CN108409780B - Method and device for cracking organic silicon hydrolysate by solvent oil thermal flooding circulation - Google Patents
Method and device for cracking organic silicon hydrolysate by solvent oil thermal flooding circulation Download PDFInfo
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Abstract
The invention relates to a cracking method and a device of organic silicon hydrolysate by solvent oil heat-drive circulation, wherein a double-spiral channel similar to a spiral plate heat exchanger is coaxially arranged in the middle of a cracking device, the upper end and the lower end of one of the double-spiral channel are not sealed and are used as a cracking channel, the upper end and the lower end of the other spiral channel are sealed to form a heat exchange medium channel, the solvent oil is distributed in an annular gap between a cylinder body formed by the cracking channel and the double-spiral channel and the cracking device, a mixture of the organic silicon hydrolysate and KOH solution is sent into the cracking channel, the heat exchange medium of the heat exchange channel provides heat for the cracking channel, the organic silicon hydrolysate is mixed with the solvent oil in the cracking channel and is vaporized while reacting, bubbles rise to drive liquid in the cracking channel to rise to the top of the cracking channel, and after gas-liquid separation, the solvent oil, the unreacted organic silicon hydrolysate and the KOH, forming a natural circulation. The invention has no stirring device, high heat and mass transfer efficiency, no local overheating, long production period of the device, low alkali consumption, and improved yield of ring body and D4And the quality of DMC, the operation is stable, safe and reliable.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a method and a device for cracking an organic silicon hydrolysate by solvent oil thermal flooding circulation.
Background
In the organosilicon industry, more than 85% of organosilicon products and products are prepared fromOrganosilicon intermediates (e.g. octamethylcyclotetrasiloxane D)4Dimethyl cyclosiloxane mixture DMC), the cleavage rearrangement of the dimethyldichlorosilane (dimethyl for short) hydrolysate is of particular importance. The cracking process is that dimethyl hydrolysate is subjected to cracking rearrangement reaction under the condition of an alkaline catalyst to obtain the product with about 60 percent of D4About 10% of D3And about 20% of D5The D with the purity of more than 99 percent (mass fraction) can be prepared by further rectifying the lysate of (2) and is called dimethyl cyclosiloxane mixture (DMC)4And (5) producing the product. In the cracking reaction process, siloxane containing three functional groups or Si-H becomes silanol sylvite and is left at the bottom of the cracking kettle.
In the cracking production of the organic silicon monomer, two processes of dry cracking and solvent oil cracking are generally adopted, and the two process routes are both realized in the industrialized production. At present, most domestic cracking devices adopt a dry cracking process, namely a semi-continuous cracking process route of hydrolysate vaporization, cracking, evaporation to dryness and loop washing. Mature process and D of main product4The DMC proportion can be properly adjusted according to the market conditions, and the DMC is divided into D4+D5"is the main. However, the process has the problems of low yield of ring bodies, poor product quality, short shutdown deslagging period, high alkali consumption, uneven heating of key equipment, difficult amplification and the like.
The alkali can not only break Si-O-Si bonds at high temperature, but also break a certain amount of Si-C bonds, so that a polymer with a cross-linked structure can be generated in the cracking process of the linear polysiloxane. To avoid the cleavage of the Si-C bond, the alkaline cleavage reaction can be carried out in an inert solvent with a high boiling point.
Foreign patents have reported on the preparation of cyclosiloxanes by cracking dimethyl hydrolysate with a solvent method since the beginning of the 80 s. The solvent oil is used as a heat carrier and added into the cracking kettle, so that the heat transfer of the cracking reaction is uniform, the local overheating phenomenon is eliminated, the occurrence of the disproportionation reaction is controlled, and the yield of the ring body is improved.
The key equipment in the solvent method continuous cracking process is a cracking kettle, and at present, a stirring type cracking kettle which is externally provided with a jacket and internally provided with a heating coil is common. The chinese patent application CN201210221210.4 discloses a stirring vane structure of an organosilicon cracking reaction kettle, wherein the shape of the stirring vane at the lowest end is consistent with that of an arc kettle, so as to shorten the distance between the stirring vane and the kettle bottom and improve the mixing effect, but the existence of a stirring device does not guarantee the sealing performance of the equipment and the safety is not high. For the cracking reaction carried out under the negative pressure condition, air is easy to be sucked to generate explosive atmosphere, and potential hazards exist in the safety production.
Chinese utility model patent 201620965364.8 discloses an organosilicon cracker, internal coil pipe heat exchanger and two U type pipe heaters of setting up of schizolysis cauldron, although improved heating area and heating efficiency, near coil pipe and U type pipe device material temperature is high, and other position temperatures are low, and it is inhomogeneous to heat, can produce the side reaction, and coil pipe and U type pipe bending portion easily deposit the dirt moreover.
The cracking kettle has the advantages that due to the existence of the jacket, the external pressure applied to the shell is increased to 1MPa (the pressure of heating steam), the thickness of the shell of the cracking kettle is inevitably increased, and the material consumption is increased. In the design, factors such as mutual avoidance of the connecting pipe, the manhole and the jacket, welding strength and safety, proper arrangement of welding seams and the like are also considered, so that the cracking kettle has a complex structure, and the manufacturing cost is improved; stirring dead angles are easily generated, scaling is generated on a heating surface, so that the heat transfer efficiency is reduced, the reaction efficiency is lowered, a large amount of sylvite can be accumulated at the bottom of the cracking kettle, frequent stopping and slag removal are needed, explosion is easily generated, and the production of cyclosiloxane is seriously influenced.
Disclosure of Invention
Aiming at the defects and shortcomings of the cracking rearrangement kettle in the current technical situation of the cracking rearrangement kettle in the organic silicon industry, the invention provides a cracking method of organic silicon hydrolysate by solvent oil heat-drive circulation, so as to overcome the defects of the traditional cracking kettle in the aspects of mass and heat transfer, full mixing and production cycle and improve the safety.
A cracking method of organic silicon hydrolysate by solvent oil heat-drive circulation is characterized in that a double-spiral channel similar to a spiral plate heat exchanger is coaxially arranged in the middle of a cracking device, the upper end and the lower end of one spiral channel in the double-spiral channel are not sealed and are used as a cracking channel, the upper end and the lower end of the other spiral channel are sealed to form a heat exchange medium channel, the solvent oil is distributed in an annular gap between a cylinder body formed by the cracking channel and the double-spiral channel and the cracking device, a mixture of the organic silicon hydrolysate and a KOH solution is fed into the cracking channel, the heat exchange medium of the heat exchange channel provides heat for the cracking channel, the organic silicon hydrolysate is mixed with solvent oil in the cracking channel and is vaporized while reacting, bubbles rise to drive liquid in the cracking channel to rise to the top of the cracking channel, and after gas-liquid separation, the solvent oil, the unreacted organic silicon hydrolysate and, forming a natural circulation.
Compared with the prior art, the double-spiral channel can not only strengthen heat transfer, provide required heat for reaction in time, but also promote mass transfer, and has the characteristics of high heat transfer rate, balanced temperature of a reactant system, full reaction of reactants and reduction of generation of byproducts.
In order to make the liquid enter the cracking channel more uniformly, it is preferable that a liquid distributor is arranged at the bottom of the cracking device, and the mixture of the organic silicon hydrolysate and the KOH solution is sent into the cracking channel through the liquid distributor.
It is preferable that: after the reaction, gas and liquid are separated at the top of the cracking channel, and the separated gas is discharged from a gas outlet of the cracking device after solvent oil is removed.
It is preferable that: the bottom of the cracking device is provided with an inverted cone section and a discharge port, and the cracking slag generated by the reaction is discharged from the discharge port after being settled by gravity in the inverted cone section. The liquid at the top of the inverted cone section flows smoothly, the liquid at the lower part is in a static state basically, and the cracking slag generated by reaction is settled on the cone body and gathered in the cone section through gravity and is discharged from the discharge port, so that long-period continuous production can be realized, and potential safety hazards are eliminated.
The second purpose of the invention is to provide a solvent oil heat-drive circulation organosilicon hydrolysate cracking device, which comprises a feed inlet, an air outlet, a heat exchange medium inlet, a heat exchange medium outlet, a solvent oil inlet and a discharge outlet, wherein the feed inlet is arranged at one side of the lower part of the cracking device, the air outlet is arranged at the center of the top of the cracking device, the heat exchange medium inlet, the heat exchange medium outlet and the solvent oil inlet are arranged at the upper part of the cracking device, and the discharge outlet is arranged at the center of the bottom of the cracking device; the middle part of the cracking device is coaxially provided with a double-spiral channel similar to a spiral plate heat exchanger, the upper end and the lower end of one spiral channel in the double-spiral channel are not sealed and are used as the cracking channel, the upper end and the lower end of the other spiral channel are sealed to form a heat exchange medium channel, solvent oil is distributed in an annular gap between a cylinder body formed by the cracking channel and the double-spiral channel and the cracking device, the upper part of a feed inlet is provided with a liquid distributor, and the liquid distributor sends a mixture of organic silicon hydrolysate and KOH solution into the cracking channel.
Compared with the prior art, the invention has simple structure, no jacket device and no stirring device, and greatly reduces the problem of scaling because the spiral plate-like structure has self-cleaning function, and the solvent oil circularly flows in the cracking channel and the annular space between the cylinder body consisting of the double-spiral channel and the cracking device.
The distance between the double spiral channels is adjustable to ensure the heat exchange effect and the mass transfer effect. The distance between the cracking channels is designed according to the capacity and the heat exchange area of the device; the space of the heat exchange channels can be designed according to the circulation quantity of the heat exchange medium, and the heat transfer coefficient is improved and the heat transfer effect is enhanced by increasing the flow speed of the heat exchange medium.
The annular space interval inside the heat-drive circulating cracking kettle body can also be designed according to the circulation quantity.
It is preferable that: the cracking device comprises a top sealing head section, a middle cylindrical section and a bottom inverted cone section, and the double-spiral channel is arranged in the middle cylindrical section and is coaxial with the cylindrical section; preferably, a demister is provided between the middle cylindrical section and the top head-sealing section to separate the solvent oil and unreacted hydrolysate entrained in the gas from the KOH solution.
It is preferable that: the liquid distributor is composed of a coil pipe, a liquid nozzle is arranged on the coil pipe, the nozzle is vertically upward, or a vertical pipe which is upwards inserted into the cracking channel is arranged, and the liquid distributor corresponds to the cracking channel to realize the uniform distribution of the liquid.
It is preferable that: the bottom of the lower inverted cone section is provided with a discharge port.
The third purpose of the invention is to provide a continuous cracking system of organosilicon hydrolysate with solvent oil heat-drive circulation, which comprises a hydrolysate heater, a cracking device according to any one of claims 5 to 8, a cracking tower, a rearrangement condenser, a water washing kettle and a solvent oil heat-drive circulation D which are connected in sequence3Column, hydrolysate tank, product column, D4A storage tank, a cracking tower kettle side line is connected with a cracking device, a rearrangement condenser is connected at the top of the tower, D3Tower top connection D3A condenser connected to the hydrolysate tank via a pump, D3The tower is connected with a product tower, the top of the product tower is connected with a product tower condenser and is connected with a finished product D4A storage tank, a side line of the product tower is connected with the DMC storage tank, and a tower kettle of the product tower is connected with a hydrolysate tank through a pump.
Compared with the prior art, the cracking device disclosed by the invention can discharge cracking slag during working, does not need to stop for slag removal, eliminates potential safety hazards, ensures continuous operation of cracking reaction and improves cracking efficiency.
The fourth purpose of the invention is to provide a method for continuously cracking the organosilicon hydrolysate by solvent oil heat-drive circulation, which comprises the following steps: mixing the organic silicon hydrolysate preheated by the hydrolysate heater with KOH solution in proportion, feeding the mixture into a cracking device as claimed in any one of claims 4-7, performing catalytic cracking reaction under the action of heat carrier solvent oil, directly feeding cyclized and rearranged gas into a cracking tower, returning the line body in the tower bottom to the cracking kettle, condensing the ring body at the top of the tower through a rearrangement condenser, feeding the condensed ring body into a water washing kettle in a purification system, purifying and washing the condensed ring body with desalted water, and feeding the purified and washed ring body into a cracking device D3Column, overhead vapor pass D3Condensing in a condenser, pumping into a hydrolysate tank, transferring the liquid from the tower bottom to a product tower, condensing the vapor from the tower top in the product tower in a condenser, pumping out the condensed vapor in the tower top in a certain reflux ratio, and feeding the condensed vapor into a finished product D4A storage tank, wherein the side line discharge of the tower is DMC and is sent into the DMC storage tank, and the high ring of the tower kettle is pressurized by a delivery pump and then returns to the hydrolysate tank; the cracked slag in the cracking device is discharged through a discharge port and sent to be buried deeply outside.
The invention has the advantages that:
(1) by utilizing the advantages of short heat transfer distance, small temperature difference, high heat transfer coefficient, large heat transfer area, large volume specific power and good flow stability of the double-spiral channel, the hydrolysate and the solvent oil are mixed and transferred quickly under the condition of constant temperature, the heat transfer is uniform and efficient, the reaction is sufficient, and the by-products are few; the cracked product is gas phase, so that the fluid in the channel is boiling while flowing, and the fluid is turbulent, so that the hydrolysate is fully contacted and mixed with the catalyst, and the reaction is facilitated.
(2) The convection and the large circulation of the liquid are realized in the device in a heat driving mode. On one hand, under the washing of the circulating solvent oil in the cracking channel, the heat exchange surface is not easy to generate precipitation and dirt, the self-cleaning effect is achieved, and the continuous and stable operation can be guaranteed. On the other hand, the reaction product is a gas phase, bubbles rise to drive the solvent oil to circularly flow, so that the heat transfer and mass transfer effects are enhanced, the full implementation of the cracking reaction is facilitated, and the yield of the product ring body is improved.
(3) Because the reaction is carried out under the vacuum condition, the requirement on the sealing property is particularly high, and if the sealing property is not achieved, air enters the cracking kettle and is mixed with siloxane steam, so that an explosive atmosphere can be formed, and danger is generated. The problem of poor sealing performance caused by the installation of the stirrer can be avoided without installing the stirrer, and the safety is improved.
(4) The process of continuous production is basically achieved, the cracking system does not need to evaporate a drying kettle, high-concentration cracking slag can be formed in a cracking device, the device does not need to be stopped, and intermittent discharge is achieved.
(5) The solvent oil circulation adopts a siphon structure, and has the advantages of high heat transfer rate, stable operation, good anti-scaling performance and the like. The annular space can be boiled to avoid bullet flow, the operation is more stable than an empty pipe, and simultaneously, ascending and descending streams are divided, so that the blockage of steam ascending is prevented. The power density of the liquid in the annular channel is high, and the optimal value can be obtained by adjusting the width of the annular gap, so that the heat transfer coefficient is greatly improved.
The invention has no stirring device, high heat and mass transfer efficiency, no local overheating, long production period of the device, low alkali consumption, and improved yield of ring body and D4And the quality of DMC, the operation is stable, safe and reliable.
Drawings
FIG. 1 is a schematic structural diagram of a heat-driven circulation-type pyrolysis kettle of the invention.
Wherein: 101 cracking kettle body, 102 demister, 103 spiral plate heat exchanger, 104 liquid distributor, 105 annular space, 106 feed inlet, 107 gas outlet, 108 heat exchange medium inlet, 109 heat exchange medium outlet, 110 solvent oil inlet and 111 discharge outlet.
FIG. 2 is a schematic diagram of a model for realizing convection and large circulation of liquid in a heat driving mode according to the invention
FIG. 3 is a schematic structural diagram of the present invention
Wherein: 1 hydrolysate, 2 hydrolysate heaters, 3 heat-driven circulation type cracking kettles, 4KOH solution tanks, 5 cracking towers, 6 rearrangement condensers, 7 rearrangement reflux tanks, 8 water washing kettles, 9 ring body storage tanks and 10D3Tower, 11D3Condenser, 12D3Column reboiler, 13D3Reflux drum, 14 product tower, 15 product tower condenser, 16 product tower reboiler, 17DMC storage tank, 18 product reflux drum
Detailed Description
Example 1
3-thousand-ton/year dimethyl hydrolysate heat-drive circulation type cracking kettle
When the heat-drive circulation type cracking kettle is used for cracking 3 ten thousand tons per year of dimethyl hydrolysate, 0.4 ton of steam is needed for 1 ton of hydrolysate, and the mass ratio of the hydrolysate: 50% KOH solution (volume) 1: 0.01, product purity: d4≥99.5％，DMC(D4+D5) More than or equal to 86.5 percent, and the heat exchange area is 80m calculated by heat quantity2Size of spiral plate heat exchanger
The structure is shown in figures 1 and 2.
The preheated mixture of dimethyl hydrolysate and KOH solution enters a cracking kettle from a lower feed inlet 106, enters a corresponding cracking channel 122 through an upper nozzle of a liquid distributor 104 to be mixed with solvent oil, absorbs heat from a heat exchange channel 121, is vaporized while reacting, bubbles rise to drive liquid in the cracking channel to rise to the top of the cracking channel 122, and after gas-liquid separation, the solvent oil, unreacted organosilicon hydrolysate and the KOH solution fall to the bottom of a cracking device through an annular gap to form natural circulation. The gas after the cyclization rearrangement is further subjected to the removal of the solvent oil by the demister 102 and then discharged from a gas phase outlet at the upper part of the cracking kettle.
The working process of the invention is as follows:
the hydrolysate preheated by the hydrolysate heater 2 is mixed with KOH solution in proportion and enters a heat-drive circulation type cracking kettle 3 to carry out catalytic cracking reaction under the action of heat carrier solvent oil, gas subjected to cyclization rearrangement directly enters a cracking tower 5, a line body in the tower kettle returns to the heat-drive circulation type cracking kettle again, a ring body at the top of the tower is condensed by a rearrangement condenser 6, sent to a water washing kettle 8 in a purification system, purified and washed by desalted water and then enters a reactor D3Column 10, overhead vapor stream D3Condensing in a condenser 11, pumping into a hydrolysate tank 1, transferring the liquid in the tower bottom to a product tower 14, condensing the vapor in the tower top in a product tower condenser 15, pumping out at a certain reflux ratio, and feeding into a finished product D4And (3) a storage tank, wherein the side line discharge of the tower is DMC and is sent into the DMC storage tank, and the high ring of the tower kettle is pressurized by a delivery pump and then returns to the hydrolysate tank 1. And discharging the cracking slag in the heat-drive circulation type cracking kettle through a discharge port, and conveying the cracking slag to be buried deeply outside.
Example 2
5.5 million tons/year dimethyl hydrolysate heat-driving circulation type cracking kettle
When the heat-drive circulation type cracking kettle is used for cracking dimethyl hydrolysate of 5.5 ten thousand tons per year, 0.392 ton of steam is needed for 1 ton of hydrolysate, and the mass ratio of the hydrolysate: 50% KOH solution (volume) 1: 0.009, product purity: d4≥99.5％，DMC(D4+D5) More than or equal to 86.7 percent, and the heat exchange area is 150m calculated by heat quantity2Size of spiral plate heat exchanger
The structure is shown in figures 1 and 2.
The preheated mixture of dimethyl hydrolysate and KOH solution enters a cracking kettle from a lower feed inlet 106, enters a corresponding cracking channel 122 through an upper nozzle of a liquid distributor 104 to be mixed with solvent oil, absorbs heat from a heat exchange channel 121, is vaporized while reacting, bubbles rise to drive liquid in the cracking channel to rise to the top of the cracking channel 122, and after gas-liquid separation, the solvent oil, unreacted organosilicon hydrolysate and the KOH solution fall to the bottom of a cracking device through an annular gap to form natural circulation. The gas after the cyclization rearrangement is further subjected to the removal of the solvent oil by the demister 102 and then discharged from a gas phase outlet at the upper part of the cracking kettle.
The working process of the invention is as follows:
the hydrolysate preheated by the hydrolysate heater 2 is mixed with KOH solution in proportion and enters a heat-drive circulation type cracking kettle 3 to carry out catalytic cracking reaction under the action of heat carrier solvent oil, gas subjected to cyclization rearrangement directly enters a cracking tower 5, a line body in the tower kettle returns to the heat-drive circulation type cracking kettle again, a ring body at the top of the tower is condensed by a rearrangement condenser 6, sent to a water washing kettle 8 in a purification system, purified and washed by desalted water and then enters a reactor D3Column 10, overhead vapor stream D3Condensing in a condenser 11, pumping into a hydrolysate tank 1, transferring the liquid in the tower bottom to a product tower 14, condensing the vapor in the tower top in a product tower condenser 15, pumping out at a certain reflux ratio, and feeding into a finished product D4And (3) a storage tank, wherein the side line discharge of the tower is DMC and is sent into the DMC storage tank, and the high ring of the tower kettle is pressurized by a delivery pump and then returns to the hydrolysate tank 1. And discharging the cracking slag in the heat-drive circulation type cracking kettle through a discharge port, and conveying the cracking slag to be buried deeply outside.
Comparative example 3
3 ten thousand tons/year dimethyl hydrolysate stirring type cracking kettle
When a common stirred tank cracker with an external jacket and a heating coil inside is used for cracking 3 million tons/year dimethyl hydrolysate, 0.42 ton of steam is needed for 1 ton of hydrolysate, and the weight of hydrolysate: 50% KOH solution (volume) 1: 0.011, product purity: d4≥99％，DMC(D4+D5)≥85％。
Comparison of a comparative example and examples 1-2 shows that the heat-drive circulating type cracking kettle has high heat transfer efficiency, reduces the alkali consumption, and improves the yield of the ring body and D4The quality of the DMC.
Claims (11)
1. A cracking method of organic silicon hydrolysate by solvent oil thermal flooding circulation is characterized in that: the middle part of the cracking device is coaxially provided with a double-spiral channel similar to a spiral plate heat exchanger, the upper end and the lower end of one spiral channel in the double-spiral channel are not sealed and are used as a cracking channel, the upper end and the lower end of the other spiral channel are sealed to form a heat exchange medium channel, solvent oil is distributed in an annular gap between a cylinder formed by the cracking channel and the double-spiral channel and the cracking device, a mixture of organic silicon hydrolysate and KOH solution is fed into the cracking channel, the heat exchange medium of the heat exchange channel provides heat for the cracking channel, the organic silicon hydrolysate is mixed with the solvent oil in the cracking channel and is vaporized while reacting, bubbles rise to drive liquid in the cracking channel to rise 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.
2. A process for cracking an organosilicon hydrolyzate with thermal flooding of solvent oil according to claim 1, characterized in that: the bottom of the cracking device is provided with a liquid distributor, and the mixture of the organic silicon hydrolysate and the KOH solution is sent into the corresponding cracking channel through the liquid distributor.
3. A process for cracking an organosilicon hydrolyzate with thermal flooding of solvent oil according to claim 1, characterized in that: after the reaction, gas and liquid are separated at the top of the cracking channel, and the separated gas is discharged from a gas outlet of the cracking device after solvent oil is removed.
4. A process for cracking an organosilicon hydrolyzate with thermal flooding of solvent oil according to claim 1, characterized in that: the bottom of the cracking device is provided with an inverted cone section and a discharge port, and the cracking slag generated by the reaction is discharged from the discharge port after being settled by gravity in the inverted cone section.
5. The utility model provides an organosilicon hydrolysate cracker of solvent oil heat-drive circulation which characterized in that: the cracking device comprises a feed inlet, an air outlet, a heat exchange medium inlet, a heat exchange medium outlet, a solvent oil inlet and a discharge outlet, wherein the feed inlet is arranged on one side of the lower part of the cracking device; the middle part of the cracking device is coaxially provided with a double-spiral channel similar to a spiral plate heat exchanger, the upper end and the lower end of one spiral channel in the double-spiral channel are not sealed and are used as the cracking channel, the upper end and the lower end of the other spiral channel are sealed to form a heat exchange medium channel, solvent oil is distributed in an annular gap between a cylinder body formed by the cracking channel and the double-spiral channel and the cracking device, the upper part of a feed inlet is provided with a liquid distributor, and the liquid distributor sends a mixture of organic silicon hydrolysate and KOH solution into the cracking channel.
6. The apparatus for cracking an organosilicon hydrolyzate fraction of solvent-oil heat-drive loop according to claim 5, wherein: the cracking device comprises a top sealing head section, a middle cylindrical section and a bottom inverted cone section, and the double-helix channel is arranged in the middle cylindrical section and is coaxial with the cylindrical section.
7. The apparatus for cracking an organosilicon hydrolyzate with a thermal drive loop of solvent oil according to claim 6, wherein: a demister is arranged between the middle cylindrical section and the top head sealing section.
8. The apparatus for cracking an organosilicon hydrolyzate fraction of solvent-oil heat-drive loop according to claim 5, wherein: the liquid distributor is composed of a coil pipe, a liquid nozzle is arranged on the coil pipe, the nozzle is vertically upward, or a vertical pipe which is upwards inserted into the cracking channel is arranged, and the liquid distributor corresponds to the cracking channel to realize the uniform distribution of the liquid.
9. The apparatus for cracking an organosilicon hydrolyzate fraction of solvent-oil heat-drive loop according to claim 5, wherein: the bottom of the inverted cone section is provided with a discharge port.
10. A continuous cracking system of organic silicon hydrolysate with solvent oil heat-drive circulation is characterized in that: the device comprises a hydrolysate heater, the cracking device as claimed in any one of claims 5 to 9, a cracking tower, a rearrangement condenser, a water washing kettle, a D3 tower, a hydrolysate tank, a product tower and a D4 storage tank, wherein the side line of the tower kettle of the cracking tower is connected with the cracking device, the rearrangement condenser is connected at the tower top, the D3 condenser is connected at the tower top of the D3 tower, the hydrolysate tank is connected through a pump, the D3 tower is connected with the product tower, the product tower top is connected with the product tower condenser and is connected with the finished product D4 storage tank, the side line of the product tower is connected with the DMC storage tank, and the tower kettle of the product tower is connected.
11. A method for continuously cracking organosilicon hydrolysate by solvent oil thermal flooding circulation is characterized in that: the method comprises the following steps:
mixing the organosilicon hydrolysate preheated by the hydrolysate heater with KOH solution in proportion, feeding the mixture into a cracking device as claimed in any one of claims 5 to 9, carrying out catalytic cracking reaction under the action of hot carrier solvent oil, directly feeding cyclized and rearranged gas into a cracking tower, returning the line body in the tower kettle to the cracking kettle, condensing the ring body at the top of the tower through a rearrangement condenser, feeding the ring body at the top of the tower into a washing kettle in a purification system, purifying and washing the ring body through desalted water, feeding the ring body into a D3 tower, condensing the steam at the top of the tower through a D3 condenser, extracting the steam at a certain reflux ratio, pumping the condensed steam into a hydrolysate tank, conveying the liquid at the bottom of the tower to a product tower, condensing the condensed steam at the top of the tower through a product tower condenser, extracting the condensed steam at a certain reflux ratio, feeding the condensed steam into a finished product D4 storage tank; the cracked slag in the cracking device is discharged through a discharge port and sent to be buried deeply outside.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1476457A (en) * | 1973-11-27 | 1977-06-16 | Gen Electric | Preparation of cyclic siloxanes |
| FR2723095A1 (en) * | 1994-07-29 | 1996-02-02 | Gen Electric | PROCESS FOR THE PREPARATION OF CYCLIC SILOXANES BY CRACKING |
| CN203663804U (en) * | 2013-12-09 | 2014-06-25 | 内蒙古恒业成有机硅有限公司 | Novel device for high boiling pyrolysis of organic silicon |
| CN203764252U (en) * | 2014-02-26 | 2014-08-13 | 江苏科圣化工机械有限公司 | Cyclosiloxane reaction kettle |
-
2018
- 2018-05-11 CN CN201810450308.4A patent/CN108409780B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1476457A (en) * | 1973-11-27 | 1977-06-16 | Gen Electric | Preparation of cyclic siloxanes |
| FR2723095A1 (en) * | 1994-07-29 | 1996-02-02 | Gen Electric | PROCESS FOR THE PREPARATION OF CYCLIC SILOXANES BY CRACKING |
| GB2291876A (en) * | 1994-07-29 | 1996-02-07 | Gen Electric | Improved siloxane cracking process |
| CN203663804U (en) * | 2013-12-09 | 2014-06-25 | 内蒙古恒业成有机硅有限公司 | Novel device for high boiling pyrolysis of organic silicon |
| CN203764252U (en) * | 2014-02-26 | 2014-08-13 | 江苏科圣化工机械有限公司 | Cyclosiloxane reaction kettle |
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