Chain-type scraper film reaction device for sulfur-containing silane coupling agent and method for producing sulfur-containing silane coupling agent by using chain-type scraper film reaction device

Abstract

The invention discloses a chain type scraper film reaction device for a sulfur-containing silane coupling agent and a method for producing the sulfur-containing silane coupling agent by adopting the chain type scraper film reaction device. Comprising a scraper film reactor, a horizontal screw centrifuge, a mixing kettle, a slurry pump, a chloropropyltriethoxysilane metering tank, an anhydrous sodium polysulfide powder tank, a condenser, a receiving tank, a Roots vacuum unit, a pipeline pump, a precision filter and a finished product tank. A discharge hole is formed in the lower part of the mixing kettle and is connected with an inlet of the slurry pump; the chained scraper film reactor is provided with a feeding hole A and a feeding hole B which are symmetrically distributed; and a chain-type scraper is arranged in the chain-type scraper film reactor. According to the invention, a suspension of chloropropyltriethoxysilane and anhydrous sodium polysulfide can enter the symmetrically distributed feed ports of the reactor through the slurry pump, and is pumped into the scraper film reactor at a certain flow rate, and a uniform film is formed through the chain type rotary scraper for reaction, so that the reaction device has efficient mass and heat transfer effects and uniform temperature distribution.

Description

Technical Field

[0001] The invention relates to the technical field of production of sulfur-containing silane coupling agents, in particular to a chain scraper thin film reaction device for sulfur-containing silane coupling agents and a method for producing sulfur-containing silane coupling agents by using the device. Background Art

[0002] The sulfur-containing silane coupling agent is a bifunctional polysulfide organosilane coupling agent with the general molecular formula of (R1R2R3SiR4)2Sn, wherein R1, R2, and R3 are C1-C4 alkyl or alkoxy groups, wherein the alkoxy group is -OCH3, -OCH2CH3, -OCH2CH2CH3, or -OCH2CH2CH2CH3, R4 is a C1-C4 alkyl group, and n=2 to 8.

[0003] Application of silane coupling agents in inorganic filler treatment: Silane coupling agents, through their unique bifunctional structure (a hydrolyzable siloxy group on one end and an organic functional group on the other), establish chemical bonds between inorganic fillers and organic matrices, significantly improving the performance of composite materials. Their mechanism of action can be divided into four steps: wetting: the silane coupling agent rapidly spreads on the inorganic material surface due to its low surface tension; hydrolysis: the alkoxy group reacts with water to form a silanol (Si-OH); condensation: the silanol forms a Si-O-Si covalent bond with the hydroxyl groups on the filler surface; and crosslinking: the organic functional group reacts with the polymer matrix to form an interfacial layer.

[0004] Application of silane coupling agents in silica processing: Silane coupling agents (such as sulfur-containing silanes) are used to modify the silica surface, reducing the polarity of the silanol group and improving its dispersion in rubber. At the same time, a "bridge" structure is formed during the vulcanization process, reducing tire hysteresis loss.

[0005] Application of silane coupling agents in ceramic materials: The surface of ceramic materials (such as alumina and silicon nitride) is rich in hydroxyl groups, and silane coupling agents can be used to achieve interfacial modification. They have good applications in the following specific application scenarios in the field of ceramics: Application in porcelain teeth: Silane coupling agents (such as porcelain treatment agents) are used to repair broken porcelain teeth, and the shear bonding strength with composite resin is improved by treating the ceramic surface (experiments show that it can be increased by more than 50%).

[0006] Modified ceramic surface coating enhancement: Silane coupling agents are used as adhesion promoters in ceramic-metal or ceramic-polymer coatings to improve adhesion and water resistance. For example, in electronic packaging, ceramic fillers are modified to enhance the interfacial bonding of thermal conductive adhesives.

[0007] At present, the synthesis routes of sulfur-containing silane coupling agents mainly include aqueous phase method and solvent method. The reaction apparatus of aqueous phase method mainly adopts batch reactor, and the reaction apparatus of solvent method mainly adopts batch reactor, tubular continuous reactor, microporous continuous reactor and other devices.

[0008] Patent application number CN201410089165.0 describes a process for preparing a sulfur-containing silane coupling agent using a polysulfide aqueous solution and 3-halopropyltrialkoxysilane as raw materials, utilizing a supported quaternary ammonium salt phase transfer catalyst. This process presents challenges such as large wastewater treatment volumes and residual phase transfer catalyst in the product, which can lead to a darker color during storage.

[0009] In the solvent method, an intermittent reactor is used for the reaction, which has problems such as low mass and heat transfer efficiency, low reaction efficiency, and large solvent loss.

[0010] In the solvent method, a tubular continuous reactor or a microchannel reactor is used for the reaction, which improves the problem of low mass and heat transfer efficiency and realizes a continuous reaction. However, since the raw material sodium polysulfide is in solid form, it is a suspension after mixing with the solvent and chloropropyltriethoxysilane. It is easy to get clogged in the pipe of the tubular reactor or in the microchannel of the microchannel reactor, resulting in the obstruction of the reaction continuity. At the same time, the introduction of multiple solvents leads to solvent loss and environmental pollution problems.

[0011] To this end, we propose a chain scraper thin film reaction device for sulfur-containing silane coupling agent and a method for producing sulfur-containing silane coupling agent using the device to solve the above problems. Summary of the Invention

[0012] The object of the present invention is to provide a chain scraper thin film reaction device for a sulfur-containing silane coupling agent and a method for producing a sulfur-containing silane coupling agent using the device, so as to solve the problems raised in the above background technology.

[0013] To achieve the above object, the present invention provides the following technical solutions: A chain scraper film reaction device for a sulfur-containing silane coupling agent, comprising a chain scraper film reactor, a horizontal screw centrifuge, a mixing kettle, a slurry pump, a chloropropyltriethoxysilane metering tank, an anhydrous sodium polysulfide powder tank, a condenser, a receiving tank, a Roots vacuum unit, a pipeline pump, a precision filter, and a finished product tank; A discharge port is provided below the mixing kettle, and the discharge port is connected to the inlet of the slurry pump; The chain scraper film reactor is provided with symmetrically distributed feed ports A and B; the feed ports A and B are connected to the discharge port of the slurry pump; The chain scraper film reactor is internally provided with a chain scraper. The upper gas phase outlet of the chain scraper film reactor is connected to the inlet of the condenser, and the lower material outlet is connected to the inlet of the horizontal screw centrifuge.

[0014] Furthermore, the width of the chain scraper is 3.0 to 4.5 cm, and the gap between the chain scraper and the inner wall of the chain scraper thin film reactor 1 is 0.15 cm.

[0015] Furthermore, a feed distributor with a tangential inlet is provided on the top of the chain scraper film reactor, and feed port A and feed port B are arranged on the feed distributor.

[0016] Furthermore, the chain scraper film reactor is externally provided with a heat transfer oil jacket.

[0017] Another object of the present invention is to provide a method for producing a sulfur-containing silane coupling agent, the method being implemented based on the above-mentioned chain scraper thin film reaction device for the sulfur-containing silane coupling agent, the method comprising the following steps: S1, add chloropropyltriethoxysilane and anhydrous sodium polysulfide into the chloropropyltriethoxysilane metering tank and the anhydrous sodium polysulfide powder tank respectively, then put them into the mixing kettle and stir evenly; S2, the chain scraper film reactor uses a Roots vacuum unit to evacuate the air, and then the material in the mixing tank is pumped into the chain scraper film reactor through a slurry pump for reaction; S3. During the thin film reaction process, a chain scraper is used to achieve efficient mass and heat transfer reaction of the suspended material. The reaction material is continuously discharged from the bottom of the chain scraper thin film reactor to the horizontal screw centrifuge for continuous separation. The filtrate is further pumped into the precision filter by a pipeline pump for filtration, and the finished product is put into the finished product tank.

[0018] Furthermore, in step S1, the stirring speed of the mixing kettle is controlled to be 80-90 rpm.

[0019] Furthermore, in step S2, when the chain scraper film reactor is evacuated, the vacuum degree is controlled to be -0.04 MPa to -0.06 MPa.

[0020] Furthermore, in step S2, when the materials in the mixing tank react in the chain scraper film reactor, the reaction temperature is controlled at 90±3°C.

[0021] Compared with the prior art, the present invention has the following beneficial effects: The present invention can allow a suspension of chloropropyltriethoxysilane and anhydrous sodium polysulfide to enter a symmetrically distributed feed port of a reactor through a slurry pump, and then be pumped into a scraper film reactor at a certain flow rate. A uniform film is formed by a chain-type rotating scraper for reaction, thereby achieving efficient mass and heat transfer effects and uniform temperature distribution.

[0022] The reaction device of the present invention has a simple process and high reaction efficiency, can realize thin film reaction under solvent-free and catalyst-free conditions, and also has the advantages of low cost and outstanding safety and environmental protection.

[0023] Compared with conventional reaction and distillation processes, the reaction device of the present invention realizes the integration of synchronous reaction and low-boiling-point separation in a thin film reactor, simplifies the process flow, and further improves production efficiency.

[0024] The reactor of the present invention offers excellent mixing performance. It achieves dynamic mixing: The continuous motion of the chain scraper not only promotes uniform distribution of the reactants but also enhances mixing between materials, resulting in a more complete reaction. Controllable residence time: By adjusting the scraper speed and reactor length, the residence time of the reactants can be precisely controlled, thereby optimizing reaction conditions and improving yield and product quality.

[0025] The reactor of the present invention is highly adaptable: the chain-type scraped-film reactor can process multiple materials simultaneously and adapt to complex reaction systems, providing greater flexibility for the preparation of sulfur-containing silanes. It avoids the clogging problem of tubular and microchannel reactors when mixing suspended solid-phase materials. Furthermore, the reactor is scalable, and its scale can be adjusted according to production needs, making it suitable for applications ranging from small laboratory equipment to large industrial production lines.

[0026] The reactor of the present invention is easy to operate and maintain, and is suitable for continuous operation: the reactor supports continuous operation mode, reducing downtime between batches and improving production efficiency. The reactor is easy to clean: the structural design of the reactor takes into account the convenience of cleaning and maintenance, reducing downtime and maintenance costs. The reactor of the present invention offers the advantages of low energy consumption: efficient heat and mass transfer allows the reaction to proceed at lower temperatures and pressures, reducing energy consumption. It also reduces waste generation: by precisely controlling reaction conditions and optimizing material ratios, it reduces byproduct generation and lowers waste disposal costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 Schematic diagram of the corresponding parameters and results of the embodiments of the present invention.

[0028] In the figure: 1. Chain scraper thin film reactor; 2. Horizontal screw centrifuge; 3. Mixing kettle; 4. Slurry pump; 5. Chloropropyltriethoxysilane metering tank; 6. Anhydrous sodium polysulfide powder tank; 7. Condenser; 8. Receiving tank; 9. Roots vacuum unit; 10. Pipeline pump; 11. Precision filter; 12. Finished product tank; 13. Feed distributor; 14. Feed port A; 15. Feed port B; 16. Thermal oil jacket; 17. Chain scraper. DETAILED DESCRIPTION

[0029] In the description of the present invention, it should be understood that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "back," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like, indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings and are intended only to facilitate the description of the present invention and simplify the description. They do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed, or operate in a specific orientation. Therefore, they should not be construed as limiting the present invention. In the description of the present invention, unless otherwise specified, "plurality" means two or more.

[0030] In the description of the present invention, it should be noted that, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "connected" should be understood in a broad sense. For example, they may refer to fixed connections, detachable connections, or integral connections; mechanical connections or electrical connections; direct connections or indirect connections through an intermediate medium; and internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0031] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0032] See also Figure 1 A chain scraper film reaction device for a sulfur-containing silane coupling agent, comprising a chain scraper film reactor 1, a horizontal screw centrifuge 2, a mixing kettle 3, a slurry pump 4, a chloropropyltriethoxysilane metering tank 5, an anhydrous sodium polysulfide powder tank 6, a condenser 7, a receiving tank 8, a Roots vacuum unit 9, a pipeline pump 10, a precision filter 11, and a finished product tank 12; The discharge ports of the chloropropyltriethoxysilane metering tank 5 and the anhydrous sodium polysulfide powder tank 6 are connected to the feed port of the mixing kettle 3. The chloropropyltriethoxysilane and the anhydrous sodium polysulfide are introduced into the mixing kettle 3 and stirred evenly. A discharge port is provided below the mixing kettle 3, and the discharge port is connected to the inlet of the slurry pump 4. A feed distributor 13 with a tangential inlet is provided on the top of the chain scraper film reactor 1. The feed distributor 13 is provided with symmetrically distributed feed ports A 14 and B 15; feed ports A 14 and B 15 is connected to the discharge port of the slurry pump 4, a chain scraper 17 is configured inside the chain scraper film reactor 1, the upper gas phase outlet of the chain scraper film reactor 1 is connected to the inlet of the condenser 7, the condenser 7 is connected to the receiving tank 8, the receiving tank 8 is connected to the Roots vacuum unit 9, the lower material outlet is connected to the inlet of the horizontal screw centrifuge 2, the outlet of the horizontal screw centrifuge 2 is connected to the pipeline pump 10, the outlet of the pipeline pump 10 is connected to the precision filter 11, and the outlet of the pipeline pump 10 is connected to the finished product tank 12.

[0033] The chain scraper film reactor 1 is externally provided with a heat transfer oil jacket 16 .

[0034] The width of the chain scraper 17 is 3.0-4.5 cm, and the gap between the chain scraper 17 and the inner wall of the chain scraper thin film reactor 1 is 0.15 cm.

[0035] A method for producing a sulfur-containing silane coupling agent is implemented based on the above-mentioned chain scraper thin film reaction device for the sulfur-containing silane coupling agent, and the method comprises the following steps: Add chloropropyltriethoxysilane and anhydrous sodium polysulfide to the chloropropyltriethoxysilane metering tank 5 and the anhydrous sodium polysulfide powder tank 6 respectively. Then put them into the mixing kettle 3 and stir evenly. 2. The chain scraper film reactor 1 is evacuated to -0.04MPa~-0.06MPa using a Roots vacuum unit 9. The materials in the mixing tank are then pumped into the chain scraper film reactor 1 via a slurry pump 4 for reaction. The reaction temperature is controlled at 90±3℃. 3. During the thin film reaction process, the chain scraper 17 is used to achieve efficient mass and heat transfer reaction of the suspended material. The reaction material is continuously discharged from the bottom of the chain scraper thin film reactor 1 to the horizontal screw centrifuge 2 for continuous separation. The filtrate is further pumped into the precision filter 11 by the pipeline pump 10 for filtration, and the obtained finished product is sent to the finished product tank 12.

[0036] In steps 2 and 3, a Roots vacuum unit 9 is used for vacuuming, and the vacuum degree is -0.04 MPa to -0.06 MPa; the reaction temperature in steps 2 and 3 is controlled at 90 ± 3 ° C; the stirring speed in steps 2 and 3 is 80 to 90 rpm; the feeding rate of chloropropyltriethoxysilane and anhydrous sodium polysulfide suspension in steps 2 and 3 is controlled at 50 to 60 kg / min; The method for collecting the low-boiling-point substances generated by the reaction in step 3 is as follows: the low-boiling-point substances generated by the reaction are mainly a small amount of ethanol, which is extracted from the reactor through the upper gas outlet of the reactor through the Roots vacuum unit 9, and then condensed in the condenser 7 and enter the receiving tank 8.

[0037] In step 3, samples are taken regularly to detect the residual amount of chloropropyltriethoxysilane in the crude reaction product. The reaction is qualified when the residual amount is less than 0.5%. The product is then separated by decanter centrifugation, and the filtrate is further passed through a precision filter 11 to obtain a clear and transparent sulfur-containing silane coupling agent product.

[0038] Specific parameters such as Figure 2 shown.

[0039] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A chain scraper thin film reaction device for sulfur-containing silane coupling agent, characterized in that: It includes a chain scraper film reactor (1), a horizontal screw centrifuge (2), a mixing kettle (3), a slurry pump (4), a chloropropyltriethoxysilane metering tank (5), an anhydrous sodium polysulfide powder tank (6), a condenser (7), a receiving tank (8), a Roots vacuum unit (9), a pipeline pump (10), a precision filter (11), and a finished product tank (12); A discharge port is provided below the mixing kettle (3), and the discharge port is connected to the inlet of the slurry pump (4); The chain scraper film reactor (1) is provided with a symmetrically distributed feed port A (14) and a feed port B (15); the feed port A (14) and the feed port B (15) are connected to the discharge port of the slurry pump (4); The chain scraper film reactor (1) is internally provided with a chain scraper (17), the upper gas phase outlet of the chain scraper film reactor (1) is connected to the inlet of the condenser (7), and the lower material outlet is connected to the inlet of the horizontal screw centrifuge (2).

2. The chain scraper thin film reaction device of sulfur-containing silane coupling agent according to claim 1, characterized in that: The width of the chain scraper (17) is 3.0 to 4.5 cm, and the gap between it and the inner wall of the chain scraper thin film reactor (1) is 0.15 cm.

3. The chain scraper thin film reaction device of sulfur-containing silane coupling agent according to claim 1, characterized in that: The chain scraper film reactor (1) is provided with a feed distributor (13) with a tangential inlet on the top, and a feed port A (14) and a feed port B (15) are provided on the feed distributor (13).

4. The chain scraper thin film reaction device of sulfur-containing silane coupling agent according to claim 1, characterized in that: The chain-type scraper film reactor (1) is externally provided with a heat-conducting oil jacket (16).

5. A method for producing a sulfur-containing silane coupling agent, characterized in that: The method is implemented based on the chain scraper thin film reaction device of any one of claims 1 to 4 containing a sulfur-containing silane coupling agent, and the method comprises the following steps: S1, chloropropyltriethoxysilane metering tank (5), anhydrous sodium polysulfide powder tank (6) are respectively added with chloropropyltriethoxysilane and anhydrous sodium polysulfide, and then placed into the mixing kettle (3) and stirred evenly; S2, the chain scraper film reactor (1) is evacuated by a Roots vacuum unit (9), and then the material in the mixing tank is pumped into the chain scraper film reactor (1) through a slurry pump (4) for reaction; S3. During the thin film reaction process, a chain scraper is used to achieve efficient mass and heat transfer reaction of the suspended material. The reaction material is continuously discharged from the bottom of the chain scraper thin film reactor (1) to the horizontal screw centrifuge (2) for continuous separation. The filtrate is further pumped into the precision filter (11) by a pipeline pump (10) for filtration, and the obtained finished product enters the finished product tank (12).

6. The method for producing a sulfur-containing silane coupling agent according to claim 5, wherein: In step S1, the stirring speed of the mixing kettle (3) is controlled to be 80-90 rpm.

7. The method for producing a sulfur-containing silane coupling agent according to claim 5, wherein: In the step S2, when the chain scraper film reactor (1) is evacuated, the vacuum degree is controlled to be -0.04 MPa to -0.06 MPa.

8. The method for producing a sulfur-containing silane coupling agent according to claim 5, wherein: In step S2, when the materials in the mixing tank react in the chain scraper film reactor (1), the reaction temperature is controlled at 90±3°C.

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