CN209778709U - Complete equipment for synthesizing bis (3-trimethoxysilylpropyl) amine by continuous method - Google Patents
Complete equipment for synthesizing bis (3-trimethoxysilylpropyl) amine by continuous method Download PDFInfo
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- CN209778709U CN209778709U CN201920651678.4U CN201920651678U CN209778709U CN 209778709 U CN209778709 U CN 209778709U CN 201920651678 U CN201920651678 U CN 201920651678U CN 209778709 U CN209778709 U CN 209778709U
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Abstract
The utility model provides a complete equipment for synthesizing bis (3-trimethoxysilylpropyl) amine by a continuous method, which comprises a synthesis kettle, a centrifuge, a crude product tank, a distillation kettle, a packed tower, 3 condensing devices and three product receiving tanks, wherein the upper end and the lower end of the synthesis kettle are respectively provided with a synthesis kettle material inlet and a synthesis kettle material outlet, the synthesis kettle material outlet is communicated with the material inlet of the centrifuge through a pipeline, the material outlet of the centrifuge is communicated with the material inlet of the crude product tank through a pipeline, the material outlet of the crude product tank is communicated with the inlet of the distillation kettle through a pipeline, and the upper end of the distillation kettle is communicated with the packed tower; the packed tower is communicated with 3 condensing units through pipelines; the 3 condensing devices are respectively communicated with the 3 product receiving tanks through pipelines; when the complete equipment of the utility model is used for synthesizing the bis (3-trimethoxysilylpropyl) amine, no catalyst is needed, the synthetic route is short, and the yield and the purity are high.
Description
Technical Field
The utility model relates to the technical field of chemical synthesis equipment, in particular to complete equipment for synthesizing bis (3-trimethoxysilylpropyl) amine by a continuous method.
Background
At present, when bis (3-trimethoxysilylpropyl) amine is produced, liquid such as 3-chloropropyltrimethoxysilane and 3-aminopropyltrimethoxysilane is mainly used as raw materials, a bis (3-trimethoxysilylpropyl) amine finished product is prepared through an organic synthesis method, and then through the working procedures of filtering, rectifying and the like, and according to technical data retrieval and market research at home and abroad, the main preparation method and production equipment of the bis (3-trimethoxysilylpropyl) amine are found to be reported.
Therefore, in combination with the process for producing bis (3-trimethoxysilylpropyl) amine, it is necessary to provide a continuous process for synthesizing bis (3-trimethoxysilylpropyl) amine in a plant, and no production apparatus comprising reacting 3-chloropropyltrimethoxysilane and 3-aminopropyltrimethoxysilane in proportion to each other in the absence of a catalyst has been reported.
SUMMERY OF THE UTILITY MODEL
In order to overcome the defects of the background art, the utility model provides a complete equipment for synthesizing bis (3-trimethoxysilylpropyl) amine by a continuous method, when the bis (3-trimethoxysilylpropyl) amine is synthesized by using the complete equipment, a catalyst is not needed, the synthetic route is short, and the yield and the purity are high.
In order to achieve the above purpose, the utility model discloses a following technical scheme realizes:
the complete equipment for synthesizing bis (3-trimethoxysilylpropyl) amine by a continuous method comprises a synthesis kettle, a centrifuge, a crude product tank, a distillation kettle, a packed tower, 3 condensing devices and three product receiving tanks, wherein the upper end and the lower end of the synthesis kettle are respectively provided with a synthesis kettle material inlet and a synthesis kettle material outlet, the synthesis kettle material outlet is communicated with the material inlet of the centrifuge through a pipeline, the material outlet of the centrifuge is communicated with the material inlet of the crude product tank through a pipeline, the material outlet of the crude product tank is communicated with the inlet of the distillation kettle through a pipeline, and the upper end of the distillation kettle is communicated with the packed tower; the packed tower is communicated with 3 condensing devices through pipelines; 3 condensing equipment passes through the pipeline respectively and receives jar intercommunication with 3 products.
Furthermore, the synthesis kettle is a vertical circular cavity, a heating jacket is arranged outside the synthesis kettle, a synthesis kettle rotating shaft driven by a motor is arranged in the synthesis kettle, and a plurality of synthesis kettle stirring blades are arranged on the synthesis kettle rotating shaft.
Further, the middle-end and the bottom of synthetic cauldron pivot respectively set up 3 synthetic cauldron stirring vane, and the distance between every synthetic cauldron stirring vane of group and the synthetic cauldron inner wall is 200mm, and the contained angle between every synthetic cauldron stirring vane place plane and the synthetic cauldron pivot is 105 degrees.
Further, a nitrogen channel is connected inside the synthesis kettle; the material inlet of the synthesis kettle is communicated with a material spray header.
Furthermore, the distillation kettle is a vertical circular cavity, a heating jacket is arranged outside the distillation kettle, a distillation kettle rotating shaft driven by a motor is arranged in the distillation kettle, and a plurality of groups of distillation kettle stirring blades are arranged on the distillation kettle rotating shaft.
furthermore, the material inlet of the synthesis kettle is connected with a raw material storage tank I, a raw material storage tank II and a raw material storage tank III through pipelines.
Furthermore, 3 condensing units are arranged at different heights of the packed tower, and the 3 condensing units are connected in parallel.
furthermore, the filler in the packed tower is filiform, blocky, annular, conical, net-shaped or plate-shaped filler, and the material of the filler is ceramic or metal.
The utility model has the advantages that:
1. Use the utility model provides a complete sets synthesizes two (3-trimethoxysilylpropyl) amine, can make production serialization, does not need to use the catalyst, easy operation, and the synthetic route is short, and the synthesis efficiency is high, and gained product purity is high, and complete sets long service life under the high temperature condition is relatively fit for with industrial production.
2. Set up three condensing equipment that is located co-altitude, be connected with the packed tower, according to the difference of material boiling point, switch when needing, reach better separation effect, ensure the purity of product.
3. The middle end and the bottom end of the resynthesis kettle are respectively provided with 3 stirring blades, the distance between each group of stirring blades and the inner wall of the cavity of the resynthesis kettle is 200mm, and the included angle between the plane where each blade is located and the rotating shaft is 105 ℃, so that the rotating shaft-blade structure can increase the flow rate and the contact surface of reaction materials, is favorable for uniform mixing of products, and ensures that the reaction is more thorough.
drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural view of the plant of the present invention;
FIG. 2 is a schematic structural view of the synthesis kettle of the present invention.
in the figure:
1. A synthesis kettle; 11. a material inlet of the synthesis kettle; 12. a material outlet of the synthesis kettle; 13. a synthetic kettle rotating shaft; 14. a synthesis kettle stirring blade; 2. a centrifuge; 3. a crude product tank; 4. a distillation kettle; 41. a distillation still rotating shaft; 42. a still stirring blade; 5. a packed tower; 61. a first condensing device; 62. a second condensing device; 63. a third condensing device; 71. a first product receiving tank; 72. a second product receiving tank; 73. a third product receiving tank; 8. a first raw material storage tank; 9. a second raw material storage tank; 10. and a third raw material storage tank.
Detailed Description
To make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the embodiments of the present invention are combined to clearly and completely describe the technical solution in the embodiments of the present invention, and obviously, the described embodiments are some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
As shown in FIGS. 1-2, a continuous process for synthesizing bis 3-trimethoxysilylpropylamine comprises a synthesis kettle 1, a centrifuge 2, a crude product tank 3, a distillation kettle 4, a packed tower 5, 3 condensing units 61, 62 and 63 and three product receiving tanks 71, 72 and 73.
The upper end and the lower end of the synthesis kettle 1 are respectively provided with a synthesis kettle material inlet 11 and a synthesis kettle material outlet 12.
The synthesis kettle material inlet 11 is connected with a raw material storage tank I8, a raw material storage tank II 9 and a raw material storage tank III 10 through pipelines, and the raw material storage tank I8, the raw material storage tank II 9 and the raw material storage tank III 10 are respectively used for storing 3-aminopropyltrimethoxysilane, 3-chloropropyltrimethoxysilane and ethylenediamine; the synthetic kettle material outlet 12 is communicated with a material inlet at the upper end of the centrifuge 2 through a pipeline, and a nitrogen channel is connected inside the synthetic kettle 1 and used for introducing nitrogen. Meanwhile, a material spray head is selectively communicated with a material inlet 11 of the synthesis kettle, and raw materials in the raw material storage tank I8, the raw material storage tank II 9 and the raw material storage tank III 10 can be sprayed into the synthesis kettle 1.
The material outlet at the lower end of the centrifuge 2 is communicated with the material inlet at the upper end of the crude product tank 3 through a pipeline, and the material outlet at the lower end of the crude product tank 3 is communicated with the inlet of the distillation still 4 through a pipeline.
Wherein, the synthesis kettle 1 and the distillation kettle 4 are both vertical round cavities, and heating jackets are arranged outside the synthesis kettle 1 and the distillation kettle 4. Be equipped with in the synthetic cauldron 1 by motor drive's synthetic cauldron pivot 13, the middle-end and the bottom of synthetic cauldron pivot 13 respectively set up 3 synthetic cauldron stirring vane 14, and the distance between every synthetic cauldron stirring vane 14 of group and the 1 inner wall of synthetic cauldron is 200mm, and the contained angle between every synthetic cauldron stirring vane 14 place plane and synthetic cauldron pivot 13 is 105 ℃.
A distillation kettle rotating shaft 41 driven by a motor is arranged in the distillation kettle 4, and a plurality of groups of distillation kettle stirring blades 42 are arranged on the distillation kettle rotating shaft 41. Alternatively, the still stirring blade 42 may be provided on the still rotating shaft 41 in the same manner as the synthesis still stirring blade 14 is provided on the synthesis still rotating shaft 13.
During production, heating jackets of the synthesis kettle 1 and the distillation kettle 4 are communicated with a low heat-conducting medium source (water vapor) at 190-200 ℃ according to the prior art.
The upper end of the distillation kettle 4 is communicated with a packed tower 5; the different heights of the packed tower 5 are communicated with 3 condensing devices 61, 62 and 63 through pipelines, and the 3 condensing devices 61, 62 and 63 are connected in parallel. The 3 condensing units 61, 62 and 63 are a first condensing unit 61, a second condensing unit 62 and a third condensing unit 63. The first condensing device 61 is positioned at a low position, the second condensing device 62 is positioned at a middle position, and the third condensing device 63 is positioned at a high position.
The 3 product receiving tanks 71, 72, 73 are a first product receiving tank 71, a second product receiving tank 72, and a third product receiving tank 73. The first condensing device 61 is communicated with the first product receiving tank 71 through a pipeline, the second condensing device 62 is communicated with the second product receiving tank 72 through a pipeline, and the third condensing device 63 is communicated with the third product receiving tank 73 through a pipeline.
The filler in the packed tower 5 is filiform, blocky, annular, conical, net-shaped or plate-shaped filler, and the material of the filler is ceramic or metal.
In the embodiment, the synthesis kettle 1 and the distillation kettle 4 are both 1.0m high and 1.0m in diameter; the diameter of the packed tower 5 is 300mm, and the height is 0.8 m. In the synthesis kettle 1 and the distillation kettle 4, the length of the corresponding rotating shaft is 0.8m, and the position 0.5m at the middle end and the position 0.8m at the bottom end of the rotating shaft are respectively provided with 3 corresponding stirring blades.
Production example:
the first step is as follows: opening a drain valve to drain water in the heating jacket of the synthesis kettle 1, and opening a steam inlet valve to heat; introducing dry nitrogen into the synthesis kettle 1, and keeping the temperature of the synthesis kettle 1 at 50 ℃ for 0.5 hour;
The second step is that: starting a feeding pump, putting 100kg of 3-aminopropyltrimethoxysilane into the synthesis kettle 1 from a raw material storage tank, heating to 90 ℃, adding 100kg of 3-chloropropyltrimethoxysilane, and continuously heating to 120 ℃ and keeping the temperature for 2 h;
The third step: cooling the synthesis kettle 1 to below 60 ℃, dropwise adding ethylenediamine, opening a valve at the bottom of the kettle, and pumping the mixed solution into a centrifuge 2;
the fourth step: filtering by a centrifuge 2 to obtain a crude product of bis (3-trimethoxysilylpropyl) amine and ammonium chloride salt;
The fifth step: pressurizing the crude bis (3-trimethoxysilylpropyl) amine product to a crude product tank 3 by using nitrogen, and collecting ammonium chloride salt from the bottom of a centrifuge 2;
And a sixth step: and (3) pumping the crude product in the crude product tank 3 into a distillation kettle 4, carrying out reduced pressure distillation, collecting ethylenediamine by a low-position condensing device I61 when the top temperature of a packed tower 5 rises to 20 ℃, collecting the front section of the product by a middle-position condensing device II 62 when the top temperature of the packed tower 5 rises to 70-100 ℃, and collecting the finished product of the bis (3-trimethoxysilylpropyl) amine by a high-position condensing device III 63 when the top temperature of the packed tower 5 rises to 150-160 ℃.
The detection of the collected products results in that: the purity of the finished bis (3-trimethoxysilylpropyl) amine product was 99.1% and the conversion was 85%.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention in its corresponding aspects.
Claims (8)
1. a complete plant for synthesizing bis (3-trimethoxysilylpropyl) amine by a continuous method is characterized in that: the device comprises a synthesis kettle (1), a centrifugal machine (2), a crude product tank (3), a distillation kettle (4), a packed tower (5), 3 condensing units (61, 62 and 63) and three product receiving tanks (71, 72 and 73), wherein the upper end and the lower end of the synthesis kettle (1) are respectively provided with a synthesis kettle material inlet (11) and a synthesis kettle material outlet (12), the synthesis kettle material outlet (12) is communicated with a material inlet of the centrifugal machine (2) through a pipeline, the material outlet of the centrifugal machine (2) is communicated with the material inlet of the crude product tank (3) through a pipeline, the material outlet of the crude product tank (3) is communicated with an inlet of the distillation kettle (4) through a pipeline, and the upper end of the distillation kettle (4) is communicated with the packed tower (5); the packed tower (5) is communicated with 3 condensing devices (61, 62 and 63) through pipelines; the 3 condensing devices (61, 62, 63) are respectively communicated with the 3 product receiving tanks (71, 72, 73) through pipelines.
2. The plant according to claim 1, wherein the synthesis kettle (1) is a vertical circular cavity, a heating jacket is arranged outside the synthesis kettle (1), a synthesis kettle rotating shaft (13) driven by a motor is arranged in the synthesis kettle (1), and a plurality of combined kettle stirring blades (14) are arranged on the synthesis kettle rotating shaft (13).
3. The plant according to claim 2, wherein 3 synthetic kettle stirring blades (14) are respectively arranged at the middle end and the bottom end of the synthetic kettle rotating shaft (13), the distance between each group of synthetic kettle stirring blades (14) and the inner wall of the synthetic kettle (1) is 200mm, and the included angle between the plane of each synthetic kettle stirring blade (14) and the synthetic kettle rotating shaft (13) is 105 degrees.
4. The plant according to claim 1, characterized in that the synthesis vessel (1) is internally connected with a nitrogen channel; the material inlet (11) of the synthesis kettle is communicated with a material spray header.
5. The plant according to claim 1, wherein the distillation kettle (4) is a vertical circular cavity, a heating jacket is arranged outside the distillation kettle (4), a distillation kettle rotating shaft (41) driven by a motor is arranged in the distillation kettle (4), and a plurality of groups of distillation kettle stirring blades (42) are arranged on the distillation kettle rotating shaft (41).
6. The plant according to claim 1, characterized in that the synthesis kettle material inlet (11) is connected with a raw material storage tank I (8), a raw material storage tank II (9) and a raw material storage tank III (10) through pipelines.
7. Plant according to claim 1, characterized in that 3 condensation devices (61, 62, 63) are provided at different heights of the packed tower (5), the 3 condensation devices (61, 62, 63) being connected in parallel.
8. The plant according to claim 1, characterized in that the packing in the packed tower (5) is wire-shaped, block-shaped, ring-shaped, cone-shaped, net-shaped or plate-shaped packing, and the material of the packing is ceramic or metal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920651678.4U CN209778709U (en) | 2019-05-08 | 2019-05-08 | Complete equipment for synthesizing bis (3-trimethoxysilylpropyl) amine by continuous method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920651678.4U CN209778709U (en) | 2019-05-08 | 2019-05-08 | Complete equipment for synthesizing bis (3-trimethoxysilylpropyl) amine by continuous method |
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| CN209778709U true CN209778709U (en) | 2019-12-13 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970785A (en) * | 2019-05-08 | 2019-07-05 | 安徽硅宝有机硅新材料有限公司 | Continuity method synthesizes the complete set of equipments of bis- (3- trimethoxy-silylpropyl) amine |
| CN115044101A (en) * | 2022-05-19 | 2022-09-13 | 湖北华欣有机硅新材料有限公司 | Production process and production device of composite silane |
-
2019
- 2019-05-08 CN CN201920651678.4U patent/CN209778709U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970785A (en) * | 2019-05-08 | 2019-07-05 | 安徽硅宝有机硅新材料有限公司 | Continuity method synthesizes the complete set of equipments of bis- (3- trimethoxy-silylpropyl) amine |
| CN109970785B (en) * | 2019-05-08 | 2024-04-26 | 安徽硅宝有机硅新材料有限公司 | Complete equipment for synthesizing bis (3-trimethoxysilylpropyl) amine by continuous method |
| CN115044101A (en) * | 2022-05-19 | 2022-09-13 | 湖北华欣有机硅新材料有限公司 | Production process and production device of composite silane |
| CN115044101B (en) * | 2022-05-19 | 2023-06-30 | 湖北华欣有机硅新材料有限公司 | Production process and production device of composite silane |
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