CN109320541A - The method of tower acid binding agent method continuous production cyanoethyl triethoxysilane - Google Patents
The method of tower acid binding agent method continuous production cyanoethyl triethoxysilane Download PDFInfo
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- acid binding
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- GBQYMXVQHATSCC-UHFFFAOYSA-N 3-triethoxysilylpropanenitrile Chemical compound CCO[Si](OCC)(OCC)CCC#N GBQYMXVQHATSCC-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000011230 binding agent Substances 0.000 title claims abstract description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000010924 continuous production Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 123
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000047 product Substances 0.000 claims abstract description 29
- 239000012043 crude product Substances 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 20
- 235000019441 ethanol Nutrition 0.000 claims abstract description 20
- OLBGECWYBGXCNV-UHFFFAOYSA-N 3-trichlorosilylpropanenitrile Chemical compound Cl[Si](Cl)(Cl)CCC#N OLBGECWYBGXCNV-UHFFFAOYSA-N 0.000 claims abstract description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000002309 gasification Methods 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 11
- 238000004821 distillation Methods 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 6
- 229940043279 diisopropylamine Drugs 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 3
- 125000001664 diethylamino group Chemical group [H]C([H])([H])C([H])([H])N(*)C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000007789 gas Substances 0.000 description 17
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 238000006386 neutralization reaction Methods 0.000 description 4
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- -1 machinery Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 150000007530 organic bases Chemical class 0.000 description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 3
- 239000005052 trichlorosilane Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 239000013070 direct material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The method of tower acid binding agent method continuous production cyanoethyl triethoxysilane, the present invention relates to the production methods of cyanoethyl triethoxysilane.The technical issues of the present invention is to solve acid value after the reaction of existing cyanoethyl triethoxysilane production method is high, at high cost, and production capacity is low, product purity is low.Method of the invention: one, building tower reactor system, which includes that lower part is the reaction towers that reaction kettle reaction zone, top are column plate reaction zone；Two, cyanoethyl triethoxysilane and acid binding agent are added to reaction kettle reaction zone, ethyl alcohol, entrainer is added separately in batch can；Three, it heats up, after reaction tower is stablized, cyanoethyltrichlorosilane, ethyl alcohol and entrainer is squeezed into reaction tower and reacted, crude product, which is drawn, from the bottom of reaction tower obtains cyanoethyl triethoxysilane after distilling, product purity of the invention is 98.5% or more, product yield >=95%.
Description
Technical field
The present invention relates to the production methods of cyanoethyl triethoxysilane.
Background technique
Cyanoethyl triethoxysilane is the direct material for synthesizing aminopropyl triethoxysilane (KH-550), due to the production
Product are in the enhancing of glass fibre, the modification of resin surface, the polymerization of textile auxiliary and the processing performance for improving silica filler etc.
Aspect has unique significant effect, is widely used in the industry neck such as coating, rubber, paint, plastics, machinery, glass fibre, electronics
Domain is one of most widely used silane product of existing market.
Existing cyanoethyl triethoxysilane production synthesis technology is broadly divided into following three kinds:
(1) still reaction: still reaction kettle is first added in cyanoethyl trichlorosilane, slow from ethanol storage tank to still reaction kettle
The ethyl alcohol of equivalent is added, after reaction, organic base is added and adjusts pH value to neutrality, filtering, distillation, rectification and purification are produced
Product.This technique acid value in generating process is excessive, and the by-product of generation is excessive, and the later period needs to be added a large amount of organic base and adjusts
PH increases the cost of reaction.
(2) tower entrainment reaction: the bottom that entrainer is first added to tower reactor is reacted in negative pressure entrainment with normal pressure entrainment,
The boiling point to heat up to column bottom temperature for cyanoethyl triethoxysilane, tower top stablizes reflux, by cyanoethyl trichlorosilane and ethyl alcohol
It is fed simultaneously by the top of tower reactor with lower part, after reaction, organic base is added and adjusts pH value to neutrality, filtering is steamed
It evaporates, rectification and purification, obtains product.This technique reduces a certain amount of acid value in production process, and by-product decreases, but in life
The serialization time is shorter during production, and production capacity is lower.
(3) hydrosilylation: using acrylonitrile and triethoxysilane in metals such as rhodium, iridium and metal complex catalyzed
Under the conditions of directly react.Since the catalyst used of reaction is noble metal catalyst, the cost of reaction is increased, is received after reaction
Rate is lower, further increases the cost of reaction.
It is above-mentioned three kinds reaction be primarily present reaction after acid value it is excessively high, it is subsequent need to be added sodium ethoxide neutralization, increase reaction at
This, Batch Process, the low problem of production capacity, while the problem low there is also the purity of product.
Summary of the invention
The present invention is to solve acid value height, at high cost, production after the reaction of existing cyanoethyl triethoxysilane production method
Can be low, product purity is low the technical issues of, and the method for tower acid binding agent method continuous production cyanoethyl triethoxysilane is provided.
The method of tower acid binding agent method continuous production cyanoethyl triethoxysilane of the invention, sequentially includes the following steps:
One, build tower reactor system: the tower reactor system include reaction tower, reboiler, receive kettle, first into
Batch can, the first feed pump, the first gasification tank, the second head tank, the second feed pump, the second gasification tank, third head tank, third into
Material pump and condenser；The lower part of reaction tower is reaction kettle reaction zone, and top is column plate reaction zone；First head tank is through the first charging
Pump is connect with the first gasification tank with the first charging aperture of column plate reaction zone lower part；Second head tank is through the second feed pump and the second gas
Change tank to connect with the second charging aperture in the middle part of column plate reaction zone；Third head tank is through third feed pump and column plate reaction zone top
The connection of third feed inlet；The gas outlet of the tower top of column plate reaction zone is connect with condenser, and the liquid that goes out of condenser flows back through return pipe
To the phegma entrance on column plate reaction zone top, connect in the entrance that column plate reaction zone top is additionally provided with exhaust outlet and condenser
It connects；Discharge port in the bottom of reaction kettle reaction zone is connect with reboiler entrance, and reboiler outlet and column plate reaction zone lower part are again
Boil the connection of gas entrance；Reception kettle is in succession on the pipeline between discharge port and reboiler；
Two, be in mass ratio (9.5~10) by cyanoethyl triethoxysilane and acid binding agent under normal pressure: 1 ratio is added
To the reaction kettle reaction zone of reaction tower, ethyl alcohol is added in the first head tank, entrainer is added in the second head tank, it will
Cyanoethyltrichlorosilane is added in third head tank；Wherein acid binding agent is diethylamine or diisopropylamine；
Three, the temperature of reaction kettle reaction zone is risen to 220~230 DEG C in stirring condition, detects first charging aperture, third
Feed inlet and overhead reflux situation, when first charging aperture temperature is 108~115 DEG C, third inlet temperature be 65~70 DEG C and
When tower top stablizes 30~40min of reflux, the metering valve charging of cyanoethyltrichlorosilane, ethyl alcohol and entrainer, control are opened simultaneously
The charging rate of cyanoethyltrichlorosilane processed is in 350~355kg/h, and the charging rate of ethyl alcohol is in 256~258kg/h, entrainer
0.1~0.12kg/h of charging rate, the temperature of reaction kettle reaction zone is 220~230 DEG C, the temperature of first charging aperture is 108
~115 DEG C, after third inlet temperature reacts 10~15min under conditions of being 65~70 DEG C, open tower reactor bottom
Crude product is squeezed into and is received in kettle by discharge port, controls 403~405kg/h of discharging speed of crude product, and the hydrochloric acid being discharged from condenser
Gas is recovered to hydrochloric acid gas storage tank；
Four, the crude product in kettle will be received to distill, obtains cyanoethyl triethoxysilane；
Method of the invention is added acid binding agent in reaction process, not only inhibits the generation of impurity well, improve product
Purity also makes the acid value of crude product be reduced to 6~7, carries out distillation getting the product after using no or little organic alkali neutralization, reduces
The cost of product reacts hydrogen chloride gas recycling generated, can do the raw material of trichlorosilane, realize the recycling of exhaust gas.Further
Cost is reduced, environmental protection is improved.Product purity of the invention is 98.5% or more, product yield >=95%.
Detailed description of the invention
Fig. 1 is the schematic diagram of tower reactor system of the invention；
Fig. 2 is the structural schematic diagram of tower reactor of the invention；
Specific embodiment
Specific embodiment 1: the side of the tower acid binding agent method continuous production cyanoethyl triethoxysilane of present embodiment
Method sequentially includes the following steps:
One, build tower reactor system: the tower reactor system includes reaction tower 1, reboiler 2, receives kettle 3, the
One head tank 4, the first feed pump 5, the first gasification tank 6, the second head tank 7, the second feed pump 8, the second gasification tank 9, third into
Batch can 10, third feed pump 11, condenser 12；The lower part of reaction tower 1 is reaction kettle reaction zone, and top is column plate reaction zone；The
One head tank 4 is connect through the first feed pump 5 with the first gasification tank 6 with the first charging aperture 1-1 of column plate reaction zone lower part；Second into
Batch can 7 is connect through the second feed pump 8 with the second gasification tank 9 with the second charging aperture 1-2 in the middle part of column plate reaction zone；Third head tank
10 connect through third feed pump 11 with the third feed inlet 1-3 on column plate reaction zone top；The gas outlet of the tower top of column plate reaction zone
1-4 is connect with condenser 12, the phegma entrance 1-5 for going out liquid and being back to column plate area top through return pipe of condenser 12, in tower
Plate reaction zone top is additionally provided with exhaust outlet 1-6 and connect with the entrance of condenser 12；Discharging in the bottom of reaction kettle reaction zone
Mouth 1-7 is connect with 2 entrance of reboiler, and the outlet of reboiler 2 is boiled gas entrance 1-8 with column plate reaction zone lower part again and connect；Kettle 3 is received to connect
It is connected on the pipeline between discharge port 1-7 and reboiler 2；
Two, be in mass ratio (9.5~10) by cyanoethyl triethoxysilane and acid binding agent under normal pressure: 1 ratio is added
To the reaction kettle reaction zone of reaction tower 1, ethyl alcohol is added in the first head tank 4, entrainer is added to the second head tank 7
In, cyanoethyltrichlorosilane is added in third head tank 10；Wherein acid binding agent is diethylamine or diisopropylamine；
Three, the temperature of reaction kettle reaction zone is risen to 220~230 DEG C in stirring condition, detection first charging aperture 1-1,
Third feed inlet 1-3 and overhead reflux situation, when first charging aperture 1-1 temperature is 108~115 DEG C, third feed inlet 1-3 temperature
At 65~70 DEG C and tower top 30~40min of stable reflux, the metering valve of cyanoethyltrichlorosilane, ethyl alcohol and entrainer is opened simultaneously
Door 15 is fed, and controls the charging rate of cyanoethyltrichlorosilane in 350~355kg/h, the charging rate of ethyl alcohol 256~
258kg/h, entrainer 0.1~0.12kg/h of charging rate, reaction kettle reaction zone temperature be 220~230 DEG C, first charging
After reacting 10~15min under conditions of the temperature of mouth 1-1 is 108~115 DEG C, third feed inlet 1-3 temperature is 65~70 DEG C, beat
The discharge port 1-7 for opening tower reactor bottom, which squeezes into crude product, to be received in kettle 3, and 403~405kg/ of discharging speed of crude product is controlled
H, and the HCl gas being discharged from condenser, are recovered to hydrochloric acid gas storage tank；
Four, the crude product in kettle 3 will be received by distillation, obtain cyanoethyl triethoxysilane；
Specific embodiment 2: the present embodiment is different from the first embodiment in that described tower in step 1
In reactor assembly, surge tank 13 and product pump 14 are set before receiving kettle 3.It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that tower reactor system
In, condenser 12 is secondary condenser.It is other the same as one or two specific embodiments.
Specific embodiment 4: tower reactor system unlike one of present embodiment and specific embodiment one to three
In system, metering valve 15 is provided on the pipeline of charging.It is other identical as one of specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four described in step 2
Entrainer be toluene.It is other identical as one of specific embodiment one to four.
Specific embodiment 6: thick in step 4 unlike one of present embodiment and specific embodiment one to five
It is -0.1MPa that product distillation condition, which is in vacuum degree, and temperature is distilled under conditions of being 130 DEG C.Other and specific embodiment
One of one to five is identical.
Specific embodiment 7: thick in step 4 unlike one of present embodiment and specific embodiment one to six
It is -0.09~-0.1MPa that product distillation condition, which is in vacuum degree, and temperature is distilled under conditions of being 130 DEG C.Other and specific reality
It is identical to apply one of mode one to six.
Specific embodiment 8: cyanogen second in step 2 unlike one of present embodiment and specific embodiment one to seven
The additional amount of ethyl triethoxy silicane alkane is a quarter of reaction kettle reaction zone volume to one third.Other and specific embodiment party
One of formula one to seven is identical.
Beneficial effects of the present invention are verified with the following examples:
Embodiment 1: the method for the tower acid binding agent method continuous production cyanoethyl triethoxysilane of the present embodiment, by following
Step carries out:
One, build tower reactor system: the tower reactor system includes reaction tower 1, reboiler 2, receives kettle 3, the
One head tank 4, the first feed pump 5, the first gasification tank 6, the second head tank 7, the second feed pump 8, the second gasification tank 9, third into
Batch can 10, third feed pump 11, condenser 12；The lower part of reaction tower 1 is 300L enamel still as reaction kettle reaction zone, and top is
Column plate reaction zone, it is regular packed tower that 9 meters of tower height, tower body diameter, which is 200mm,；First head tank 4 through the first feed pump 5 with
First gasification tank 6 is connect with the first charging aperture 1-1 of column plate reaction zone lower part；Second head tank 7 is through the second feed pump 8 and second
Gasification tank 9 is connect with the second charging aperture 1-2 in the middle part of column plate reaction zone；Third head tank 10 is anti-through third feed pump 11 and column plate
The third feed inlet 1-3 connection on the top Ying Qu；The gas outlet 1-4 of the tower top of column plate reaction zone is connect with condenser 12, condenser
The 12 phegma entrance 1-5 for going out liquid and being back to column plate reaction zone top through return pipe, is additionally provided on column plate reaction zone top
Exhaust outlet 1-6 is connect with the entrance of condenser 12；Condenser 12 is secondary condenser；Discharging in the bottom of reaction kettle reaction zone
Mouth 1-7 is connect with 2 entrance of reboiler, and the outlet of reboiler 2 is boiled gas entrance 1-8 with column plate reaction zone lower part again and connect；Kettle 3 is received to connect
It is connected on the pipeline between discharge port 1-7 and reboiler 2；Surge tank 13 and product pump 14 are set before receiving kettle 3；In charging
Metering valve 15 is provided on pipeline；
Two, it under normal pressure, after 100kg cyanoethyl triethoxysilane and 10kg diethylamine are mixed, is added under reaction tower 1
Ethyl alcohol is added in the first head tank 4 by the reaction kettle reaction zone in portion, and entrainer toluene is added in the second head tank 7, will
Cyanoethyltrichlorosilane is added in third head tank 10；
Three, the temperature of reaction kettle reaction zone is risen to 224 DEG C under agitation, detection first charging aperture 1-1, third into
Material mouth 1-3 and overhead reflux situation, when first charging aperture 1-1 temperature is 108 DEG C, third feed inlet 1-3 temperature is 70 DEG C and tower
After reflux 30min is stablized on top, the metering valve 15 for opening simultaneously cyanoethyltrichlorosilane, ethyl alcohol and entrainer toluene is fed, control
The charging rate of cyanoethyltrichlorosilane processed is in 300kg/h, and the charging rate of ethyl alcohol is in 220kg/h, entrainer charging rate
0.1kg/h, the temperature in reaction kettle area is 224 DEG C, first charging aperture 1-1 temperature is 108 DEG C, third feed inlet 1-3 temperature is
10min is reacted under conditions of 70 DEG C, the discharge port 1-7 for then opening tower reactor bottom, which squeezes into crude product, to be received in kettle 3, control
The hydrogen chloride gas of the discharging speed 345kg/h of crude product processed, the reaction being discharged from condenser are recovered to hydrochloric acid gas storage tank；In reaction process
Every 2h sampling monitoring, the purity for monitoring cyanoethyl triethoxysilane in crude product stop reaction all after 98.5% or more, 48h；
Four, the crude product in kettle 3 will be received to take out, is born under conditions of vacuum degree degree is -0.098MPa, temperature is 130 DEG C
Pressure distillation, obtains cyanoethyl triethoxysilane.
The structural formula for the cyanoethyl triethoxysilane that the present embodiment obtains is
Diethylamine is added as acid binding agent in reaction process in the present embodiment, not only inhibits the generation of impurity well, mentions
High product purities, the purity for the cyanoethyl triethoxysilane product that the present embodiment obtains are 99.4%, product yield 96%.
The use of acid binding agent also makes the acid value of crude product be reduced to 7 simultaneously, does not have to organic alkali neutralization, cyanogen second is obtained after directly being distilled
Ethyl triethoxy silicane alkane product, reduces the cost of product；Hydrogen chloride gas recycling generated is reacted, the original of trichlorosilane can be done
Material, realizes the recycling of exhaust gas, further reduces the cost, and improves environment protecting.
Embodiment 2: the method for the tower acid binding agent method continuous production cyanoethyl triethoxysilane of the present embodiment, by following
Step carries out:
One, build tower reactor system: the tower reactor system is identical as embodiment 1；
Two, under normal pressure, 100kg cyanoethyl triethoxysilane and 10kg diisopropylamine after mixing, are added to reaction
Ethyl alcohol is added in the first head tank 4 by the reaction kettle reaction zone of 1 lower part of tower, and entrainer toluene is added to the second head tank 7
In, cyanoethyltrichlorosilane is added in third head tank 10；
Three, the temperature of reaction kettle reaction zone is increased to 226 DEG C under agitation, detects first charging aperture 1-1, third
Feed inlet 1-3 and overhead reflux situation, when first charging aperture 1-1 temperature is 110 DEG C, third feed inlet 1-3 temperature be 72 DEG C and
After tower top stablizes reflux 30min, the metering valve 15 for opening simultaneously cyanoethyltrichlorosilane, ethyl alcohol and entrainer toluene is fed；
The charging rate of cyanoethyltrichlorosilane is controlled in 300kg/h, the charging rate of ethyl alcohol in 220kg/h, entrainer toluene into
Speed 0.1kg/h is expected, the temperature of reaction kettle reaction zone is 226 DEG C, first charging aperture 1-1 temperature is 110 DEG C, third feed inlet
After 1-3 temperature reacts 12min under conditions of being 72 DEG C, crude product is squeezed into reception by the discharge port 1-7 for opening tower reactor bottom
In kettle 3, the discharging speed 345kg/h of crude product is controlled, the hydrogen chloride gas being discharged from condenser is recovered to hydrochloric acid gas storage tank；Reaction process
In every 2h sampling monitoring, monitor the purity of cyanoethyl triethoxysilane in crude product and stop all after 98.5% or more, 48h instead
It answers；
Four, negative pressure under conditions of vacuum degree degree is -0.098MPa, temperature is 130 DEG C of the crude product in kettle 3 will be received to steam
It evaporates, obtain cyanoethyl triethoxysilane.
The structural formula for the cyanoethyl triethoxysilane that the present embodiment obtains is
Diisopropylamine is added as acid binding agent in reaction process in the present embodiment, not only inhibits the generation of impurity well,
Product purity is improved, the purity for the cyanoethyl triethoxysilane product that the present embodiment obtains is 99.8%, and product yield is
97%.The use of acid binding agent also makes the acid value of crude product be reduced to 7 simultaneously, does not have to organic alkali neutralization, after directly being distilled to obtain the final product
To cyanoethyl triethoxysilane product, the cost of product is reduced；Hydrogen chloride gas recycling generated is reacted, trichlorosilane can be done
Raw material, realize the recycling of exhaust gas.It further reduces the cost, improves environment protecting.
Claims (7)
1. the method for tower acid binding agent method continuous production cyanoethyl triethoxysilane, it is characterised in that this method is according to the following steps
It carries out:
One, build tower reactor system: the tower reactor system include reaction tower (1), reboiler (2), receive kettle (3),
First head tank (4), the first feed pump (5), the first gasification tank (6), the second head tank (7), the second feed pump (8), the second gas
Change tank (9), third head tank (10), third feed pump (11), condenser (12)；The lower part of reaction tower (1) is reaction kettle reaction
Area, top are column plate reaction zones；First head tank (4) is through under the first feed pump (5) and the first gasification tank (6) and column plate reaction zone
The first charging aperture (1-1) in portion connects；Second head tank (7) is reacted through the second feed pump (8) with the second gasification tank (9) with column plate
Second charging aperture (1-2) connection in the middle part of area；Third head tank (10) is through third feed pump (11) and column plate reaction zone top
Third feed inlet (1-3) connection；The gas outlet (1-4) of the tower top of column plate reaction zone is connect with condenser (12), condenser (12)
The liquid that goes out the phegma entrance (1-5) on column plate reaction zone top is back to through return pipe, be additionally provided on column plate reaction zone top
Exhaust outlet (1-6) is connect with the entrance of condenser (12)；Discharge port (1-7) and reboiler in the bottom of reaction kettle reaction zone
(2) entrance connects, and reboiler (2) outlet is boiled gas entrance (1-8) with column plate reaction zone lower part again and connect；Kettle (3) are received to exist in succession
On pipeline between discharge port (1-7) and reboiler (2)；
Two, under normal pressure, be in mass ratio (9.5~10) by cyanoethyl triethoxysilane and acid binding agent: 1 ratio is added to instead
Ethyl alcohol is added in the first head tank (4) by the reaction kettle reaction zone for answering tower (1), and entrainer is added to the second head tank (7)
In, cyanoethyltrichlorosilane is added in third head tank (10)；Wherein acid binding agent is diethylamine or diisopropylamine；
Three, the temperature of reaction kettle reaction zone is risen to 220~230 DEG C in stirring condition, detection first charging aperture (1-1), the
Three feed inlets (1-3) and overhead reflux situation, when 108~115 DEG C of first charging aperture (1-1) temperature, third feed inlet (1-3) temperature
Degree opens simultaneously the meter of cyanoethyltrichlorosilane, ethyl alcohol and entrainer for 65~70 DEG C and when tower top stablizes 30~40min of reflux
Valve (15) charging is measured, controls the charging rate of cyanoethyltrichlorosilane in 350~355kg/h, the charging rate of ethyl alcohol is 256
~258kg/h, entrainer 0.1~0.12kg/h of charging rate, reaction kettle reaction zone temperature be 220~230 DEG C, first into
Under conditions of the temperature of material mouth (1-1) is 108~115 DEG C, third feed inlet (1-3) temperature is 65~70 DEG C reaction 10~
After 15min, the discharge port (1-7) for opening tower reactor bottom, which squeezes into crude product, to be received in kettle (3), controls the discharging speed of crude product
403~405kg/h, and the HCl gas being discharged from condenser are spent, hydrochloric acid gas storage tank is recovered to；
Four, the crude product in kettle (3) will be received by distillation, obtain cyanoethyl triethoxysilane.
2. the method for tower acid binding agent method continuous production cyanoethyl triethoxysilane according to claim 1, feature
It is in the tower reactor system in step 1, setting surge tank (13) and product pump (14) before receiving kettle (3).
3. the method for tower acid binding agent method continuous production cyanoethyl triethoxysilane according to claim 1 or 2, special
It levies in the tower reactor system being in step 1, condenser (12) is secondary condenser.
4. the method for tower acid binding agent method continuous production cyanoethyl triethoxysilane according to claim 1 or 2, special
Sign is in tower reactor system described in step 1, and metering valve (15) are provided on the pipeline of charging.
5. the method for tower acid binding agent method continuous production cyanoethyl triethoxysilane according to claim 1 or 2, special
Sign is that entrainer described in step 2 is toluene.
6. the method for tower acid binding agent method continuous production cyanoethyl triethoxysilane according to claim 1 or 2, special
Sign be cyanoethyl triethoxysilane in step 2 additional amount be reaction kettle reaction zone volume a quarter to three/
One.
7. the method for tower acid binding agent method continuous production cyanoethyl triethoxysilane according to claim 1 or 2, special
It is -0.09~-0.1MPa that levy the crude product distillation condition that is in step 4, which be in vacuum degree, temperature be 130 DEG C under conditions of into
Row distillation.
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| CN110563754A (en) * | 2019-08-05 | 2019-12-13 | 潜江宜生新材料有限公司 | A alcoholysis reaction system for producing chloromethyl triethoxysilane |
| CN111925388A (en) * | 2020-08-18 | 2020-11-13 | 苏州欣溪源新材料科技有限公司 | Preparation method of titanium tetraisopropoxide |
| CN113457582A (en) * | 2021-07-21 | 2021-10-01 | 江西宏柏新材料股份有限公司 | Device for continuously producing cyanoethyl trichlorosilane |
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| CN110563754A (en) * | 2019-08-05 | 2019-12-13 | 潜江宜生新材料有限公司 | A alcoholysis reaction system for producing chloromethyl triethoxysilane |
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