Chlorosilane esterification reaction apparatus

Abstract

The utility model provides a kind of chlorosilane esterification reaction device, by setting pre-reactor, and two esterification reactors, methanol is shunted to reaction raw material, it is realized to carry out preliminary reaction in pre-reactor and then enter esterification reactor one condensing section and carry out preliminary reaction, then enter esterification reactor two and another methanol carries out sufficient esterification reaction, can effectively reduce the risk that the liquid phase of excessive pressure impact backflow caused by a large amount of reaction heat in turn leads to flooding, improve the security of production.

Description

Technical Field

[0001] This utility model relates to the chemical industry, specifically to a chlorosilane esterification reaction apparatus. Background Technology

[0002] In the esterification reaction of chlorosilanes, due to the special reaction conditions and differences in material properties, the problem of material overflowing into the reaction condenser often occurs. This not only causes some materials to undergo unnecessary reactions in the condenser, generating difficult-to-handle byproducts, but also affects the normal operation of the entire reaction system, and may even lead to equipment damage, thereby reducing production efficiency and economic benefits.

[0003] While existing technologies include various chlorosilane esterification reaction devices, such as the vinyltrichlorosilane esterification gas-phase reaction tower device (patent publication number CN207025291U), which optimizes reaction conditions and improves reaction efficiency by setting up multi-stage reaction trays and heating / cooling coils, it does not offer an effective solution to the problem of material overflow. Similarly, the hydrogen chloride recovery and purification system generated during chlorosilane esterification (patent publication number CN214936054U) mainly focuses on the recovery and purification of hydrogen chloride, without addressing the material overflow problem. The harmless treatment mechanism for 3-chloropropyltrichlorosilane synthesis tail gas (patent publication number CN208542003U) focuses on the harmless treatment of tail gas, also failing to solve the material overflow problem. Although an esterification reaction device (patent publication number CN220940693U) optimizes the esterification reaction process and improves the degree of esterification by setting up small and large circulation pipelines, it also does not offer specific measures to address the material overflow problem. Utility Model Content

[0004] This invention proposes a chlorosilane esterification reaction device to reduce the problem of material overflow and improve safety.

[0005] The technical solution of this utility model is implemented as follows: A chlorosilane esterification reaction apparatus includes a pre-reactor, an esterification reactor one, and an esterification reactor two connected in sequence; the pre-reactor is used for activation to the critical reaction temperature, and both esterification reactor one and esterification reactor two are used for the esterification reaction, each including an upper condensation section and a lower vessel body; the vessel body is equipped with a heating pipeline; wherein: The feed end of the pre-reactor is connected to a chlorosilane feed pipe and a methanol feed pipe 1, respectively. The bottom of the pre-reactor is connected to the condensation section of the esterification reactor 1 via a pipeline. The vessel body of the esterification reactor 1 is connected to the condensation section of the esterification reactor 2 via a pipeline. The condensation section of the esterification reactor 2 is also connected to a methanol feed pipe 2. The vessel body is also equipped with a crude product collection pipe.

[0006] Furthermore, the top of the pre-reactor is connected to the upper part of the pre-reactor via the material channel of the condensation unit; the material output pipeline of the condensation unit is also connected to a demister, the lower part of which is connected to the upper part of the pre-reactor.

[0007] Preferably, the condensation unit includes multiple condensers connected in series, with the material output end of the last condenser connected to the demister via the medium channel of the first condenser.

[0008] More preferably, the condensation unit includes condenser one, condenser two, and condenser three. The top of the pre-reactor is provided with pipelines that sequentially pass through the material channels of condenser one, condenser two, and condenser three and return to the upper part of the pre-reactor. Each of condenser one and condenser two has a separate pipeline at its material output end that connects to the upper part of the pre-reactor. The material output end of condenser three is provided with a pipeline that passes through the medium channel of condenser one and connects to the demister.

[0009] Preferably, the top of the condensation section of the esterification reactor is connected to the upper part of the pre-reactor via a pipeline through the condenser.

[0010] Furthermore, the vessel of the esterification reactor is provided with a circulation pipe connected to its own condensation section.

[0011] Furthermore, the second esterification reactor is equipped with a second circulation pipe connected to its own condensation section.

[0012] Furthermore, the top of the condensation section of the second esterification reactor is provided with a circulation pipe three that is connected to the condensation section of the first esterification reactor.

[0013] Furthermore, the condensation section of the esterification reactor is equipped with a vent pipe at the top.

[0014] Furthermore, the second esterification reactor is equipped with a mother liquor feed pipe.

[0015] Compared with the prior art, the beneficial effects of this utility model are as follows: This invention, by setting up a pre-reactor and two esterification reactors, diverts the methanol raw material for reaction. After pre-reaction in the pre-reactor, the methanol enters the condensation section of the first esterification reactor for preliminary reaction, and then enters the second esterification reactor to undergo a full esterification reaction with another stream of methanol. This effectively reduces the risk of excessive pressure caused by the generation of a large amount of reaction heat, which could impact the backflow of liquid phase and lead to flooding, thus improving the safety of production. Attached Figure Description

[0016] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram of an overall chlorosilane esterification reaction apparatus provided by the present invention.

[0018] The attached figures are labeled as follows: L1, Chlorosilane feed pipe; L2, Methanol feed pipe one; L3, Methanol feed pipe two; L4, Crude product collection pipe; L5, Circulation pipe one; L6, Circulation pipe two; L7, Circulation pipe three; L8, Vent pipe; L9, Mother liquor feed pipe; C1, Condenser one; C2, Condenser two; C3, Condenser three; C4, Condenser four; D1, Demister; E1, Vaporizer; R1, Pre-reactor; R2, Esterification reactor one; R3, Esterification reactor two. Detailed Implementation

[0019] The technical solution of this utility model will be clearly and completely described below with reference to its embodiments. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of this utility model.

[0020] Reference Figure 1 This embodiment provides a chlorosilane esterification reaction apparatus, including a pre-reactor R1, an esterification reactor one R2, and an esterification reactor two R3 connected in sequence; the pre-reactor R1 is used to activate to the critical reaction temperature, and the esterification reactor one R2 and the esterification reactor two R3 are both reactors with their own condensation sections for the esterification reaction, each including an upper condensation section and a lower vessel body, the vessel body being equipped with heating pipelines for heating to the temperature required for the esterification reaction; wherein: The feed end of the pre-reactor R1 is connected to a chlorosilane feed pipe L1 and a methanol feed pipe L2. The bottom of the pre-reactor R1 is connected to the condensation section of the esterification reactor R2. The vessel of the esterification reactor R2 is connected to the condensation section of the esterification reactor R3. The condensation section of the esterification reactor R3 is also connected to a methanol feed pipe L3. The vessel is also equipped with a crude product collection pipe L4.

[0021] The esterification reaction between chlorosilanes and methanol is a typical exothermic reaction. Therefore, if conventional feeding methods are used, there is a risk of overflow due to the exothermic reaction. In the above embodiment, the first stream of methanol from methanol feed pipe L2 and chlorosilane enter the pre-reactor R1 and are preheated to the critical temperature to undergo a pre-reaction. Then, they enter the condensation section of esterification reactor R2 for a preliminary reaction. In the condensation section, the heat of reaction is promptly carried away by the condensing medium, and the resulting esterified liquid can smoothly enter the lower vessel. Subsequently, the material in the vessel of esterification reactor R2 enters the condensation section of esterification reactor R3 and undergoes a further esterification reaction with the second stream of methanol vaporized from methanol feed pipe L3. After heat exchange, the material enters the vessel of esterification reactor R3, and the crude esterified product is collected.

[0022] In a preferred embodiment, the methanol feed pipe L3 is connected to the middle section of the condensation section of the esterification reactor R3, and the pipeline from the vessel of the esterification reactor R2 is connected to the upper section of the condensation section. After feeding, the methanol and the condensed esterification liquid form a countercurrent to achieve further esterification.

[0023] In a preferred embodiment, to capture the small amount of hydrogen chloride gas produced by the esterification reaction in the pre-reactor and recover the escaped material, the top of the pre-reactor R1 is connected to the upper part of the pre-reactor R1 via the material conveying channel of the condensation unit; the material output pipeline of the condensation unit is also connected to a demister D1, the lower part of which is connected to the upper part of the pre-reactor R1. The function of the demister D1 is to capture droplets to form a liquid phase that converges to the bottom, allowing the gas phase to escape through the upper part and the liquid phase to enter the pre-reactor R1 for recycling. Specifically, the condensation unit includes condenser C1, condenser C2, and condenser C3. The top of the pre-reactor R1 is provided with a pipeline that sequentially passes through the material channels of condenser C1, condenser C2, and condenser C3 and returns to the upper part of the pre-reactor R1; condenser C1 and condenser C2 each have separate pipelines at their material output ends connected to the upper part of the pre-reactor R1. Furthermore, to reduce energy consumption, the material output end of condenser C3 is connected to the demister D1 via a pipeline through the medium channel of condenser C1. Since condenser C3 is located at the end, the temperature of its material after condensation is relatively low, and it can be used as a cooling medium to condense condenser C1.

[0024] In a preferred embodiment, to balance pressure, capture hydrogen chloride, and improve material utilization, a pipeline is installed at the top of the condensation section of the esterification reactor R2, connecting it to the upper part of the pre-reactor R1 via condenser C4. Material escaping from the condensation section of the esterification reactor R2 is condensed by condenser C4 and returned to the pre-reactor R1, where it is further treated by demister D1 to remove hydrogen chloride gas.

[0025] In a preferred embodiment, to improve the conversion rate of chlorosilanes, a circulation pipeline can be installed within or between the esterification reactors to achieve material circulation and increase the esterification rate. This is particularly important for some polychlorinated silanes, where a certain esterification rate needs to be maintained to improve product quality. For example, a circulation pipe L5 can be installed in the vessel of esterification reactor R2, connecting it to its own condensation section. A circulation pipe L6 can be installed in the vessel of esterification reactor R3, connecting it to its own condensation section. A circulation pipe L7 can be installed at the top of the condensation section of esterification reactor R3, connecting it to the condensation section of esterification reactor R2.

[0026] In a preferred embodiment, the top of the condensation section of the esterification reactor R2 is provided with a vent pipe L8 for releasing the pressure inside the reactor in an emergency.

[0027] In the above embodiments, the crude product collection pipe L4 can be connected to an external post-processing unit, such as a falling film evaporator, to collect crystals and obtain the product through falling film evaporation, and separate the mother liquor. The mother liquor can preferably be connected to the vessel of the esterification reactor R3 through the mother liquor feed pipe L9, so as to realize the recycling of some unreacted materials for further esterification.

[0028] 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. A chlorosilane esterification reaction apparatus, characterized in that, It includes a pre-reactor (R1), an esterification reactor one (R2), and an esterification reactor two (R3) connected in sequence; the pre-reactor (R1) is used to activate to the critical reaction temperature, and both esterification reactor one (R2) and esterification reactor two (R3) are used for the esterification reaction, each containing an upper condensation section and a lower vessel body; wherein: The feed end of the pre-reactor (R1) is connected to a chlorosilane feed pipe (L1) and a methanol feed pipe (L2). The bottom of the pre-reactor (R1) is connected to the condensation section of the esterification reactor (R2). The vessel body of the esterification reactor (R2) is connected to the condensation section of the esterification reactor (R3). The condensation section of the esterification reactor (R3) is also connected to a methanol feed pipe (L3). The vessel body is also equipped with a crude product collection pipe (L4).

2. The reaction apparatus as described in claim 1, characterized in that, The top of the pre-reactor (R1) is connected to the upper part of the pre-reactor (R1) via the material channel of the condensation unit; the material output pipeline of the condensation unit is also connected to a demister (D1), and the lower part of the demister (D1) is connected to the upper part of the pre-reactor (R1).

3. The reaction apparatus as described in claim 2, characterized in that, The condensation unit includes multiple condensers connected in series, with the material output end of the last condenser connected to the demister (D1) via the medium channel of the first condenser.

4. The reaction apparatus as described in claim 3, characterized in that, The condensation unit includes condenser one (C1), condenser two (C2), and condenser three (C3). The top of the pre-reactor (R1) is provided with pipelines that sequentially pass through the material channels of condenser one (C1), condenser two (C2), and condenser three (C3) and return to the upper part of the pre-reactor (R1). Each of condenser one (C1) and condenser two (C2) has a separate pipeline at its material output end that connects to the upper part of the pre-reactor (R1). The material output end of condenser three (C3) is provided with a pipeline that passes through the medium channel of condenser one (C1) and connects to the demister (D1).

5. The reaction apparatus as described in claim 2, characterized in that, The top of the condensation section of the esterification reactor (R2) is connected to the upper part of the pre-reactor (R1) via a pipeline through condenser (C4).

6. The reaction apparatus as described in claim 1, characterized in that, The esterification reactor (R2) is equipped with a circulation pipe (L5) connected to its own condensation section.

7. The reaction apparatus as described in claim 1, characterized in that, The vessel of the second esterification reactor (R3) is connected to its own condensation section via a second circulation pipe (L6).

8. The reaction apparatus as described in claim 1, characterized in that, The top of the condensation section of the second esterification reactor (R3) is connected to the condensation section of the first esterification reactor (R2) via a circulation pipe (L7).

9. The reaction apparatus as described in claim 1, characterized in that, The condensation section of the esterification reactor (R2) is equipped with a vent pipe (L8).

10. The reaction apparatus as claimed in claim 1, characterized in that, The second esterification reactor (R3) is equipped with a mother liquor feed pipe (L9).

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