CN115945144A - Methyl chloride synthesis and siloxane recovery device and method for organic silicon - Google Patents
Methyl chloride synthesis and siloxane recovery device and method for organic silicon Download PDFInfo
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Abstract
The invention belongs to the field of methyl chloride synthesis in the organosilicon industry, and particularly relates to a methyl chloride synthesis and siloxane recovery device and method for organosilicon. The methyl chloride synthesis and siloxane recovery device provided by the invention comprises a methyl chloride synthesis reactor, wherein a gas-phase methanol inlet and a crude hydrogen chloride inlet are formed in one side of the methyl chloride synthesis reactor; the other side is provided with a siloxane outlet; an oleic acid separation component is arranged inside the oil tank; the bottom is provided with a circulating washing liquid outlet; the top is provided with a spraying facility and a washing facility, and is also provided with a circulating washing pump, and the circulating washing liquid outlet and the hydrogen chloride replenishing pipeline are connected with the spraying facility through the circulating washing pump to form a circulating loop. The device has simple structure and low operation cost, can recover siloxane carried in hydrogen chloride, improves the conversion rate of the hydrogen chloride and methanol, and simultaneously prolongs the operation period of methyl chloride synthesis.
Description
Technical Field
The invention relates to the organosilicon industry, in particular to a chloromethane synthesis and siloxane recovery device and method for organosilicon.
Background
The organosilicon generally refers to a large class of compounds containing silicon-carbon bonds or silicon-oxygen, silicon-sulfur bonds and the like in organosilicon products, and is an important component of the chemical high-performance new material industry, wherein the upstream is a basic chemical raw material such as metallic silicon, hydrogen chloride, methanol, chloromethane and the like, and the downstream products are mainly three classes of silicone oil, silicone resin, special organosilicon products and the like. Due to the characteristics of organic polymers and inorganic polymers, the monosodium glutamate has many unique characteristics in performance, has many excellent properties such as high temperature resistance, low temperature resistance, weather aging resistance, electrical insulation, physiological inertia and the like, and has a very wide application range, and the summary of the industrial monosodium glutamate is best explained. The development of the domestic organic silicon industry is rapid due to the benefit of new energy and the economic target of 'double carbon'.
The hydrogen chloride in the upstream raw material of the organic silicon is mainly obtained by hydrolyzing dimethyl dichlorosilane with concentrated acid, and due to the characteristics of a hydrolysis process, the generated hydrogen chloride can carry oily liquid drops containing siloxane in the actual production. The partial hydrogen chloride enters the chloride synthesis device, which not only causes material waste, but also causes the problems of reduced activity of reaction catalyst, system blockage, shortened operation period and the like due to the siloxane entering the methyl chloride synthesis device. On the other hand, the industry generally adopts a liquid phase catalysis method to produce methyl chloride, the HCl conversion rate of the process is low, a large amount of dilute acid is generated to cause the processing difficulty, and the HCl conversion rate is about 90 to 95 percent; excessive HCl can reduce the generation of byproducts but greatly inhibit the conversion rate of HCl, generate more waste acid and even need to wash unreacted HCl in the synthesis gas by alkali liquor in a post system, and the economic operation of the device is influenced by the existence of the problems.
The synthesis of methyl chloride by the reaction of hydrogen chloride and methanol is an exothermic reaction, and the problem that the system is blocked and the like is easily caused due to impurities carried in the hydrogen chloride, so that the reaction heat cannot be effectively utilized, and the reaction temperature is controlled by generally adopting a mode of condensing a refrigerant and then refluxing into a reactor in the industry, thereby causing heat loss. At present, a plurality of devices or methods for synthesizing methyl chloride by hydrogen chloride and methanol liquid-phase catalysis exist, but the current devices and methods have various problems, and are not ideal and suitable for the aspects of siloxane material recycling, siloxane-containing waste acid generation, siloxane-containing hydrogen chloride and methanol conversion rate, energy effective utilization and the like.
In order to solve the above problems in the prior art, the following different technical means are mainly adopted:
the preparation of methyl chloride from hydrogen chloride (gas) and methanol is described in patent EP0428166A1, however, the siloxane in the hydrogen chloride used is not discussed.
Patent CN111892479 a discloses a method and apparatus for increasing the primary conversion rate of methanol in synthetic methyl chloride, in which hydrogen chloride gas, methanol and high temperature catalyst solution are added into an ejector to obtain reaction fluid, but the patent still has the problem that siloxane is mixed in hydrogen chloride and enters a chloride synthesis apparatus.
Patent CN113896613A discloses a method and apparatus for synthesizing methyl chloride, the method is: taking gaseous hydrogen chloride, preheated hydrochloric acid solution and preheated gaseous methanol as raw materials, introducing the raw materials into a first reaction kettle for synthesis reaction, and adjusting the ratio of the hydrochloric acid solution in the raw materials and/or the preheating temperature of the hydrochloric acid solution and/or the preheating temperature of the gaseous methanol according to the reaction temperature in the first reaction kettle in the reaction process; hydrochloric acid solution is added into a second reaction kettle, the mixed gas of methyl chloride, hydrogen chloride and methanol at the outlet of the first reaction kettle is introduced into the second reaction kettle, and liquid methanol is introduced for synthesis reaction.
Therefore, in order to solve the above-mentioned problems in methyl chloride synthesis in the organosilicon industry, there is a need to develop a low-cost, efficient and energy-saving methyl chloride synthesis apparatus or method.
Disclosure of Invention
Aiming at the defects of the prior art, particularly the problem of low primary conversion rate of hydrogen chloride, the invention firstly provides the problem that siloxane impurities in the hydrogen chloride influence the conversion rate of the hydrogen chloride, and provides a device and a method for synthesizing organic silicon by using methyl chloride and recovering siloxane.
A methyl chloride synthesis and siloxane recovery device for organic silicon comprises a methyl chloride synthesis reactor and a hydrogen chloride supplement pipeline, wherein a gas-phase methanol inlet and a crude hydrogen chloride inlet are formed in one side of the methyl chloride synthesis reactor; the other side is provided with a siloxane outlet; an oleic acid separation component is arranged inside the oil tank; the top is provided with a gas phase outlet.
The bottom of the methyl chloride synthesis reactor, which is close to the outlet side of siloxane, is provided with a circulating washing liquid outlet, and the circulating washing liquid outlet and a hydrogen chloride replenishing pipeline are respectively connected with the inlet end of a circulating washing pump. And the outlet end of the circulating washing pump is connected with the gas phase outlet to form a circulating loop.
And a spraying facility is arranged at the gas phase outlet, and a washing facility is arranged below the spraying facility. The gas-phase methanol inlet and the crude hydrogen chloride inlet are connected with a gas mixing device and used for mixing methanol gas and crude hydrogen chloride gas.
The gas mixing device is connected with a feeding distribution pipe, the length of the feeding distribution pipe accounts for 1/3~1/2 of the length of the methyl chloride synthesis reactor, and the feeding distribution pipe is provided with small injection holes with the diameter of 1-3mm.
In order to ensure the conversion rate of hydrogen chloride and methanol and reduce the entrainment of outlet liquid phase siloxane, the height of the washing facility is 20 to 50 times of the diameter of the washing facility;
preferably, the height of the washing facility is 30 to 50 times of the diameter of the washing facility.
The washing facility comprises cross flow tower plates and oblique flow tower plates, the number ratio of the cross flow tower plates to the oblique flow tower plates is (2~1): 1, and the included angle between the oblique flow tower plates and the inner wall of the washing facility is 110-130 degrees;
in order to improve the layering effect of the washed oil, the bottom of the washing facility is provided with the oblique flow baffle, so that the influence of fluid disturbance on the separation of the oleic acid is reduced.
Preferably, two sets of oleic acid separation components, namely a first oleic acid separation component and a second oleic acid separation component, are arranged in the methyl chloride synthesis reactor and are used for separating siloxane (oil phase) and hydrogen chloride.
The oleic acid separation assembly comprises a packing gasket and a packing plate;
the filler plate is inclined downwards, and the included angle between the filler plate and the axial lead of the filler gasket is 30 to 70 degrees; preferably, the included angle between the axial lead of the filler plate and the axial lead of the filler gasket is 45 to 60 degrees. When the included angle is too small, the liquid flow resistance is too large, and the liquid flow is limited; when the included angle is too large, the liquid is not easy to coalesce, and the separation effect is poor.
The lower surface of the filler plate is made of a hydrophilic material, and preferably, the hydrophilic material is ethylene-tetrafluoroethylene copolymer (ETFE) with hydrophilic and oleophobic properties after surface treatment.
The packing gasket is of a hollow structure.
The separation principle of the oleic acid separation component is as follows: the oleic acid mixed phase enters the oleic acid separation component along the vertical direction of the axial lead of the packing gasket, the acid phase is wetted and coalesced on the lower surface of the packing plate and sinks under the action of gravity to be separated from the oil phase, and then the oleic acid mixed phase flows out of the oleic acid separation component in a state that the upper layer is the oil phase and the lower layer is the acid phase.
The oleic acid separation component is made of materials suitable for high temperature of over 155 ℃ and has acid corrosion resistance;
preferably, the packing gasket is made of polytetrafluoroethylene.
In order to guarantee the operation period, a first liquid purging port is arranged right below the first oleic acid separation assembly, and a second liquid purging port is arranged right below the second oleic acid separation assembly. The first liquid purging port and the second liquid purging port are respectively connected with the outlet end of the circulating washing pump, so that the mixed liquid of the supplemented hydrogen chloride solution and the circulating washing liquid purges the oleic acid separation assembly.
The gas phase outlet is arranged at the gas phase methanol inlet side, and the distance between the gas phase outlet and the first oleic acid separation assembly is 0.2-0.5 m in order to reduce the influence on the oleic acid separation assembly; preferably, the distance between the gas phase outlet and the first oleic acid separation component is 0.3-0.5 m.
Preferably, the siloxane outlet is positioned at a height of 2/3~4/5 of the methyl chloride synthesis reactor, and if the height of the siloxane outlet is too high, the liquid level is too high to easily entrain siloxane impurities.
Preferably, the spraying facility comprises a spraying facility fixing structure, a dry-type pipe and a nozzle;
the number of the nozzles is 6-10, the nozzle vertical drop is 8-15mm, and the flow of each nozzle is 0.3-1m 3 The material is PVC.
The nozzle is a solid cone spiral nozzle, and the spraying angle is 90 degrees.
The invention also provides a method for synthesizing organic silicon by using methyl chloride and recovering siloxane, which comprises the following steps:
a. adding crude hydrogen chloride gas, methanol gas and a catalyst solution to carry out methyl chloride synthesis reaction to obtain synthesis gas;
b. spraying and washing the synthesis gas, and recovering chlorosilane;
c. the hydrogen chloride solution was replenished.
The feeding temperature of the crude hydrogen chloride gas and the methanol gas in the step a is 90-150 ℃, and the volume ratio of the crude hydrogen chloride gas to the methanol gas is 1-1.3; preferably, the volume ratio of the crude hydrogen chloride gas to the methanol gas is 1.05 to 1.1.
In the step a, the reaction temperature of the synthesis reaction is 120-165 ℃, and the reaction pressure is 0.1-0.25Mpa.
The catalyst solution is a zinc chloride solution, and the mass fraction of the zinc chloride solution is 40 to 65 percent;
after the catalyst solution is added, controlling the liquid level in the reaction container to be 40-80% of the height of the reaction container; preferably, the liquid level in the reaction container is controlled to be 60% -80% of the height of the reaction container.
In the step b, the spraying temperature is controlled to be 90-110 ℃, the control of the reaction temperature is not facilitated due to overhigh temperature, and the blockage of the tray is caused due to the crystallization of siloxane in the tower caused by overlow temperature.
Mixing the supplemented hydrogen chloride solution and the circulating washing liquid in the step c to obtain a mixed liquid, wherein 2-10% of the flow of the mixed liquid is used for blowing the oleic acid separation assembly; the remainder is used to scrub the syngas.
The mass fraction of the supplemented hydrogen chloride solution is 25-30%. The supplemented hydrogen chloride solution can fully utilize reaction heat release, the released heat is used for carrying out hydrogen chloride analysis on the supplemented hydrogen chloride solution, the analyzed hydrogen chloride participates in the reaction again, and moisture in the solution is discharged out of the system along with the reaction gas. The flow of the supplementary hydrogen chloride solution is adjusted according to the temperature of the reactor, and the heat released by the reaction is controlled, so that the aim of controlling the spraying temperature is fulfilled.
The method comprises the steps that a catalyst solution enters a methyl chloride synthesis reactor through a hydrogen chloride supplement pipeline, crude hydrogen chloride gas containing siloxane and methanol gas enter a gas mixing device to be mixed, then the mixture enters the methyl chloride synthesis reactor, the reaction is carried out under the catalytic action of the catalyst solution to obtain synthesis gas (methyl chloride, methanol and hydrogen chloride), then the synthesis gas enters a washing facility, methanol and hydrogen chloride in the synthesis gas are removed after washing, washing liquid rich in hydrogen chloride and methanol enters the methyl chloride synthesis reactor again to participate in the reaction, meanwhile, the mass fraction of the supplementary hydrogen chloride solution added into the washing liquid is 25% -30%, the supplementary hydrogen chloride solution can be analyzed by reaction heat, and silicon oxygen impurities in the methyl chloride synthesis reactor pass through an oleic acid separation assembly and then are recovered through a siloxane outlet. The hydrogen chloride solution supplemented through the hydrogen chloride supplement pipeline is mixed with the circulating washing liquid flowing out of the circulating washing liquid outlet to obtain a mixed liquid, and a part of the mixed liquid enters the methyl chloride synthesis reactor through a spraying facility to participate in reaction; the other part of mixed liquor sweeps first oleic acid separation module and second oleic acid separation module through first liquid sweep mouth and second liquid sweep mouth respectively, prolongs the live time of oleic acid separation module.
Compared with the prior art, the invention has the following beneficial effects:
1. the inventor discovers the influence of impurities of siloxane in hydrogen chloride on the conversion rate of the hydrogen chloride in the synthesis process of the methyl chloride for the first time, and the oleic acid separation component and the circulating washing system adopted by the device act together to improve the conversion rate of the hydrogen chloride: after unreacted hydrogen chloride in the methyl chloride synthesis reactor is separated by the oleic acid separation component, the siloxane is timely removed out of the methyl chloride synthesis reactor, the purity of the hydrogen chloride is improved, and meanwhile, the unreacted hydrogen chloride enters the methyl chloride synthesis reactor for reaction through the circulating washing system, so that the conversion rate of the hydrogen chloride is improved.
2. The device is additionally provided with the liquid blowing port, and the oleic acid separation component can be blown by part of the circulating washing liquid through the liquid blowing port, so that the service time of the oleic acid separation component can be prolonged, and meanwhile, the blowing liquid is the circulating washing liquid, so that the recycling is realized, and the material consumption is reduced.
3. The device provided by the invention is provided with a hydrogen chloride supplementing pipeline and a circulating washing system, and supplies washing liquid for the synthesis gas so as to remove methanol and hydrogen chloride in the synthesis gas and improve the recovery rate of methanol; meanwhile, the washed methanol and the washed hydrogen chloride enter the methyl chloride synthesis reactor again along with the washing liquid to participate in the reaction, so that the conversion rate of the hydrogen chloride and the methanol is improved.
4. The device provided by the invention is provided with a hydrogen chloride replenishing pipeline, and fully utilizes reaction heat to provide heat for analysis of the hydrogen chloride.
5. The device provided by the invention has the advantages of low energy consumption and low cost, and efficiently solves the problems of short operation period, low conversion rate and the like in the chloromethane synthesis process in the organic silicon production process.
Drawings
FIG. 1 is a schematic diagram of the apparatus of the present invention;
FIG. 2 is a schematic longitudinal sectional view of a spray facility;
FIG. 3 is a schematic cross-sectional view of a spray installation;
FIG. 4 is a schematic view of an oleic acid separation module;
wherein, 1 is a chloromethane synthesis reactor; 2 is a gas phase methanol inlet; 3 is a crude hydrogen chloride inlet; 4 is a gas mixing device; 5 is a first liquid purge port; 6 is a second liquid purging port; 7 is a circulating washing liquid outlet; 8 is a circulating washing pump; 9 is a hydrogen chloride replenishing pipeline; 10 is a siloxane outlet; 11 is a second oleic acid separation module; 12 is a first oleic acid separation module; 13 is a washing facility; 14 is a spraying facility; 15 is an oblique flow baffle; 16 is a feed distribution pipe; 12-1 is a packing gasket; 12-2 filler plates; 14-1 is a spiral nozzle; 14-2 is a fixed structure of a spraying facility; 14-3 are "dry" type tubes.
Detailed Description
Example 1
The device adopted in the embodiment is a methyl chloride synthesis and siloxane recovery device for organic silicon, and comprises a methyl chloride synthesis reactor 1 as shown in fig. 1, wherein a gas-phase methanol inlet 2 and a crude hydrogen chloride inlet 3 are arranged on one side of the methyl chloride synthesis reactor 1. The gas-phase methanol inlet 2 and the crude hydrogen chloride inlet 3 are connected with a gas mixing device 4 and are used for mixing methanol gas and crude hydrogen chloride gas. The gas mixing device 4 is connected with a feed distribution pipe 16, the length of the feed distribution pipe 16 accounts for 1/3 of that of the methyl chloride synthesis reactor, and the feed distribution pipe 16 is provided with small injection holes with the diameter of 2 mm.
The other side of the methyl chloride synthesis reactor 1 is provided with a siloxane outlet 10, and the siloxane outlet 10 is arranged at the height of 4/5 of the methyl chloride synthesis reactor 1.
Two oleic acid separation components, namely a first oleic acid separation component 12 and a second oleic acid separation component 11, are arranged in the methyl chloride synthesis reactor 1; in order to ensure the operation period, a first liquid purging port 5 and a second liquid purging port 6 are respectively arranged right below the two oleic acid separation assemblies; the oleic acid separation assembly comprises a packing gasket 12-1 and a packing plate 12-2, in order to improve the oleic acid separation efficiency, the packing plate 12-2 is inclined downwards, an included angle between the axial line of the packing plate 12-2 and the axial line of the packing gasket 12-1 is 50 degrees, as shown in fig. 4, the oleic acid separation assembly is made of polytetrafluoroethylene, the width of the packing plate 12-2 is 140mm, the stacking height between the packing plates 12-2 is 21mm, and the lower surface of the packing plate 12-2 is made of ETFE (F-40).
The top of the methyl chloride synthesis reactor 1 is provided with a gas phase outlet, the distance between the gas phase outlet and the first oleic acid separation component 12 is 0.5m, the gas phase outlet is provided with a spraying facility 14, a washing facility 13 is arranged below the spraying facility 14, and the bottom of the washing facility 13 is provided with an oblique flow baffle 15. The washing facility 13 comprises cross flow trays and inclined flow trays, the number ratio of the cross flow trays to the inclined flow trays is 1.5, and the angle between the inclined flow trays and the inner wall of the washing facility 13 is 120 degrees. A spraying facility 14 is arranged on the washing facility 13, the spraying facility 14 comprises 3 dry type pipes 14-3 and a spraying facility fixing structure 14-2, and the dry type pipes 14-3 are provided with two rows of parallel nozzles as shown in fig. 3; the nozzle is a solid cone spiral nozzle 14-1, as shown in fig. 2, the spiral nozzle 14-1 is made of PVC, the number of the nozzles is 15, the diameter of the nozzles is 8mm, and the flow rate of each nozzle is 1m 3 /h。
The bottom of the chloromethane synthesis reactor 1 at the side of the siloxane outlet 10 is provided with a circulating washing liquid outlet 7; the circulating washing liquid outlet 7 and the hydrogen chloride replenishing pipeline 9 are respectively connected with the inlet end of a circulating washing pump 8, and the outlet end of the circulating washing pump 8 is respectively connected with a spraying facility 14, a first liquid purging port 5 and a second liquid purging port 6.
The method for synthesizing the organic silicon by using the chloromethane and recovering the siloxane in the embodiment comprises the following steps:
a. 1834m 3 Crude hydrogen chloride gas,/h 1667m 3 The methanol gas is respectively added into a gas mixing device 4 through a crude hydrogen chloride inlet 3 and a gas phase methanol inlet 2, mixed and then enters a methyl chloride synthesis reactor 1 through a feeding distribution pipe 16, and the volume of the methyl chloride synthesis reactor is 45m 3 Adding zinc chloride solution with mass fraction of 60% through a recycle pump inlet hydrogen chloride make-up pipeline 9, and carrying out chlorine treatment at reaction temperature of 155 ℃ and reaction pressure of 0.1MPaPerforming methane synthesis reaction to obtain synthesis gas;
b. the synthesis gas enters a washing facility 13, after washing, methanol and hydrogen chloride in the synthesis gas are absorbed by washing liquid, and the washing liquid rich in hydrogen chloride and methanol enters the methyl chloride synthesis reactor 1 again to participate in reaction; siloxane in the hydrogen chloride gas passes through the first oleic acid separation component 12 and the second oleic acid separation component 11 and then is recovered through a siloxane outlet 10;
c. a supplementary hydrogen chloride solution with the mass fraction of 25% is added through a hydrogen chloride supplementary pipeline 9, and the supplementary hydrogen chloride solution is mixed with the circulating washing liquid to obtain a mixed liquid for washing the synthesis gas and purging the oleic acid separation assembly.
The conversion rate of hydrogen chloride is kept at 96% in the reaction process, the conversion rate of methanol is 99.5%, no waste acid is generated basically in the reaction process, and entrained siloxane can be effectively recovered.
Example 2
In this example, the volume ratio of the crude hydrogen chloride gas to the methanol gas was 1.05, the mass fraction of the supplemented hydrogen chloride solution was 30%, and the rest was the same as in example 1.
The conversion rate of hydrogen chloride is kept to be 98.5 percent and the conversion rate of methanol is 99.5 percent in the reaction process, no waste acid is generated basically in the reaction process, and the entrained siloxane can be effectively recovered.
Example 3
The volume ratio of the crude hydrogen chloride gas to the methanol gas in the present example was 1.3, the mass fraction of the supplemented hydrogen chloride solution was 30%, and the rest was the same as in example 1.
The conversion rate of hydrogen chloride is kept at 96% in the reaction process, the conversion rate of methanol is 99.5%, no waste acid is generated basically in the reaction process, and entrained siloxane can be effectively recovered.
Example 4
The present embodiment is the same as embodiment 1 except that the shower facility 14 and the washing facility 13 are not provided.
In the reaction process, the conversion rate of the hydrogen chloride is kept to be 92 percent, the conversion rate of the methanol is 94 percent, no waste acid is generated basically in the reaction process, and the entrained siloxane can be effectively recovered.
Example 5
The present embodiment is the same as embodiment 1 except that the oblique flow baffle 15 is not provided.
In the reaction process, the conversion rate of hydrogen chloride is kept at 93%, the conversion rate of methanol is 95%, no waste acid is generated basically in the reaction process, and the entrained siloxane part can be effectively recovered.
Comparative example 1
This comparative example was the same as example 1 except that no oleic acid separation module was provided.
During the reaction, the conversion rate of hydrogen chloride is kept at 90%, the conversion rate of methanol is 92%, waste acid is generated during the reaction, and entrained siloxane can not be effectively recovered.
Claims (10)
1. A methyl chloride synthesizing and siloxane recovering device for organic silicon, which is characterized in that,
the device comprises a methyl chloride synthesis reactor (1) and a hydrogen chloride solution replenishing pipeline (9);
a gas-phase methanol inlet (2) and a crude hydrogen chloride inlet (3) are arranged on one side of the chloromethane synthesis reactor (1); the other side is provided with a siloxane outlet (10); an oleic acid separation component is arranged inside the oil tank; the top is provided with a gas phase outlet;
the bottom of methyl chloride synthesis reactor (1) near siloxane export (10) side sets up circulation washing liquid export (7), hydrogen chloride make-up pipeline (9) are connected with the entry end of circulation scrubbing pump (8) respectively, the exit end and the gaseous phase exit linkage of circulation scrubbing pump (8), form circulation circuit.
2. The apparatus for synthesizing methyl chloride and recovering siloxane from organosilicon according to claim 1,
a spraying facility (14) is arranged at the gas phase outlet, and a washing facility (13) is arranged below the spraying facility (14);
the washing means (13) comprise cross-flow trays and inclined-flow trays,
the number ratio of the cross flow trays to the inclined flow trays is (2~1) to 1,
the included angle between the inclined flow tower plate and the inner wall of the washing facility (13) is 110-130 degrees.
3. The apparatus for synthesizing methyl chloride and recovering siloxane from organosilicon according to claim 1,
two sets of oleic acid separating assemblies are arranged in the methyl chloride synthesis reactor (1), and each oleic acid separating assembly comprises: a first oleic acid separation component (12) and a second oleic acid separation component (11);
the oleic acid separation component comprises a packing gasket (12-1) and a packing plate (12-2);
the filler plate (12-2) is inclined downwards, and the included angle between the axial lead of the filler plate (12-2) and the axial lead of the filler gasket (12-1) is 30-70 degrees;
the lower surface of the filler plate (12-2) is made of hydrophilic material;
the packing gasket (12-1) is of a hollow structure.
4. The organosilicon chloromethane synthesis and siloxane recovery device according to claim 3,
a first liquid purging port (5) is arranged below the first oleic acid separation component (12), and a second liquid purging port (6) is arranged below the second oleic acid separation component (11);
the first liquid purging port (5) and the second liquid purging port (6) are respectively connected with the outlet end of the circulating washing pump (8).
5. The organosilicon chloromethane synthesis and siloxane recovery device according to claim 1, wherein,
the gas-phase methanol inlet (2) and the crude hydrogen chloride inlet (3) are connected with a gas mixing device (4);
the gas mixing device (4) is connected with a feeding distribution pipe (16);
the length of the feed distribution pipe (16) accounts for 1/3~1/2 of the length of the methyl chloride synthesis reactor (1);
the feeding distribution pipe (16) is provided with small injection holes with the diameter of 1-3mm.
6. The apparatus for synthesizing organosilicon chloromethane and recovering siloxane according to claim 2,
and an inclined flow baffle (15) is arranged at the bottom of the washing facility (13).
7. A method for synthesizing organic silicon by methyl chloride and recovering siloxane is characterized by comprising the following steps:
a. adding crude hydrogen chloride gas, methanol gas and a catalyst solution into an organic silicon chloromethane synthesis and siloxane recovery device to perform chloromethane synthesis reaction to obtain synthesis gas;
b. spraying and washing the synthesis gas, and recovering chlorosilane;
c. make up the hydrogen chloride solution.
8. The method for synthesizing the organic silicon by using the methyl chloride and recovering the siloxane as claimed in claim 7, wherein the spraying temperature is controlled to be 90-110 ℃;
the mass fraction of the supplemented hydrogen chloride solution is 25% -30%.
9. The method of organosilicon methyl chloride synthesis and siloxane recovery according to claim 7,
the feeding temperature of the crude hydrogen chloride gas and the methanol gas is 90-150 ℃, and the volume ratio of the crude hydrogen chloride gas to the methanol gas is 1-1.3;
the catalyst solution is a zinc chloride solution, and the mass fraction of the zinc chloride solution is 40-65%.
10. The method for synthesizing organic silicon by methyl chloride and recovering siloxane according to claim 7,
the reaction temperature of the synthesis reaction in the step a is 120-165 ℃, and the reaction pressure is 0.1-0.25Mpa.
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| CN113548941A (en) * | 2020-04-24 | 2021-10-26 | 蓝星（北京）技术中心有限公司 | Synthesis method and device of methane chloride |
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