CN201614355U - Gamma-chloropropyl triethoxy silane esterification reaction device - Google Patents
Gamma-chloropropyl triethoxy silane esterification reaction device Download PDFInfo
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- CN201614355U CN201614355U CN2009202909297U CN200920290929U CN201614355U CN 201614355 U CN201614355 U CN 201614355U CN 2009202909297 U CN2009202909297 U CN 2009202909297U CN 200920290929 U CN200920290929 U CN 200920290929U CN 201614355 U CN201614355 U CN 201614355U
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Abstract
The utility model discloses a gamma-chloropropyl triethoxy silane esterification reaction device, comprising a main esterification kettle and a main condenser, wherein the main esterification kettle is respectively provided with an upper material inlet and a lower material outlet, the main condenser is communicated with the main esterification kettle; the reaction device further comprises a secondary esterification reaction device communicated with the main esterification kettle. The reaction device is used for the esterification reaction of gamma-chloropropyl triethoxy silane, and can shorten the esterification reaction period, improve the conversion utilization ratio of raw materials, and reduce raw material loss and production cost.
Description
Technical field
The utility model relates to the chemical industry equipment field, relates in particular to the esterification device in a kind of γ-chloropropyl triethoxysilane production.
Background technology
γ-chloropropyl triethoxysilane is a kind of important silane coupling agent and other kind silane coupling agent synthetic key intermediate, be used for coupling organic polymer and mineral filler, strengthen its cohesiveness, improve the machinery of product, performance such as electric, water-fast and anti-aging.Be usually used in industries such as glass, casting, yarn fabric auxiliary agent, insulating material and glue paste, vast market prospect is arranged.
Traditional γ-chloropropyl triethoxysilane esterification is that γ-chloropropyl trichloro-silane and dehydrated alcohol are at 60～80 ℃, under-the 0.096MPa in common reaction kettle of the esterification esterification takes place, adopt γ-chloropropyl trichloro-silane once to add, the mode that dehydrated alcohol adds in batches, react after about 6 hours the 4h that refluxes under-0.096MPa, total reaction time of esterification is more than the 10h.After the neutralizations such as the thick product process sodium ethylate after the esterification, squeeze into still kettle rectifying, make γ-chloropropyl triethoxysilane product.The tradition esterification device is simple because of equipment, reaction conditions is wayward, therefore the processing condition such as constant of temperature and vacuum tightness are had relatively high expectations, so not only exist to operational condition require harsh, reaction time is long, reaction not exclusively and problems such as energy consumption height, and the feedstock conversion utilization ratio is low, makes thick product foreign matter content height.Therefore the technical problem that exists at prior art, combined process research, by esterification device is improved, to shorten reaction time to greatest extent, improve the conversion and the utilization ratio of raw material, reduce production costs, the production of γ-chloropropyl trichloro-silane is had important economic implications and realistic meaning.
Summary of the invention
Technical problem to be solved in the utility model provides a kind of improved γ-chloropropyl triethoxysilane esterification device, to shorten the esterification cycle and to improve the feedstock conversion utilization ratio.
For solving the problems of the technologies described above, the technical solution of the utility model is:
γ-chloropropyl triethoxysilane esterification device, comprise the main esterifying kettle that is respectively arranged with material inlet and following material inlet, with the main condenser that is communicated with described main esterifying kettle, described reaction unit also comprises the secondary esterification device that is communicated with described main esterifying kettle.
Described secondary esterification device comprises counter-current reactor, secondary esterifying kettle and secondary condenser, the outlet of described counter-current reactor bottom is communicated with the import that is positioned at secondary esterifying kettle top, the outlet at described counter-current reactor top is communicated with described secondary condenser import, is positioned at the import of described counter-current reactor bottom and the outlet of secondary esterifying kettle bottom and is communicated with described main esterifying kettle by adverse current feeding pipeline and feed back pipeline respectively.
Be provided with the filler that contains catalyst component in the described counter-current reactor.
The top of described counter-current reactor is provided with material inlet.
Described main condenser is two condensers that connect with series system.
Owing to adopted technique scheme, the beneficial effects of the utility model are:
1, the utility model carries out carrying out the secondary esterification again after the counter-current separation to raw material by increasing the secondary esterification device, makes the raw material recycle, and make esterification be in dynamic balance state, improve the conversion and the utilization ratio of raw material, reduced significant loss, reduced production cost.
2, behind the increase secondary esterification device, increased the esterification progress, make original rhythmic reaction process become the semicontinuous reaction process of semi-batch, shortened reaction time, reaction times has on average shortened 1 times when using traditional esterification device, and the unit operation period ratio shortens more than 1/4 when using traditional esterification device.
3, be provided with the filler that contains catalyzer in the counter-current reactor of the present utility model, not only can effectively separate with hydrogen chloride gas with γ-chloropropyl trichloro-silane feed ethanol, the catalyst component that filler contains can also fast reaction speed.
4, counter-current reactor of the present utility model top is provided with material inlet, raw material γ-chloropropyl trichloro-silane enters reactor from the material inlet spray, the high-temperature gas material that comes with the autonomic response still meets, be convenient to the mutual mass-and heat-transfer of cold and hot storeroom, can more completely hydrogen chloride gas be separated with raw material, and the raw material uniform mixing when being beneficial to the secondary esterification, be beneficial to the carrying out of secondary esterification.
5, the top of main reaction still of the present utility model and lower end are respectively arranged with material inlet, and raw material adds fashionablely can adopt the backward feed mode, is convenient to raw material and mixes, and improves speed of response and reaction uniformity.
6, utilizing the utility model to carry out γ-chloropropyl triethoxysilane esterification, can association reaction be SN
2The reaction mechanism of reversible reaction by to material properly distributed and thorough mixing, has been enlivened the generation of reaction intermediate, has further accelerated speed of response.
Description of drawings
Accompanying drawing is a structural representation of the present utility model.
Among the figure, 1. main esterifying kettle; 11. last material inlet; 12. following material inlet; 2. condensing reflux pipeline; 3. main condenser; 31. first main condenser; 32. second main condenser; 4. counter-current reactor; 41. filler; 42. reflux condenser material inlet; 5. secondary esterifying kettle; 6. secondary condenser; 7. adverse current feeding pipeline; 8. feed back pipeline.
Embodiment
As shown in drawings, γ-chloropropyl triethoxysilane esterification device, comprise the main esterifying kettle 1 that is respectively arranged with material inlet 11 and following material inlet 12, with the main condenser 3 that is communicated with described main esterifying kettle 1, described reaction unit also comprises the secondary esterification device that is communicated with described main esterifying kettle 1
Described secondary esterification device comprises counter-current reactor 4, secondary esterifying kettle 5 and secondary condenser 6, the outlet of described counter-current reactor 4 bottoms is communicated with the import that is positioned at secondary esterifying kettle 5 tops, the outlet at described counter-current reactor 4 tops is communicated with described secondary condenser 6 imports, is positioned at the import of described counter-current reactor 4 bottoms and the outlet of secondary esterifying kettle 5 bottoms and is communicated with described main esterifying kettle 1 by adverse current feeding pipeline 7 and feed back pipeline 8 respectively.
Described main condenser 3 is first main condenser 31 and second main condenser 32 that connects with series system.
Be provided with filler 41 in the described counter-current reactor 4, its top is provided with material inlet 42.
During the utility model work, the main reaction still adopts the adverse current feeding mode, γ-chloropropyl trichloro-silane once adds (add-on is 2/3rds when using legacy equipment) from the last material inlet 11 of main reaction still 1, following material inlet 12 from main reaction still 1 adds dehydrated alcohol gradually then, main esterification begins, open the valve on the condensation return line 2, add temperature of reaction with alcoholic acid and rise to 50 ℃ gradually from 25 ℃.React about 1h, and amount of alcohol added is about and stops the ethanol charging two of total add-on/a period of time, with the valve closes on the condensing reflux pipeline 2, open the valve on the adverse current feeding pipeline 7 simultaneously, main esterification reaction temperature is increased to 120～123 ℃ rapidly, because under the normal pressure, the boiling point of γ-chloropropyl trichloro-silane is 179～180 ℃, the alcoholic acid boiling point is 78.3 ℃, the boiling point of γ-chloropropyl triethoxysilane is 221 ℃, and hydrogenchloride is gaseous state, therefore ethanol content is the highest in the feed liquid that steams under 120～123 ℃ of temperature, secondly be chloropropyl trichloro-silane, unreacted ethanol and a small amount of unreacted γ-chloropropyl trichloro-silane vaporization is with after mother liquor separates, enter counter-current reactor 4 by condensing reflux pipeline 7, and under the effect of the filler in being arranged on counter-current reactor 4 41, hydrogen chloride gas is separated, this moment, the material inlet 42 from counter-current reactor 4 entered counter-current reactor 4 with certain speed with raw material γ-chloropropyl trichloro-silane spray, with the pyritous gaseous state material mass-and heat-transfer that comes from main esterifying kettle, be more conducive to hydrogen chloride gas is separated the hydrogen chloride gas of the separating gas recovery system that after condenser 6 condensations, truncates.
Material in counter-current reactor 4 under reflux enters secondary esterifying kettle 5, and the temperature of controlling secondary esterifying kettle 5 is 60～80 ℃ and carries out the secondary esterification.When feed liquid reaches the reaction needed amount in secondary esterifying kettle 5, the reflux pipeline 7 of main esterifying kettle 1 is switched to condensing reflux pipeline 2, simultaneously autonomous 1 time material inlet of esterifying kettle 12 continues to add ethanol, and temperature of charge in the main esterifying kettle 1 is controlled at 60～80 ℃ proceeds main esterification.
After reaction for some time, secondary esterifying kettle intensive amount is met the requirements of γ-chloropropyl triethoxysilane, be back to main reaction still 1 by feed back pipeline 8.
More than the reaction control process repeated once in per 3 hours, and γ in main esterifying kettle 1-chloropropyl triethoxysilane content reaches the content that needs.
In the esterification reaction process, the pressure of reactive system all is controlled at-below the 0.096Mpa.
Claims (5)
1. γ-chloropropyl triethoxysilane esterification device, comprise the main esterifying kettle that is respectively arranged with material inlet and following material inlet, main condenser with being communicated with described main esterifying kettle is characterized in that: described reaction unit also comprises the secondary esterification device that is communicated with described main esterifying kettle.
2. γ as claimed in claim 1-chloropropyl triethoxysilane esterification device, it is characterized in that: described secondary esterification device comprises counter-current reactor, secondary esterifying kettle and secondary condenser, the outlet of described counter-current reactor bottom is communicated with the import that is positioned at secondary esterifying kettle top, the outlet at described counter-current reactor top is communicated with described secondary condenser import, is positioned at the import of described counter-current reactor bottom and the outlet of secondary esterifying kettle bottom and is communicated with described main esterifying kettle by adverse current feeding pipeline and feed back pipeline respectively.
3. γ as claimed in claim 2-chloropropyl triethoxysilane esterification device is characterized in that: be provided with the filler that contains catalyst component in the described counter-current reactor.
4. γ as claimed in claim 2-chloropropyl triethoxysilane esterification device is characterized in that: the top of described counter-current reactor is provided with material inlet.
5. as claim 1,2,3 or 4 described γ-chloropropyl triethoxysilane esterification devices, it is characterized in that: two condensers of described main condenser for connecting with series system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2009202909297U CN201614355U (en) | 2009-12-25 | 2009-12-25 | Gamma-chloropropyl triethoxy silane esterification reaction device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009202909297U CN201614355U (en) | 2009-12-25 | 2009-12-25 | Gamma-chloropropyl triethoxy silane esterification reaction device |
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| CN2009202909297U Expired - Fee Related CN201614355U (en) | 2009-12-25 | 2009-12-25 | Gamma-chloropropyl triethoxy silane esterification reaction device |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086214A (en) * | 2010-12-04 | 2011-06-08 | 郭学阳 | Method for producing gamma-chloropropyl triethoxysilane |
| 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 |
| CN106699801A (en) * | 2016-11-22 | 2017-05-24 | 山东硅科新材料有限公司 | Synthetic process of silicon-based imidazole epoxy resin curing agent |
-
2009
- 2009-12-25 CN CN2009202909297U patent/CN201614355U/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086214A (en) * | 2010-12-04 | 2011-06-08 | 郭学阳 | Method for producing gamma-chloropropyl triethoxysilane |
| CN102086214B (en) * | 2010-12-04 | 2013-07-31 | 郭学阳 | Method for producing gamma-chloropropyl triethoxysilane |
| 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 |
| CN106699801A (en) * | 2016-11-22 | 2017-05-24 | 山东硅科新材料有限公司 | Synthetic process of silicon-based imidazole epoxy resin curing agent |
| CN106699801B (en) * | 2016-11-22 | 2019-09-20 | 山东硅科新材料有限公司 | The synthesis technology of silicon substrate imidazoles based epoxy resin curing agent |
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| C14 | Grant of patent or utility model | ||
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101027 Termination date: 20111225 |