CN220143335U - Continuous synthesizer of diisooctyl terephthalate plasticizer - Google Patents

Continuous synthesizer of diisooctyl terephthalate plasticizer Download PDF

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CN220143335U
CN220143335U CN202321564865.1U CN202321564865U CN220143335U CN 220143335 U CN220143335 U CN 220143335U CN 202321564865 U CN202321564865 U CN 202321564865U CN 220143335 U CN220143335 U CN 220143335U
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inlet
outlet
section
esterification
water separator
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曹翠琼
李江华
高俊
孙乾
李峻
储阳阳
纪静
杨娟
荆晓平
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Jiangsu Zhengdan Chemical Industry Co ltd
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Jiangsu Zhengdan Chemical Industry Co ltd
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Abstract

The utility model discloses a continuous synthesis device of a diisooctyl terephthalate plasticizer in the field of chemical production equipment, wherein a reaction tower consists of an upper dealcoholization section and a lower esterification section, the top of the dealcoholization section is connected to the top of a water separator after passing through a condenser, the bottom of the water separator is provided with a water outlet, and the side surface of the water separator is provided with an alcohol outlet; a discharge hole is formed in the side surface of the bottom of the esterification section, and an alcohol reflux port and a feed inlet are formed in the side surface of the upper part of the esterification section; a guide lifting cylinder with openings at the upper and lower parts is arranged in the esterification section, a catalyst layer is arranged in an annular cavity between the guide lifting cylinder and the inner wall of the reaction tower, and a feed inlet and an alcohol reflux port are positioned above the catalyst layer; the discharge port is connected with one inlet of the dispersing pump, the other inlet of the dispersing pump is connected with the diatomite inlet, the outlet of the dispersing pump is connected to the inlet of the continuous filter, and the outlet of the continuous filter is connected with the finished product receiving device. The device has compact structure, can be used for continuous synthesis of the diisooctyl terephthalate, and improves the production efficiency.

Description

Continuous synthesizer of diisooctyl terephthalate plasticizer
Technical Field
The utility model relates to chemical production equipment, in particular to a device for synthesizing a diisooctyl terephthalate plasticizer.
Background
The diisooctyl terephthalate (DOTP) is a novel plasticizer which starts to be produced and used in the 1980 s, and compared with the conventional diisooctyl phthalate (DOP), the DOTP has the advantages of high insulation, low volatilization, heat resistance, cold resistance, extraction resistance, good flexibility, good compatibility with PVC resin and the like, is widely used for processing polyvinyl chloride, vinyl chloride copolymer and cellulose resin, is also used for manufacturing plastic products and sheet materials of films, wire and cable insulation, artificial leather, mould and the like, and can also be used as an additive of a coating additive and a lubricant, and a softener of rubber and paper. In recent years, attention is paid to the rubber and plastic industry, and the rubber and plastic industry has become a substitute for DOP.
At present, the diisooctyl terephthalate in China is more in production factories, and the production methods of most factories are direct esterification of terephthalic acid. The production process adopts an intermittent production mode of an acid catalyst esterification process, and the intermittent synthesis mode is to directly esterify and synthesize DOTP by taking terephthalic acid and isooctyl alcohol as raw materials under the catalysis of tetraisopropyl titanate. The esterification and refining of the synthesis process are carried out in two reaction kettles, the refining process needs to be carried out once alkali washing and twice water washing, and then the finished product is obtained after dealcoholization and filter pressing by a stripping device. However, the actual production situation has the following problems: (1) the esterification efficiency is not ideal, and the unit consumption is high; (2) the product quality (acid value, resistance) is unstable; (3) high oil content in sewage, large waste water content, etc.
The semicontinuous synthesis mode is to feed slurry at a clear point of the material, and in order to effectively increase the alcohol concentration and the forward reaction speed and adopt a certain pressurizing mode for esterification, the raw materials are considered to react above the normal pressure boiling point, so that the reaction rate can be effectively improved, and the energy consumption is saved. However, due to the high temperature requirements of the reaction, there is too high requirements for equipment and process operations during synthetic applications, and there is room for improvement for application in industrial production.
Patent CN111960943a discloses a process for producing dioctyl terephthalate by semi-continuous method, firstly making batch esterification reaction, then continuously making neutralization water washing, dealcoholization stripping, decoloring and filtering to obtain dioctyl terephthalate.
Patent CN114276238A discloses a process for the preparation of diisooctyl terephthalate, comprising: the method comprises the steps of primary esterification, secondary esterification distillation, neutralization, filtration and the like. The utility model shortens the time required by primary esterification through secondary esterification, and excessive octanol forms azeotropy with glycol generated in the reaction, so that glycol can be removed directly in an esterification kettle, and glycol is separated out and recovered through water washing, standing and layering.
Patent CN110698345a discloses a continuous stripping dealcoholization method of diisooctyl terephthalate, which comprises washing a crude diisooctyl terephthalate product obtained by catalytic esterification of terephthalic acid and excessive isooctyl alcohol with alkali wash water, heating to 165-175 ℃ by a stripping feed heater, and feeding the crude diisooctyl terephthalate product between an upper packing layer and a lower packing layer in a stripping dealcoholization tower by a feed distributor; maintaining the pressure in the tower body at 1-6KPa, and obtaining the diisooctyl phthalate after steam stripping, wherein the temperature at the top of the tower is 140-150 ℃.
The existing device for producing the diisooctyl terephthalate has the defects that: 1. these devices are produced by a gap method or a semi-continuous method, and the production efficiency is low. 2. The devices are complex, the primary esterification and the secondary esterification are completed in different reaction devices, and the whole production device comprises equipment such as an esterification device, a dealcoholization device, a neutralization and water washing device, a stripping device, an adsorption and filtration device, a wastewater treatment device and the like, and has the advantages of more equipment, complex process and difficult control.
Disclosure of Invention
The utility model aims to provide a continuous synthesis device for a diisooctyl terephthalate plasticizer, which can be used for continuous synthesis of the diisooctyl terephthalate plasticizer, improves the production efficiency, has a more compact structure, and can reduce the equipment manufacturing cost and the management cost for producing the diisooctyl terephthalate.
The purpose of the utility model is realized in the following way: the continuous synthesis device of the diisooctyl terephthalate plasticizer comprises a vertically arranged cylindrical reaction tower, wherein a heat-preserving jacket is arranged outside the reaction tower, the reaction tower consists of an upper dealcoholization section and a lower esterification section, a gas phase outlet is arranged at the top of the dealcoholization section, a filler is arranged in the dealcoholization section, a gas phase space connected with the gas phase outlet is reserved above the filler, the gas phase outlet is connected to the top of a water separator after passing through a condenser, a water outlet is arranged at the bottom of the water separator, an alcohol outlet is arranged on the side surface of the water separator, and a vacuum air extractor is further connected to the top of the water separator; a discharge hole is formed in the side face of the bottom of the esterification section, an alcohol reflux port and a feed port for feeding a mixed material of terephthalic acid and isooctyl alcohol are formed in the side face of the upper part of the esterification section, and the alcohol reflux port is connected with an alcohol outlet on the side face of the water separator; a guide lifting cylinder with openings at the upper and lower parts is arranged in the esterification section, the upper part of the guide lifting cylinder extends to the lower side of the filler, the lower part of the guide lifting cylinder extends to the upper part of the discharge hole, a catalyst layer is arranged in an annular cavity between the guide lifting cylinder and the inner wall of the reaction tower, a feed inlet and an alcohol reflux port are positioned above the catalyst layer, and the guide lifting cylinder isolates the feed inlet and the alcohol reflux port from the filler; the discharge port is connected with one inlet of the dispersing pump, the other inlet of the dispersing pump is connected with the diatomite inlet, the outlet of the dispersing pump is connected to the inlet of the continuous filter, and the outlet of the continuous filter is connected with the finished product receiving device.
When the method works, the reaction tower is kept to have a certain vacuum degree, the mixed material of the terephthalic acid and the isooctanol firstly enters an esterification section, the dosage mole ratio of the terephthalic acid to the isooctanol is 1:3, the isooctanol is excessive, the temperature of the esterification section is 210+/-2 ℃, the terephthalic acid reacts with the isooctanol to generate the diisooctyl terephthalate under the action of a catalyst, the diisooctyl terephthalate is light yellow or colorless transparent oily liquid, the density of the diisooctyl terephthalate is about 0.981-0.986 g/cm at normal temperature, and the boiling point of the diisooctyl terephthalate is about 400 ℃; and isooctanol density of 0.833g/cm 3 Under the condition of heating, water generated by esterification and excessive isooctanol form an azeotrope and go upward from the bottom of the tower through the upflow cylinder, isooctanol and water are firstly steamed out, filler can prevent steamed out matters from entraining diisooctyl terephthalate, water is continuously discharged from the bottom of the water separator, isooctanol returns to the esterification section from the alcohol reflux port, generated crude diisooctyl terephthalate accumulates to the bottom of the tower, the discharged material of the discharge port and diatomite are pumped into a continuous filter through a dispersion pump, the diatomite acts as adsorption and decoloration, and finished DOTP is obtained after filtering. The above working process can continuously carry out the production of DOTP. Compared with the prior art, the utility model has the beneficial effects that: the device sets up esterification, dealcoholization in a reaction tower, and it is used for the continuous synthesis of terephthalic acid diisooctyl plasticizer, has improved production efficiency, and simultaneously, its structure is compacter, can reduce the equipment manufacturing cost and the management cost of terephthalic acid diisooctyl production.
In order to ensure that the raw materials are fully mixed, the feed inlet is connected with the grinding pump outlet, the grinding pump inlet is connected with the jet mixer outlet, the jet mixer comprises two paths of inlets, one path of inlet is connected with the terephthalic acid inlet, and the other path of inlet is connected with the isooctanol inlet. Terephthalic acid is solid at normal temperature, isooctanol is liquid, and is fed through a jet mixer, and the isooctanol is used for injecting terephthalic acid, so that the material is convenient to feed, and the terephthalic acid can be ground into micro-nano grade slurry through grinding of a grinding pump, and isooctanol not only can be used as a conveying carrier, but also has the effects of lubrication and cooling, so that smooth grinding is ensured, and the raw materials are fully mixed.
Further, the catalyst layer comprises a catalyst bed of layered structure, on which a spherical catalyst (produced according to the formulation of example 6 of patent CN 112958065B) is loaded. The catalyst bed with the layered structure is convenient for loading the catalyst, soluble mixed materials between gaps of the spherical catalyst pass up and down, so that the materials are not easy to accumulate, and meanwhile, the catalyst layer is well contacted with the materials, the energy efficiency of the catalyst is ensured, and the catalyst is not easy to run off.
Further, the lifting guide cylinder comprises an upper conical cylinder body and a lower cylindrical cylinder body, and the conical cylinder body gradually contracts from top to bottom and is connected with the upper end of the cylindrical cylinder body. The gas phase materials in the reaction comprise distilled alcohol and water, and the structure of the guide lifting cylinder ensures that the upper part has a larger evaporation space, so that the alcohol materials and the water are easier to be distilled.
Further, a circulating liquid inlet is arranged above the catalyst layer on the esterification section, a circulating liquid outlet is arranged below the catalyst layer, and a circulating pump is connected between the circulating liquid outlet and the circulating liquid inlet through an external pipeline. By cyclically increasing the chance of contact of the reaction mass with the catalyst, the reaction proceeds more rapidly.
Further, a liquid outlet is arranged at the bottom of the esterification section. The liquid outlet is used for cleaning and placing the residue.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model.
In the figure, a circulating pump 1, a grinding pump 2, a jet mixer 3, a condenser 4, a water separator 5, a dispersing pump 6, a continuous filter 7, a reaction tower 8, a liquid outlet 801, a circulating liquid outlet 802, a circulating liquid inlet 803, a feeding port 804, a gas outlet 805, a gas space 806, a filler 807, a reflux inlet 808, a 809 lifting cylinder, a 810 heat-insulating jacket, a 811 discharging port and a 812 catalyst layer.
Detailed Description
As shown in fig. 1, the continuous synthesis device of the diisooctyl terephthalate plasticizer comprises a vertically arranged cylindrical reaction tower 8, a heat-insulating jacket 810 is arranged outside the reaction tower 8, the reaction tower 8 consists of an upper dealcoholization section and a lower esterification section, a gas phase outlet 805 is arranged at the top of the dealcoholization section, a filler 807 is arranged in the dealcoholization section, a gas phase space 806 connected with the gas phase outlet 805 is reserved above the filler 807, the gas phase outlet 805 is connected to the top of a water separator 5 after passing through a condenser 4, a water outlet is arranged at the bottom of the water separator 5, and an alcohol outlet is arranged on the side surface of the water separator 5; the side surface of the bottom of the esterification section is provided with a discharge hole 811, the side surface of the upper part of the esterification section is provided with an alcohol reflux hole 808 and a feed hole 804 for feeding the mixed material of terephthalic acid and isooctyl alcohol, and the alcohol reflux hole 808 is connected with an alcohol outlet on the side surface of the water separator 5; a lift guiding cylinder 809 with openings at the upper and lower sides is arranged in the esterification section, the upper part of the lift guiding cylinder 809 extends to the lower side of the filler 807, the lower part of the lift guiding cylinder 809 extends to the upper part of the discharge hole 811, a catalyst layer 812 is arranged in an annular cavity between the lift guiding cylinder 809 and the inner wall of the reaction tower 8, a feed inlet 804 and an alcohol reflux inlet 808 are positioned above the catalyst layer, and the lift guiding cylinder 809 isolates the feed inlet 804 and the alcohol reflux inlet 808 from the filler 807; the discharge port 811 is connected to one inlet of the dispersion pump 6, the other inlet of the dispersion pump 6 is connected to the diatomite inlet, the outlet of the dispersion pump 6 is connected to the inlet of the continuous filter 7, and the outlet of the continuous filter 7 is connected to the finished product receiving device.
To ensure adequate mixing of the materials, the feed inlet 804 is connected to the outlet of the grinding pump 2, the inlet of the grinding pump 2 is connected to the outlet of the jet mixer 3, and the jet mixer 3 comprises two inlets, one of which is connected to the terephthalic acid inlet and the other of which is connected to the isooctanol inlet. Terephthalic acid is solid at normal temperature, isooctanol is liquid, and is fed through the jet mixer 3, and the isooctanol is used for injecting terephthalic acid, so that the material is convenient to feed, and the terephthalic acid can be ground into micro-nano grade slurry through the grinding of the grinding pump 2, and isooctanol not only can be used as a conveying carrier, but also has the effects of lubrication and cooling, so that the grinding is smooth, and the raw materials are fully mixed.
Further, the catalyst layer 812 includes a catalyst bed of a layered structure, on which a spherical catalyst is loaded. The catalyst bed with the layered structure is convenient for loading the catalyst, soluble mixed materials between gaps of the spherical catalyst pass up and down, so that the materials are not easy to accumulate, and meanwhile, the catalyst bed is well contacted with the materials, the energy efficiency of the catalyst is ensured, and the catalyst is not easy to run off.
Further, the lift guide 809 includes an upper tapered cylinder and a lower cylindrical cylinder, the tapered cylinder gradually shrinking from top to bottom and being connected to the upper end of the cylindrical cylinder. The gas phase material in the reaction comprises distilled alcohol and water, and the structure of the lifting guide 809 ensures that the upper part has a larger evaporation space, so that the alcohol material and the water are easier to be distilled out.
Further, a circulating liquid inlet 803 is arranged above the catalyst layer on the esterification section, a circulating liquid outlet 802 is arranged below the catalyst layer, and a circulating pump 1 is connected between the circulating liquid outlet 802 and the circulating liquid inlet 803 through an external pipeline. By cyclically increasing the chance of contact of the reaction mass with the catalyst, the reaction proceeds more rapidly.
Further, a liquid outlet 801 is arranged at the bottom of the esterification section. The drain 801 is used for cleaning and removing residue.
When the device works, terephthalic acid and isooctanol enter a grinding pump 2 through a jet mixer 3, are ground into micro-nano grade slurry, then enter an esterification section, a catalyst bed layer is loaded with spherical catalyst, a side discharge hole 811 at the bottom of the tower generates coarse ester, meanwhile, water generated by the esterification reaction and excessive isooctanol form an azeotrope, enter a dealcoholization section from the bottom of the tower through a flow-up cylinder, enter a water separator 5 after condensation, isooctanol flows back into the esterification section again to continuously participate in the esterification reaction, water is discharged, and products after dealcoholization at the bottom of the tower and diatomite are pumped into a continuous filter 7 through a dispersion pump 6 to be adsorbed, decolorized and filtered to obtain a finished product DOTP.
The specific continuous esterification dealcoholization decoloration filtration process parameters are as follows:
the dosage mole ratio of terephthalic acid and isooctyl alcohol is 1:3, the particle size of particles in micro-nano grade slurry is 100nm-50um, the temperature of an esterification section is 210+/-2 ℃, and the airspeed is 3 h -1 The temperature of the circulating liquid is 190+/-2 ℃. The vacuum at the top of the tower is 90+/-2 KPa, and the temperature of the dealcoholization section is 180+/-2 ℃. The dealcoholized product was added with 0.5wt% diatomaceous earth.
When the device works, the conversion rate of dioctyl terephthalate is more than or equal to 99.9 percent. Continuous production can be performed.
The utility model is not limited to the above embodiments, and based on the technical solution disclosed in the utility model, a person skilled in the art may make some substitutions and modifications to some technical features thereof without creative effort according to the technical content disclosed, and all the substitutions and modifications are within the protection scope of the utility model.

Claims (6)

1. The utility model provides a continuous synthesizer of diisooctyl terephthalate plasticizer, includes the cylinder reaction tower of vertical setting, the reaction tower is equipped with heat preservation jacket, its characterized in that outward: the reaction tower consists of an upper dealcoholization section and a lower esterification section, wherein the top of the dealcoholization section is provided with a gas phase outlet, a filler is arranged in the dealcoholization section, a gas phase space connected with the gas phase outlet is reserved above the filler, the gas phase outlet is connected to the top of a water separator after passing through a condenser, the bottom of the water separator is provided with a water outlet, the side surface of the water separator is provided with an alcohol outlet, and the top of the water separator is also connected with a vacuum air extractor; a discharge hole is formed in the side face of the bottom of the esterification section, an alcohol reflux port and a feed port for feeding a mixed material of terephthalic acid and isooctyl alcohol are formed in the side face of the upper part of the esterification section, and the alcohol reflux port is connected with an alcohol outlet on the side face of the water separator; a guide lifting cylinder with openings at the upper and lower parts is arranged in the esterification section, the upper part of the guide lifting cylinder extends to the lower side of the filler, the lower part of the guide lifting cylinder extends to the upper part of the discharge hole, a catalyst layer is arranged in an annular cavity between the guide lifting cylinder and the inner wall of the reaction tower, a feed inlet and an alcohol reflux port are positioned above the catalyst layer, and the guide lifting cylinder isolates the feed inlet and the alcohol reflux port from the filler; the discharge port is connected with one inlet of the dispersing pump, the other inlet of the dispersing pump is connected with the diatomite inlet, the outlet of the dispersing pump is connected to the inlet of the continuous filter, and the outlet of the continuous filter is connected with the finished product receiving device.
2. The continuous synthesis apparatus of diisooctyl terephthalate plasticizer according to claim 1, characterized in that: the feed inlet is connected with the grinding pump outlet, the grinding pump inlet is connected with the jet mixer outlet, the jet mixer comprises two paths of inlets, one path of inlet is connected with the terephthalic acid inlet, and the other path of inlet is connected with the isooctanol inlet.
3. The continuous synthesis apparatus of diisooctyl terephthalate plasticizer according to claim 1 or 2, characterized in that: the catalyst layer comprises a catalyst bed with a layered structure, and a spherical catalyst is loaded on the catalyst bed.
4. The continuous synthesis apparatus of diisooctyl terephthalate plasticizer according to claim 1 or 2, characterized in that: the lifting guide cylinder comprises a conical cylinder body at the upper part and a cylindrical cylinder body at the lower part, and the conical cylinder body gradually contracts from top to bottom and is connected with the upper end of the cylindrical cylinder body.
5. The continuous synthesis apparatus of diisooctyl terephthalate plasticizer according to claim 1 or 2, characterized in that: the esterification section is provided with a circulating liquid inlet above the catalyst layer, a circulating liquid outlet below the catalyst layer, and a circulating pump is connected between the circulating liquid outlet and the circulating liquid inlet through an external pipeline.
6. The continuous synthesis apparatus of diisooctyl terephthalate plasticizer according to claim 1 or 2, characterized in that: the bottom of the esterification section is provided with a liquid outlet.
CN202321564865.1U 2023-06-19 2023-06-19 Continuous synthesizer of diisooctyl terephthalate plasticizer Active CN220143335U (en)

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CN202321564865.1U CN220143335U (en) 2023-06-19 2023-06-19 Continuous synthesizer of diisooctyl terephthalate plasticizer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202321564865.1U CN220143335U (en) 2023-06-19 2023-06-19 Continuous synthesizer of diisooctyl terephthalate plasticizer

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CN220143335U true CN220143335U (en) 2023-12-08

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