CN109529729B - Fine chemical production organosilicon device - Google Patents

Fine chemical production organosilicon device Download PDF

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Publication number
CN109529729B
CN109529729B CN201811510127.2A CN201811510127A CN109529729B CN 109529729 B CN109529729 B CN 109529729B CN 201811510127 A CN201811510127 A CN 201811510127A CN 109529729 B CN109529729 B CN 109529729B
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rod
kettle
rod body
kettle body
stirring
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CN109529729A (en
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李宁
胡江林
尹彭霞
张双平
胡适
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China National Chemical Engineering Sixth Construction Co Ltd
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China National Chemical Engineering Sixth Construction Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10Chemical 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/06Preparatory processes

Abstract

The invention discloses a device for producing organic silicon in fine chemical industry, which comprises a dehydration kettle and a reaction kettle which are connected in sequence; the reaction kettle comprises: the middle part of the top of the kettle body is provided with a detachable top cover, the upper part of the kettle body is provided with a feeding hole, and the lower part of the kettle body is provided with a discharging hole; the stirring rod is composed of a first rod body, a second rod body and a third rod body which are sequentially connected from top to bottom, the first rod body coaxially and vertically penetrates through a top cover at the top of the kettle body and is fixed with the top cover, the length of the second rod body is 2/3 of the length of the kettle body, and the third rod body is positioned at the lower part of the kettle body; the third body of rod is hollow structure, and it does not communicate with the second body of rod, the third body of rod is provided with a plurality of screw holes along its circumference and vertically. The invention can accelerate the reaction rate and shorten the reaction time.

Description

Fine chemical production organosilicon device
Technical Field
The invention relates to the field of chemical product production devices. More specifically, the invention relates to a device for producing organic silicon by fine chemical engineering.
Background
The organic silicone oil is dimethyl silicone oil, which is polyorganosiloxane with chain structures of different polymerization degrees and is liquid at normal temperature. The dimethyl silicone oil is the silicone oil with the largest yield and the widest application. Because of the excellent characteristics of high and low temperature resistance, weather resistance, shear resistance, hydrophobicity, chemical stability, electrical insulation, low surface tension, physiological inertia and the like, the high-temperature-resistant and low-temperature-resistant composite material has been widely applied to the fields of machinery, electricity, textiles, coatings, medicine and the like as a lubricant, transformer oil, shockproof oil, a heat carrier, an additive and the like.
Disclosure of Invention
The invention aims to provide a device for producing organic silicon in a fine chemical industry, which can accelerate the reaction rate and shorten the reaction time.
To achieve these objects and other advantages in accordance with the present invention, there is provided a fine chemical production apparatus for organosilicon, comprising a dehydration kettle and a reaction kettle connected in sequence; the reaction kettle comprises:
the middle part of the top of the kettle body is provided with a detachable top cover, the upper part of the kettle body is provided with a feeding hole, and the lower part of the kettle body is provided with a discharging hole;
the stirring rod is composed of a first rod body, a second rod body and a third rod body which are sequentially connected from top to bottom, the first rod body coaxially and vertically penetrates through a top cover at the top of the kettle body and is fixed with the top cover, the length of the second rod body is 2/3 of the length of the kettle body, and the third rod body is positioned at the lower part of the kettle body; the third rod body is of a hollow structure and is not communicated with the second rod body, and a plurality of threaded holes are formed in the third rod body along the circumferential direction and the longitudinal direction of the third rod body;
the spiral air inlet pipe is connected with the first air bottle and comprises a straight pipe part and a spiral pipe part which are communicated with each other, the straight pipe part penetrates into the kettle body from the side edge of the top of the kettle body and extends to the height of the upper end of the second rod body, the straight pipe part is provided with a first valve, the spiral pipe part surrounds the second rod body and extends to the bottom end of the second rod body, the spiral pipe part is uniformly provided with a plurality of air injection pipes, the air injection pipes are communicated with the spiral pipe part, and the air injection pipes are arranged in a circular arc transition and tangent mode with the joints of the spiral pipe part; the diameter of the spiral pipe part is 1/30-1/40 of the diameter of the kettle body;
the first stirring rods are obliquely and downwards connected to the stirring rod at intervals, and the included angle between the first stirring rods and the lower part of the stirring rod is 60 degrees, and the length of each first stirring rod is set to be not interfered with the spiral air inlet pipe when the first stirring rod rotates;
the second air inlet pipe coaxially penetrates into the third rod body from the bottom of the kettle, and the stirring rod can rotate relative to the second air inlet pipe;
a plurality of second stirring rods, it is hollow structure, the second stirring rod 6 passes through screw hole threaded connection and intercommunication with the third body of rod, be provided with the gas pocket on the second stirring rod.
Preferably, 2-3 air injection holes are arranged at intervals on the spiral pipe part between the adjacent air injection pipes, and the diameter of each air injection hole is 1/30-1/40 of the diameter of the spiral pipe part.
Preferably, a switchable window is arranged on the side face of the kettle body opposite to the third rod body.
Preferably, one side of the upper part of the kettle body is provided with a vacuum-pumping pipe and a vacuum instrument, and the vacuum-pumping pipe is connected with a vacuum pump.
Preferably, a heating assembly is further included, comprising:
the shell is arranged outside the kettle body and forms a sealed interlayer space between the kettle body and the outer wall of the kettle body, the heating pipe is spirally arranged in the interlayer, and heat conduction oil is filled in the interlayer space.
Preferably, the first stirring rod is of a cubic grid structure;
its face up and face down of first stirring rod are provided with the multiunit charging tray along its length direction, the charging tray sets up along the width direction of first stirring rod, the charging tray is convex structure and concave surface upwards.
The invention also provides a method for preparing organic silicon by using the fine chemical production organic silicon device, which comprises the following steps:
adding a dimethyl siloxane mixed ring body and an end-capping agent hexamethyldisiloxane into a dehydration kettle according to a mass ratio of 6-10: 1-3, introducing nitrogen under reduced pressure to remove water in raw materials, simultaneously opening a top cover in the kettle body and taking out the top cover together with a stirring rod, dispersing and placing catalyst cation exchange resin on a material tray, wherein the addition amount of the catalyst is 8% of the total mass of the raw materials, covering the top cover, and introducing nitrogen under reduced pressure to remove water in the catalyst;
secondly, adding the dehydrated raw materials into a reaction kettle through a feeding hole, and reacting for 4 hours at a vacuum degree of-0.06 MPa and a nitrogen atmosphere at 85 ℃ until the viscosity of the mixed solution is not changed any more;
and step three, cooling the mixed solution, transferring the cooled mixed solution to a filtering device, filtering and collecting the catalyst, and removing low-boiling-point substances from the filtered mixed solution to obtain the simethicone.
The invention at least comprises the following beneficial effects: set up charging tray and first stirring rod and avoid the catalyst to concentrate on an area of the cauldron body completely, adopt the charging tray not only to make the catalyst dispersion more even, after the reaction, partial catalyst still stays on the charging tray, more conveniently gets rid of the catalyst in the dimethyl silicon oil.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a schematic structural diagram of a device for producing organic silicon in a fine chemical industry;
FIG. 2 is a schematic structural view of a spiral tube section and a gas lance arrangement;
FIG. 3 is a schematic view of the arrangement of the trays;
FIG. 4 is a schematic view of the structure of the reaction vessel used in comparative example 1.
The reactor comprises a reactor body 1, a first rod body 2, a second rod body 3, a third rod body 4, a straight pipe portion 5, a spiral pipe portion 6, a first valve 7, an air injection pipe 8, a first stirring rod 9, a second air inlet pipe 10, a second stirring rod 11, a vacuum pipe 12, a vacuum instrument 13, a shell 14 and a material tray 15.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It is to be noted that the experimental methods described in the following embodiments are all conventional methods unless otherwise specified, and the reagents and materials, if not otherwise specified, are commercially available; in the description of the present invention, the terms "lateral", "longitudinal", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
As shown in figures 1-3, the invention provides a device for producing organic silicon in fine chemical industry, which comprises a dehydration kettle and a reaction kettle which are connected in sequence; the reaction kettle comprises:
the middle part of the top of the kettle body 1 is provided with a detachable top cover;
the stirring rod is composed of a first rod body 2, a second rod body 3 and a third rod body 4 which are sequentially connected from top to bottom, the first rod body 2 coaxially and vertically penetrates through a top cover at the top of the kettle body 1, the length of the second rod body 3 is 2/3 of the length of the kettle body 1, and the third rod body 4 is positioned at the lower part of the kettle body 1; the third rod body 4 is of a hollow structure and is not communicated with the second rod body 3, a plurality of threaded holes are formed in the third rod body 4 along the circumferential direction and the longitudinal direction of the third rod body, and the second rod body 3 is in threaded connection with the third rod body 4;
the spiral air inlet pipe is connected with the first air bottle and comprises a straight pipe portion 5 and a spiral pipe portion 6 which are communicated with each other, the straight pipe portion 5 penetrates into the kettle body 1 from the side of the top of the kettle body 1 and extends to the height of the upper end of the second rod body 3, a first valve 7 is arranged on the straight pipe portion 5, the spiral pipe portion 6 surrounds the second rod body 3 and extends to the bottom end of the second rod body 3, a plurality of air injection pipes 8 are uniformly arranged on the spiral pipe portion 6, the air injection pipes 8 are communicated with the spiral pipe portion 6, and the air injection pipes 8 are arranged in arc transition and tangent with the connecting part of the spiral pipe portion 6; so that the flow direction of the gas in the gas ejector 8 is the same as the gas flow direction at the tangent point of the corresponding spiral gas inlet pipe. The diameter of the spiral pipe part 6 is 1/30-1/40 of the diameter of the kettle body 1; as shown in figure 2, the gas outlet direction of the gas injection pipe 8 is the same as the movement direction of the gas at the tangent point of the spiral pipe part 6, so that the gas flow enters the gas injection pipe 8 to be sprayed into the kettle body 1 in an accelerated state after accelerating in spiral movement, and is in a turbulent flow state, thereby realizing uniform mixing of raw materials and improving the reaction speed.
A plurality of first stirring rods 9, its interval downward sloping is connected on the second body of rod 3, and is 60 with the contained angle of second body of rod 3 lower part, the length of first stirring rod 9 sets up to do not interfere with spiral intake pipe when it rotates, and first stirring rod 9 still can be used for bearing the catalyst.
The second air inlet pipe 10 coaxially penetrates into the third rod body 4 from the bottom of the kettle in a sealing manner, and the stirring rod can rotate relative to the second air inlet pipe 10;
a plurality of second stirring rod 11, it is hollow structure, second stirring rod 11 passes through screw hole threaded connection and intercommunication with the third body of rod 4, around its axial and the even a plurality of gas pockets that are provided with of circumference on the second stirring rod 11.
In another technical scheme, 2-3 air injection holes are arranged at intervals in the spiral pipe part 6 between the adjacent air injection pipes 8, and the diameter of each air injection hole is 1/30-1/40 of the diameter of the spiral pipe part 6.
In another technical scheme, a switchable window is arranged on the side surface of the kettle body 1 opposite to the third rod body 4.
In another technical scheme, one side of the upper part of the kettle body 1 is provided with a vacuum-pumping pipe 12 and a vacuum instrument 13, and the vacuum-pumping pipe 12 is connected with a vacuum pump.
In another aspect, the apparatus further comprises a heating assembly comprising:
the shell 14 is arranged outside the kettle body 1 and forms a sealed interlayer space between the outer wall of the kettle body 1, a heating pipe is spirally arranged in the interlayer, and heat conduction oil is filled in the interlayer space.
In another technical scheme, the first stirring rod 9 is of a cubic grid structure;
its up face of first stirring rod 9 and face down are provided with multiunit charging tray 15 along its length direction, charging tray 15 sets up along the width direction of first stirring rod 9, charging tray 15 is convex structure and concave surface upwards, and first stirring rod 9 drives the catalyst on charging tray 15 and rotates when rotating, avoids the catalyst to concentrate on a region of the cauldron body 1 completely, and it is more even to adopt charging tray 15 not only to make the catalyst dispersion, and after the reaction, partial catalyst still stays on charging tray 15, more conveniently gets rid of the catalyst in the dimethyl silicon oil.
Example 1
A method for preparing organic silicon by using a device for producing organic silicon in fine chemical industry comprises the following steps:
adding a dimethyl siloxane mixed ring body (commonly called DMC) and an end-capping agent hexamethyldisiloxane (MM) into a dehydration kettle according to a mass ratio of 10:1, introducing nitrogen under reduced pressure to remove water in raw materials, simultaneously opening a top cover in the kettle body and taking out the top cover together with a stirring rod, dispersing and placing catalyst cation exchange resin (the mass molar concentration of hydrogen ions is 8mmol/g, and the particle size is 0.7MM) on a material tray, wherein the addition amount of the catalyst is 8% of the total mass of the raw materials (DMC and MM), then covering the top cover, introducing nitrogen under reduced pressure to remove water in the catalyst, and introducing nitrogen through a spiral air inlet pipe and a second air inlet pipe.
And step two, adding the dehydrated raw materials into a reaction kettle through a feeding hole, reacting for 4 hours at 85 ℃ in a nitrogen atmosphere at a vacuum degree of-0.06 MPa, wherein the viscosity of the mixed solution is not changed any more, the dynamic viscosity of the mixed solution is 567 mPa.s, nitrogen is introduced through a spiral air inlet pipe and a second air inlet pipe and is uniformly dispersed in each space of the kettle body, and the effects of fully mixing the materials, accelerating the reaction speed and preventing the catalyst from sinking to the bottom of the kettle are achieved.
And step three, cooling the mixed solution, transferring the cooled mixed solution to a filtering device, filtering and collecting the catalyst, and removing low-boiling-point substances from the filtered mixed solution to obtain the simethicone.
Comparative example 1
Adding dimethyl siloxane mixed ring bodies (commonly called DMC) and an end-capping agent hexamethyldisiloxane (MM) into a dehydration kettle according to the mass of the embodiment 1, and introducing nitrogen under reduced pressure to remove water in the raw materials; simultaneously removing water from the catalyst cation exchange resin (the mass molar concentration of hydrogen ions is 8mmol/g, and the particle size is 0.7 mm);
and step two, adding the dimethyl siloxane mixed ring body, the end-capping agent hexamethyldisiloxane and the catalyst cation exchange resin into a reaction kettle, wherein the reaction kettle is a common reaction kettle, the structure of the reaction kettle is shown in figure 4, the viscosity of the mixture does not change after the reaction is carried out for 5 hours at the temperature of 85 ℃, and the dynamic viscosity of the mixture is 536mPa & s.
And step three, cooling the mixed solution, transferring the cooled mixed solution to a filtering device, filtering and collecting the catalyst, and removing low-boiling-point substances from the filtered mixed solution to obtain the simethicone.
Based on example 1 and comparative example 1, it can be seen that the reaction rate can be accelerated from 5 hours to 4 hours by using the silicone device of the present application.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.

Claims (1)

1. A method for preparing organic silicon by using an organic silicon device produced by fine chemical engineering is characterized by comprising the following steps:
adding a dimethyl siloxane mixed ring body and an end-capping agent hexamethyldisiloxane into a dehydration kettle according to a mass ratio of 6-10: 1-3, introducing nitrogen under reduced pressure to remove water in raw materials, simultaneously opening a top cover in the kettle body and taking out the top cover together with a stirring rod, dispersing and placing catalyst cation exchange resin on a material tray, wherein the addition amount of the catalyst is 8% of the total mass of the raw materials, covering the top cover, and introducing nitrogen under reduced pressure to remove water in the catalyst;
secondly, adding the dehydrated raw materials into a reaction kettle through a feeding hole, and reacting for 4 hours at a vacuum degree of-0.06 MPa and a nitrogen atmosphere at 85 ℃ until the viscosity of the mixed solution is not changed any more;
step three, cooling the mixed solution, transferring the cooled mixed solution to a filtering device, filtering and collecting the catalyst, and removing low-boiling-point substances from the filtered mixed solution to obtain the dimethyl silicone oil;
the fine chemical production organic silicon device comprises a dehydration kettle and a reaction kettle which are connected in sequence; the reaction kettle comprises:
the middle part of the top of the kettle body is provided with a detachable top cover, the upper part of the kettle body is provided with a feeding hole, and the lower part of the kettle body is provided with a discharging hole; a vacuumizing pipe and a vacuum instrument are arranged on one side of the upper part of the kettle body, and the vacuumizing pipe is connected with a vacuum pump;
the stirring rod is composed of a first rod body, a second rod body and a third rod body which are sequentially connected from top to bottom, the first rod body coaxially and vertically penetrates through a top cover at the top of the kettle body and is fixed with the top cover, the length of the second rod body is 2/3 of the length of the kettle body, and the third rod body is positioned at the lower part of the kettle body; the third rod body is of a hollow structure and is not communicated with the second rod body, and a plurality of threaded holes are formed in the third rod body along the circumferential direction and the longitudinal direction of the third rod body; a switchable window is arranged on the side surface of the kettle body opposite to the third rod body;
the spiral air inlet pipe is connected with the first air bottle and comprises a straight pipe part and a spiral pipe part which are communicated with each other, the straight pipe part penetrates into the kettle body from the side edge of the top of the kettle body and extends to the height of the upper end of the second rod body, the straight pipe part is provided with a first valve, the spiral pipe part surrounds the second rod body and extends to the bottom end of the second rod body, the spiral pipe part is uniformly provided with a plurality of air injection pipes, the air injection pipes are communicated with the spiral pipe part, and the air injection pipes are arranged in a circular arc transition and tangent mode with the joints of the spiral pipe part; the diameter of the spiral pipe part is 1/30-1/40 of the diameter of the kettle body; 2-3 air injection holes are arranged at intervals on the spiral pipe part between every two adjacent air injection pipes, and the diameter of each air injection hole is 1/30-1/40 of the diameter of the spiral pipe part;
the first stirring rods are obliquely and downwards connected to the second rod body at intervals, the included angle between the first stirring rods and the lower part of the second rod body is 60 degrees, and the length of each first stirring rod is set to be not interfered with the spiral air inlet pipe when the first stirring rod rotates; the first stirring rod is of a square grid structure; a plurality of groups of material trays are arranged on the upward surface and the downward surface of the first stirring rod along the length direction of the first stirring rod, the material trays are arranged along the width direction of the first stirring rod, and the material trays are of circular arc structures and have upward concave surfaces;
the second air inlet pipe coaxially penetrates into the third rod body from the bottom of the kettle, and the stirring rod can rotate relative to the second air inlet pipe;
the second stirring rods are of hollow structures, the second stirring rods 6 are in threaded connection and communication with the third rod body through threaded holes, and air holes are formed in the second stirring rods;
a heating assembly, comprising: the shell is arranged outside the kettle body and forms a sealed interlayer space between the kettle body and the outer wall of the kettle body, the heating pipe is spirally arranged in the interlayer, and heat conduction oil is filled in the interlayer space.
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