An intermittent production and separation system for octadecyl acrylate

Abstract

The utility model discloses a kind of intermittent production, separation combination system of octadecyl acrylate, it includes the reaction kettle for reaction, the washing tank for removing excess acid, catalyst and polymerization inhibitor, the filter washing dryer for post-treatment of the solid-liquid product obtained by reaction, waste liquid tank for collecting filter washing dryer waste liquid, vacuum pump for providing vacuum state, waste water tank for collecting vacuum pump waste water etc..The utility model can control reaction progress, improve product purity in the production of octadecyl acrylate process.The utility model adopts vacuum distillation mode, accurately adjusts reaction progress, improves reaction conversion rate, ensures that the reactant of entire system is converted fully, simultaneously in the drying process of refined product, vacuum heating mode is used, reduce the moisture in product, improve the purity of product.Through above operation, under the premise of excess acrylate, the conversion rate of octadecanol is close to 100%, and the purity of obtained octadecyl acrylate is ≥98wt%.

Description

Technical Field

[0001] This utility model relates to an intermittent production and separation system for octadecyl acrylate, belonging to the technical field of chemical reaction systems. Background Technology

[0002] Octadecyl acrylate is an important organic chemical raw material whose chemical structure contains acrylic acid groups and octadecyl alcohol groups. Its chemical formula is C1. 21 H 40 O2 has a relative molecular mass of 328.54 g / mol. Octadecyl acrylate is usually a white solid or waxy solid with low viscosity at room temperature.

[0003] Octadecyl acrylate has a wide range of applications in many fields. Here are some of the important applications:

[0004] Polymer Materials: Octadecyl acrylate is an important monomer that plays multiple roles in the synthesis of various polymers. It can be copolymerized with other monomers to form polymer materials with specific properties. Unlike traditional external plasticizers, the long alkyl side chains of octadecyl acrylate act as "internal plasticizers," reducing intermolecular forces and enhancing chain mobility, thereby effectively lowering the glass transition temperature of the material, making it more flexible, and improving its processing performance.

[0005] Coatings and inks: Octadecyl acrylate can be used as an additive in coatings and inks. It can improve the adhesion, bonding strength, and abrasion resistance of coatings and inks. In addition, it can also improve the gloss and weather resistance of coatings.

[0006] Surfactants: Octadecyl acrylate can be used to synthesize surfactants, such as certain preservatives and emulsifiers. These surfactants can play emulsifying, dispersing, and stabilizing roles in a variety of applications.

[0007] Functional lubricants: Lubricants made from octadecyl acrylate can be used in a variety of lubrication applications, such as lubricating oils, greases, and pastes. They can reduce the coefficient of friction, improve lubrication performance, and prevent wear and corrosion of metal parts.

[0008] There are many methods for synthesizing octadecyl acrylate, mainly including esterification, transesterification, and acyl chloride synthesis.

[0009] Esterification is a direct esterification reaction between acrylic acid and octadecyl alcohol under the action of a catalyst, producing octadecyl acrylate and water. The reaction is reversible, so timely removal of the generated water during the reaction can allow the forward reaction to continue. Esterification is further divided into direct esterification and melt esterification. In direct esterification, an organic solvent that can azeotropically react with water is used as a water-carrying agent during the reaction. The generated water is removed by vacuum distillation during the reaction, improving the conversion rate. Melt esterification does not use a water-carrying agent during the reaction. Optimal material ratios, catalyst dosage, polymerization inhibitor dosage, and reaction time are determined through orthogonal experiments and programmed temperature rise, thereby driving the reaction in the forward direction.

[0010] There are three types of transesterification: ester-to-ester transesterification, ester-to-alcohol transesterification, and ester-to-acid transesterification. When preparing higher acrylates via transesterification, methyl acrylate is often used as the lower ester. Because of its low boiling point (around 80°C), the reaction can only proceed at lower temperatures, prolonging the reaction time. The azeotrope formed by methanol and methyl acrylate has a boiling point of 62–63°C, easily carrying away the reactants and reducing the reaction yield. Furthermore, copolymerization or homopolymerization of methyl acrylate and higher acrylates also reduces the yield of higher acrylates. Considering cost and post-processing difficulties, this method is no longer commonly used industrially.

[0011] The acyl chloride process involves the esterification reaction of phthalic acid with alcohol in the presence of alkaline substances such as sodium ethoxide, sodium carbonate, pyridine, and triethylamine to produce esters. Acyl chloride is obtained by reacting acrylic acid with thionyl chloride. The acyl chloride process has high raw material costs and involves the handling of hazardous chemicals.

[0012] Other methods: In recent years, researchers have developed methods using solid superacids to replace traditional liquid acid catalysts, which can lower the esterification temperature to below 100°C and simplify post-processing steps; microwave-assisted technology can shorten the reaction time to one-third of traditional methods; molecular sieve dehydration processes can significantly improve reaction conversion rates. Strict temperature control (<140°C) and maintaining nitrogen protection in the system are required during production to prevent premature monomer polymerization. These methods offer varying degrees of improvement in efficiency and conversion rates compared to traditional methods, and given time, they will undoubtedly become the mainstay for the industrial production of high-chain acrylic acid esters. Summary of the Invention

[0013] The technical problem to be solved by this utility model is to provide an intermittent production and separation system for producing octadecyl acrylate.

[0014] The present invention solves the above-mentioned technical problem through the following technical solution:

[0015] A batch production and separation system for octadecyl acrylate, comprising:

[0016] The reactor used for the reaction has an inlet, a feed port, and a gas phase outlet at the top. The inlet is connected to a liquid feed line, and the liquid feed mainly consists of acrylic acid, water-carrying agents, etc. The feed port is for adding solid materials in the reactants, including octadecyl alcohol, catalysts, and polymerization inhibitors. The gas phase outlet is connected to a vacuum pump via a pipeline. The reactor has a discharge port at the bottom.

[0017] A washing tank for removing excess acid, catalyst, and polymerization inhibitor is provided. The top of the washing tank has a feed inlet, a washing liquid inlet, and a vent. The feed inlet is connected to the bottom outlet of the reactor via a pipeline. The washing liquid inlet is connected to a deionized water feed line and a NaOH solution feed line. A spray nozzle is installed inside the washing tank, connected to the washing liquid inlet via a pipeline. The washing liquid consists of two types: NaOH solution and deionized water, with the NaOH solution being applied first, followed by the deionized water. The bottom of the washing tank has a discharge outlet, connected to a filter washing and drying machine via a pipeline.

[0018] A filtration washing and drying machine is provided for post-processing of the solid-liquid products obtained from the reaction. The top of the filtration washing and drying machine is equipped with a feed inlet, a gas phase outlet, and a washing liquid inlet. The feed inlet is connected to the outlet of the washing tank. The washing liquid inlet is connected to the washing water feed line. The lower side of the cylinder of the filtration washing and drying machine is equipped with a solid discharge outlet, which is connected to a solid material tank for collecting the target product. The bottom of the filtration washing and drying machine is equipped with a drain outlet, which is connected to a waste liquid tank through a pipeline.

[0019] The waste liquid tank is used to collect waste liquid from the filter washing and drying machine. The top of the waste liquid tank is equipped with an inlet and a vent, and the bottom is equipped with a discharge port. The inlet is connected to the liquid outlet of the filter washing and drying machine through a pipeline, the vent is connected to the main vent pipe through a pipeline, and the discharge port is connected to the waste liquid outlet line.

[0020] A vacuum pump is used to provide a vacuum state. The vacuum pump is equipped with an inlet, a liquid phase outlet, and a gas phase outlet. The inlet is connected to the gas phase outlet of the reaction vessel and the filter washing and drying machine.

[0021] A wastewater tank for collecting vacuum pump wastewater has an inlet and a vent at the top, and a liquid outlet and a water outlet on both sides of the bottom.

[0022] The gas phase outlets of the washing tank, vacuum pump, wastewater tank, and waste liquid tank are connected to the vent manifold. The drying process of the filter washing dryer uses vacuum operation to remove moisture from the product.

[0023] Preferably, the reactor is equipped with a cooling coil, the two ends of which are connected to the refrigerant inlet line and refrigerant outlet line at the top of the reactor, respectively. A jacket is provided outside the reactor, the upper part of which is connected to the heat medium inlet line, and the lower part to the heat medium outlet line. The heat medium heats the molten solid reactants, providing the heat required for the reaction; the refrigerant in the cooling coil removes the heat generated by the reaction, working in conjunction with the heat medium in the jacket to maintain the reaction temperature. The reactor operates intermittently, with its top connected to a vacuum pump. Vacuum distillation is used to remove the water generated by the reaction, thus driving the reaction forward. Given the intermittent operation, the vacuum pumps used for the reactor and the filter washing and drying machine are from the same unit, and can be switched according to the operating procedure.

[0024] Preferably, the reaction vessel, washing tank, and filter washing and drying machine are respectively equipped with stirring paddle one, stirring paddle two, and stirring paddle three, which are driven by motor one, motor two, and motor three, respectively. The motors are equipped with frequency converters.

[0025] Preferably, the washing tank and the filter washing and drying machine are each equipped with a pH analyzer and a pH analyzer, respectively. The washing process is determined based on the analysis results.

[0026] Preferably, the filter washing and drying machine is equipped with a jacket, a heat medium inlet and a heat medium outlet, which are respectively connected to the heat medium feed line and the heat medium discharge line.

[0027] Preferably, a weighing scale is provided at the bottom of the solid material hopper.

[0028] This invention allows for control of the reaction process and improved product purity during the production of octadecyl acrylate. It employs vacuum distillation to precisely regulate the reaction process, increasing the conversion rate and ensuring complete conversion of reactants throughout the system. Simultaneously, vacuum heating is used during the drying process of the refined product to reduce moisture content and further enhance purity. Through these operations, with excess acrylic acid, the conversion rate of octadecyl alcohol approaches 100%, yielding octadecyl acrylate with a purity ≥98 wt%. Attached Figure Description

[0029] Figure 1 A schematic diagram of the intermittent production, separation and combination system of octadecyl acrylate provided by this utility model. Detailed Implementation

[0030] To make this utility model more apparent and understandable, preferred embodiments are described in detail below with reference to the accompanying drawings.

[0031] Example

[0032] like Figure 1As shown, this utility model provides an intermittent production and separation system for octadecyl acrylate, comprising:

[0033] Reactor 1: The top of reactor 1 is equipped with a gas phase outlet, which is externally connected to vacuum pump 4 via pipeline 18. The top of reactor 1 has five openings: the first is a feed port 9 for solid material inlet; the second is a feed inlet, mainly for liquid materials, connected to feed line 13; the third is a refrigerant inlet connected to refrigerant feed line 14; the fourth is a refrigerant outlet connected to refrigerant discharge line 15; a cooling coil 12 is installed inside the reactor, connected to the refrigerant inlet and refrigerant outlet respectively; and the fifth is a stirring paddle connection port. At the top center of reactor 1, a stirring paddle 11 inside the reactor is driven by motor 10; the bottom of reactor 1 is connected to the inlet of washing tank 2 via pipeline 19, and NaOH solution feed line 21 is also connected to pipeline 19, while deionized water feed line 20 is connected to NaOH solution feed line 21. The two feed lines sequentially rinse washing tank 2; reactor 1 is equipped with a jacket, with a heat medium inlet at the top connected to heat medium feed line 16, and a heat medium outlet at the bottom connected to heat medium discharge line 17.

[0034] Washing tank 2: Washing tank 2 is used to remove excess acid, catalyst and polymerization inhibitor. The washing tank 2 is equipped with a stirring paddle 26, which is driven by a motor 22 to assist in washing. The top of the washing tank 2 is equipped with a feed inlet, which is connected to the discharge port at the bottom of the reactor 1 through a pipeline 19. The top side of the washing tank 2 is equipped with a washing liquid inlet, which is connected to a nozzle 25 through a pipeline. The number of nozzles 25 is determined according to the volume of the washing tank 2. The outside is connected to the NaOH solution feed line 21 and the deionized water feed line 20 through a pipeline 24. The bottom of the washing tank 2 is equipped with a discharge port, which is connected to the filter washing dryer 3 through a pipeline 27. A pH analyzer 43 is installed on the side of the washing tank 2. The top of the washing tank 2 is equipped with a vent, which is connected to the vent main through a pipeline 23.

[0035] Filter washing and drying machine 3: The filter washing and drying machine 3 has a feed inlet at the top, which is connected to the discharge outlet of the washing tank 1 through pipeline 27; a gas phase outlet is provided on one side of the top, which is connected to the inlet of the vacuum pump 4 through pipeline 33; a washing water inlet is provided on the other side, which is connected to the washing water feed line 28; a solid discharge outlet is provided at the bottom of the side of the filter washing and drying machine 3, which is connected to the solid material tank 7 through pipeline 30; a liquid outlet is provided at the bottom, which is connected to the waste liquid tank 6 through liquid outlet line 35; an agitator 34 is provided inside the filter washing and drying machine 3, which is driven by motor 29; a jacket is provided on the outside of the filter washing and drying machine 3, with a heat medium inlet at the lower part of the jacket connected to the heat medium feed line 31, and a heat medium outlet at the upper part connected to the heat medium discharge line 32; a pH analyzer 44 is provided on the side of the filter washing and drying machine 3 cylinder;

[0036] Vacuum pump 4: The inlet of vacuum pump 4 is connected to the gas phase outlet at the top of reactor 1 through pipeline 18; the liquid phase outlet of vacuum pump 4 is connected to wastewater tank 5 through pipeline 38; the vent is connected to the vent main through pipeline 39.

[0037] Wastewater tank 5: The upper part of the wastewater tank 5 has an inlet on one side, which is connected to the liquid phase outlet of the vacuum pump 4 through pipeline 9 38; the other side has a vent, which is connected to the vent main through pipeline 10 40; the wastewater tank is equipped with a partition to divide the inside of the tank into a water zone and an oil zone; the bottom side has a liquid outlet connected to pipeline 12 42; the bottom side has a water outlet connected to pipeline 11 41.

[0038] Waste liquid tank 6: The upper part of the waste liquid tank 6 has an inlet on one side, which is connected to the filter washing and drying machine 3 through the liquid outlet line 35; the other side has an vent, which is connected to the vent main pipe through pipeline fourteen 36; the lower part has a drain port connected to pipeline thirteen 37.

[0039] Solid material hopper 7: It is equipped with a feed inlet at the top, which is connected to the solid material outlet of the filter washing and drying machine 3 through pipeline 30;

[0040] This invention employs a batch reactor with intermittent vacuum operation. A top feed port is provided for adding solid materials, while a liquid inlet is also provided for feeding liquid materials. Based on esterification, solid materials, such as octadecyl alcohol, catalysts, and polymerization inhibitors, are added through the feed port. Liquid materials for the reaction, such as acrylic acid and water-carrying agents (in melt esterification), are added through the inlet. All materials are added to the reactor in a specific ratio. The heat required for the reaction is supplied through a jacketed heat transfer medium. Following the reaction scheme, the reactor sequentially reaches the melting temperature, the first-stage reaction temperature, and the second-stage reaction temperature. Water generated during the reaction is vaporized and removed by reducing the boiling point through vacuum, thus ensuring the reaction proceeds towards the target product. The reaction is exothermic, and the released heat is dissipated through cooling coils inside the reactor, while the temperature inside the reactor is controlled by the jacketed heat transfer medium.

[0041] A washing tank is used to wash the reaction products and residual materials. First, NaOH solution is used to clean the residual acid, catalyst and polymerization inhibitor in the materials. Then, deionized water is used to rinse the materials washed with NaOH solution into the integrated filter washing and drying machine. A certain number of nozzles are set in the washing tank to flush the materials attached to the inside of the washing tank into the integrated filter washing and drying machine without dead angles. The process of NaOH solution washing is determined according to the results of pH value analyzer.

[0042] The integrated filtration, washing, and drying machine combines these processes into a single unit, minimizing the number of hazardous materials passing through and reducing the overall hazard of the reaction. After the material brought in by deionized water enters the machine, the solid-liquid mixture continues to be washed with deionized water. A spray system inside the filter ensures the washing liquid is evenly distributed within the container, enabling both internal cleaning and material slurry washing. The filter cake and washing liquid are mixed by agitation using lifting paddles, ensuring thorough washing of the remaining filter cake. The deionized water washing process is determined based on pH analysis results. The filtration system uses a high-precision filter screen, which can intercept solid materials with a particle size of 10μm or larger. The filtration process can be combined with vacuum operation to maximize the recovery of filtrate and effectively achieve solid-liquid separation. During filtration, the filter cake is flat and the solid-liquid separation effect is good. After filtration, the remaining filter cake is loosened layer by layer by the stirring blades. The equipment's heating device heats the filter cake evenly. Under vacuum, the integrated machine's jacket introduces heating medium to heat the wet material, accelerate evaporation, and achieve the drying purpose. After drying, the material is loosened by the stirring blades and then automatically discharged from the discharge port on the side of the tank wall by the pushing of the stirring blades. The washed liquid is sent to the waste liquid tank.

[0043] A vacuum pump is used to provide the vacuum required for the reaction and drying. The vacuum level is controlled between 15 and 100 kPa(a). The pump selection can be determined according to the actual site conditions and vacuum requirements.

Claims

1. A batch production, separation, and combination system for octadecyl acrylate, characterized in that, include: The reactor (1) used for the reaction has a feed inlet, a feeding port (9) and a gas phase outlet at the top. The feed inlet is connected to the feed line (13). The bottom of the reactor (1) has a discharge port. A washing tank (2) for removing excess acid, catalyst and polymerization inhibitor. The washing tank (2) is provided with a feed inlet and a vent at the top. The feed inlet is connected to the deionized water feed line (20), the NaOH solution feed line (21) and the outlet of the reactor (1). The washing tank (2) is provided with a nozzle (25) which is connected to the deionized water feed line (20) and the NaOH solution feed line (21). The washing tank (2) is provided with an outlet at the bottom. A filter washing and drying machine (3) is used to post-process the solid and liquid products obtained from the reaction. The filter washing and drying machine (3) has a feed inlet and a gas phase outlet at the top. The feed inlet is connected to the outlet of the washing tank (2). The upper part of the filter washing and drying machine (3) has a washing liquid inlet, which is connected to the washing water feed line (28). The washing water feed line (28) is connected to the deion feed line (20) and the NaOH solution feed line (21). The lower part of the side of the filter washing and drying machine (3) has a solid outlet, which is connected to the solid material tank (7). The bottom of the filter washing and drying machine (3) has an outlet. Waste liquid tank (6) for collecting waste liquid from filter washing and drying machine. The top of the waste liquid tank (6) is provided with a feed inlet and a vent, and the bottom is provided with a discharge outlet. The feed inlet is connected to the discharge outlet of filter washing and drying machine (3) through a liquid outlet line (35). A vacuum pump (4) is used to provide a vacuum state. The vacuum pump (4) is equipped with an inlet, a liquid phase outlet, and a vent. The inlet is connected to the gas phase outlet of the reactor (1) and the filter washing dryer (3). Wastewater tank (5) for collecting vacuum pump wastewater. The top of the wastewater tank (5) is provided with a feed inlet and a vent, and the bottom sides are provided with a liquid outlet and a water outlet, respectively. The vents of the washing tank (2), vacuum pump (4), wastewater tank (5), and waste liquid tank (6) are connected to the venting manifold.

2. The intermittent production, separation, and combination system for octadecyl acrylate as described in claim 1, characterized in that, The reactor (1) is equipped with a cooling coil (12), and the two ends of the cooling coil (12) are connected to the refrigerant feed line (14) and the refrigerant discharge line (15) at the top of the reactor (1), respectively. The reactor (1) is equipped with a jacket, the upper part of which is connected to the heat medium feed line (16) and the lower part of which is connected to the heat medium discharge line (17).

3. The intermittent production, separation, and combination system for octadecyl acrylate as described in claim 1, characterized in that, The reactor (1), washing tank (2), and filter washing dryer (3) are respectively equipped with a stirring paddle one (11), a stirring paddle two (26), and a stirring paddle three (34), which are driven by a motor one (10), a motor two (22), and a motor three (29), respectively.

4. The intermittent production, separation, and combination system for octadecyl acrylate as described in claim 1, characterized in that, The washing tank (2) and the filter washing and drying machine (3) are respectively equipped with pH analyzer one (43) and pH analyzer two (44).

5. The intermittent production, separation, and combination system for octadecyl acrylate as described in claim 1, characterized in that, The filter washing and drying machine (3) is equipped with a jacket. The lower part of the jacket is equipped with a heat medium inlet connected to the heat medium feed line 31, and the upper part is equipped with a heat medium outlet connected to the heat medium discharge line 32.

6. The intermittent production, separation, and combination system for octadecyl acrylate as described in claim 1, characterized in that, The solid material hopper (7) is equipped with a weighing scale (8) at the bottom.

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