Automatic temperature control system for preparing triisopropyl chlorosilane
By using an inner and outer jacket structure and an automatic temperature control system, the problems of time-consuming and labor-intensive temperature control and safety hazards in the preparation of triisopropylsilane have been solved, and automatic temperature adjustment and safety improvement have been achieved.
Patent Information
- Application Number
- CN202422770378.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-13
- Publication Date
- 2025-10-31
- Estimated Expiration
- 2034-11-13
AI Technical Summary
In the current process of preparing triisopropylsilane, the temperature control of the reactor relies on manual operation, which is time-consuming, labor-intensive, and poses safety hazards. Furthermore, the reagents can easily cause an explosion when they come into contact with water or air.
The system employs an inner and outer jacket structure, combined with an automatic temperature control system using temperature sensors and solenoid valves, to achieve automatic switching between hot and cold media. Heating and cooling are achieved by introducing cold and hot oil through the inner and outer jackets, and nitrogen purging is used to prevent reagents from coming into contact with water and air.
This enabled timely control of the reactor temperature, reduced the frequency of manual operation, improved production safety, and avoided safety hazards and reagent leakage risks.
Smart Images
Figure CN223501337U_ABST
Abstract
Description
Technical fields:
[0001] This utility model relates to an automatic temperature control system for the preparation of triisopropylchlorosilane, and particularly to an automatic temperature control system for the preparation of triisopropylchlorosilane. Background technology:
[0002] Triisopropylsilane is a raw material for synthesizing sterically hindered organosilicon protective agents. It is mainly used to protect various types of hydroxyl groups, especially in polyfunctional hydroxyl compounds, where selective protection and deprotection are possible. This is very important for the synthesis of nucleotides, nucleotide acids, and sugar compounds. It is also a raw material for synthesizing antifouling coating compositions that have excellent water resistance and can effectively produce antifouling effects for a long time, even when immersed in seawater for a long time, and that can prevent or inhibit the adhesion of slime. This composition reduces the content of volatile organic compounds evaporated into the air and has high environmental safety.
[0003] The current method for preparing triisopropylsilane involves adding Grignard reagent to a synthesis reactor, followed by the dropwise addition of a mixture of trichlorosilane, n-butyl ether, and trimethoxysilane. A Grignard reaction occurs in the reactor, requiring temperature control. This necessitates manually circulating cooling water or heating steam into the reactor's jacket. This method is time-consuming and labor-intensive, and it cannot effectively control the reactor temperature, posing a significant safety hazard. Furthermore, if the reactor punctures, causing the Grignard reagent to come into contact with water or air, an explosion risk is highly probable. Utility Model Content:
[0004] The purpose of this invention is to provide an automatic temperature control system for the preparation of triisopropylchlorosilane that has a simple connection structure, reduces labor costs, and improves production safety.
[0005] This utility model is implemented by the following technical solution: The purpose of this patent is to provide an automatic temperature control system for the preparation of triisopropylchlorosilane, which includes a synthesis reactor. An inner jacket and an outer jacket are respectively provided inside and outside the synthesis reactor. The oil outlet of the cold oil pipeline is connected to the liquid inlet of the inner jacket, and the oil outlet of the hot oil pipeline is connected to the oil inlet of the outer jacket. A first temperature sensor is provided inside the synthesis reactor. A first solenoid valve is provided on the cold oil pipeline, and a second solenoid valve is provided on the hot oil pipeline. The signal output terminal of the first temperature sensor is connected to the signal input terminal of the controller via a signal connection. The signal output terminal of the controller is connected to the signal input terminals of the first solenoid valve and the second solenoid valve via a signal connection.
[0006] Furthermore, it also includes a cold oil cooling vessel and a hot oil heating vessel; the oil outlet of the inner jacket is connected to the liquid inlet of the cold oil cooling vessel, the liquid outlet of the cold oil cooling vessel is connected to the oil inlet of the cold oil pipeline, and the water outlet of the chilled brine pipeline is connected to the liquid inlet of the outer jacket of the cold oil cooling vessel; the oil outlet of the outer jacket is connected to the liquid inlet of the hot oil heating vessel, the liquid outlet of the hot oil heating vessel is connected to the oil inlet of the hot oil pipeline, and the steam outlet of the steam pipeline is connected to the steam inlet of the outer jacket of the hot oil heating vessel.
[0007] Furthermore, a second temperature sensor and a third temperature sensor are respectively installed in the cold oil cooling vessel and the hot oil heating vessel; a first regulating valve is installed on the chilled brine pipeline, and a second regulating valve is installed on the steam pipeline; the signal output terminals of the second temperature sensor and the third temperature sensor are both connected to the signal input terminal of the controller via signal connection; the signal output terminal of the controller is connected to the signal input terminals of the first regulating valve and the second regulating valve via signal connection.
[0008] Furthermore, it also includes a nitrogen pipeline, the outlet of which is connected to the inlet of the cold oil cooling vessel, the inlet of the hot oil heating vessel, the inlet on the oil outlet pipeline of the inner jacket, and the inlet on the oil outlet pipeline of the outer jacket, respectively.
[0009] It also includes a cooler, wherein the oil outlet of the inner jacket is connected to the hot medium inlet of the cooler, the hot medium outlet of the cooler is connected to the liquid inlet of the cold oil cooling vessel, and the water outlet of the chilled brine pipeline is connected to the cold medium inlet of the cooler.
[0010] Advantages of this utility model: 1. The connection structure of this utility model is simple and easy to implement. By setting a first temperature sensor, a first solenoid valve and a second solenoid valve, the automatic switching of hot and cold media is realized, which reduces the frequency of personnel operating the hot and cold media to enter the inner and outer jackets, saving time and effort, reducing labor costs, and at the same time realizing timely control of the temperature inside the synthesis reactor, avoiding safety hazards caused by excessive temperature.
[0011] 2. The synthesis reactor is heated and cooled by circulating cold and hot oil through the inner and outer jackets, which avoids contact between the reagents and water. When the system is shut down, nitrogen is used for purging, achieving nitrogen sealing and preventing the reagents from coming into contact with air, thus improving production safety. Attached image description:
[0012] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.
[0013] Figure 1 This is a schematic diagram of the overall structure of this utility model.
[0014] Synthesis vessel 1, inner jacket 101, outer jacket 102, cold oil cooling vessel 2, hot oil heating vessel 3, nitrogen pipeline 4, cold oil pipeline 5, hot oil pipeline 6, first temperature sensor 7, first solenoid valve 8, second solenoid valve 9, controller 10, chilled brine pipeline 11, steam pipeline 12, second temperature sensor 13, third temperature sensor 14, first regulating valve 15, second regulating valve 16, cooler 17. Detailed implementation method:
[0015] Example: Figure 1 As shown, an automatic temperature control system for the preparation of triisopropylchlorosilane includes a synthesis reactor 1, a cold oil cooling reactor 2, a hot oil heating reactor 3, a nitrogen pipeline 4, and a cooler 17. An inner jacket 101 and an outer jacket 102 are respectively installed inside and outside the synthesis reactor 1. The oil outlet of the cold oil pipeline 5 is connected to the liquid inlet of the inner jacket 101, and the oil outlet of the hot oil pipeline 6 is connected to the oil inlet of the outer jacket 102. A first temperature sensor 7 is installed inside the synthesis reactor 1. A first solenoid valve 8 is installed on the cold oil pipeline 5, and a second solenoid valve 9 is installed on the hot oil pipeline 6. The signal output terminal of the first temperature sensor 7 is connected to the signal input terminal of a controller 10 via a signal connection. The signal output terminal of the controller 10 is connected to the signal input terminals of the first solenoid valve 8 and the second solenoid valve 9 via signal connections. Heating and cooling of the synthesis reactor 1 are achieved by introducing cold oil and hot oil into the inner jacket 101 and the outer jacket 102 of the synthesis reactor 1, respectively, avoiding contact between the reagents and water and improving production safety.
[0016] The oil outlet of the inner jacket 101 is connected to the hot medium inlet of the cooler 17, the hot medium outlet of the cooler 17 is connected to the liquid inlet of the cold oil cooling vessel 2, and the water outlet of the chilled brine pipeline 11 is connected to the cold medium inlet of the cooler 17; the liquid outlet of the cold oil cooling vessel 2 is connected to the oil inlet of the cold oil pipeline 5, and the water outlet of the chilled brine pipeline 11 is connected to the liquid inlet of the jacket outside the cold oil cooling vessel 2; the oil outlet of the outer jacket 102 is connected to the liquid inlet of the hot oil heating vessel 3, the liquid outlet of the hot oil heating vessel 3 is connected to the oil inlet of the hot oil pipeline 6, and the steam outlet of the steam pipeline 12 is connected to the steam inlet of the jacket outside the hot oil heating vessel 3.
[0017] A second temperature sensor 13 and a third temperature sensor 14 are respectively installed in the cold oil cooling vessel 2 and the hot oil heating vessel 3; a first regulating valve 15 is installed on the chilled brine pipeline 11, and a second regulating valve 16 is installed on the steam pipeline 12; the signal output terminals of the second temperature sensor 13 and the third temperature sensor 14 are both connected to the signal input terminal of the controller 10 via signal connection; the signal output terminal of the controller 10 is connected to the signal input terminals of the first regulating valve 15 and the second regulating valve 16 via signal connection.
[0018] The outlet of nitrogen pipeline 4 is connected to the inlet of cold oil cooling vessel 2, the inlet of hot oil heating vessel 3, the inlet of the oil outlet pipeline of inner jacket 101, and the inlet of the oil outlet pipeline of outer jacket 102.
[0019] Working principle:
[0020] When a mixture of trichlorosilane, n-butyl ether, and trimethoxysilane is added dropwise to synthesis vessel 1, the first temperature sensor 7 continuously monitors the temperature inside synthesis vessel 1. When the temperature rise rate exceeds 2℃ / min or the temperature exceeds 55℃, the controller 10 controls the first solenoid valve 8 to open, allowing cooling oil to flow into the inner jacket 101 for cooling, thus maintaining the temperature inside synthesis vessel 1 at 40-50℃ to ensure stable reaction and prevent safety hazards due to excessive temperature. After the mixture addition is complete, the controller 10 controls the first solenoid valve 8... Close the second solenoid valve 9 and open it to introduce hot oil into the outer jacket 102 for heating, so that the temperature inside the synthesis reactor 1 is controlled at 60-70℃. When the temperature reaches 70℃, the controller 10 adjusts the second solenoid valve 9 to close it slightly. When the temperature reaches 60℃, the controller 10 adjusts the second solenoid valve 9 to open it wider. After maintaining the temperature for a certain period of time, the reactants in the synthesis reactor 1 are released. At the same time, the controller 10 controls the second solenoid valve 9 to close and introduces nitrogen gas for replacement, thus achieving nitrogen sealing, preventing the reagents from coming into contact with air, and improving production safety.
[0021] After the cold oil in the inner jacket 101 has completed heat exchange, it first enters the cooler 17 for preliminary cooling, and then enters the cold oil cooling vessel 2. The frozen brine is passed through the jacket outside the cold oil cooling vessel 2 for cooling, so that the cold oil in the cold oil cooling vessel 2 is cooled to -10-0℃. The second temperature sensor 13 constantly detects the temperature of the cold oil in the cold oil cooling vessel 2 and transmits it to the controller 10. When the temperature reaches -10℃, the controller 10 controls the first regulating valve 15 to open slightly, and when the temperature reaches 0℃, the controller 10 controls the first regulating valve 15 to open wider.
[0022] After the hot oil in the outer jacket 102 has completed heat exchange, it enters the hot oil heating vessel 3. Steam is introduced into the jacket outside the hot oil heating vessel 3 for heating, so that the hot oil in the hot oil heating vessel 3 is heated to 70-90℃. The third temperature sensor 14 detects the temperature of the hot oil in the hot oil heating vessel 3 at all times and transmits it to the controller 10. When the temperature reaches 90℃, the controller 10 controls the second regulating valve 16 to open slightly. When the temperature reaches 70℃, the controller 10 controls the second regulating valve 16 to open wider.
[0023] This utility model has a simple and easy-to-implement connection structure, realizes automatic switching of hot and cold media, reduces the frequency of personnel operation of hot and cold media to be introduced into the inner jacket 101 and the outer jacket 102, saves time and effort, reduces labor costs, and at the same time realizes timely control of the temperature inside the synthesis reactor 1, avoiding safety hazards due to excessive temperature.
[0024] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.
Claims
1. An automatic temperature control system for the preparation of triisopropylchlorosilane, characterized in that: It includes a synthesis reactor, with an inner jacket and an outer jacket respectively provided inside and outside the synthesis reactor. The oil outlet of the cold oil pipeline is connected to the liquid inlet of the inner jacket, and the oil outlet of the hot oil pipeline is connected to the oil inlet of the outer jacket. A first temperature sensor is provided inside the synthesis reactor, a first solenoid valve is provided on the cold oil pipeline, and a second solenoid valve is provided on the hot oil pipeline. The signal output terminal of the first temperature sensor is connected to the signal input terminal of the controller via a signal connection, and the signal output terminal of the controller is connected to the signal input terminals of the first solenoid valve and the second solenoid valve via a signal connection.
2. The automatic temperature control system for the preparation of triisopropylchlorosilane according to claim 1, characterized in that: It also includes a cold oil cooling vessel and a hot oil heating vessel; the oil outlet of the inner jacket is connected to the liquid inlet of the cold oil cooling vessel, the liquid outlet of the cold oil cooling vessel is connected to the oil inlet of the cold oil pipeline, and the water outlet of the chilled brine pipeline is connected to the liquid inlet of the outer jacket of the cold oil cooling vessel; the oil outlet of the outer jacket is connected to the liquid inlet of the hot oil heating vessel, the liquid outlet of the hot oil heating vessel is connected to the oil inlet of the hot oil pipeline, and the steam outlet of the steam pipeline is connected to the steam inlet of the outer jacket of the hot oil heating vessel.
3. The automatic temperature control system for the preparation of triisopropylchlorosilane according to claim 2, characterized in that: A second temperature sensor and a third temperature sensor are respectively installed in the cold oil cooling tank and the hot oil heating tank; a first regulating valve is installed on the chilled brine pipeline and a second regulating valve is installed on the steam pipeline; the signal output terminals of the second temperature sensor and the third temperature sensor are both connected to the signal input terminal of the controller; the signal output terminal of the controller is connected to the signal input terminals of the first regulating valve and the second regulating valve respectively.
4. An automatic temperature control system for the preparation of triisopropylchlorosilane according to any one of claims 1-3, characterized in that: It also includes a nitrogen pipeline, the outlet of which is connected to the inlet of the cold oil cooling vessel, the inlet of the hot oil heating vessel, the inlet of the oil outlet pipeline of the inner jacket, and the inlet of the oil outlet pipeline of the outer jacket.
5. The automatic temperature control system for the preparation of triisopropylchlorosilane according to claim 4, characterized in that: It also includes a cooler, wherein the oil outlet of the inner jacket is connected to the hot medium inlet of the cooler, the hot medium outlet of the cooler is connected to the liquid inlet of the cold oil cooling vessel, and the water outlet of the chilled brine pipeline is connected to the cold medium inlet of the cooler.