CN101092426A - Reaction system and synthetic method for producing chloropropyl triethoxy silicane continuously - Google Patents
Reaction system and synthetic method for producing chloropropyl triethoxy silicane continuously Download PDFInfo
- Publication number
- CN101092426A CN101092426A CN 200710072565 CN200710072565A CN101092426A CN 101092426 A CN101092426 A CN 101092426A CN 200710072565 CN200710072565 CN 200710072565 CN 200710072565 A CN200710072565 A CN 200710072565A CN 101092426 A CN101092426 A CN 101092426A
- Authority
- CN
- China
- Prior art keywords
- heat exchanger
- communicated
- esterifier
- chloropropyl
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
This invention relates to reaction system and synthesis method for continuously producing chloropropyl triethoxy silane by esterification reaction. This invention solves the problems of long synthesis period, high energy consumption, high production cost and high HCl content in the crude product faced by the present chloropropyl triethoxy silane synthesis reaction. The liquid outlet at the bottom of the ethanol storage tank of the reaction system is through connected with the liquid inlet of the second heat exchanger. The gas outlet of the second heat exchanger is through connected with the gas inlet at the lower part of the stripping column. The gas outlet at the top of the stripping column is through connected with the gas inlet of the third heat exchanger. The gas outlet of the third heat exchanger is through connected with the gas inlet of the first ceramic suction pump. The liquid out of the third heat exchanger is through connected with the liquid inlet of the esterification reactor. This invention has such advantages as simple apparatus structure, easy operation and low space occupation.
Description
Technical field
The present invention relates to a kind of reaction unit and synthetic method of synthetic chloropropyl triethoxysilane.
Background technology
The synthetic route of traditional chloropropyl triethoxysilane is chloropropyl trichloro-silane and ethanol under 80～100 ℃, 0.03MPa, and esterification takes place.Reaction formula is:
ClCH
2CH
2CH
2SiCl
3+CH
3CH
2OH→ClCH
2CH
2CH
2Si(OCH
2CH
3)
3+HCl
The ethanol batch-wise adds, and the reaction times is about 6 hours, refluxes about 3 hours under 0.03MPa in the reaction back, and total reaction times was about more than 10 hours.At last with thick product through in the neutralizing agent sodium ethylate and after, squeeze into rectifying tower and carry out rectifying, make chloropropyl triethoxysilane.The main drawback of traditional technology is to carry out esterification under the processing condition of constant temperature, constant vacuum, certainly will cause like this reaction time long, energy consumption is high, contain more problems such as hydrogenchloride in the head product, simultaneously because the price comparison costliness of sodium ethylate improves production cost greatly.In addition, the head product after the neutralization also will pass through distillation operation again, has strengthened the cost input of manpower and materials so again.
Summary of the invention
The objective of the invention is long for the synthesis reaction period that solves present chloropropyl triethoxysilane, energy consumption is high, production cost is high, contain more problems such as hydrogenchloride in the head product, and provides a kind of reactive system and synthetic method thereof of continuous production chloropropyl triethoxysilane.The present invention adopts the continuous reaction apparatus system, and utilization chemical equilibrium principle of dynamics is carried out the continuous production chloropropyl triethoxysilane under temperature that continues to change and vacuum tightness.
Reactive system of the present invention is made up of chloropropyl trichloro-silane storage tank, ethanol storage tank, esterifier, safety valve, tensimeter, agitator, first heat exchanger, thermopair, well heater and temperature regulator, temperature control resistance wire, head product storage tank, second heat exchanger, gas stripping column, the 3rd heat exchanger, liquid-outlet valve, sampling valve, first ceramic pump and second ceramic pump of bleeding of bleeding; The liquid outlet of its chloropropyl trichloro-silane tank top is communicated with the fluid inlet at esterifier top, the liquid outlet of ethanol storage tank bottom is communicated with the fluid inlet of second heat exchanger, the air outlet of second heat exchanger is communicated with the inlet mouth of gas stripping column bottom, the air outlet at gas stripping column top is communicated with the inlet mouth of the 3rd heat exchanger, the air outlet of the 3rd heat exchanger is communicated with first inlet mouth of bleeding ceramic pump, the liquid outlet of the 3rd heat exchanger is communicated with the fluid inlet of esterifier, the air outlet at esterifier top is communicated with the inlet mouth of first heat exchanger, the bleed inlet mouth of ceramic pump of the air outlet of first heat exchanger and second, first the bleed air outlet of ceramic pump of ceramic pump and second of bleeding is communicated with the inlet mouth of hydrogenchloride treatment facility, esterifier is provided with agitator, safety valve, tensimeter, thermopair and well heater and temperature regulator, the liquid outlet of esterifier bottom is communicated with the fluid inlet of head product tank top, the liquid outlet of head product tank bottom is communicated with the fluid inlet on gas stripping column top, gas stripping column is equipped with the temperature control resistance wire outward, filler is housed in the gas stripping column, and the liquid outlet of gas stripping column bottom is communicated with the fluid inlet of liquid-outlet valve and sampling valve respectively.
The synthetic method of chloropropyl triethoxysilane of the present invention is as follows: with purity is that 99% chloropropyl trichloro-silane and dehydrated alcohol feed in raw material by 1: 3.15～3.3 mol ratio, reaction pressure maintains-0.03～-0.09MPa between, be 3～3.5h reaction time, in reaction time, add continuously dehydrated alcohol, be warming up to 50 ℃ from 25 ℃ with the adding temperature of reaction of dehydrated alcohol; In reaction process, chloropropyl trichloro-silane directly adds esterifier, dehydrated alcohol is warming up to 90～115 ℃ of vaporizations earlier, enter stripping tower from the stripping tower bottom, in Ta Nei and the head product chloropropyl triethoxysilane mass transfer, the heat transfer that are dissolved with a large amount of hydrogenchloride, hydrogenchloride in the head product is broken away from, thereby to the higher chloropropyl triethoxysilane of purity, gasiform ethanol, unreacted chloropropyl trichloro-silane are liquefied as liquid by heat exchanger then, enter in the esterifier and chloropropyl trichloro-silane generation esterification again; The head product that reaction generates in vacuum tightness is-0.096MPa, temperature be under ℃ condition of 1l0～120, carry out mass transfer and heat transfer with pyritous dehydrated alcohol adverse current in gas stripping column, dissolved hydrogenchloride in the product chloropropyl triethoxysilane is separated, unreacted chloropropyl trichloro-silane and ethanol vaporization simultaneously and product separation, enter esterifier through liquefaction again and participate in reaction again, simultaneously the hydrogenchloride that reaction generates in the esterifier and through the hydrogenchloride of alcohol desorption through over-heat-exchanger, detach by the ceramic pump of bleeding, handle by the hydrogenchloride treatment facility again.
The inventive method has the advantage that power consumption is low, product purity is high, reaction time is short, production cost is low.Device structure of the present invention is simple, is convenient to operation, saves to take up an area of the space.
Description of drawings
Fig. 1 is the synoptic diagram that reactive system of the present invention connects, Reference numeral 3 expression valves, 4 expression under meters, 21 expression pumps among the figure.
Embodiment
Embodiment one: the reactive system of (referring to Fig. 1) present embodiment is made up of chloropropyl trichloro-silane storage tank 1, ethanol storage tank 2, esterifier 5, safety valve 6, tensimeter 7, agitator 8, first heat exchanger 9, thermopair 10, well heater and temperature regulator 11, temperature control resistance wire 12, head product storage tank 13, second heat exchanger 14, gas stripping column 15, the 3rd heat exchanger 16, liquid-outlet valve 17, sampling valve 18, first ceramic pump 19 and second ceramic pump 20 of bleeding of bleeding; The liquid outlet at chloropropyl trichloro-silane storage tank l top is communicated with the fluid inlet at esterifier 5 tops, the liquid outlet of ethanol storage tank 2 bottoms is communicated with the fluid inlet of second heat exchanger 14, the air outlet of second heat exchanger 14 is communicated with the inlet mouth of gas stripping column 15 bottoms, the air outlet at gas stripping column 15 tops is communicated with the inlet mouth of the 3rd heat exchanger 16, the air outlet of the 3rd heat exchanger 16 is communicated with first inlet mouth of bleeding ceramic pump 19, the liquid outlet of the 3rd heat exchanger 16 is communicated with the fluid inlet of esterifier 5, the air outlet at esterifier 5 tops is communicated with the inlet mouth of first heat exchanger 9, the bleed inlet mouth of ceramic pump 20 of the air outlet of first heat exchanger 9 and second, first the bleed air outlet of ceramic pump 20 of ceramic pump 19 and second of bleeding is communicated with the inlet mouth of hydrogenchloride treatment facility, esterifier 5 is provided with agitator 8, safety valve 6, tensimeter 7, thermopair 10 and well heater and temperature regulator 11, the liquid outlet of esterifier 5 bottoms is communicated with the fluid inlet at head product storage tank 13 tops, the liquid outlet of head product storage tank 13 bottoms is communicated with the fluid inlet on gas stripping column 15 tops, the gas stripping column 15 outer temperature control resistance wires 12 that are equipped with, in the gas stripping column 15 filler is housed, the liquid outlet of gas stripping column 15 bottoms is communicated with the fluid inlet of liquid-outlet valve 17 and sampling valve 18 respectively.
Embodiment two: the present embodiment filler is ceramic Pall ring filler, Raschig ring, ceramic rectangular saddle ring filler or saddle packing.Other structure is identical with embodiment one with mode of connection.
Embodiment three: present embodiment adopts the synthetic chloropropyl triethoxysilane of the reactive system in the embodiment one, synthetic method is as follows: with purity is that 99% chloropropyl trichloro-silane and dehydrated alcohol feed in raw material by 1: 3.15～3.3 mol ratio, reaction pressure maintains-0.03～-0.09MPa between, be 3～3.5h reaction time, in reaction time, add continuously dehydrated alcohol, be warming up to 50 ℃ from 25 ℃ with the adding temperature of reaction of dehydrated alcohol; In reaction process, chloropropyl trichloro-silane directly adds esterifier 5, dehydrated alcohol is warming up to 90～115 ℃ by second heat exchanger 14 and enters stripping tower 15 again, and is entered in the esterifier 5 and chloropropyl trichloro-silane generation esterification by the 3rd heat exchanger 16 by stripping tower 15 tops behind the head product generation mass-and heat-transfer; Head product that reaction generates and pyritous ethanol are in the vacuum tightness of-0.096MPa, under 117～120 ℃, adverse current is carried out mass transfer and heat transfer in stripping tower 15, dissolved hydrogenchloride in the product chloropropyl triethoxysilane is separated, unreacted chloropropyl trichloro-silane and dehydrated alcohol vaporization simultaneously and product separation, enter esterifier 5 through liquefaction again and participate in reaction again, the hydrogenchloride of hydrogenchloride that reaction generates in the esterifier 5 and stripping tower 15 inner desorbs is through over-heat-exchanger simultaneously, detach by the ceramic pump 19 and 20 of bleeding, handle by the hydrogenchloride treatment facility again.
Mass transfer and heat transfer in gas stripping column with head product and high temperature ethanol in the present embodiment, unreacted chloropropyl trichloro-silane is dropped into reactor again, and hydrogenchloride is got rid of outside the reaction system, help improving degree of purity of production, improve conversion of raw material, reduce reaction cost.The productive rate of product is more than 99% in the present embodiment.
Embodiment four: in the present embodiment dehydrated alcohol is warming up to 90～110 ℃ by second heat exchanger 14.Other step is identical with embodiment three.
Embodiment five: in the present embodiment dehydrated alcohol is warming up to 110 ℃ by second heat exchanger 14.Other step is identical with embodiment three.
Claims (5)
1, a kind of reactive system of continuous production chloropropyl triethoxysilane, it is by chloropropyl trichloro-silane storage tank (1), ethanol storage tank (2), esterifier (5), safety valve (6), tensimeter (7), agitator (8), first heat exchanger (9), thermopair (10), well heater and temperature regulator (11), temperature control resistance wire (12), head product storage tank (3), second heat exchanger (14), gas stripping column (15), the 3rd heat exchanger (16), liquid-outlet valve (17), sampling valve (18), first ceramic pump (19) and second ceramic pump (20) of bleeding of bleeding is formed; The liquid outlet that it is characterized in that chloropropyl trichloro-silane storage tank (1) top is communicated with the fluid inlet at esterifier (5) top, the liquid outlet of ethanol storage tank (2) bottom is communicated with the fluid inlet of second heat exchanger (14), the air outlet of second heat exchanger (14) is communicated with the inlet mouth of gas stripping column (15) bottom, the air outlet at gas stripping column (15) top is communicated with the inlet mouth of the 3rd heat exchanger (16), the bleed inlet mouth of ceramic pump (19) of the air outlet of the 3rd heat exchanger (16) and first is communicated with, the liquid outlet of the 3rd heat exchanger (16) is communicated with the fluid inlet of esterifier (5), the air outlet at esterifier (5) top is communicated with the inlet mouth of first heat exchanger (9), the bleed inlet mouth of ceramic pump (20) of the air outlet of first heat exchanger (9) and second, first the bleed air outlet of ceramic pump (20) of ceramic pump (19) and second of bleeding is communicated with the inlet mouth of hydrogenchloride treatment facility, esterifier (5) is provided with agitator (8), safety valve (6), tensimeter (7), thermopair (10) and well heater and temperature regulator (11), the liquid outlet of esterifier (5) bottom is communicated with the fluid inlet at head product storage tank (13) top, the liquid outlet of head product storage tank (13) bottom is communicated with the fluid inlet on gas stripping column (15) top, the outer temperature control resistance wire (12) that is equipped with of gas stripping column (15), gas stripping column is equipped with filler in (15), and the liquid outlet of gas stripping column (15) bottom is communicated with the fluid inlet of liquid-outlet valve (17) and sampling valve (18) respectively.
2, the reactive system of continuous production chloropropyl triethoxysilane according to claim 1 is characterized in that filler is ceramic Pall ring filler, Raschig ring, ceramic rectangular saddle ring filler or saddle packing.
3, utilize the method for the synthetic chloropropyl triethoxysilane of reactive system of the described continuous production chloropropyl triethoxysilane of claim 1, it is characterized in that this synthetic method thes contents are as follows: with purity is that 99% chloropropyl trichloro-silane and dehydrated alcohol feed in raw material by 1: 3.15～3.3 mol ratio, reaction pressure maintains-0.03～-0.09MPa between, be 3～3.5h reaction time, in reaction time, add continuously dehydrated alcohol, be warming up to 50 ℃ from 25 ℃ with the adding temperature of reaction of dehydrated alcohol; In reaction process, chloropropyl trichloro-silane directly adds esterifier, dehydrated alcohol is warming up to 90～115 ℃ of vaporizations earlier, enter stripping tower from the stripping tower bottom, in Ta Nei and the head product chloropropyl triethoxysilane mass transfer, the heat transfer that are dissolved with a large amount of hydrogenchloride, hydrogenchloride in the head product is broken away from, thereby to the higher chloropropyl triethoxysilane of purity, gasiform ethanol, unreacted chloropropyl trichloro-silane are liquefied as liquid by heat exchanger then, enter in the esterifier and chloropropyl trichloro-silane generation esterification again; The head product that reaction generates in vacuum tightness is-0.096MPa again, temperature is under 110～120 ℃ of conditions, carry out mass transfer and heat transfer with pyritous dehydrated alcohol adverse current in gas stripping column, dissolved hydrogenchloride in the product chloropropyl triethoxysilane is separated, unreacted chloropropyl trichloro-silane and ethanol vaporization simultaneously and product separation, enter esterifier through liquefaction again and participate in reaction again, simultaneously the hydrogenchloride that reaction generates in the esterifier and through the hydrogenchloride of alcohol desorption through over-heat-exchanger, detach by the ceramic pump of bleeding, handle by the hydrogenchloride treatment facility again.
4, the synthetic method of continuous production chloropropyl triethoxysilane according to claim 3 is characterized in that dehydrated alcohol is warming up to 90～110 ℃ earlier.
5, the synthetic method of continuous production chloropropyl triethoxysilane according to claim 3 is characterized in that dehydrated alcohol is warming up to 110 ℃ earlier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710072565 CN101092426A (en) | 2007-07-25 | 2007-07-25 | Reaction system and synthetic method for producing chloropropyl triethoxy silicane continuously |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710072565 CN101092426A (en) | 2007-07-25 | 2007-07-25 | Reaction system and synthetic method for producing chloropropyl triethoxy silicane continuously |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101092426A true CN101092426A (en) | 2007-12-26 |
Family
ID=38990881
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710072565 Pending CN101092426A (en) | 2007-07-25 | 2007-07-25 | Reaction system and synthetic method for producing chloropropyl triethoxy silicane continuously |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101092426A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101671355B (en) * | 2009-09-30 | 2011-04-06 | 哈尔滨工业大学 | Method for synthezing trialkoxysilanes by adopting multistage fluidized bed |
| CN101333292B (en) * | 2008-07-22 | 2011-08-24 | 株洲时代新材料科技股份有限公司 | Raw material feeding manner and device for producing silicone resin |
| CN102199168A (en) * | 2010-03-25 | 2011-09-28 | 日照岚星化工工业有限公司 | Novel synthetic technology of gamma-chloropropyl triethoxysilane |
| CN101648966B (en) * | 2009-09-03 | 2012-01-04 | 潍坊中业化学有限公司 | Method capable of increasing content and yield of gamma-chloropropyltriethoxysilane simultaneously |
| CN102432633A (en) * | 2011-12-07 | 2012-05-02 | 诺贝尔（九江）高新材料有限公司 | Alcoholysis process of chloropropyltriethoxysilane |
| CN103254224A (en) * | 2013-03-27 | 2013-08-21 | 青岛晟科材料有限公司 | Preparation method of gamma-chloropropyl triethoxysilane coupling agent |
| CN104086582A (en) * | 2014-07-15 | 2014-10-08 | 江西晨光新材料有限公司 | Clean production method of 3-chloropropyltrialkoxysilane |
| CN105440069A (en) * | 2015-10-14 | 2016-03-30 | 日照岚星化工工业有限公司 | Method for neutralizing chloride ions in gamma-chloropropyltriethoxysilane synthetic liquid |
| CN109663559A (en) * | 2018-12-14 | 2019-04-23 | 浙江开化合成材料有限公司 | A kind of dedicated phenyl trichlorosilane process units of food-grade silicone resin |
| CN113150026A (en) * | 2021-05-06 | 2021-07-23 | 兰州康鹏威耳化工有限公司 | Continuous preparation method and system of phenyltrimethoxysilane |
-
2007
- 2007-07-25 CN CN 200710072565 patent/CN101092426A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101333292B (en) * | 2008-07-22 | 2011-08-24 | 株洲时代新材料科技股份有限公司 | Raw material feeding manner and device for producing silicone resin |
| CN101648966B (en) * | 2009-09-03 | 2012-01-04 | 潍坊中业化学有限公司 | Method capable of increasing content and yield of gamma-chloropropyltriethoxysilane simultaneously |
| CN101671355B (en) * | 2009-09-30 | 2011-04-06 | 哈尔滨工业大学 | Method for synthezing trialkoxysilanes by adopting multistage fluidized bed |
| CN102199168A (en) * | 2010-03-25 | 2011-09-28 | 日照岚星化工工业有限公司 | Novel synthetic technology of gamma-chloropropyl triethoxysilane |
| CN102432633A (en) * | 2011-12-07 | 2012-05-02 | 诺贝尔（九江）高新材料有限公司 | Alcoholysis process of chloropropyltriethoxysilane |
| CN102432633B (en) * | 2011-12-07 | 2014-05-07 | 江西晨光新材料有限公司 | Alcoholysis process of chloropropyltriethoxysilane |
| CN103254224A (en) * | 2013-03-27 | 2013-08-21 | 青岛晟科材料有限公司 | Preparation method of gamma-chloropropyl triethoxysilane coupling agent |
| CN104086582A (en) * | 2014-07-15 | 2014-10-08 | 江西晨光新材料有限公司 | Clean production method of 3-chloropropyltrialkoxysilane |
| CN105440069A (en) * | 2015-10-14 | 2016-03-30 | 日照岚星化工工业有限公司 | Method for neutralizing chloride ions in gamma-chloropropyltriethoxysilane synthetic liquid |
| CN105440069B (en) * | 2015-10-14 | 2018-05-15 | 日照岚星化工工业有限公司 | A kind of method of chlorion in neutralization γ-chloropropyl triethoxysilane Synthesis liquid |
| CN109663559A (en) * | 2018-12-14 | 2019-04-23 | 浙江开化合成材料有限公司 | A kind of dedicated phenyl trichlorosilane process units of food-grade silicone resin |
| CN113150026A (en) * | 2021-05-06 | 2021-07-23 | 兰州康鹏威耳化工有限公司 | Continuous preparation method and system of phenyltrimethoxysilane |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101092426A (en) | Reaction system and synthetic method for producing chloropropyl triethoxy silicane continuously | |
| CN104437295A (en) | Device and method for preparing tetramethoxysilane | |
| CN101249312A (en) | Separation apparatus and method of high precision rectification purify trichlorosilane | |
| CN202359049U (en) | System for producing methyl silicate by hydrolyzing methyl trichlorosilane | |
| CN105000564B (en) | Production method of dichlorosilane for preparing silane | |
| CN102674368B (en) | Method and system for preparing trichlorosilane | |
| CN204380655U (en) | Prepare the device of tetramethoxy-silicane | |
| CN107986234B (en) | System for preparing deuterium-depleted water by electrolysis-catalytic exchange combined process and implementation method thereof | |
| CN201037131Y (en) | Modified device for producing methyl t-butyl ether | |
| CN202346934U (en) | Trimethoxy hydrogen silicon alcoholysis esterification pre-reaction device | |
| CN201981013U (en) | Trichlorosilane production system | |
| CN102134080B (en) | Heat-pump energy-saving separating device for extracting trichlorosilane by adopting static mixing booster and method | |
| CN202543171U (en) | Methanol recovery equipment for biodiesel production | |
| CN103755532B (en) | Chloromethyl ether continuous production system and production process utilizing same | |
| CN104045087A (en) | Device for preparing trichlorosilane | |
| CN102532181B (en) | Alcoholysis process of trimethoxy hydrosilicon | |
| CN202246100U (en) | Trichlorosilane separating and purifying system in polysilicon production process | |
| CN101805248B (en) | Method for continuously synthesizing trichloracetic aldehyde and device thereof | |
| CN209093326U (en) | A kind of organosilicon production system | |
| CN104263761A (en) | Method and device for layered fermentation of ethanol through illumination heating | |
| CN202099066U (en) | Device for preparing silicane | |
| CN112047834A (en) | Device and method for continuously preparing isobutyric anhydride | |
| CN206624653U (en) | A kind of device for preparing dichlororosilane eiectronic grade | |
| CN105036137B (en) | Method for preparing silane by disproportionation of dichlorosilane as raw material | |
| CN206739249U (en) | A kind of pure steam generator |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |