CN105542168B - A kind of poly- methyltriethoxysilane double tower continuous production technology - Google Patents
A kind of poly- methyltriethoxysilane double tower continuous production technology Download PDFInfo
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- CN105542168B CN105542168B CN201510969329.3A CN201510969329A CN105542168B CN 105542168 B CN105542168 B CN 105542168B CN 201510969329 A CN201510969329 A CN 201510969329A CN 105542168 B CN105542168 B CN 105542168B
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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
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
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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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- 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
- C08G77/32—Post-polymerisation treatment
- C08G77/34—Purification
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Abstract
The invention discloses a kind of poly- methyltriethoxysilane double tower continuous production technologies, include the following steps: (a) cleaning equipment；(b) hydraulic pressure detects；(c) the first tower reactor and the second tower reactor are heated；(d) poly- methyltriethoxysilane is prepared；(e) poly- methyltriethoxysilane crude product is refined.The present invention carries out cleaning to equipment, remove the dirt and impurity on the inner wall of the first tower, the first tower reactor, the second tower and the second tower reactor, the cleannes of reaction environment are improved, reduces in reaction mass and is mixed into impurity, by being detected to equipment hydraulic pressure, improve safety, and reaction is carried out continuously using double tower, production capacity is improved, production efficiency is increased substantially, recruitment number and labor intensity are significantly reduced, and the quality of poly- methyltriethoxysilane finished product obtained is uniform, stablizes.
Description
Technical field
The invention belongs to poly- methyltriethoxysilane synthesis technical fields, and in particular to a kind of poly- methyltriethoxy silane
Alkane double tower continuous production technology.
Background technique
Organosilicon is that one kind is wide in variety, has excellent performance, using wide novel chemical product.In organoalkoxysilane
Containing the group completely different there are two chemical property in intermediate, the two groups can be close with organic matter, inorganic matter respectively
In conjunction with, become the bridge between organic matter and inorganic matter, thus it is widely used as inorganic filler surface modifying agent, modified paint agent
And modifier etc..Currently, all kinds of silane, silicone intermediate and the silicone oil as made from them, silicon rubber, silicone resin
Products such as (including their secondary operation product), in electric, building, automobile, weaving, light industry, cosmetics, medical treatment, food
The industries such as product are widely applied, and have played positive effect.
Over the past decade, organosilicon product at home and abroad have developed rapidly, quick with national economy especially in China
Development, be engaged in organosilicon scientific research, production and application unit spring up like bamboo shoots after a spring rain as development and growth.Come for years, has
The consumption figure of machine silicon product is pushed ahead with annual more than ten percent or even tens percent speed, and is always maintained at strong
The growth momentum of strength.Poly- methyltriethoxysilane is the oligomer of methyltriethoxysilane, and average degree of polymerization is 2~3, tool
There is special fragrance, be the liquid that can be burnt, in the presence of having acid or alkali, meets water facile hydrolysis, condensation, hydrolysis condensation product is high
Molecular compound, finally crosslinking forms a film.Poly- methyltriethoxysilane is one of organic silicon water-proofing agent series products, belongs to solvent
Type, for neutral waterproofing agent.This product has good weather-proof, ageing-resistant, anti-pollution, chemical-resistant resistance and hydrophobic, gas permeability.
The conventional method for synthesizing poly- methyltriethoxysilane is that the monomethyl trichlorine silicon measured is squeezed into reaction kettle
Alkane is warming up to 60~90 degree, and dehydrated alcohol is added dropwise in kettle from dehydrated alcohol head tank, is passed through nitrogen bubbling and flow back instead
It answers.In temperature rising reflux reaction process, Trichloromethyl silane is reacted with dehydrated alcohol generates poly- methyltriethoxysilane and chlorine
Change hydrogen, the air-flow of rising enters condenser, and condensate liquid flows back into reaction kettle, and not solidifying gas chlorination hydrogen removes tail gas absorption.Reaction knot
Beam, remaining reaction solution is exactly poly- methyltriethoxysilane product in kettle.The reaction time of this production method is long, a batch of material
Time-consuming 30h or more is wanted, production efficiency is low.
Summary of the invention
Above-mentioned technical problem present in present invention aims to solve the prior art provides a kind of poly- methyl triethoxy
Silane double tower continuous production technology carries out cleaning, the first tower of removal, the first tower reactor, the second tower and the second tower to equipment
Dirt and impurity on the inner wall of kettle improve the cleannes of reaction environment, reduce in reaction mass and are mixed into impurity, by equipment
Hydraulic pressure detection improves safety, and is carried out continuously reaction using double tower, improves production capacity, increases substantially production efficiency, recruitment
Number and labor intensity are significantly reduced, and the quality of poly- methyltriethoxysilane finished product obtained is uniform, stablizes.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme:
A kind of poly- methyltriethoxysilane double tower continuous production technology, it is characterised in that preparation step includes:
(a) cleaning equipment: first preparing the clear water of two barrels of 120L, and the temperature of clear water is controlled at 20~22 DEG C, then by one
The clear water of bucket 120L directly rinses the first tower, while the clear water of another barrel of 120L is directly rinsed the second tower, is cleaning the first tower
Before kettle and the second tower reactor, detection work is carried out, then using two high-pressure nozzles to the inner wall and the second tower reactor of the first tower reactor
Inner wall directly washed away, the hard dirt on the inner wall of the first tower reactor and the inner wall of the second tower reactor is smashed, flushing time
Continue 10~15min, then the first tower, the second tower, the first tower reactor and the second tower reactor are estimated by operator, reach mark
On time, cleaning can be terminated；
(b) hydraulic pressure detects: after completing cleaning, the first tower being connect with the first tower reactor, by the second tower and the second tower
Kettle connection detects the first tower and the first tower reactor using hydraulic pressure detection, first empties the air in the first tower and the first tower reactor, connect
The pressure of water is slowly increased to 0.7MPa, keep pressure 30min, pressure be then down to 0.6MPa, keep 1~2h, detection
The leakage situation of the junction of first tower and the first tower reactor drains water after detection is qualified, then to the first tower and the first tower reactor into
The drying of row compressed air, the second tower and the second tower reactor use and the first tower hydraulic pressure identical as the first tower reactor detects, detection second
The leakage situation of the junction of tower and the second tower reactor drains water, then press the second tower and the second tower reactor after detection is qualified
Contracting air blow drying；
(c) the first tower reactor and the second tower reactor are heated: opening the jacket steam valve of the first tower reactor and the second tower reactor respectively,
Boiler Steam is passed through in the jacket steam valve of first tower reactor, the air pressure controlled in the collet of the first tower reactor is less than 0.2MPa, steams
For the heat transfer of vapour into the first tower reactor, steam heats the first tower reactor, while being passed through in the jacket steam valve of the second tower reactor
Boiler Steam, the air pressure controlled in the collet of the second tower reactor are less than 0.2MPa, and the heat transfer of steam is into the second tower reactor, steam
The second tower reactor is heated, temperature detection then is carried out to the first tower reactor and the second tower reactor, detect every 8min primary, control the
The temperature of the temperature of one tower reactor and the second tower reactor is greater than 90 DEG C；
(d) prepare poly- methyltriethoxysilane: reaction raw materials liquid ethyl alcohol is passed into the second tower after calculating by metering pump
In, and the ethyl alcohol of entrance is heated and is vaporized, then heating work is carried out to the second tower, while the temperature for controlling the second tower reactor is big always
In 90 DEG C, when the tower top temperature of the first tower detects 60 DEG C, start metering pump, starts to throw monomethyl into from the top of the first tower
Trichlorosilane, while the feed rate for controlling Trichloromethyl silane and ethyl alcohol is adjusted, it is maintained at monomethyl in the unit time
The molar ratio 1:2.9 of trichlorosilane and ethyl alcohol starts magnetic force when the liquid level of the first tower reactor reaches the l/2~2/3 of tower reactor volume
The material of first tower reactor is transported to the top of the second tower by pump, and remains that material liquid level is in the l/ of total volume in the first tower reactor
Reaction balance will gradually be tended in 2~2/3 sections, after system feeding, Trichloromethyl silane and ethyl alcohol are in the second tower and second
It comes into full contact with and reacts in tower reactor, the tower top of the second tower reacts remaining gas and is passed into the first tower, and the gas of the first tower is passed through
It condenses into condenser, is flowed back into the first tower reactor by the condensate liquid after condenser, the tail gas of condenser discharge is passed into hydrogen
In sodium hydroxide solution, the hydrogen chloride gas in tail gas is absorbed, Trichloromethyl silane and ethyl alcohol are simultaneously in the first tower and the first tower
It is reacted in kettle, to 8~9h of reaction in reaction, the second tower and the second tower reactor in the first tower and the first tower reactor, the second tower
Material gradually increases in kettle, when material reaches 2/3 volume in the second tower reactor, starts discharging pump, carries out continuous discharge, protect simultaneously
Holding material liquid level in the second tower reactor, in the section l/2~2/3 of total volume, continuous outputting material obtains poly- methyltriethoxy silane
Alkane crude product；
(e) it refines poly- methyltriethoxysilane crude product: obtained poly- methyltriethoxysilane crude product is first passed into
In first rectifying column, the light impurities and heavy impurity of poly- methyltriethoxysilane crude product are removed, first rectifying column is obtained
Material be passed into Second distillation column by tilting down channel, using reboiler to Second distillation column heat, to material carry out
Poly- methyltriethoxysilane crude product refining is obtained poly- methyltriethoxysilane finished product by rectification and purification.
Further, in step (a), detection work is carried out before cleaning the first tower reactor and the second tower reactor and specifically includes cleaning
The installation of the model and technical parameter, cleaning pump of pump, each component seat in the plane, connecting pipe connection and supply water tank water level.
Further, in step (c), the lower head selection standard elliposoidal of the collet of the first tower reactor and the second tower reactor, upper envelope
Head selects 90 ° of flanged conical heads.
Further, in step (d), during the reaction, material liquid in the first tower reactor and the second tower reactor is observed using visor
The height of position.
The present invention is by adopting the above-described technical solution, have the advantages that
The present invention carries out cleaning to equipment, is rinsed work using inner wall of the room temperature clear water to the first tower and the second tower
Make, the impurity on the inner wall of the first tower and the second tower is discharged with clear water, and uses high-pressure nozzle directly in the first tower reactor
Wall and the inner wall of the second tower reactor are washed away, and the hard dirt on the inner wall of the first tower reactor and the inner wall of the second tower reactor is smashed,
The dirt and impurity on the inner wall of the first tower reactor and the second tower reactor are removed, the cleannes of reaction environment can be effectively improved, is reduced
Impurity is mixed into reaction mass.The present invention by detecting to equipment hydraulic pressure, let out with the junction of the first tower reactor by the first tower of detection
Situation is leaked, guarantees to seal between the first tower and the first tower reactor, prevents reaction process gas from leaking, detect the second tower and the second tower reactor
Junction leakage situation, guarantee to seal between the second tower and the second tower reactor, prevent reaction process gas from leaking, improve safety
Property.And reaction raw materials liquid dehydrated alcohol is passed into the second tower by the present invention, throws monomethyl trichlorine into from the top of the first tower
Silane, while the feed rate for controlling Trichloromethyl silane and ethyl alcohol is adjusted, start magnetic drive pump for the material of the first tower reactor
The top of the second tower, Trichloromethyl silane and ethyl alcohol is transported to come into full contact with and react in the second tower and the second tower reactor, the
The tower top of two towers reacts remaining gas and is passed into the first tower, and the gas of the first tower, which is passed into condenser, to be condensed, and condensation is passed through
Condensate liquid after device flows back into the first tower reactor, and Trichloromethyl silane and ethyl alcohol carry out in the first tower and the first tower reactor simultaneously
Reaction can be achieved with double tower in this way and be carried out continuously reaction, in reaction process, the temperature and the second tower reactor of the first tower reactor of strict control
Temperature, while adjusting and controlling the feed rate of Trichloromethyl silane and ethyl alcohol, be maintained at monomethyl three in the unit time
The molar ratio 1:2.9 of chlorosilane and ethyl alcohol improves the production capacity of poly- methyltriethoxysilane product, increases substantially production effect
Rate, recruitment number and labor intensity are significantly reduced, and the quality of poly- methyltriethoxysilane finished product obtained is uniform, stablizes,
With high economic value.
Detailed description of the invention
The present invention will be further explained below with reference to the attached drawings:
Fig. 1 is the flow chart for inventing a kind of poly- methyltriethoxysilane double tower continuous production technology；
Fig. 2 is the structural block diagram for inventing a kind of poly- methyltriethoxysilane double tower continuous production technology.
Specific embodiment
It as depicted in figs. 1 and 2, is a kind of poly- methyltriethoxysilane double tower continuous production technology of the present invention, preparation
Step includes:
(a) cleaning equipment: judge the first tower 1, the second tower 3, the first tower reactor 2 and the second tower reactor 4 without bright before washing
Aobvious damage, if there is the place of apparent damage, should repair work in time.When to the first tower 1 and the cleaning of the second tower 3, by
It is smaller in its bore, high pressure washing, meeting waste water resource are such as used, therefore be directly rinsed with room temperature clear water.Prepare two barrels
The clear water of 120L, the temperature of clear water are controlled at 20~22 DEG C, and the clear water of one barrel of 120L is directly then rinsed the first tower 1, behaviour
Make personnel to be directly flushed on the inner wall of the first tower 1 using container, the opening close to the first tower 1 is rinsed clockwise, and water is suitable
The first tower 1 inner wall outflow, take away impurity, while the clear water of another barrel of 120L is directly rinsed into the second tower 3, operator adopts
It is directly flushed to container on the inner wall of the second tower 3, the opening close to the second tower 3 is rinsed clockwise, and water is along the first tower 1
Inner wall outflow, take away impurity, when the basic residue 1/3 of the clear water in two barrels, the first tower 1 and the second tower 3 estimated, if first
When tower 1 and the second tower 3 are without foreign matter and trace is evident that, the cleaning to the first tower 1 and the second tower 3 can be stopped, if
First tower 1 and the second tower 3 can continue for remaining clear water to be finished there are when visible foreign matter and trace.First tower 1 and the second tower
Impurity on 3 inner wall is discharged with clear water, can effectively improve the cleannes of reaction environment, reduce be mixed into reaction mass it is miscellaneous
Matter.
Before cleaning the first tower reactor 2 and the second tower reactor 4, check whether the model of cleaning pump and technical parameter meet cleaning
Work, checks whether cleaning pump is horizontally mounted, and checks each component seat in the plane whether there is or not damage, and whether each connecting pipe connects reliably, and
And also to check whether the water level in the water tank of supply reaches standard, when being washed away using high pressure, need in routine observation water tank
Water level should be replenished in time when water level is low.When confirmation checks and meets regulation, starting cleaning pump 8~12min of idle running, using two
A high-pressure nozzle directly washes away the inner wall of the first tower reactor 2 and the inner wall of the second tower reactor 4, and the pressure process of high-pressure nozzle is answered
This slowly pressurizes, and in pressure process, the operator of high-pressure nozzle must with pressure regulation personnel's effective communication, when boosting
Specific instruction should be given, forbids increasing hydraulic pressure in the unwitting situation of operator of high-pressure nozzle, be washed away entirely
Journey, it is necessary to high-pressure nozzle be put into the first tower reactor 2 and the second tower reactor 4, safety is improved.In the souring of high-pressure nozzle
Under, the hard dirt on the inner wall of the first tower reactor 2 and the inner wall of the second tower reactor 4 is smashed, flushing time continues 10~15min,
Then the first tower reactor 2 and the second tower reactor 4 are estimated by operator, if the first tower reactor 2 and the second tower reactor 4 are without clearly visible
Foreign matter and trace when, cleaning can be terminated.Operator need to be into when high pressure washes away the first tower reactor 2 and the second tower reactor 4
Row effective protection measure, specific as shown in table 1:
| Protect position | Safeguard procedures |
| Cephalic protection | Damage of the water to eyes is prevented using the side bumper of goggles. |
| Body protection | The impact of jet stream backwash is blocked using protective garment. |
| Hand protection | Using gloves, increases frictional force, prevent high-pressure nozzle from sliding. |
1 safeguard procedures of table
(b) hydraulic pressure detects: after completing cleaning, the first tower 1 being connect with the first tower reactor 2, by the second tower 3 and second
Tower reactor 4 connects, and is detected using hydraulic pressure detection to the first tower 1 and the first tower reactor 2, first by the air in the first tower 1 and the first tower reactor 2
The pressure of water is then slowly increased to 0.7MPa by emptying, keeps pressure 30min, and pressure is then down to 0.6MPa, keep 1~
The leakage situation of the junction of 2h, the first tower 1 of detection and the first tower reactor 2 drains water after detection is qualified, then to the first tower 1 and
First tower reactor 2 carries out compressed air drying, and the second tower 3 and the second tower reactor 4 use and the identical water of the first tower 1 and the first tower reactor 2
Pressure detection detects the leakage situation of the junction of the second tower 3 and the second tower reactor 4 and drains water, then after detection is qualified to second
Tower 3 and the second tower reactor 4 carry out compressed air drying.Hydraulic pressure detection prevents reaction process gas from leaking, and improves safety.
(c) lower head for heating the collet of the first tower reactor 2 and 4: the first tower reactor 2 of the second tower reactor and the second tower reactor 4 selects mark
Quasi- elliposoidal is 8mm according to rigidity condition design wall thickness, and material is stainless steel making, and upper cover selects 90 ° of flanging taper envelopes
Head, according to the big end of end socket and collet butt welding, small end and autoclave body fillet welding, therefore design wall thickness is 8mm, material is stainless steel
It makes.Then the jacket steam valve for opening the first tower reactor 2 and the second tower reactor 4 respectively, in the jacket steam valve of the first tower reactor 2
It is passed through Boiler Steam, controls the air pressure in the collet of the first tower reactor 2 and be less than 0.2MPa, the heat transfer of steam to the first tower reactor 2
In, steam heats the first tower reactor 2, while Boiler Steam is passed through in the jacket steam valve of the second tower reactor 4, controls the second tower reactor
Air pressure in 4 collet is less than 0.2MPa, and the heat transfer of steam is into the second tower reactor 4, and steam heats the second tower reactor 4, then
Temperature detection is carried out to the first tower reactor 2 and the second tower reactor 4, detect every 8min it is primary, control the first tower reactor 2 temperature and
The temperature of second tower reactor 4 is greater than 90 DEG C.
(d) poly- methyltriethoxysilane is prepared: before reactions, it can be achieved that being passed through in the first tower reactor 2 and the second tower reactor 4
Petroleum ether, petroleum ether are used as solvent, and hydrogen chloride gas, chlorination can be generated by being primarily due to Trichloromethyl silane and ethanol synthesis
Hydrogen physical efficiency and ethanol synthesis generate water, and the presence of water can reduce the yield of poly- methyltriethoxysilane, and hydrogen chloride gas
Insoluble in organic solvent, Trichloromethyl silane and ethyl alcohol are dissolved in organic solvent, therefore are used as solvent using petroleum ether, will react
The hydrogen chloride gas of generation is discharged.Reaction raw materials liquid ethyl alcohol is passed into the second tower 3 after being calculated by metering pump, and to entrance
Ethyl alcohol heating vaporization, then heating work is carried out to the second tower 3, while the temperature for controlling the second tower reactor 4 is consistently greater than 90 DEG C.?
When the tower top temperature of one tower 1 detects 60 DEG C, start metering pump, start to throw Trichloromethyl silane into from the top of the first tower 1,
Adjust simultaneously and control the feed rate of Trichloromethyl silane and ethyl alcohol, be maintained in the unit time Trichloromethyl silane with
The charging of the molar ratio 1:2.9 of ethyl alcohol, Trichloromethyl silane and ethyl alcohol have larger impact to the selectivity of product, due to a first
When base trichlorosilane and ethanol synthesis, fraction Trichloromethyl silane can have little time reaction just as tail gas volatilizes together
Come, therefore the molar ratio of Trichloromethyl silane and ethyl alcohol can be 1:3.0 with appropriate adjustment.Reach in the liquid level of the first tower reactor 2
When the l/2 of tower reactor volume~2/3, the material of the first tower reactor 2 is transported to the top of the second tower 3 by starting magnetic drive pump 6, and is protected always
Hold material liquid level in the first tower reactor 2 will gradually tend in the section l/2~2/3 of total volume, after system feeding reaction balance, one
Methyl trichlorosilane and ethyl alcohol come into full contact in the second tower 3 and the second tower reactor 4 and are reacted, and the tower top of the second tower 3 reacts remaining
Gas be passed into the first tower 1, the gas of the first tower 1, which is passed into condenser 5, to be condensed, pass through the condensate liquid after condenser 5 return
It flowing in the first tower reactor 2, the tail gas that condenser 5 is discharged is passed into sodium hydroxide solution, the hydrogen chloride gas in tail gas is absorbed,
Trichloromethyl silane and ethyl alcohol are reacted in the first tower 1 and the first tower reactor 2 simultaneously.To in the first tower 1 and the first tower reactor 2
Reaction, 8~9h of reaction in the second tower 3 and the second tower reactor 4, organic synthesis is a veryer long process, it is necessary to assure
There is the sufficient time to carry out fully reacting for Trichloromethyl silane and ethyl alcohol, but 10h is not to be exceeded in the reaction time, not only wastes
Time reduces production efficiency, and increases the degree that side reaction occurs, and causes product to hydrolyze, reduces yield.In second tower reactor 4
Material gradually increases, and when material reaches 2/3 volume in the second tower reactor 4, starts discharging pump 7, carries out continuous discharge, keep simultaneously
For material liquid level in the section l/2~2/3 of total volume, continuous outputting material obtains poly- methyltriethoxy silane in second tower reactor 4
Alkane crude product.
During the reaction, the height for needing to be observed material liquid level in the first tower reactor 2 and the second tower reactor 4 using visor, is answered
It observes at regular intervals, and the material liquid surface altitude record that will be observed that facilitates operator to operate into table.Depending on
Material used by mirror plays an important role in the height deterministic process of material liquid level, the main material of visor such as 2 institute of table
Show:
| Title | Material | Quantity |
| Endoscopy glass | Pyrex | 1 |
| Liner | Asbestos packing sheet | 2 |
| Compression ring | — | 1 |
| Connect edge | — | 1 |
The main material of 2 visor of table
(e) it refines poly- methyltriethoxysilane crude product: obtained poly- methyltriethoxysilane crude product is first passed into
In first rectifying column 8, the light impurities and heavy impurity of poly- methyltriethoxysilane crude product are removed, first rectifying column 8 is obtained
To material be passed into Second distillation column 9 by tilting down channel, using reboiler to Second distillation column 9 heat, to material
Rectification and purification is carried out, poly- methyltriethoxysilane crude product refining is obtained into poly- methyltriethoxysilane finished product.
The present invention carries out cleaning to equipment, removes the first tower 1, the first tower reactor 2, the second tower 3 and the second tower reactor 4
Dirt and impurity on inner wall improve the cleannes of reaction environment, reduce in reaction mass and are mixed into impurity, by equipment hydraulic pressure
Detection improves safety, and is carried out continuously reaction using double tower, improves production capacity, increases substantially production efficiency, recruitment number
It is significantly reduced with labor intensity, the quality of poly- methyltriethoxysilane finished product obtained is uniform, stablizes.
Present invention packaging and storing: poly- methyltriethoxysilane finished product 50/200/250L plastic barrel is packed.Storage
In shady and cool, dry, draughty storehouse, far from kindling material, heat source, storehouse temperature is no more than 30 DEG C.Packing instructions sealing, can not be in
Air contact should separately be stored with acid, bases, should not be deposited long.The equipment such as illumination, energy wind in storage should use explosion-proof type,
Switch is located at outside storehouse.Tank stores Shi Yaoyou technical measures for fire and explosion prevention.It fills and wants coutroi velocity, pay attention to preventing electrostatic accumulation.Operation
Scene must not smoke, drinks water, feed.It wants with light packs when carrying gently to unload, prevents packing container from damaging.
The above is only specific embodiments of the present invention, but technical characteristic of the invention is not limited thereto.It is any with this hair
Based on bright, to solve essentially identical technical problem, essentially identical technical effect is realized, made simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (4)
1. a kind of poly- methyltriethoxysilane double tower continuous production technology, it is characterised in that include the following steps:
(a) cleaning equipment: first prepare the clear water of two barrels of 120L, the temperature of clear water is controlled at 20~22 DEG C, then by one barrel
The clear water of 120L directly rinses the first tower, while the clear water of another barrel of 120L is directly rinsed the second tower, is cleaning the first tower reactor
Before the second tower reactor, detection work is carried out, then using two high-pressure nozzles to the inner wall of the first tower reactor and the second tower reactor
Inner wall is directly washed away, and the hard dirt on the inner wall of the first tower reactor and the inner wall of the second tower reactor is smashed, flushing time is held
Continuous 10~15min, then estimates the first tower, the second tower, the first tower reactor and the second tower reactor by operator, reaches without bright
When showing visible foreign matter and trace, cleaning can be terminated；
(b) hydraulic pressure detects: after completing cleaning, the first tower being connect with the first tower reactor, the second tower and the second tower reactor are connected
It connects, the first tower and the first tower reactor is detected using hydraulic pressure detection, first empty the air in the first tower and the first tower reactor, then will
The pressure of water is slowly increased to 0.7MPa, keeps pressure 30min, and pressure is then down to 0.6MPa, keeps 1~2h, detection first
The leakage situation of the junction of tower and the first tower reactor drains water, then press the first tower and the first tower reactor after detection is qualified
Contracting air blow drying, the second tower and the second tower reactor use and identical with the first tower reactor the hydraulic pressure of the first tower detects, detect the second tower and
The leakage situation of the junction of second tower reactor drains water after detection is qualified, then carries out compression sky to the second tower and the second tower reactor
Air-blowing is dry；
(c) the first tower reactor and the second tower reactor are heated: the jacket steam valve of the first tower reactor and the second tower reactor is opened respectively, first
Boiler Steam is passed through in the jacket steam valve of tower reactor, the air pressure controlled in the collet of the first tower reactor is less than 0.2MPa, steam
For heat transfer into the first tower reactor, steam heats the first tower reactor, while being passed through boiler in the jacket steam valve of the second tower reactor
Steam, the air pressure controlled in the collet of the second tower reactor are less than 0.2MPa, and the heat transfer of steam is into the second tower reactor, steam heating
Then second tower reactor carries out temperature detection to the first tower reactor and the second tower reactor, detect every 8min primary, the first tower of control
The temperature of the temperature of kettle and the second tower reactor is greater than 90 DEG C；
(d) prepare poly- methyltriethoxysilane: reaction raw materials liquid ethyl alcohol is passed into the second tower after being calculated by metering pump, and
Vaporization is heated to the ethyl alcohol of entrance, then heating work is carried out to the second tower, while the temperature for controlling the second tower reactor is consistently greater than 90
DEG C, when the tower top temperature of the first tower detects 60 DEG C, start metering pump, starts to throw monomethyl trichlorine into from the top of the first tower
Silane, while the feed rate for controlling Trichloromethyl silane and ethyl alcohol is adjusted, it is maintained at monomethyl trichlorine in the unit time
The molar ratio 1:2.9 of silane and ethyl alcohol, when the liquid level of the first tower reactor reaches the l/2~2/3 of tower reactor volume, starting magnetic drive pump will
The material of first tower reactor is transported to the top of the second tower, and remain material liquid level in the first tower reactor total volume l/2~
Reaction balance will gradually be tended in 2/3 section, after system feeding, Trichloromethyl silane and ethyl alcohol are in the second tower and the second tower reactor
It inside comes into full contact with and reacts, the tower top of the second tower reacts remaining gas and is passed into the first tower, and the gas of the first tower is passed into cold
It condenses in condenser, is flowed back into the first tower reactor by the condensate liquid after condenser, the tail gas of condenser discharge is passed into hydroxide
In sodium solution, the hydrogen chloride gas in tail gas, Trichloromethyl silane and ethyl alcohol are absorbed while in the first tower and the first tower reactor
It is reacted, to 8~9h of reaction in reaction, the second tower and the second tower reactor in the first tower and the first tower reactor, in the second tower reactor
Material gradually increases, and when material reaches 2/3 volume in the second tower reactor, starts discharging pump, carries out continuous discharge, while keeping the
For material liquid level in the section l/2~2/3 of total volume, it is thick that continuous outputting material obtains poly- methyltriethoxysilane in two tower reactors
Product；
(e) it refines poly- methyltriethoxysilane crude product: obtained poly- methyltriethoxysilane crude product is first passed into first
In rectifying column, the light impurities and heavy impurity of poly- methyltriethoxysilane crude product, the object that first rectifying column is obtained are removed
Material is passed into Second distillation column by tilting down channel, is heated using reboiler to Second distillation column, carries out rectifying to material
Purification, obtains poly- methyltriethoxysilane finished product for poly- methyltriethoxysilane crude product refining.
2. a kind of poly- methyltriethoxysilane double tower continuous production technology according to claim 1, it is characterised in that:
In step (a), model and technology that detection work specifically includes cleaning pump are carried out before cleaning the first tower reactor and the second tower reactor
Parameter, the installation of cleaning pump, each component seat in the plane, connecting pipe connection and supply water tank water level.
3. a kind of poly- methyltriethoxysilane double tower continuous production technology according to claim 1, it is characterised in that:
In step (c), the lower head selection standard elliposoidal of the collet of the first tower reactor and the second tower reactor, upper cover selects 90 ° of flanging cones
Shape end socket.
4. a kind of poly- methyltriethoxysilane double tower continuous production technology according to claim 1, it is characterised in that:
In step (d), during the reaction, the height of material liquid level in the first tower reactor and the second tower reactor is observed using visor.
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