CN210385810U - Dimethyl dichlorosilane hydrolysate cracking device - Google Patents
Dimethyl dichlorosilane hydrolysate cracking device Download PDFInfo
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- CN210385810U CN210385810U CN201920879541.4U CN201920879541U CN210385810U CN 210385810 U CN210385810 U CN 210385810U CN 201920879541 U CN201920879541 U CN 201920879541U CN 210385810 U CN210385810 U CN 210385810U
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Abstract
The utility model relates to a cracking device for dimethyl dichlorosilane hydrolysate, wherein a hydrolysate storage tank is connected with a hydrolysate preheater through a hydrolysate delivery pump; the hydrolysate preheater is connected with the Venturi mixer; the catalyst storage tank is connected with the Venturi mixer through a catalyst delivery pump; the Venturi mixer is connected with the cracking reaction kettle; the cracking reaction kettle is connected with the cracking tower, and the cracking tower is connected with the cracking tower condenser. Injecting a proper amount of solvent oil into a horizontal cracking reaction kettle, preheating a part of dimethyldichlorosilane hydrolysate, uniformly mixing with a catalyst, and then feeding the preheated part of dimethyldichlorosilane hydrolysate into the cracking reaction kettle, and directly feeding the rest of the preheated dimethyldichlorosilane hydrolysate into a cracking tower to act together with cracking reflux liquid to control the temperature of the cracking tower; the utility model discloses dimethyldichlorosilane hydrolysate pyrolysis cycle can improve to 35 days, and the energy consumption can descend about 25%, and catalyst unit consumption can reduce to less than 2 thousandth, pyrolysis ring body yield can promote to 99.5%.
Description
Technical Field
The utility model belongs to the technical field of organosilicon product production, concretely relates to dimethyl dichlorosilane hydrolysate cracker.
Background
The organic silicon product is a novel high-tech material, and has been widely applied to the fields of electronics, electrical appliances, aviation, aerospace, construction, textile, medicine and the like since the industrial production in the 40 th generation of the 20 th century. Statistically, in the prior silicone industry, more than 85% of silicone polymers are produced from silicone intermediate methyl cyclosiloxane mixture (abbreviated as DMC), and therefore, DMC production is very important.
At present, most of domestic methyl chlorosilane production plants adopt a cracking process to produce DMC, and the cracking process mainly comprises a traditional dry cracking process and a novel solvent cracking process. Wherein, the dry cracking method has been gradually replaced due to the defects of larger catalyst adding amount, lower ring body yield, high cracking energy consumption and the like; the cracking by the novel solvent method has the advantages of low catalyst addition amount, high ring body yield and the like. Chinese patent CN 104059099A introduces a method for cracking dimethyl dichlorosilane hydrolysate, namely, strong-basicity macroporous anion exchange resin, potassium hydroxide, potassium trimethylsilanolate and [ bmin ] BF4 ionic liquid are subjected to load reaction to obtain a composite catalyst, a methyl dichlorosilane hydrolysate product, solvent oil and hydrolysate are added into a cracking kettle, a ring body mixture is obtained after the hydrolysate is cracked and rearranged, and then a DMC product is obtained after water washing and high-boiling residue and low-boiling residue removal. The yield of the obtained ring body by adopting the method is more than 90 percent, but the obtained ring body product still needs to be washed by water and the like, which is particularly shown in 1, the ring body product obtained after cracking needs to be additionally provided with a washing procedure; 2. the cracked product is not primarily rectified to remove high-boiling-point substances and low-boiling-point substances, and the subsequent rectifying tower has higher design requirement, heavier processing load and higher energy consumption. Chinese patent CN 108409780a describes a method and apparatus for cracking organosilicon hydrolysate by thermal driving circulation of solvent oil, that is, a double-spiral channel in the form of a spiral plate-like heat exchanger is coaxially arranged in the middle of the cracking apparatus, wherein the upper and lower ends of one spiral channel are not sealed and are used as the cracking channel, the upper and lower ends of the other spiral channel are sealed to form a heat exchange medium channel, and the solvent oil is distributed in the annular gap between the cracking apparatus and the column body formed by the cracking channel and the double-spiral channel. Liquid of the hydrolysate in the cracking channel rises to the top of the cracking channel, and after gas-liquid separation, the solvent oil, the unreacted organic silicon hydrolysate and the KOH solution fall to the bottom of the cracking device through the annular gap to form natural circulation. The invention can not generate local overheating phenomenon, has less alkali consumption, but has higher requirements on equipment, which is particularly shown in 1, the cracking kettle has higher manufacturing and processing difficulty; 2. the reactor annulus may limit the cracking capacity and may, in the later stages of production, cause a reduction in the efficiency of the reaction due to an increase in the viscosity of the reactants and even block the annulus.
Disclosure of Invention
The utility model aims to overcome the shortcomings of the prior art and provide a dimethyl dichlorosilane hydrolysate cracking device.
The utility model provides a dimethyl dichlorosilane hydrolysate cracking process and device includes following step:
a dimethyl dichlorosilane hydrolysate cracking device, a hydrolysate storage tank is connected with a hydrolysate preheater through a hydrolysate delivery pump; the hydrolysate preheater is connected with the Venturi mixer;
the catalyst storage tank is connected with the Venturi mixer through a catalyst delivery pump;
the Venturi mixer is connected with the cracking reaction kettle;
the cracking reaction kettle is connected with the cracking tower, the cracking tower is connected with a condenser of the cracking tower, the condenser of the cracking tower is connected with a reflux tank of the cracking tower, and the reflux tank of the cracking tower is connected to the DMC storage tank through a reflux pump of the cracking tower.
The hydrolysate storage tank is connected with the cracking tower through a hydrolysate delivery pump.
The connecting pipeline of the cracking tower and the cracking reaction kettle is a bidirectional pipeline.
The reflux tank of the cracking tower is connected with the upper part of the cracking tower through a reflux pump of the cracking tower.
The tower decomposing condenser and the tower decomposing reflux tank are respectively connected to the vacuum unit through pipelines.
The dimethyl dichlorosilane hydrolysate cracking process with the device comprises the following steps:
(A) the dimethyl dichlorosilane hydrolysate is divided into two parts, one part is preheated to the temperature of 130-160 ℃ by the steam of the hydrolysate preheater, and then is uniformly mixed with the catalyst in the Venturi mixer and enters a cracking reaction kettle containing solvent oil; the other part directly enters the cracking tower without preheating;
(B) and (3) feeding the ring steam generated from the cracking kettle into a cracking tower through a bidirectional pipe, feeding the ring steam into a cracking condenser after mass transfer and heat transfer with the preheated dimethyl dithiosilane hydrolysate and cracking reflux, collecting liquid of the cracking condenser, and using part of the collected liquid to a subsequent rectification section and using part of the collected liquid to control the temperature of the cracking tower through cracking tower reflux liquid, thereby completing the cracking process of the dimethyl dichlorosilane hydrolysate.
The preheated dimethyldichlorosilane hydrolysate in the step (A) accounts for 50-100% of the total fed dimethyldichlorosilane hydrolysate. The solvent oil comprises octadecanol, C8-C20 normal and unsaturated alkanes or the mixture thereof.
In the step (A), the catalyst is potassium hydroxide, and the mass ratio of the hydrolysate to the catalyst is 1: 0.005-0.0005.
In the step (A), the catalyst is potassium hydroxide, and the mass ratio of the hydrolysate to the catalyst is 1: 0.005-0.0005.
In the step (B), the temperature of the top of the cracking tower is controlled to be 70-110 ℃ by controlling the reflux amount of the cracking tower and the amount of the dimethyldichlorosilane hydrolysate directly entering the cracking tower; the temperature of the cracking kettle is controlled at 160 ℃ and the pressure is 10-20kPa by controlling the steam opening of the cracking kettle.
In the step (B), the medium in the bidirectional pipe between the cracking tower and the cracking reaction kettle is a gas-liquid mixture; the non-preheated hydrolysate enters the cracking tower from 1/3-2/3 through a feed distributor; regular packing is filled in the cracking tower above the feeding distributor, and random pall ring packing is filled below the feeding distributor.
Compared with the prior art, the utility model its advantage lies in:
1. part of hydrolysate directly enters a cracking tower, light component substances such as a ring body, water and the like in the hydrolysate absorb heat and evaporate,
heavy component substances such as the linear body and the like transfer heat and mass with the ascending gas flow of the cracking kettle and then return to the cracking kettle for cracking again, so that the production energy consumption is reduced by 10-35%, the possibility that water in hydrolysate enters the cracking kettle to form foam (substances formed after mixing water, a ring body, a catalyst and the like in the reaction process) is reduced, the cracking reaction space 1/4-1/3 is increased, and the cracking period is prolonged by about 2-15 days;
2. the catalyst is conveyed by a precision metering pump, is uniformly mixed with the hydrolysate and then enters the cracking kettle, so that the contact degree of the catalyst and the hydrolysate is enhanced; a cracking distribution device is adopted, so that the mixture of the catalyst and the hydrolysate is distributed more uniformly in a cracking kettle, and the cracking efficiency is improved by 20-50%;
3. the solvent oil with low viscosity and high stability is used as a heat carrier, the viscosity of a reaction system is reduced (the viscosity of materials in a cracking reaction kettle reaches 50-100cp after 3-5 days without the solvent oil, and the viscosity can be controlled to be 10-20cp after the solvent oil is used for a process for 10 days), so that the heat transfer of the system is uniform, the local overheating phenomenon is eliminated, the cracking period is long, and the yield of ring bodies is high; the horizontal cracking reaction kettle is adopted to avoid the defect that the vertical reaction kettle is not tightly sealed due to the stirring device, so that the reaction system is always stable under the high-vacuum reaction condition, the cracking reaction efficiency is improved, and the potential safety hazard that the system sucks air to generate explosion under the negative pressure production condition is also avoided.
4. Two different fillers are added in the cracking tower, the obtained ring body can directly enter a subsequent rectification process without washing, the loss of the ring body is avoided, and the yield of the ring body can reach more than 99.5 percent.
Drawings
FIG. 1 shows a dimethyl dichlorosilane hydrolysate cracking apparatus, wherein, 1, a hydrolysate storage tank, 1-1, a hydrolysate delivery pump, 2, a hydrolysate preheater, 3, a catalyst storage tank, 3-1, a catalyst delivery pump, 4, a cracking tower, 5, a cracking reaction kettle, 6, a cracking tower condenser, 7, a cracking tower reflux tank, 7-1, a cracking tower reflux pump, and 8, a Venturi mixer.
Detailed Description
Example 1
A dimethyl dichlorosilane hydrolysate cracking device, a hydrolysate storage tank 1 is connected with a hydrolysate preheater 2 through a hydrolysate delivery pump 1-1; the hydrolysate preheater 2 is connected with a Venturi mixer 8;
the catalyst storage tank 3 is connected with a Venturi mixer 8 through a catalyst delivery pump 3-1;
the Venturi mixer 8 is connected with the cracking reaction kettle 5;
the cracking reaction kettle 5 is connected with the cracking tower 4, the cracking tower 4 is connected with the cracking tower condenser 6, the cracking tower condenser 6 is connected with the cracking tower reflux tank 7, and the cracking tower reflux tank 7 is connected to the DMC storage tank through the cracking tower reflux pump 7-1.
The hydrolysate storage tank 1 is connected with the cracking tower 4 through a hydrolysate delivery pump 1-1.
The connecting pipeline of the cracking tower 4 and the cracking reaction kettle 5 is a bidirectional pipeline.
The cracking tower reflux tank 7 is connected with the upper part of the cracking tower 4 through a cracking tower reflux pump 7-1.
The cracking tower condenser 6 and the cracking tower reflux tank 7 are respectively connected to a vacuum unit through pipelines.
Example 2
Injecting 10m into a horizontal cracking reaction kettle3Mineral spirits (mixture of C18, C19, C20 saturated hydrocarbons), 5m3Heating the hydrolysate/h dimethyl dichlorosilane to 150 ℃ by a preheater, then uniformly mixing the hydrolysate/h dimethyl dichlorosilane hydrolysate with 15kg/h catalyst (KOH) in a Venturi mixer, and feeding the mixture into a cracking reaction kettle through a cracking distributor (the cracking kettle contains a plurality of micropores so as to uniformly distribute liquid, which is not described in the figure), wherein the temperature of the cracking reaction kettle is controlled to be 160 ℃ and the absolute pressure is 10 kPa; the ring steam generated by cracking enters a cracking tower through a gas phase pipe (the temperature at the top of the tower is controlled at 90 ℃, and the temperature at the bottom of the tower is controlled at
160 ℃ C.), and 2.5m3H dimethyl dichloro chloride without preheatingAnd (3) after mass transfer and heat transfer of the silane hydrolysate and the cracking reflux liquid, feeding the silane hydrolysate and the cracking reflux liquid into a cracking condenser, collecting the liquid of the cracking condenser, extracting a part of the liquid to a subsequent rectification section, and using a part of the liquid in the cracking tower reflux liquid to control the temperature of the cracking tower. Through statistical analysis: average feed of hydrolysate from 6m3The per hour is increased to 7.5m3The cracking efficiency is improved by about 25 percent, the cracking period is prolonged from 23 days to 28 days, the steam consumption is saved by about 0.3t/h, the cold energy is reduced by about 700MJ/h (the energy consumption is reduced by about 22 percent), the unit consumption of the catalyst is reduced from 7 per mill to 2 per mill, and the yield of a cracking ring body is 99.5 percent.
Example 3
The other conditions were the same as 1, the feed rate of the dimethyldichlorosilane hydrolyzate was increased to 6m by the preheater3The adding amount of the catalyst is kept at 15kg/h, the solvent oil is octadecanol, and the amount of the un-preheated hydrolysate is 2.8m3Statistical analysis at/h: the cracking efficiency of the hydrolysate is improved by about 46 percent, the cracking period is prolonged from 23 days to 25 days, the steam consumption is saved by about 0.34t/h, the cold energy is reduced by about 780MJ/h (the energy consumption is reduced by about 25 percent), the unit consumption of the catalyst is reduced from 7 per mill to 1.7 per mill, and the yield of the cracking ring body is 99.3 percent.
Example 4
The other conditions were the same as 1, the feed rate of the dimethyldichlorosilane hydrolyzate was increased to 4.5m by the preheater3The catalyst is added in an amount of 15kg/h, the solvent oil is octadecanol, and the amount of the non-preheated hydrolysate is kept at 2.3m3Statistical analysis at/h: the cracking efficiency of the hydrolysate is improved by about 13 percent, the cracking period is prolonged from 23 days to 35 days, the steam consumption is saved by about 0.28t/h, the cold energy is reduced by about 640MJ/h (the energy consumption is reduced by about 21 percent), the unit consumption of the catalyst is reduced from 7 per mill to 2.2 per mill, and the yield of the cracking ring body is 99.5 percent.
Example 5
The other conditions were the same as 1, the feed rate of the dimethyldichlorosilane hydrolyzate was increased to 5.5m by the preheater3The catalyst addition was kept at 15kg/h and the amount of non-preheated hydrolysate was kept at 2.5m3Statistical analysis at/h: the cracking efficiency of the hydrolysate is improved by about 33 percent, the cracking period is prolonged from 23 days to 27 days, the steam consumption is saved by about 0.3t/h, the cold quantity is reduced by about 800MJ/h (the energy consumption is reduced by about 22 percent), and the unit consumption of the catalyst is reduced by 7 percentThe permillage is reduced to 1.88 permillage, and the yield of cracking ring body is 99.5 percent.
Claims (5)
1. A dimethyl dichlorosilane hydrolysate cracking device is characterized in that a hydrolysate storage tank (1) is connected with a hydrolysate preheater (2) through a hydrolysate delivery pump (1-1); the hydrolysate preheater (2) is connected with the Venturi mixer (8);
the catalyst storage tank (3) is connected with the Venturi mixer (8) through the catalyst delivery pump (3-1);
the Venturi mixer (8) is connected with the cracking reaction kettle (5);
the cracking reaction kettle (5) is connected with the cracking tower (4), the cracking tower (4) is connected with the cracking tower condenser (6), the cracking tower condenser (6) is connected with the cracking tower reflux tank (7), and the cracking tower reflux tank (7) is connected to the DMC storage tank through the cracking tower reflux pump (7-1).
2. The dimethyldichlorosilane hydrolysate splitting apparatus as set forth in claim 1, wherein the hydrolysate storage tank (1) is connected to the splitting tower (4) via a hydrolysate transfer pump (1-1).
3. The dimethyldichlorosilane hydrolysate cracking apparatus as claimed in claim 1, wherein the connecting pipeline between the cracking tower (4) and the cracking reaction kettle (5) is a bidirectional pipeline.
4. The dimethyldichlorosilane hydrolysate cracking apparatus according to claim 1, wherein the cracking tower reflux drum (7) is connected to the upper part of the cracking tower (4) via a cracking tower reflux pump (7-1).
5. The dimethyldichlorosilane hydrolysate cracking apparatus according to claim 1, wherein the cracking tower condenser (6) and the cracking tower reflux drum (7) are respectively connected to a vacuum unit through a pipeline.
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| CN114516976A (en) * | 2022-01-28 | 2022-05-20 | 云南能投硅材科技发展有限公司 | Dimethyl dichlorosilane hydrolysis waste pretreatment process |
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| CN114516976A (en) * | 2022-01-28 | 2022-05-20 | 云南能投硅材科技发展有限公司 | Dimethyl dichlorosilane hydrolysis waste pretreatment process |
| CN114516976B (en) * | 2022-01-28 | 2024-01-12 | 云南能投硅材科技发展有限公司 | Pretreatment process for hydrolysis waste of dimethyl dichlorosilane |
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