Preparation Device for N-(β-Aminoethyl)-γ-aminopropyltrimethoxysilane and Its Usage Method

Abstract

The invention discloses a preparation device for N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and a using method thereof, comprising: an inclined cylinder body; a spiral cavity body; a side opening which is arranged on the outer peripheral surface of the spiral cavity body near the lowest end of the inclined cylinder body; an end opening which is arranged at one end of the spiral cavity body near the highest end of the inclined cylinder body; a chloropropyltrimethoxysilane pipeline; a chloropropyltrimethoxysilane storage tank; an ethylenediamine pipeline, one end of which is communicated with the lower surface of the inclined cylinder body; an ethylenediamine storage tank which is communicated with the other end of the ethylenediamine pipeline; a contraction part which is formed at the highest end of the inclined cylinder body; and a liquid extraction cavity, the side surface of which is communicated with the contraction part. The beneficial effect of the invention is that through the rotation of the spiral cavity body, the intermediate mixing layer of the reaction product is stirred, the stratification of the reaction product is accelerated, the structure is compact, and the use is convenient.

Description

Technical Field

[0001] The present invention relates to the field of synthesis devices for amino silane coupling agents, and particularly to a preparation device for N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and its usage method. Background Art

[0002] Silane coupling agents are a class of organic compounds containing silicon atoms, which can enhance the affinity between organic and inorganic compounds, and can strengthen and improve the physical and chemical properties of composite materials, and are known as the "industrial flavor enhancer". N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane is a very representative silane coupling agent. However, there are still many problems in its actual production and application. For a long time, the production of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane has mostly been intermittent reactions, single-pot batch production, with a long reaction cycle, high energy consumption, low efficiency, requiring a high level of manual labor, and complex operating conditions. In batch production, the molar ratio of raw material ethylenediamine to chloropropyltrimethoxysilane needs to reach 12 - 30:1, the consumption of ethylenediamine is large, the product purity is only about 97%, there are many impurities, and the yield is only about 80%. Moreover, the process conditions for each pot of production need to be manually controlled by workers, and process differences will inevitably occur, thereby affecting product quality, and the product quality is uneven.

[0003] The Chinese invention patent authorization announcement number CN103408581B discloses a continuous production reaction device and method for N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane. A mixed solution of ethylenediamine and chloropropyltrimethoxysilane sprayed downward from the top of the reaction tower (2) completes the reaction during the falling process in the reaction tower (2) under the overprotection of the rising ethylenediamine vaporized liquid, and is automatically pumped into a continuous sedimentation separator by a transfer pump (12) that automatically controls the amount of reaction liquid in the automatic control reaction kettle (3) for continuous liquid separation. The obtained clear liquid is subjected to rectification to obtain N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane. This reaction device has a complex structure, many component devices, occupies a large area, and is costly.

[0004] The Chinese invention patent publication number CN113501840A discloses a method for preparing N-(2-aminoethyl)-3-aminopropyltrimethoxysilane using a pipeline reactor. The raw materials composed of ethylenediamine and 3-chloropropyltrimethoxysilane react in the pipeline reactor. The residence time of the raw materials in the pipeline reactor is 20 - 50 min, and the reaction temperature of the pipeline reactor is controlled at 80°C - 130°C; the reaction product discharged from the outlet of the pipeline reactor is separated and processed to obtain N-(2-aminoethyl)-3-aminopropyltrimethoxysilane as the product. This method controls the reaction in the pipeline, the reaction space is narrow, it is impossible to ensure sufficient reaction, and it is also impossible to layer the reaction products. Summary of the Invention

[0005] The technical problem to be solved by the present invention is that the existing method for preparing N-(2-aminoethyl)-3-aminopropyltrimethoxysilane cannot shorten the layering time, or can shorten the layering time but at a high cost. Therefore, a preparation device for N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and its use method are provided.

[0006] The technical solution of the present invention is: a preparation device for N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, comprising: an inclined cylinder, the lowest end of the inclined cylinder is closed, and the highest end of the inclined cylinder is open; a spiral cavity, one end of the spiral cavity passes through the center of the lowest end of the inclined cylinder and is connected to a driving mechanism, and the other end of the spiral cavity extends towards the highest end of the inclined cylinder; a side opening, the side opening is opened on the outer peripheral surface of the part of the spiral cavity close to the lowest end of the inclined cylinder; an end opening, the end opening is opened at one end of the spiral cavity close to the highest end of the inclined cylinder; a chloropropyltrimethoxysilane pipeline, one end of the chloropropyltrimethoxysilane pipeline is communicated with the upper surface of the inclined cylinder; a chloropropyltrimethoxysilane storage tank, the chloropropyltrimethoxysilane storage tank is communicated with the other end of the chloropropyltrimethoxysilane pipeline; an ethylenediamine pipeline, one end of the ethylenediamine pipeline is communicated with the lower surface of the inclined cylinder; an ethylenediamine storage tank, the ethylenediamine storage tank is communicated with the other end of the ethylenediamine pipeline; a contraction part, the contraction part is formed at the highest end of the inclined cylinder; a liquid extraction cavity, the side of the liquid extraction cavity is communicated with the contraction part.

[0007] An improvement of the above solution is that a freely rolling rolling body is provided in the spiral cavity, and the outer diameter of the rolling body is larger than the side opening and the end opening.

[0008] A further improvement of the above solution is that an overflow plate is provided at the connection between the side of the liquid extraction cavity and the contraction part, and an overflow space is left between the overflow plate and the top of the contraction part.

[0009] A further improvement of the above solution is that a one-way valve is installed in the overflow space.

[0010] A further improvement of the above solution is that the inclined cylinder is coated with a heating layer.

[0011] In the above solution, the inclined cylinder is supported by a bracket.

[0012] Usage method of a preparation device for N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, comprising the following steps: respectively pump the chloropropyltrimethoxysilane in the chloropropyltrimethoxysilane storage tank and the ethylenediamine in the ethylenediamine storage tank through the chloropropyltrimethoxysilane pipeline and the ethylenediamine pipeline to the inclined cylinder body for reaction; start the driving mechanism to drive the rotation of the spiral cavity body, stratify the reaction products to form the supernatant liquid in the upper layer and ethylenediamine hydrochloride in the lower layer; the reaction products flow into the liquid extraction cavity through the contraction part, ensuring that most of the ethylenediamine hydrochloride remains in the inclined cylinder body, and the supernatant liquid flows into the liquid extraction cavity; extract the liquid in the upper part of the liquid extraction cavity, and then high-purity N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane can be obtained.

[0013] The beneficial effect of the present invention is that the ethylenediamine with a lower density is transported from below to the inclined cylinder body, and the chloropropyltrimethoxysilane with a higher density is transported from above to the inclined cylinder body, enabling the two to be fully mixed and reacted. By rotating the spiral cavity body, the intermediate mixed layer of the reaction products is stirred to accelerate the stratification of the reaction products. Due to the inclination of the inclined cylinder body, most of the lower-layer products remain in the inclined cylinder body, and the supernatant liquid after stratification enters the liquid extraction cavity. The structure is compact and convenient to use. Description of the Drawings

[0014] Figure 1 is a schematic diagram of the preparation device for N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane of the present invention;

[0015] Figure 2 is a schematic diagram of a preferred example of the present invention;

[0016] Figure 3 is a schematic diagram of another preferred example of the present invention;

[0017] In the figure, 1, inclined cylinder body; 2, spiral cavity body; 3, side opening; 4, end opening; 5, chloropropyltrimethoxysilane pipeline; 6, chloropropyltrimethoxysilane storage tank; 7, ethylenediamine pipeline; 8, ethylenediamine storage tank; 9, contraction part; 10, liquid extraction cavity; 11, rolling body; 12, overflow plate; 13, one-way valve; 14, pump. Detailed Embodiments

[0018] The present invention will be further described below in conjunction with the drawings and embodiments.

[0019] Such as Figure 1As shown in the figure, the preparation device of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane includes: an inclined cylinder 1, the lowest end of the inclined cylinder is closed, and the highest end of the inclined cylinder is open; a spiral cavity 2, one end of the spiral cavity passes through the center of the lowest end of the inclined cylinder and is connected to a driving mechanism, and the driving mechanism can be a motor or a motor, which can drive the spiral cavity to rotate. The other end of the spiral cavity extends towards the highest end of the inclined cylinder; a side opening 3, which is opened on the outer peripheral surface of the part of the spiral cavity close to the lowest end of the inclined cylinder, and there can be one or more side openings; an end opening 4, which is opened at one end of the spiral cavity close to the highest end of the inclined cylinder; a chloropropyltrimethoxysilane pipeline 5, one end of the chloropropyltrimethoxysilane pipeline is communicated with the upper surface of the inclined cylinder; a chloropropyltrimethoxysilane storage tank 6, the chloropropyltrimethoxysilane storage tank is communicated with the other end of the chloropropyltrimethoxysilane pipeline; an ethylenediamine pipeline 7, one end of the ethylenediamine pipeline is communicated with the lower surface of the inclined cylinder; an ethylenediamine storage tank 8, the ethylenediamine storage tank is communicated with the other end of the ethylenediamine pipeline; a contraction part 9, which is formed at the highest end of the inclined cylinder; a liquid extraction cavity 10, the side of the liquid extraction cavity is communicated with the contraction part.

[0020] The usage method of the preparation device of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane includes the following steps: respectively pump the chloropropyltrimethoxysilane in the chloropropyltrimethoxysilane storage tank and the ethylenediamine in the ethylenediamine storage tank into the inclined cylinder through the chloropropyltrimethoxysilane pipeline and the ethylenediamine pipeline by a pump 14 for reaction. The ethylenediamine and chloropropyltrimethoxysilane are fully mixed and reacted, and reactants are formed in the inclined cylinder. The reactants include by-product ethylenediamine hydrochloride in the lower layer and supernatant liquid, i.e., N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, in the upper layer. A mixed layer is formed between the two. Start the driving mechanism to drive the spiral cavity to rotate. Since the spiral cavity is located near the central axis of the inclined cylinder, the reaction products, especially the mixed layer, can be stratified to form supernatant liquid in the upper layer and ethylenediamine hydrochloride in the lower layer. At the same time, part of the reactants enter the spiral cavity through the side opening and are finally discharged from the end opening. The reaction products flow into the liquid extraction cavity through the contraction part. The contraction part can accelerate the flow of the supernatant liquid into the liquid extraction cavity and inhibit the flow of the lower-layer ethylenediamine hydrochloride into the liquid extraction cavity, ensuring that most of the ethylenediamine hydrochloride remains in the inclined cylinder, and the supernatant liquid flows into the liquid extraction cavity. By taking the liquid in the upper part of the liquid extraction cavity, high-purity N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane can be obtained.

[0021] As a preferred example of the present invention, as Figure 2As shown, a freely rolling rolling body 11 is provided in the spiral cavity. The outer diameter of the rolling body is larger than the side opening and the end opening. When the spiral cavity rotates, the rolling body also rolls therein, disturbing the reactants in the spiral cavity and promoting their stratification.

[0022] As another preferred example of the present invention, as Figure 3 shown, in order to prevent the lower-layer ethylenediamine hydrochloride from flowing into the liquid extraction cavity, an overflow plate 12 is provided at the connection between the side of the liquid extraction cavity and the contraction part. An overflow space is left between the overflow plate and the top of the contraction part, and the overflow plate intercepts the lower-layer ethylenediamine hydrochloride. Further, a one-way valve 13 is installed in the overflow space to ensure that the liquid in the liquid extraction cavity will not flow back into the inclined cylinder body.

[0023] To ensure the progress of the reaction, the inclined cylinder body is covered with a heating layer, and the temperature of the heating layer can be set. For example, the initial temperature is relatively low, such as 60°C - 80°C, and then the temperature gradually rises to 100°C. The inclined cylinder body is supported on the ground by a bracket.

Claims

1. Preparation device for N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, characterized in that: Comprising: An inclined cylinder body (1), the lowest end of the inclined cylinder body being closed and the highest end being open; A helical cavity body (2), one end of the helical cavity body passing through the center of the lowest end of the inclined cylinder body and connecting to a driving mechanism, and the other end of the helical cavity body extending towards the highest end of the inclined cylinder body; a side opening (3) formed on the outer peripheral surface of a part of the helical cavity body near the lowest end of the inclined cylinder body; an end opening (4) formed at one end of the helical cavity body near the highest end of the inclined cylinder body; a 3-chloropropyltrimethoxysilane pipeline (5), one end of the 3-chloropropyltrimethoxysilane pipeline communicating with the upper surface of the inclined cylinder body; a 3-chloropropyltrimethoxysilane storage tank (6), the 3-chloropropyltrimethoxysilane storage tank communicating with the other end of the 3-chloropropyltrimethoxysilane pipeline; an ethylenediamine pipeline (7), one end of the ethylenediamine pipeline communicating with the lower surface of the inclined cylinder body; an ethylenediamine storage tank (8), the ethylenediamine storage tank communicating with the other end of the ethylenediamine pipeline; a contraction part (9) formed at the highest end of the inclined cylinder body; a liquid extraction cavity (10), the side surface of the liquid extraction cavity communicating with the contraction part; a freely rolling rolling body (11) provided in the helical cavity body, the outer diameter of the rolling body being larger than that of the side opening and the end opening.

2. The preparation device of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane according to claim 1, characterized in that: An overflow plate (12) is provided at the connection between the side surface of the liquid extraction cavity and the contraction part, and a flow-through space is left between the overflow plate and the top of the contraction part.

3. The preparation device of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane according to claim 2, characterized in that: A one-way valve (13) is installed in the flow-through space.

4. The preparation device of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane according to claim 1, characterized in that: The inclined cylinder body is coated with a heating layer.

5. The preparation device of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane according to claim 1, characterized in that: The inclined cylinder body is supported by a bracket.

6. The usage method of the preparation device of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane according to any one of claims 1-5, characterized in that: Comprising the following steps: Respectively pump 3-chloropropyltrimethoxysilane in the 3-chloropropyltrimethoxysilane storage tank and ethylenediamine in the ethylenediamine storage tank into the inclined cylinder body through the 3-chloropropyltrimethoxysilane pipeline and the ethylenediamine pipeline for reaction, start the driving mechanism to drive the helical cavity body to rotate, layer the reaction products to form supernatant liquid in the upper layer and ethylenediamine hydrochloride in the lower layer, the reaction products flow through the contraction part into the liquid extraction cavity, ensuring that most of the ethylenediamine hydrochloride remains in the inclined cylinder body, the supernatant liquid flows into the liquid extraction cavity, and extract the liquid in the upper part of the liquid extraction cavity to obtain high-purity N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane.

Images