siloxane which are hydrolysis products of methyl chlorosilane are important intermediates of a plurality of organosilicon products. At present, hydrolysis modes of the dimethyldichlorosilane mainly comprise saturated acid hydrolysis and unsaturated acid hydrolysis, and a large amount of hydrogen chloride can be recovered by utilizing the saturated acid hydrolysis, but because the primary hydrolysis reaction of the dimethyldichlorosilane adopts pressurized saturated hydrochloric acid for hydrolysis, the consumption of the hydrochloric acid is high, the operation cost is high, a large amount of acid water is discharged, the subsequent acid water treatment is heavy in burden and difficult; unsaturated acid is utilized for hydrolysis, the acid concentration is low, the dechlorination effect is not ideal, a large amount of energy consumption is required to be provided for the dissolution and heat release of hydrogen chloride, the obtained acid water cannot be recycled or is difficult to recycle, the phenomenon of acid discharge can occur, and the cost and the difficulty of wastewater treatment are still increased. Therefore, it is objectively needed to develop a stably controlled deep dechlorination system for dimethyldichlorosilane hydrolysate, which has reasonable structural design, stable operation, remarkable dechlorination effect and no waste water generation.
Disclosure of Invention
An object of the utility model is to provide a structural design is reasonable, the operation is stable, dechlorination effect is showing, the degree of depth dechlorination system of the dimethyldichlorosilane hydrolysate of the stable control that no waste water produced.
The utility model aims at realizing like this, including hydrolysis unit and degasser, degasser's gas outlet is connected with the absorption tower through the blast pipe, degasser's liquid outlet has connected gradually one-level washing device through first fluid-discharge tube, second grade washing device and tertiary washing device, be provided with the desalinized water import pipe on the tertiary washing device, tertiary washing device's liquid outlet is through the liquid inlet intercommunication of first back flow with second grade washing device, second grade washing device's liquid outlet is through the liquid inlet intercommunication of second back flow with the absorption tower, the liquid outlet of absorption tower is through the liquid inlet intercommunication of second back flow with one-level washing device, be provided with the hydrochloric acid additional pipe on the first washing device, the liquid outlet of one-level washing device passes through the liquid inlet intercommunication of third back flow with hydrolysis unit.
The system has the beneficial effects that: firstly, a primary washing device, a secondary washing device and a tertiary washing device are used for carrying out tertiary washing on the dimethyldichlorosilane hydrolysate, and after the tertiary washing, the viscosity of the dimethyldichlorosilane hydrolysate is improved, the chlorine content is reduced, and the product quality is effectively improved; when the primary washing device, the secondary washing device and the tertiary washing device are used, desalted water is supplemented to the tertiary washing device through a desalted water inlet pipe, fresh hydrochloric acid with the concentration of 31 percent by weight is supplemented to the primary washing device through a hydrochloric acid supplementing pipe, on one hand, the supplemented fresh hydrochloric acid can supplement water to the whole washing system, the water consumption and the water inflow are balanced, the balance of the whole system is maintained, on the other hand, the hydrochloric acid concentration in the primary washing device can be improved, and further, the hydrochloric acid concentration of the primary washing is stably controlled, so that the high-efficiency dechlorination of the dimethyldichlorosilane hydrolysate is realized, the hydrochloric acid after the primary washing is reused in the hydrolysis device, and the recovery rate of hydrogen chloride can be further improved; thirdly, the dilute hydrochloric acid that one-level washing device, second grade washing device and tertiary washing device washing produced all recycles whole washing system, and entire system can realize the high-efficient recovery and the recycle of hydrochloric acid, and the thorough solution the appearance that the sour water was arranged outward, the effectual cost that reduces the operation has the advantage that structural design is reasonable, the operation is stable, the chlorine dechlorination effect is showing, can produce better economic benefits, easily uses widely.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention;
in the figure: the method comprises the following steps of 1-a hydrolysis device, 2-a degassing device, 3-an exhaust pipe, 4-an absorption tower, 5-a first liquid discharge pipe, 6-a first-stage water washing device, 7-a second-stage water washing device, 8-a third-stage water washing device, 9-a desalted water inlet pipe, 10-a first return pipe, 11-a second return pipe, 12-a second liquid discharge pipe, 13-a hydrochloric acid supplement pipe, 14-a third return pipe, 15-a buffer tank, 16-a mixer, 17-a phase separator, 171-a liquid distribution pipe, 172-a separation filler component, 18-a circulation pipe and 19-a condenser.
Detailed Description
The following further describes the present invention with reference to the attached drawings, but the present invention is not limited in any way, and any changes or improvements based on the teaching of the present invention all belong to the protection scope of the present invention.
As shown in fig. 1, the utility model comprises a hydrolysis device 1 and a degassing device 2, the hydrolysis device 1 is used for hydrolyzing dimethyldichlorosilane monomer and hydrochloric acid, realizes the separation of dimethyldichlorosilane hydrolysate and hydrogen chloride gas, the degassing device 2 is used for carrying out secondary separation hydrogen chloride gas to dimethyldichlorosilane, the gas outlet of the degassing device 2 is connected with an absorption tower 4 through an exhaust pipe 3, the absorption tower 4 is used for absorbing the hydrogen chloride gas separated by the degassing device 2, the liquid outlet of the degassing device 2 is connected with a primary washing device 6, a secondary washing device 7 and a tertiary washing device 8 in sequence through a first liquid discharge pipe 5, the primary washing device 6, the secondary washing device 7 and the tertiary washing device 8 are used for washing the dimethyldichlorosilane hydrolysate, a desalted water inlet pipe 9 is arranged on the tertiary washing device 8, the desalted water entering the desalted water inlet pipe 9 used by the tertiary washing device 8 is used for washing the dimethyldichlorosilane, the liquid outlet of the tertiary washing device 8 is communicated with the liquid inlet of the secondary washing device 7 through a first backflow pipe 10, the liquid outlet of the secondary washing device 7 is communicated with the liquid inlet of the secondary washing device 6, the hydrochloric acid backflow pipe 13 is arranged on the tertiary washing device 7, the hydrochloric acid backflow pipe, the tertiary washing device 7 is communicated with a hydrochloric acid backflow pipe used by a hydrochloric acid backflow pipe, the absorption device 13, the absorption tower is communicated with a hydrochloric acid backflow pipe used by a hydrochloric acid backflow pipe 4, and a hydrochloric acid backflow pipe 4, a hydrochloric acid backflow pipe used by a hydrochloric acid backflow pipe 13, the primary washing device 6 uses the hydrochloric acid discharged from the absorption tower 4 and the fresh hydrochloric acid with the concentration of 31 percent by weight supplemented outside the hydrochloric acid supplementing pipe to wash the dimethyldichlorosilane, the primary washing device 6, the secondary washing device 7 and the tertiary washing device 8 are used, desalted water is supplemented to the tertiary washing device 8 through the desalted water inlet pipe 9, the fresh hydrochloric acid with the concentration of 31 percent by weight is supplemented to the primary washing device 6 through the hydrochloric acid supplementing pipe 13, the supplemented fresh hydrochloric acid can realize water supplementation to the whole washing system on the one hand, the water consumption and the water inflow are balanced, the whole system balance is maintained, on the other hand, the hydrochloric acid concentration in the primary washing device 6 can be improved, the hydrochloric acid concentration of washing primary can be further stably controlled, the efficient dechlorination of the dimethyldichlorosilane is realized, the hydrochloric acid after primary washing is recycled to the hydrolysis device 1, the recovery rate of hydrogen chloride can be further improved, meanwhile, the whole system can realize the efficient recovery and reutilization of the hydrochloric acid, the phenomenon of the hydrochloric acid is thoroughly solved, and the running cost is effectively reduced.
The working process of the system is as follows: the dimethyl dichlorosilane hydrolysate which is hydrolyzed by the hydrolysis device 1 and degassed and separated by the degassing device 2 enters the primary water washing device 1 through the first liquid discharge pipe 5, at the moment, the hydrochloric acid which enters through the second liquid discharge pipe 12 and 31 percent by weight of fresh hydrochloric acid which is supplemented outside the hydrochloric acid supplementing pipe 13 also enter the primary water washing device 1, the dimethyl dichlorosilane is subjected to primary water washing separation by utilizing the hydrochloric acid and the external fresh hydrochloric acid, the dilute hydrochloric acid separated by the primary water washing is recycled into the hydrolysis device 6 through the third return pipe 14, the dimethyl dichlorosilane hydrolysate which is separated by the primary water washing enters the secondary water washing device 2, at the moment, the dilute hydrochloric acid which enters through the first return pipe 10 also enters the secondary water washing device 7, utilizing dilute hydrochloric acid to carry out second-stage washing separation on the dimethyldichlorosilane hydrolysate, enabling dilute hydrochloric acid separated by the second-stage washing to enter the absorption tower 4 through the second return pipe 11, enabling the dimethyldichlorosilane hydrolysate separated by the second-stage washing to enter the third-stage washing device 8, enabling desalted water entering through a desalted water inlet pipe 9 to enter the third-stage washing device 8, utilizing the desalted water to carry out third-stage washing separation on the dimethyldichlorosilane hydrolysate, enabling the viscosity of the dimethyldichlorosilane hydrolysate separated by the third-stage washing to be 15-25 Cp, enabling the chlorine content to be 1-ppmwt, and enabling the dilute hydrochloric acid separated by the third-stage washing to enter the first return pipe 10.
Further, in order to improve the effect of the primary washing, the hydrochloric acid concentration in the primary washing device 6 is guaranteed to be balanced, the liquid inlet of the primary washing device 6 is provided with a buffer tank 15, a hydrochloric acid supplement pipe 13 is arranged on the buffer tank 15, the hydrochloric acid discharged from the absorption tower 4 by using the buffer tank 15 and the fresh hydrochloric acid which is supplemented from the hydrochloric acid supplement pipe 13 and has the concentration of 31 percent wt are mixed to adjust the concentration, and then the hydrochloric acid enters the primary washing device 6, so that the dechlorination effect of the primary washing can be improved, the hydrogen chloride separation efficiency of the hydrolysis device 1 can be improved, and the recovery efficiency of the hydrogen chloride is enhanced.
Further, the first-stage water washing device 6, the second-stage water washing device 7 and the third-stage water washing device 8 all comprise a mixer 16 and a phase separator 17 which are sequentially arranged. The mixer 16 is used for mixing the dimethyldichlorosilane hydrolysate with hydrochloric acid or desalted water, the phase separator 17 is used for separating oil from water of the dimethyldichlorosilane hydrolysate, and the mixer 16 is a pipeline mixer, a stirred tank mixer or a static mixer. A liquid distribution pipe 171 and a separation packing assembly 172 are sequentially arranged in the phase separator 17 along the liquid inlet and liquid outlet directions
Preferably, liquid distribution pipe 171 is responsible for and many evenly distributed liquid distribution pipes on the liquid inlet is responsible for including the vertical liquid inlet that arranges, and liquid distribution pipe horizontal installation is responsible for at the liquid inlet, and the tip of liquid inlet is responsible for and liquid distribution pipe is sealed, and the equipartition is provided with a plurality of liquid holes in every liquid inlet is responsible for. The liquid distribution pipe 171 can further distribute the flow of the dimethyldichlorosilane and hydrochloric acid mixture, and serves to buffer the mixture feed for uniform distribution.
Preferably, the separation packing assembly 172 comprises a plurality of baffle plates which are vertically and alternately arranged in the phase separator 17, the diameter of each baffle plate is larger than the diameter of the phase separator 17, the radius of each baffle plate is smaller than that of the phase separator 17, a packing layer is arranged between every two adjacent baffle plates, and a mixture of dimethyldichlorosilane and hydrochloric acid sequentially passes through the packing layers in a curved flow channel formed by the baffle plates, so that the contact area of the mixture and the packing layers is effectively increased, the time of oil-water separation is prolonged, the oil-water separation is fully realized, and after the separation of the packing layers, the oil-water separation is realized, and the dechlorinated dimethyldichlorosilane hydrolysate floats above the hydrochloric acid. The filler of packing layer adopts not trompil buckled plate filler, and thereby the mixture passes through not trompil buckled plate filler, thereby the dispersed phase can fully collide, coalesce and reach the purpose of oil-water stratification, improves oil-water separation efficiency.
In order to control the concentration of hydrochloric acid entering the primary water washing device 6 and improve the washing dechlorination effect, the second liquid discharge pipe 12 is provided with a circulating pipe 18 communicated with the absorption tower 4, the circulating pipe 18 is provided with a condenser 19, chilled water with the temperature below-15 ℃ is introduced into the condenser 19, and the chilled water is used for circularly condensing the dilute hydrochloric acid with the increased concentration returned to the absorption tower 4, so that the temperature stability of the dilute hydrochloric acid returned to the absorption tower 4 can be ensured, the temperature stability of washing absorption in the absorption tower 4 can be further ensured, and the washing absorption effect of hydrogen chloride gas can be improved.
Claims (9)
1. The deep dechlorination system of the dimethyl dichlorosilane hydrolysate comprises a hydrolysis device (1) and a degassing device (2), and is characterized in that: the gas outlet of degasser (2) is connected with absorption tower (4) through blast pipe (3), the liquid outlet of degasser (2) has connected gradually one-level washing device (6), second grade washing device (7) and tertiary washing device (8) through first drain pipe (5), be provided with demineralized water import pipe (9) on tertiary washing device (8), the liquid outlet of tertiary washing device (8) is through the liquid inlet intercommunication of first back flow (10) with second grade washing device (7), the liquid outlet of second grade washing device (7) is through the liquid inlet intercommunication of second back flow (11) with absorption tower (4), the liquid outlet of absorption tower (4) is through the liquid inlet intercommunication of second drain pipe (12) with one-level washing device (6), be provided with hydrochloric acid on one-level washing device (6) and supply pipe (13), the liquid outlet of one-level washing device (6) is through the liquid inlet intercommunication of third back flow (14) with hydrolysis unit (1).
2. The deep dechlorination system of dimethyldichlorosilane hydrolysate according to claim 1, wherein: a buffer tank (15) is arranged at a liquid inlet of the primary water washing device (6), and the hydrochloric acid supplementing pipe (13) is arranged on the buffer tank (15).
3. The deep dechlorination system of dimethyldichlorosilane hydrolysate according to claim 1, wherein: one-level washing device (6), second grade washing device (7) and tertiary washing device (8) all include blender (16) and phase separator (17) that set gradually.
4. The deep dechlorination system of dimethyldichlorosilane hydrolysate according to claim 3, wherein: the mixer (16) is a pipeline mixer, a stirred tank mixer or a static mixer.
5. The deep dechlorination system of dimethyldichlorosilane hydrolysate according to claim 3, wherein: and a liquid distribution pipe (171) and a separation packing component (172) are sequentially arranged in the phase separator (17) along the liquid inlet and liquid outlet directions.
6. The deep dechlorination system of dimethyldichlorosilane hydrolysate according to claim 5, wherein: liquid distribution pipe (171) are responsible for and many evenly distributed liquid distribution pipes on the liquid inlet is responsible for including the vertical liquid inlet that arranges, and the liquid inlet is responsible for and the tip of liquid distribution pipe is sealed, and every liquid inlet is responsible for and is gone up the equipartition and is provided with a plurality of liquid holes.
7. The deep dechlorination system of dimethyldichlorosilane hydrolysate according to claim 5, wherein: the separation packing assembly (172) comprises a plurality of baffle plates which are arranged in the phase separator (17) in an up-and-down staggered mode, the diameter of each baffle plate is larger than that of the phase separator (17) and smaller than that of the phase separator (17), and a packing layer is arranged between every two adjacent baffle plates.
8. The deep dechlorination system of dimethyldichlorosilane hydrolysate according to claim 7, wherein: the filler of the filler layer is corrugated plate filler without holes.
9. The deep dechlorination system of dimethyldichlorosilane hydrolysate according to claim 1, wherein: and a circulating pipe (18) communicated with the absorption tower (4) is arranged on the second liquid discharge pipe (12), and a condenser (19) is arranged on the circulating pipe (18).
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| Application Number | Priority Date | Filing Date | Title |
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| CN202221355236.3U CN217535876U (en) | 2022-06-01 | 2022-06-01 | Deep dechlorination system for dimethyl dichlorosilane hydrolysate |
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| CN202221355236.3U CN217535876U (en) | 2022-06-01 | 2022-06-01 | Deep dechlorination system for dimethyl dichlorosilane hydrolysate |
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