CN110538616A - Device and method for producing low-viscosity methyl silicone oil - Google Patents
Device and method for producing low-viscosity methyl silicone oil Download PDFInfo
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- CN110538616A CN110538616A CN201910880605.7A CN201910880605A CN110538616A CN 110538616 A CN110538616 A CN 110538616A CN 201910880605 A CN201910880605 A CN 201910880605A CN 110538616 A CN110538616 A CN 110538616A
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- kettle body
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/005—Separating solid material from the gas/liquid stream
- B01J8/006—Separating solid material from the gas/liquid stream by filtration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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Abstract
The invention provides a device and a method for producing low-viscosity methyl silicone oil, wherein the device comprises the following components: a reaction kettle body; the upper part of the reaction kettle body is provided with a feeding hole, the inside of the reaction kettle body is provided with an anchor stirrer, the bottom of the reaction kettle body is an outward convex arc surface, and the lowest end of the arc surface is provided with a discharging hole; a cylindrical baffle surrounding the discharge port; the bottom end of the cylindrical baffle is attached to the arc surface, and the top end of the cylindrical baffle is provided with a metal filter screen. Compared with the prior art, the device and the method for producing the low-viscosity methyl silicone oil can avoid the solid catalyst from flowing out along with the reaction product, reduce the abrasion of the catalyst, reduce the loss rate of the catalyst, ensure that most of the solid catalyst is soaked in the reaction product, effectively protect the catalyst and prolong the service life of the catalyst.
Description
Technical Field
The invention relates to the technical field of production of methyl silicone oil, in particular to a device and a method for producing low-viscosity methyl silicone oil.
Background
The methyl silicone oil is linear polysiloxane which takes inorganic Si-O-Si as a main chain and is connected with methyl on the Si, has the advantages of high and low temperature resistance, weather resistance, shear resistance, hydrophobicity, chemical stability, electric insulation, low surface tension, physiological inertia and the like, is widely used in the fields of machinery, electricity, instruments, textile, coating, medicine and the like as a lubricant, transformer oil, instrument oil, heat carrier, additive and the like, and is a silicone oil product with the largest output and the widest application.
At present, the acidic solid catalyst with the advantages of strong catalytic activity, recyclability and reutilization, convenient preparation, environmental protection and the like gradually replaces concentrated sulfuric acid and becomes a main catalyst for catalytically synthesizing low-viscosity dimethyl silicone oil. However, in the production process, it is found that after a polymerization equilibration reaction is carried out in a common batch reaction kettle by using a solid acid catalyst, solid catalyst particles easily flow out of the bottom of the reaction kettle along with the discharging process, the catalyst can be recycled only by adding a filtering operation, the abrasion of the solid catalyst is increased by repeated filtering operation, the loss rate of the catalyst is increased, the catalyst discharged along with a reaction product loses the protection of the reaction product, and the service life of the catalyst is shortened.
Disclosure of Invention
In view of this, the present invention provides an apparatus and a method for producing low viscosity methyl silicone oil, which can prevent the solid catalyst from flowing out along with the reaction product, reduce catalyst abrasion, reduce catalyst loss rate, and simultaneously ensure that most of the solid catalyst is in the reaction product immersion, so as to be effectively protected, and prolong the service life of the catalyst.
The invention provides a device for producing low-viscosity methyl silicone oil, which comprises:
A reaction kettle body; the upper part of the reaction kettle body is provided with a feeding hole, the inside of the reaction kettle body is provided with an anchor stirrer, the bottom of the reaction kettle body is an outward convex arc surface, and the lowest end of the arc surface is provided with a discharging hole;
A cylindrical baffle surrounding the discharge port; the bottom end of the cylindrical baffle is attached to the arc surface, and the top end of the cylindrical baffle is provided with a metal filter screen.
preferably, the anchor type stirrer is controlled by a stirring motor arranged outside the reaction kettle body.
Preferably, the discharge hole is provided with a discharge valve.
Preferably, the mesh size of the metal filter screen is 100-200 meshes.
preferably, the cylindrical baffle is not in contact with the anchor agitator at all times.
The invention also provides a method for producing the low-viscosity methyl silicone oil, and the device adopting the technical scheme comprises the following steps:
a) Adding octamethylcyclotetrasiloxane, hexamethyldisiloxane and a solid catalyst into a reaction kettle body, and reacting under the stirring condition to obtain the low-viscosity methyl silicone oil.
Preferably, the mass ratio of the octamethylcyclotetrasiloxane, the hexamethyldisiloxane and the solid catalyst in the step a) is (8-12): 1: (0.1 to 1).
Preferably, the solid catalyst in step a) is a strong acid cation exchange resin, wherein the solid catalyst with the particle size of 0.4 mm-1.2 mm accounts for more than 90%.
Preferably, the rotating speed of the stirring in the step a) is 200r/min to 2000 r/min.
Preferably, the reaction temperature in the step a) is 75-95 ℃ and the reaction time is 6-10 h.
The invention provides a device and a method for producing low-viscosity methyl silicone oil, wherein the device comprises the following components: a reaction kettle body; the upper part of the reaction kettle body is provided with a feeding hole, the inside of the reaction kettle body is provided with an anchor stirrer, the bottom of the reaction kettle body is an outward convex arc surface, and the lowest end of the arc surface is provided with a discharging hole; a cylindrical baffle surrounding the discharge port; the bottom end of the cylindrical baffle is attached to the arc surface, and the top end of the cylindrical baffle is provided with a metal filter screen. Compared with the prior art, the device and the method for producing the low-viscosity methyl silicone oil can avoid the solid catalyst from flowing out along with the reaction product, reduce the abrasion of the catalyst, reduce the loss rate of the catalyst, ensure that most of the solid catalyst is soaked in the reaction product, effectively protect the catalyst and prolong the service life of the catalyst.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for producing low-viscosity methyl silicone oil according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an apparatus for producing low-viscosity methyl silicone oil provided in a comparative example.
Detailed Description
the technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a device for producing low-viscosity methyl silicone oil, which comprises:
A reaction kettle body; the upper part of the reaction kettle body is provided with a feeding hole, the inside of the reaction kettle body is provided with an anchor stirrer, the bottom of the reaction kettle body is an outward convex arc surface, and the lowest end of the arc surface is provided with a discharging hole;
A cylindrical baffle surrounding the discharge port; the bottom end of the cylindrical baffle is attached to the arc surface, and the top end of the cylindrical baffle is provided with a metal filter screen.
Referring to fig. 1, fig. 1 is a schematic structural diagram of an apparatus for producing low-viscosity methyl silicone oil according to an embodiment of the present invention; wherein, 1 is the reation kettle cauldron body, 2 is the feed inlet, 3 is anchor agitator, 4 is cylindrical baffle, 5 is the metal filter screen, 6 is the blowing valve.
In the invention, the reaction kettle body (1) is used for carrying out batch reaction. In the invention, a feeding hole (2) is arranged at the upper part of the reaction kettle body (1) and is used for adding reaction raw materials into the reaction kettle body (1); one or more feed ports may be provided, and the present invention is not particularly limited thereto.
in the invention, an anchor stirrer (3) is arranged in the reaction kettle body (1) and is used for stirring and mixing the raw materials in the reaction kettle body (1) and carrying out reaction under the stirring condition. In the invention, the anchor stirrer (3) is preferably controlled by a stirring motor (marked by M in the figure) arranged outside the reaction kettle body.
In the invention, the bottom of the reaction kettle body (1) is an outwardly convex arc surface, and the lowest end of the arc surface is provided with a discharge hole; therefore, when the discharge port is opened, the materials in the reaction kettle body (1) can be smoothly discharged out of the reaction kettle body (1) through the discharge port under the action of gravity. In the invention, the discharge port is preferably provided with a discharge valve (6) for controlling the opening and closing of the discharge port.
in the invention, the cylindrical baffle (4) surrounds the discharge opening; the bottom end of the cylindrical baffle plate (4) is attached to the arc surface, and the top end of the cylindrical baffle plate is provided with a metal filter screen (5). The reaction kettle body (1) is isolated from the discharge hole to a certain extent by adopting the cylindrical baffle (4) with the specific structure, and materials in the reaction kettle body (1) need to be accumulated to a certain extent, so that the materials can be discharged through the discharge hole after passing through the metal filter screen (5) when the liquid level is higher than the top end of the cylindrical baffle (4); and the metal filter screen (5) can realize the interception effect on the solid catalyst.
In the present invention, the mesh size of the metal mesh is preferably 100 to 200 mesh, and more preferably 150 mesh.
in the invention, the cylindrical baffle (4) is not contacted with the anchor stirrer (3) all the time; namely, the anchor stirrer (3) does not touch the cylindrical baffle (4) in the working process, and the anchor stirrer also has a certain dispersion effect on the solid catalyst intercepted by the metal filter screen (5).
The invention also provides a method for producing the low-viscosity methyl silicone oil, and the device adopting the technical scheme comprises the following steps:
a) Adding octamethylcyclotetrasiloxane, hexamethyldisiloxane and a solid catalyst into a reaction kettle body, and reacting under the stirring condition to obtain the low-viscosity methyl silicone oil.
The method comprises the steps of adding octamethylcyclotetrasiloxane, hexamethyldisiloxane and a solid catalyst into a reaction kettle body (1), and reacting under a stirring condition to obtain the low-viscosity methyl silicone oil. The sources of the octamethylcyclotetrasiloxane and hexamethyldisiloxane in the present invention are not particularly limited, and commercially available products well known to those skilled in the art may be used.
in the present invention, the solid catalyst is preferably a strongly acidic cation exchange resin; wherein the solid catalyst with a particle size of 0.4mm to 1.2mm is preferably > 90%, more preferably 95%.
in the invention, the mass ratio of the octamethylcyclotetrasiloxane, the hexamethyldisiloxane and the solid catalyst is preferably (8-12): 1: (0.1 to 1), more preferably 10: 1: (0.2 to 0.8), most preferably 10: 1: 0.5.
In the invention, the octamethylcyclotetrasiloxane, the hexamethyldisiloxane and the solid catalyst respectively enter the reaction kettle body (1) through the feed inlet (2).
In the invention, the stirring condition is realized by an anchor stirrer (3); the rotation speed of the stirring is preferably 200r/min to 2000r/min, more preferably 200r/min to 1000r/min, and most preferably 500 r/min.
in the invention, the reaction temperature is preferably 75-95 ℃, and more preferably 80-90 ℃; the reaction time is preferably 6 to 10 hours, more preferably 8 hours.
After the reaction is finished, the obtained low-viscosity methyl silicone oil is discharged out of the reaction kettle body (1) from a discharge port after the solid catalyst is intercepted by the metal filter screen (5).
The device and the method for producing the low-viscosity methyl silicone oil can avoid the solid catalyst from flowing out along with reaction products, reduce the abrasion of the catalyst, reduce the loss rate of the catalyst, ensure that most of the solid catalyst is soaked in the reaction products, effectively protect the catalyst and prolong the service life of the catalyst.
The invention provides a device and a method for producing low-viscosity methyl silicone oil, wherein the device comprises the following components: a reaction kettle body; the upper part of the reaction kettle body is provided with a feeding hole, the inside of the reaction kettle body is provided with an anchor stirrer, the bottom of the reaction kettle body is an outward convex arc surface, and the lowest end of the arc surface is provided with a discharging hole; a cylindrical baffle surrounding the discharge port; the bottom end of the cylindrical baffle is attached to the arc surface, and the top end of the cylindrical baffle is provided with a metal filter screen. Compared with the prior art, the device and the method for producing the low-viscosity methyl silicone oil can avoid the solid catalyst from flowing out along with the reaction product, reduce the abrasion of the catalyst, reduce the loss rate of the catalyst, ensure that most of the solid catalyst is soaked in the reaction product, effectively protect the catalyst and prolong the service life of the catalyst.
To further illustrate the present invention, the following examples are provided for illustration.
Example 1
The structural schematic diagram of the device for producing the low-viscosity methyl silicone oil provided by the embodiment 1 of the invention is shown in figure 1; wherein, 1 is the reation kettle cauldron body, 2 is the feed inlet, 3 is anchor agitator, 4 is cylindrical baffle, 5 is the metal filter screen, 6 is the blowing valve.
The working process of producing the low-viscosity methyl silicone oil by adopting the device is as follows:
Mixing the components in a mass ratio of 10: 1: 0.5 of octamethylcyclotetrasiloxane, hexamethyldisiloxane and strong acid cation exchange resin (95 percent of granularity of 0.4-1.2 mm) respectively enter a reaction kettle body (1) through a feed inlet (2), and react under the stirring condition of the rotating speed of 500r/min at the reaction temperature of 80-90 ℃ for 8 hours to obtain low-viscosity methyl silicone oil; opening a discharge valve (6), intercepting the strong acid cation exchange resin by a metal filter screen (5) with the mesh size of 150 meshes, and discharging the reaction mixture out of the reaction kettle body (1) from a discharge port.
comparative example
The schematic structural diagram of the apparatus for producing low-viscosity methyl silicone oil provided in the comparative example is shown in fig. 2; wherein, 1 is the reaction kettle body, 2 is the feed inlet, 3 is the anchor agitator, 4 is the blowing valve.
the working process of producing the low-viscosity methyl silicone oil by adopting the device is as follows:
Mixing the components in a mass ratio of 10: 1: 0.5 of octamethylcyclotetrasiloxane, hexamethyldisiloxane and strong acid cation exchange resin (95 percent of granularity of 0.4-1.2 mm) respectively enter a reaction kettle body (1) through a feed inlet (2), and react under the stirring condition of the rotating speed of 500r/min at the reaction temperature of 80-90 ℃ for 8 hours to obtain low-viscosity methyl silicone oil; opening a discharging valve (4), and discharging the reaction mixture out of the reaction kettle body (1) through a discharging hole; and finally, recovering the strong-acid cation exchange resin by a filtration mode.
The effect data of the low-viscosity methyl silicone oil produced by the example 1 and the comparative example are compared, and the results are shown in the table 1.
TABLE 1 Effect data of example 1 and comparative example on the production of low-viscosity methyl silicone oils
| Example 1 | Comparative example | |
| Size of metal filter screen | 150 mesh | — |
| Time of filtration | - | 1h |
| Product yield | 85.7％ | 85.5％ |
| Recovery rate of solid catalyst | 100％ | 97％ |
In the comparative example 1, the outflow rate of the solid catalyst along with the reaction materials is 20-30%, and the solid catalyst can be recovered by about 95% of the outflow rate after being filtered, so that the loss rate of the solid catalyst for producing the one-kettle product is 2-3%; meanwhile, the service life of the solid catalyst is about 800 hours, and the solid catalyst needs to be supplemented periodically in the production process to meet the production requirement. In the embodiment 1 of the invention, the solid catalyst can not flow out along with the reaction materials, and the recovery rate can be up to 100% without filtration operation; and because of being protected by the methyl silicone oil product in the kettle, the service life is prolonged to more than 1000h, and meanwhile, the regular supplement is not needed.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. An apparatus for producing low viscosity methyl silicone oil comprising:
A reaction kettle body; the upper part of the reaction kettle body is provided with a feeding hole, the inside of the reaction kettle body is provided with an anchor stirrer, the bottom of the reaction kettle body is an outward convex arc surface, and the lowest end of the arc surface is provided with a discharging hole;
A cylindrical baffle surrounding the discharge port; the bottom end of the cylindrical baffle is attached to the arc surface, and the top end of the cylindrical baffle is provided with a metal filter screen.
2. The apparatus of claim 1, wherein the anchor agitator is controlled by an agitator motor disposed outside the reactor tank body.
3. the apparatus of claim 1, wherein the outlet port is provided with a discharge valve.
4. The apparatus of claim 1, wherein the metal screen has a mesh size of 100-200 mesh.
5. The apparatus of claim 1, wherein the cylindrical baffle is always out of contact with the anchor agitator.
6. A method for producing low-viscosity methyl silicone oil, characterized in that the device of any one of claims 1 to 5 is used, and the method comprises the following steps:
a) Adding octamethylcyclotetrasiloxane, hexamethyldisiloxane and a solid catalyst into a reaction kettle body, and reacting under the stirring condition to obtain the low-viscosity methyl silicone oil.
7. the method according to claim 6, wherein the mass ratio of the octamethylcyclotetrasiloxane, the hexamethyldisiloxane and the solid catalyst in step a) is (8-12): 1: (0.1 to 1).
8. The process according to claim 6, wherein the solid catalyst in step a) is a strong acid cation exchange resin, wherein the solid catalyst has a particle size of 0.4mm to 1.2mm in a proportion of > 90%.
9. The method according to claim 6, wherein the stirring speed in step a) is 200r/min to 2000 r/min.
10. The process according to claim 6, wherein the reaction in step a) is carried out at a temperature of 75 ℃ to 95 ℃ for a time of 6h to 10 h.
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| CN201910880605.7A CN110538616B (en) | 2019-09-18 | 2019-09-18 | Device and method for producing low-viscosity methyl silicone oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111318236A (en) * | 2020-03-02 | 2020-06-23 | 宁夏美邦寰宇化学有限公司 | Device and method for preparing tetrahydrofuran |
| CN114984888A (en) * | 2022-04-28 | 2022-09-02 | 华东理工大学 | Continuous esterification circulating reactor system for producing plasticizer |
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