CN109529729A - Fine chemistry industry produces Organic Silicon Plant - Google Patents
Fine chemistry industry produces Organic Silicon Plant Download PDFInfo
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- CN109529729A CN109529729A CN201811510127.2A CN201811510127A CN109529729A CN 109529729 A CN109529729 A CN 109529729A CN 201811510127 A CN201811510127 A CN 201811510127A CN 109529729 A CN109529729 A CN 109529729A
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- rod
- autoclave body
- stirring rod
- organic silicon
- tube portion
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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
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
Abstract
The invention discloses fine chemistry industries to produce Organic Silicon Plant, including sequentially connected dehydrating kettle and reaction kettle；The reaction kettle, comprising: autoclave body, at the top of middle part there is dismountable top cover, upper part is provided with feed inlet, and lower part is provided with discharge port；Stirring rod, its by under upper sequentially connected first body of rod, second body of rod and the third body of rod constitute, first body of rod coaxial vertical passes through the top cover and fixed thereto at the top of autoclave body, and the length of second body of rod is the 2/3 of autoclave body length, and the third body of rod is located at the lower part of the autoclave body；The third body of rod is hollow structure, is not connected to second body of rod, the third body of rod is circumferentially and longitudinally provided with multiple threaded holes along it.The present invention can speed up reaction rate, shorten the reaction time.
Description
Technical field
The present invention relates to chemical products process units fields.It is more particularly related to a kind of fine chemistry industry production
Organic Silicon Plant.
Background technique
Organic silicone oil is typically all dimethicone, it is a kind of poly organo of different polymerization degree chain structure
Alkane is liquid under room temperature.Dimethicone is yield maximum, most widely used silicone oil kind.Because having resistant of high or low temperature, weather-proof
The excellent characteristics such as property, shear resistant, hydrophobicity, chemical stability, electrical insulating property, low surface tension and physiological inertia, are made
It is widely used in mechanical, electrical, weaving, coating and medicine for lubricant, transformer oil, shockproof oil, heat carrier and additive etc.
Equal fields.
Summary of the invention
The object of the present invention is to provide fine chemistry industries to produce Organic Silicon Plant, can speed up reaction rate, when shortening reaction
Between.
In order to realize these purposes and other advantages according to the present invention, fine chemistry industry production Organic Silicon Plant is provided,
Including sequentially connected dehydrating kettle and reaction kettle；The reaction kettle, comprising:
Autoclave body, at the top of middle part there is dismountable top cover, upper part is provided with feed inlet, and lower part is provided with discharging
Mouthful；
Stirring rod, by under upper sequentially connected first body of rod, second body of rod and the third body of rod constitute, described first
Body of rod coaxial vertical passes through the top cover and fixed thereto at the top of autoclave body, and the length of second body of rod is the 2/3 of autoclave body length, institute
State the lower part that the third body of rod is located at the autoclave body；The third body of rod is hollow structure, is not connected to second body of rod, described the
Three bodies of rod are circumferentially and longitudinally provided with multiple threaded holes along it；
Spiral air inlet is connect with the first gas cylinder, and the spiral air inlet includes interconnected straight-tube portion and spiral shell
Coil sections, the straight-tube portion is as the height where the avris at the top of autoclave body penetrates the autoclave body and extends to the second body of rod upper end
Degree, the straight-tube portion are provided with the first valve, and the spiral tube portion encloses the second body of rod winding, and extends to second body of rod
Bottom end, spiral tube portion is evenly arranged with multiple air jet pipes, and the air jet pipe is connected to the spiral tube portion, and air jet pipe is set
It is set to and the junction arc transition of spiral tube portion and tangent；The helix tube section diameter is the 1/30~1/ of autoclave body diameter
40；
Multiple first stirring rod, interval, which tilts down, to be connected on stirring rod, and is with the angle of stirring rod lower part
60 °, the length of first stirring rod is set as its rotation Shi Buyu spiral air inlet and interferes；
Second air inlet pipe is coaxially penetrated by bottom in the third body of rod, and the stirring rod can be with respect to the second air inlet
Pipe rotation；
Multiple second stirring rod, are hollow structure, and second stirring rod 6 is connected with the third body of rod by threaded hole screw thread
It connects and is connected to, be provided with stomata in second stirring rod.
Preferably, the spiral tube portion between adjacent air jet pipe is arranged at intervals with 2-3 fumarole, the jet bore dia
For helix tube section diameter 1/30~1/40.
Preferably, the autoclave body side is with respect to being provided with switchable window at the third body of rod.
Preferably, the side on the autoclave body top is provided with vacuum-pumping tube and vacuum instrumentation, the vacuum-pumping tube with
Vacuum pump is connected.
It preferably, further include heating component comprising:
Shell is set to outside autoclave body, forms the interlayer space of sealing between the autoclave body outer wall, in the interlayer
It spirals and is provided with heating tube, be filled with conduction oil in the interlayer space.
Preferably, first stirring rod is cube network；
Its face upward of first stirring rod and face directed downwardly are provided with multiple groups charging tray, the material along its length
Disk is arranged along the width direction of the first stirring rod, and the charging tray is arc-shaped structure and concave upright.
The method that Organic Silicon Plant prepares organosilicon is produced using fine chemistry industry the present invention also provides a kind of, including following
Step:
Step 1: by dimethyl siloxane mixed methylcyclosiloxane and end-capping reagent hexamethyldisiloxane 6~10:1~3 in mass ratio
Be added dehydrating kettle in, decompression be passed through nitrogen removal raw material in moisture, while in autoclave body open top cover together with stirring rod together
It takes out, catalyst cation exchanger resin is scattered on charging tray, the additional amount of catalyst is the 8% of total mass of raw material,
Top cover is covered later, decompression is passed through the moisture in nitrogen removal catalyst；
Step 2: dewatered raw material is added in reaction kettle by feed inlet, vacuum degree, nitrogen in -0.06MPa
4 hours are reacted in atmosphere at 85 DEG C, the viscosity of mixed liquor is no longer changed；
Step 3: being filtered collection, filtered mixing to catalyst for filter device is transferred to after mixed liquor cooling
Liquid carries out de- low-boiling-point substance processing to get dimethicone.
The present invention is include at least the following beneficial effects: setting charging tray and the first stirring rod avoid catalyst from being totally absorbed in kettle
One region of body can not only make catalyst dispersion more evenly using charging tray, and after reaction, partial catalyst also stays in charging tray
On, it is more convenient to remove the catalyst in dimethicone.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of fine chemistry industry production Organic Silicon Plant；
Fig. 2 is the structural schematic diagram of spiral tube portion and air jet pipe setting；
Fig. 3 is the setting schematic diagram of charging tray；
Fig. 4 is the structural schematic diagram of the reaction kettle used in comparative example 1.
1 autoclave body, 2 first bodies of rod, 3 second bodies of rod, the 4 third bodies of rod, 5 straight-tube portions, 6 spiral tube portions, 7 first valves, 8
Air jet pipe, 9 first stirring rod, 10 second air inlet pipe, 11 second stirring rod, 12 vacuum-pumping tubes, 13 vacuum instrumentations, 14 shells, 15
Charging tray.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
It should be noted that experimental method described in following embodiments is unless otherwise specified conventional method, institute
Reagent and material are stated, unless otherwise specified, is commercially obtained；In the description of the present invention, term " transverse direction ", " vertical
To ", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", the instructions such as "outside" side
Position or positional relationship are to be based on the orientation or positional relationship shown in the drawings, and are merely for convenience of description of the present invention and simplification of the description,
It is not that the device of indication or suggestion meaning or element must have a particular orientation, be constructed and operated in a specific orientation, because
This is not considered as limiting the invention.
As shown in Figures 1 to 3, the present invention provides a kind of fine chemistry industry production Organic Silicon Plant, including sequentially connected dehydration
Kettle and reaction kettle；The reaction kettle, comprising:
Autoclave body 1, at the top of middle part have dismountable top cover；
Stirring rod, by under upper sequentially connected first body of rod 2, second body of rod 3 and the third body of rod 4 constitute, it is described
First body of rod, 2 coaxial vertical passes through the top cover at 1 top of autoclave body, and the length of second body of rod 3 is the 2/3 of 1 length of autoclave body, described
The third body of rod 4 is located at the lower part of the autoclave body 1；The third body of rod 4 is hollow structure, is not connected to second body of rod 3, described
The third body of rod 4 is circumferentially and longitudinally provided with multiple threaded holes along it, and second body of rod 3 is threadedly coupled with the third body of rod 4；
Spiral air inlet is connect with the first gas cylinder, and the spiral air inlet includes interconnected straight-tube portion 5 and spiral shell
Coil sections 6, the straight-tube portion 5 penetrate the autoclave body 1 by the avris at 1 top of autoclave body and extend to second body of rod, 3 upper end institute
Height, the straight-tube portion 5 is provided with the first valve 7, and the spiral tube portion 6 encloses second body of rod, 3 winding, and extends
To the bottom end of second body of rod 3, spiral tube portion 6 is evenly arranged with multiple air jet pipes 8, the air jet pipe 8 and the spiral pipe portion
Points 6 connections, air jet pipe 8 are set as and the junction arc transition of spiral tube portion 6 and tangent；To make gas in air jet pipe 8
Flow direction it is identical as airflow direction at corresponding spiral air inlet point of contact.6 diameter of spiral tube portion is 1 diameter of autoclave body
1/30~1/40；As shown in Fig. 2, 8 outgassing direction of air jet pipe is identical as the direction of motion of gas at the point of contact of spiral tube portion 6,
After guaranteeing that flow spiral movement accelerates, enters back into air jet pipe 8 and acceleration mode is kept to spray into autoclave body 1, be in turbulence state, realize
Raw material is uniformly mixed and improves reaction speed.
Multiple first stirring rod 9, interval, which tilts down, to be connected on second body of rod 3, and the folder with second body of rod, 3 lower part
Angle is 60 °, and the length of first stirring rod 9 is set as its rotation Shi Buyu spiral air inlet and interferes, the first stirring rod 9
It can also be used to carry catalyst.
Second air inlet pipe 10 is penetrated in the third body of rod 4 by bottom co-axial seal, and the stirring rod can be with respect to
The rotation of two air inlet pipe 10；
Multiple second stirring rod 11, are hollow structure, and second stirring rod 11 passes through threaded hole spiral shell with the third body of rod 4
Line is connected to and in communication with, and is evenly provided with multiple stomatas around its axial and circumferential in second stirring rod 11.
In another technical solution, the spiral tube portion 6 between adjacent air jet pipe 8 is arranged at intervals with 2-3 fumarole, institute
Stating jet bore dia is 6 diameter 1/30~1/40 of spiral tube portion.
In another technical solution, 1 side of autoclave body is with respect to being provided with switchable window at the third body of rod 4.
In another technical solution, the side on 1 top of autoclave body is provided with vacuum-pumping tube 12 and vacuum instrumentation 13,
The vacuum-pumping tube 12 is connected with vacuum pump.
It further include heating component in another technical solution comprising:
Shell 14 is set to outside autoclave body 1, and the interlayer space of sealing, the folder are formed between 1 outer wall of autoclave body
Layer inside turn is provided with heating tube, is filled with conduction oil in the interlayer space.
In another technical solution, first stirring rod 9 is cube network；
Its face upward of first stirring rod 9 and face directed downwardly are provided with multiple groups charging tray 15, institute along its length
The width direction that charging tray 15 is stated along the first stirring rod 9 is arranged, and the charging tray 15 is arc-shaped structure and concave upright, the first stirring
Stick 9 drives the catalyst rotation on charging tray 15, avoids catalyst from being totally absorbed in a region of autoclave body 1, use in rotation
Charging tray 15 can not only make catalyst dispersion more evenly, and after reaction, partial catalyst also stays on charging tray 15, be more convenient removal
Catalyst in dimethicone.
Embodiment 1
A method of organosilicon is prepared using fine chemistry industry production Organic Silicon Plant, comprising the following steps:
Step 1: by dimethyl siloxane mixed methylcyclosiloxane (being commonly called as DMC) and end-capping reagent hexamethyldisiloxane (MM) by matter
Amount is added in dehydrating kettle than 10:1, and decompression is passed through the moisture in nitrogen removal raw material, while opening top cover together with stirring in autoclave body
It mixes bar to take out together, by catalyst cation exchanger resin, (hydrionic molality is 8mmol/g, partial size is
It 0.7mm) is scattered on charging tray, the additional amount of catalyst is the 8% of raw material (DMC and MM) gross mass, later by top cover lid
On, decompression is passed through the moisture in nitrogen removal catalyst, and the nitrogen being passed through can pass through spiral air inlet and the second air inlet pipe.
Step 2: dewatered raw material is added in reaction kettle by feed inlet, vacuum degree, nitrogen in -0.06MPa
4 hours are reacted in atmosphere at 85 DEG C, the viscosity of mixed liquor is no longer changed, dynamic viscosity 567mPas, and nitrogen is logical
It crosses spiral air inlet and the second air inlet pipe is passed through, be dispersed in each space of autoclave body, play and mix well material acceleration instead
Speed is answered, prevents catalyst from sinking to the effect of bottom.
Step 3: being filtered collection, filtered mixing to catalyst for filter device is transferred to after mixed liquor cooling
Liquid carries out de- low-boiling-point substance processing to get dimethicone.
Comparative example 1
Step 1: by dimethyl siloxane mixed methylcyclosiloxane (being commonly called as DMC) and end-capping reagent hexamethyldisiloxane (MM) by real
The quality for applying example 1 is added in dehydrating kettle, and decompression is passed through the moisture in nitrogen removal raw material；Catalyst cation exchange is sloughed simultaneously
The moisture of resin (hydrionic molality is 8mmol/g, partial size 0.7mm)；
Step 2: dimethyl siloxane mixed methylcyclosiloxane, end-capping reagent hexamethyldisiloxane and catalyst cation are exchanged
Resin is added in reaction kettle, and reaction kettle is common response kettle, and structure is as shown in figure 4, react 5 hours at being 85 DEG C in temperature
The viscosity of mixture is no longer changed afterwards, dynamic viscosity 536mPas.
Step 3: being filtered collection, filtered mixing to catalyst for filter device is transferred to after mixed liquor cooling
Liquid carries out de- low-boiling-point substance processing to get dimethicone.
It is small by 5 based on embodiment 1 and comparative example 1 it is found that the Organic Silicon Plant using the application can speed up reaction speed
When can foreshorten to 4 hours.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (7)
1. fine chemistry industry produces Organic Silicon Plant, which is characterized in that including sequentially connected dehydrating kettle and reaction kettle；The reaction
Kettle, comprising:
Autoclave body, at the top of middle part there is dismountable top cover, upper part is provided with feed inlet, and lower part is provided with discharge port；
Stirring rod, by under upper sequentially connected first body of rod, second body of rod and the third body of rod constitute, first body of rod
Coaxial vertical passes through the top cover and fixed thereto at the top of autoclave body, and the length of second body of rod is the 2/3 of autoclave body length, and described the
Three bodies of rod are located at the lower part of the autoclave body；The third body of rod is hollow structure, is not connected to second body of rod, the third bar
Body is circumferentially and longitudinally provided with multiple threaded holes along it；
Spiral air inlet is connect with the first gas cylinder, and the spiral air inlet includes interconnected straight-tube portion and helix tube
Part, the straight-tube portion as the height where the avris at the top of autoclave body penetrates the autoclave body and extends to the second body of rod upper end,
The straight-tube portion is provided with the first valve, and the spiral tube portion encloses the second body of rod winding, and extends to second body of rod
Bottom end, spiral tube portion are evenly arranged with multiple air jet pipes, and the air jet pipe is connected to the spiral tube portion, air jet pipe setting
For the junction arc transition with spiral tube portion and tangent；The helix tube section diameter is the 1/30~1/ of autoclave body diameter
40；
Multiple first stirring rod, interval, which tilts down, to be connected on second body of rod, and is with the angle of the second body of rod lower part
60 °, the length of first stirring rod is set as its rotation Shi Buyu spiral air inlet and interferes；
Second air inlet pipe is coaxially penetrated by bottom in the third body of rod, and the stirring rod can turn with respect to the second air inlet pipe
It is dynamic；
Multiple second stirring rod, are hollow structure, and second stirring rod 6 is threadedly coupled simultaneously with the third body of rod by threaded hole
It is connected to, is provided with stomata in second stirring rod.
2. fine chemistry industry as described in claim 1 produces Organic Silicon Plant, which is characterized in that the spiral between adjacent air jet pipe
Tube portion is arranged at intervals with 2-3 fumarole, and the jet bore dia is helix tube section diameter 1/30~1/40.
3. fine chemistry industry as described in claim 1 produces Organic Silicon Plant, which is characterized in that the autoclave body side is with respect to third
Switchable window is provided at the body of rod.
4. fine chemistry industry as described in claim 1 produces Organic Silicon Plant, which is characterized in that the side on the autoclave body top is set
It is equipped with vacuum-pumping tube and vacuum instrumentation, the vacuum-pumping tube is connected with vacuum pump.
5. fine chemistry industry as described in claim 1 produces Organic Silicon Plant, which is characterized in that it further include heating component, packet
It includes:
Shell is set to outside autoclave body, and the interlayer space of sealing, the interlayer inside turn are formed between the autoclave body outer wall
It is provided with heating tube, is filled with conduction oil in the interlayer space.
6. fine chemistry industry as described in claim 1 produces Organic Silicon Plant, which is characterized in that first stirring rod is cube
Network；
Its face upward of first stirring rod and face directed downwardly are provided with multiple groups charging tray, the charging tray edge along its length
The width direction of first stirring rod is arranged, and the charging tray is arc-shaped structure and concave upright.
7. a kind of method for preparing organosilicon using fine chemistry industry production Organic Silicon Plant, which comprises the following steps:
Step 1: dimethyl siloxane mixed methylcyclosiloxane and end-capping reagent hexamethyldisiloxane 6~10:1 in mass ratio~3 are added
In dehydrating kettle, decompression is passed through the moisture in nitrogen removal raw material, while opening top cover in autoclave body and taking out together together with stirring rod,
Catalyst cation exchanger resin is scattered on charging tray, the additional amount of catalyst is the 8% of total mass of raw material, later will
Top cover covers, and decompression is passed through the moisture in nitrogen removal catalyst；
Step 2: dewatered raw material is added in reaction kettle by feed inlet, vacuum degree, nitrogen atmosphere in -0.06MPa
In 4 hours are reacted at 85 DEG C, the viscosity of mixed liquor is no longer changed；
Step 3: by mixed liquor it is cooling after be transferred to filter device, collection is filtered to catalyst, filtered mixed liquor into
The de- low-boiling-point substance processing of row is to get dimethicone.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811510127.2A CN109529729B (en) | 2018-12-11 | 2018-12-11 | Fine chemical production organosilicon device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811510127.2A CN109529729B (en) | 2018-12-11 | 2018-12-11 | Fine chemical production organosilicon device |
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| CN109529729B CN109529729B (en) | 2021-11-02 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116574262A (en) * | 2023-05-15 | 2023-08-11 | 浙江佳汇新材料有限公司 | Vinyl silicone oil preparation process |
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