Continuous production system for 6, 6-dimethyl fulvene

Abstract

The utility model discloses a 6, 6-dimethyl fulvene continuous production system, which relates to the technical field of fine chemical engineering, and comprises a mixing device, a reaction device and a control device, the reaction device is used for reacting the mixture conveyed by the tetrahydropyrrole catalytic mixing device; the rectification device is used for separating a product from an unreacted substrate after the reaction of the reaction device; and the falling film evaporator is used for separating the 6, 6-dimethyl fulvene from the by-product. According to the continuous production device disclosed by the utility model, the continuous production of 6, 6-dimethyl fulvene is realized.

Description

Technical Field

[0001] This utility model relates to the field of fine chemical technology, and in particular to a continuous production system for 6,6-dimethyl-rich ene. Background Technology

[0002] 6,6-Dimethylfulene is an important starting compound for the synthesis of organometallic compounds, and there are several synthetic methods. One method involves reacting cyclopentadiene with potassium / sodium to generate potassium cyclopentadiene or sodium cyclopentadiene, which is then reacted directly with a ketone, followed by hydrolysis to obtain fulene compounds.

[0003] Another method involves the condensation reaction of cyclopentadiene and aldehydes / ketones in the presence of a catalyst. The reaction proceeds as follows: In a Shrek flask, acetone and cyclopentadiene are dissolved in methanol. The solution is cooled to 0°C, and then tetrahydropyrrole is slowly added. The reaction mixture is stirred at 0°C for 2 hours, followed by neutralization of the tetrahydropyrrole with glacial acetic acid. The organic phase is extracted with water and pentane, and the combined organic phases are dried over anhydrous magnesium sulfate. After removing the solvent, distillation yields 6,6-dimethylfulne.

[0004] The two methods described above have the following problems: First, both methods are intermittent, multi-step operations, which cannot achieve large-scale continuous production; second, the reaction solvent cannot be fully recovered, resulting in a large amount of waste liquid, which significantly increases the product cost during large-scale production, thereby affecting the product's competitiveness. Utility Model Content

[0005] Based on the technical problems existing in the background technology, this utility model proposes a continuous production system for 6,6-dimethyl-rich ene, which realizes the continuous production of 6,6-dimethyl-rich ene.

[0006] The continuous production system for 6,6-dimethyl-rich ene proposed in this utility model includes:

[0007] A mixing device for mixing methanol, acetone and cyclopentadiene;

[0008] A reaction apparatus for reacting a mixture supplied by a tetrahydropyrrole catalytic mixing unit;

[0009] A distillation apparatus is used to separate the products from the unreacted substrate after a reaction in a reaction apparatus.

[0010] Falling film evaporators are used to separate 6,6-dimethyl-richene from byproducts in distillation equipment.

[0011] Preferably, the mixing device is further connected to:

[0012] A methanol purification unit is used to purify methanol and transport it to a mixing unit.

[0013] An acetone purification unit is used to purify acetone and transport it to a mixing unit.

[0014] A pyrolysis unit for pyrolyzing dicyclopentene into cyclopentadiene and conveying it to a mixing unit.

[0015] Preferably, the cyclopentadiene separated by the distillation unit is transported to the cracking unit via pipeline; the methanol separated by the distillation unit is transported to the methanol purification unit via pipeline.

[0016] Preferably, the reaction apparatus is also connected to a tetrahydropyrrole purification device for purifying tetrahydropyrrole and conveying it to the reaction apparatus.

[0017] Preferably, the falling film evaporator is also connected to a waste liquid recovery device and a condenser, the condenser being used for cooling 6,6-dimethyl-richene.

[0018] The beneficial technical effects of this utility model are as follows:

[0019] This invention improves the purity of methanol, acetone, and tetrahydropyrrole entering the mixing device through methanol purification, acetone purification, and tetrahydropyrrole purification devices; the vacuum distillation device enables the recovery and reuse of reaction products and unreacted substrates methanol, tetrahydropyrrole, and cyclopentadiene; through the combined use of these devices, this invention achieves continuous production of 6,6-dimethyl-rich ene, with all unreacted solvents and catalysts recovered and reused, reducing waste liquid generation, significantly lowering product costs, and improving economic efficiency. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the continuous production system for 6,6-dimethyl-richene proposed in this utility model.

[0021] In the diagram: 1-Methanol purification unit, 2-Acetone purification unit, 3-Cracking unit, 4-Mixing unit, 5-Tetrahydropyrrole purification unit, 6-Reaction unit, 7-Distillation unit, 8-Falling film evaporator, 9-Condenser, 10-Waste liquid recovery unit. Detailed Implementation

[0022] The present invention will be further explained below with reference to specific embodiments.

[0023] Reference Figure 1 The present invention proposes a continuous production system for 6,6-dimethyl-rich ene, comprising: a mixing device 4 for mixing methanol, acetone and cyclopentadiene; a reaction device 6 for reacting the mixture conveyed by the tetrahydropyrrole catalytic mixing device 4; a distillation device 7 for separating the product from the unreacted substrate after the reaction in the reaction device 6; and a falling film evaporator 8 for separating 6,6-dimethyl-rich ene from the byproducts in the product after the distillation device 7.

[0024] To remove water from methanol, acetone, and tetrahydropyrrole components, the mixing device 4 is also connected to: a methanol purification device 1 for purifying methanol and conveying it to the mixing device 4; an acetone purification device 2 for purifying acetone and conveying it to the mixing device 4; a cracking device 3 for cracking dicyclopentene into cyclopentadiene and conveying it to the mixing device 4; and a tetrahydropyrrole purification device 5 for purifying tetrahydropyrrole and conveying it to the reaction device 6.

[0025] To recover unreacted substrates, the cyclopentadiene separated by the distillation unit 7 is transported to the cracking unit 3 via pipeline; the methanol separated by the distillation unit 7 is transported to the methanol purification unit 1 via pipeline.

[0026] In addition, the falling film evaporator 8 is also connected to a waste liquid recovery device 10 and a condenser 9, which is used for cooling 6,6-dimethyl-richene.

[0027] In this embodiment, the distillation apparatus is a four-stage distillation column. The upper section of the first distillation column produces cyclopentadiene, methanol, tetrahydropyrrole, and water, while the bottom section produces 6,6-dimethyl-richene and other products. The upper section of the second distillation column produces cyclopentadiene, methanol, and tetrahydropyrrole, while the bottom section produces water which goes to a waste liquid recovery device. The upper section of the third distillation column produces cyclopentadiene and methanol, while the bottom section produces tetrahydropyrrole. The upper section of the fourth distillation column produces cyclopentadiene, while the bottom section produces methanol.

[0028] Application examples

[0029] Anhydrous methanol from the methanol tank farm and methanol returned from the vacuum distillation unit, at 30°C, are dehydrated and pumped into the mixing unit at a flow rate of 500 L / h. Acetone, dried with anhydrous calcium sulfate, is pumped into the mixing unit at a flow rate of 69.4 L / h. Dicyclopentadiene from the boundary area is heated and liquefied, then mixed with cyclopentadiene returned from the vacuum distillation unit before entering the cracking unit, where it is cracked into cyclopentadiene. The condensed cyclopentadiene is pumped into the mixing unit at a flow rate of 195 L / h. The mixing unit uses an ice-brine jacket, maintaining the temperature at 0°C, with a molar ratio of acetone to cyclopentadiene of 1:2.

[0030] The mixed methanol, acetone and cyclopentadiene were pumped into the reaction unit. Tetrahydropyrrole from the tank farm and tetrahydropyrrole returned from the vacuum distillation unit were dehydrated with anhydrous magnesium sulfate and then pumped into the reaction unit at a flow rate of 155 L / h. The temperature of the reaction unit was kept at 0°C and the pressure at atmospheric pressure. The reaction time was 2 hours.

[0031] The reaction apparatus adopts a plug flow heat exchange reactor to ensure that the residence time of the above four raw materials in the reactor is greater than 2 hours.

[0032] The product mixture from the reaction unit is pumped into the first distillation column. The top fraction of the first distillation column is cyclopentadiene, methanol, tetrahydropyrrole, and water, while the bottom fraction is 6,6-dimethyl-richene and high-boiling-point substances produced by the reaction. The cyclopentadiene, methanol, tetrahydropyrrole, and water distilled from the top of the first distillation column enter the second distillation column. The upper part of the second distillation column distills cyclopentadiene, methanol, and tetrahydropyrrole, while the bottom fraction, water, goes to the waste liquid recovery unit. The cyclopentadiene, methanol, and tetrahydropyrrole distilled from the top of the second distillation column enter the third distillation column. The top of the third distillation column distills cyclopentadiene and methanol, while the bottom fraction, tetrahydropyrrole, is distilled. The top of the fourth distillation column distills cyclopentadiene, while the bottom fraction, methanol, is distilled.

[0033] Cyclopentadiene, methanol, and tetrahydropyrrole are condensed and returned to their respective feed sections.

[0034] 6,6-Dimethyl-Fupe and the high-boiling-point substances produced in the reaction enter a falling film evaporator. 6,6-Dimethyl-Fupe is discharged from the top of the falling film evaporator and condensed for storage as a product. The unevaporated high-boiling-point substances in the falling film evaporator and the water produced at the bottom of the second distillation column are sent to the wastewater treatment process as waste liquid.

[0035] The falling film evaporator operates at a pressure of -0.098 MPaG and a shell-side temperature of 120℃.

[0036] The flow rate of the 6,6-dimethylfulne product was approximately 93.1 kg / h, and the product yield was approximately 93%.

[0037] Although embodiments of this application have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of this application. The scope of this application is defined by the appended claims and their equivalents, all of which should be included within the protection scope of this application.

Claims

A continuous production system for 1,6,6-dimethyl-rich olefins, characterized in that, include: Mixing device (4) for mixing methanol, acetone and cyclopentadiene; The reaction apparatus (6) is used for the reaction of the mixture delivered by the tetrahydropyrrole catalytic mixing apparatus (4); Distillation apparatus (7) is used to separate the reaction products from the unreacted substrate in reaction apparatus (6); Falling film evaporator (8) is used to separate 6,6-dimethyl-richene from by-products in the product after distillation unit (7); The mixing device (4) is also connected to: Methanol purification unit (1) is used to purify methanol and transport it to the mixing unit (4). Acetone purification device (2) is used to purify acetone and transport it to the mixing device (4). The cracking unit (3) is used to crack dicyclopentene into cyclopentadiene and transport it to the mixing unit (4). The reaction apparatus (6) is also connected to a tetrahydropyrrole purification device (5) for purifying tetrahydropyrrole and transporting it to the reaction apparatus (6).

2. The continuous production system for 6,6-dimethyl-rich olefins according to claim 1, characterized in that, The cyclopentadiene separated by the distillation unit (7) is transported to the cracking unit (3) via pipeline; the methanol separated by the distillation unit (7) is transported to the methanol purification unit (1) via pipeline.

3. The continuous production system for 6,6-dimethyl-rich olefins according to claim 1, characterized in that, The falling film evaporator (8) is also connected to a waste liquid recovery device (10) and a condenser (9), which is used for cooling 6,6-dimethyl-richene.

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