NL2021197B1 - A device and method for continuously producing environment-friendly plasticizer - Google Patents
A device and method for continuously producing environment-friendly plasticizer Download PDFInfo
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- NL2021197B1 NL2021197B1 NL2021197A NL2021197A NL2021197B1 NL 2021197 B1 NL2021197 B1 NL 2021197B1 NL 2021197 A NL2021197 A NL 2021197A NL 2021197 A NL2021197 A NL 2021197A NL 2021197 B1 NL2021197 B1 NL 2021197B1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
Abstract
A device and method for continuously producing environment-friendly plasticizer. Solid acid and liquid alcohol material is added into a preheating and dehydrating reactor, stirred and heated until not water comes out, to realize material preheating and dehydration; The above mentioned reaction material which is preheated and dehydrated is conveyed from the preheating and dehydrating reactor to multi-stage esterification reactors connected in series through a pump or high potential difference, and catalyst is added into the first-stage esterification reactor, stirred and heated to realize reaction; With continuous input of the reaction material, when reaching the material outlet at the upper part of the esterification reactor, the reaction material in the reactor is conveyed to a next-stage esterification reactor for further reaction; the flow rate of the material into the esterification reactor is adjusted, and the liquid material generated at the end of the reaction is conveyed to a dealcoholization reactor for further dealcoholization. The device of the invention has advantages that the layout is reasonable, the working procedures are simple, the production efficiency is high, the operation is stable, the yield in unit time is effectively improved, and thus continuous and large-scale production of environment-friendly plasticizer is realized.
Description
Technical Field
The invention belongs to the technical field of environment-friendly plastic additive preparation, and especially relates to a method for continuously producing environmentfriendly plasticizer.
Background Technology
Cables are praised as “blood vessels” and “nerves” of national economy. The wire and cable manufacturing industry is one of the largest auxiliary industry in national economy, and the second largest industry in machinery, next to the automobile industry. Wire and cable products are broadly applied in energy, traffic, communication, automobiles, petrochemical engineering, etc. In recent years, the wire and cable industry of China maintains fast growth, and continues occupying an important position in national economy. With further development of industrialization, completion of infrastructure construction and improvement of urbanization level of China, the wire and cable industry will surely and quickly develop to maturity.
Environment-friendly plasticizer, DOTP, is a fine chemical product having broad application range and excellent performance. DOTP is mainly applied in PVC plastic products and is main additive in cable material production. Along with fast development of the cable industry, DOTP will be increasingly demanded and have broad market prospect.
Currently, industrial DOTP production is conducted by the batch method, which mainly has the following disadvantages: 1) match production consumes longer time, and generates greatly fluctuating and unstable product quality; 2) the process is outdated and requires high labor intensity; 3) batch esterification consumes more energy and materials, but gives low product yield; 4) the scale is small, and thus large-scale production cannot be realized, and the plasticizer output is restrained. Since a large amount of recovered PTA material is used as the raw material of reaction, the particle sizes are non-uniform, and thus compatibility between the esterification reaction of solid and liquid is low, and the reaction consumes long time. The invention proposes a
AO 18.06.1059 NL new method with stable process and high economic efficiency, which can realize continuous and large-scale production of environment-friendly plasticizer.
Description of Invention
Technical problem: the invention aims to provide a device and method for continuously producing environment-friendly plasticizer.
Technical scheme: a method for continuously producing environment-friendly plasticizer, comprising the following steps: (1) material preheating and dehydration: the solid acid and liquid alcohol material is added into a preheating and dehydrating reactor at a mass ratio of 1:2.4-1:3.2, stirred, and heated to a temperature over 160°C until no water comes out, to realize material preheating and dehydration; (2) continuous esterification reaction: the above mentioned reaction material which is preheated and dehydrated is conveyed from the preheating and dehydrating reactor to multi-stage esterification reactors connected in series through a pump or high potential difference, and catalyst, i.e., tetrabutyl titanate is added into the first-stage esterification reactor at an amount which is ().lwt.%-().5 wt.% of the total reaction material, stirred and heated to 180-240°C to realize reaction; with continuous input of the reaction material, when reaching the material outlet at the upper part of the esterification reactor, the reaction material in the reactor overflows naturally through a pipe or is conveyed to a next-stage esterification reactor for further reaction; the reaction temperature in the esterification reactors connected in series is controlled within 180-240°C, the flow rate of the material into the esterification reactor is adjusted such that the acid value of the liquid material flowing out of the final esterification reactor is lower than 0.50 mgKOH/g, and the liquid material generated at the end of the reaction is conveyed to a dealcoholization reactor for further dealcoholization.
The solid acid material in the step (1) is purified terephthalic acid (PTA), precipitated PTA, fallen PTA or recovered material from the alkali decrement process in the polyester fiber industry (commonly known as alkali dissolved PTA).
The multi-stage esterification reactors connected in series have two stages at least.
AO 18.06.1059 NL
The esterification reaction is performed in multi-stage fluidized bed reactors connected in series, which have two stages at least.
The addition amount of the catalyst, i.e., tetrabutyl titanate in the step (2) is 0.1wt.%-0.3 wt.% of the total reaction material.
A device for continuously producing environment-friendly plasticizer, in which a preheating and dehydrating reactor, multi-stage esterification reactors connected in series and a dealcoholization reactor are connected in sequence through pipes in the device; The preheating and dehydrating reactor is provided with a condenser and a wastewater receiving tank; the multi-stage esterification reactors connected in series are composed of esterification reactors connected in series or fluidized bed reactors connected in series which have two stages at least, the first-stage esterification reactor is connected with a catalyst tank through a metering pump, and the final-stage esterification reactor is connected with the dealcoholization reactor through a pipe.
Each stage of reactor in the multi-stage esterification reactors is installed at gradually lower height, and the reaction material overflows naturally to the adjacent next-stage esterification reactor.
Each stage of reactor in the multi-stage esterification reactors is installed at equal height, and the reaction material is conveyed to the next-stage esterification reactor through the pump.
A condenser and an alcohol-water separator are connected at the top of each stage of esterification reactor, and iso-octyl alcohol generated through condensation flows from the alcohol-water separator to the corresponding esterification reactor through a pipe. The esterification reactors connected in series are connected to a condenser for centralized condensation and heat exchange, and iso-octyl alcohol generated through condensation is conveyed to each stage of esterification reactor.
Beneficial effects: the invention provides a device and method for continuously producing environment-friendly plasticizer. Before reaction, the solid and liquid
AO 18.06.1059 NL reaction materials are preheated and dehydrated through the dehydrating reactor, to realize overall uniform mobility of the materials and remarkably improve the material conveying speed and reaction speed. In the invention, the esterification reactors or fluidized bed reactors connected in series are used to realize continuous reaction through natural overflow and pump conveying; in addition, the device of the invention has advantages that the layout is reasonable, the working procedures are simple, the production efficiency is high, the operation is stable, the yield in unit time is effectively improved, and thus continuous and large-scale production of environment-friendly plasticizer is realized.
Brief Description of Drawings
Lig. 1 shows the diagram of a preferred device for continuously producing the environment-friendly plasticizer with four esterification reactors connected in series in the invention.
Lig. 2 shows the diagram of a preferred device for continuously producing the environment-friendly plasticizer with six esterification reactors connected in series in the invention.
In the figures, 1: preheating and dehydrating reactor; 2: first esterification reactor; 3: catalyst metering pump; 4: second esterification reactor; 5: third esterification reactor; 6: fourth esterification reactor; 7: fifth esterification reactor; 8: sixth esterification reactor; 9: dealcoholization reactor.
Lig. 1 shows the diagram of a preferred device for continuously producing the environment-friendly plasticizer with four esterification reactors connected in series in the invention. As shown in Lig. 1, the reaction material which is preheated and dehydrated is conveyed from the preheating and dehydrating reactor to the first esterification reactor in the esterification system through a pump, the four esterification reactors in the esterification system are installed at gradually lower height, and the reaction material overflows naturally to the next esterification reactor.
Lig. 2 shows the diagram of a preferred device for continuously producing the
AO 18.06.1059 NL environment-friendly plasticizer with six esterification reactors connected in series in the invention. As shown in Eig. 2, the reaction material which is preheated and dehydrated is conveyed from the preheating and dehydrating reactor to the first esterification reactor in the esterification system through high potential difference, the six esterification reactors in the esterification system are installed at equal height, and the reaction material is conveyed to the next esterification reactor at certain flow rate.
Specific Implementation
The following embodiments further describe the invention, but the invention is not limited thereto.
Embodiment 1
Precipitated PTA and 98% iso-octyl alcohol with a mass ratio of 1:2.8 are added into the preheating and dehydrating reactor, stirred mechanically and heated through heat transfer oil, with the temperature in the reactor not lower than 160°C during mechanical stirring, to realize material preheating and dehydration; the reaction material which is preheated and dehydrated is conveyed from the preheating and dehydrating reactor to the first esterification reactor in the esterification system through a pump (or high potential difference), the catalyst metering pump at the top of the reactor is turned on, and mechanical stirring and heating are started for reaction; with continuous input of the reaction material, when reaching the material outlet at the upper part of the first esterification reactor, the reaction material in the reactor overflows naturally through the pipe or is conveyed to the second esterification reactor through the pump for further reaction at certain flow rate; along with the reaction progress, similarly, when reaching the material outlet at the upper part of the second esterification reactor, the reaction material in the reactor overflows naturally through the pipe or is conveyed to the third esterification reactor through the pump for further reaction, and so on; the reaction material finally flows into the final fourth esterification reactor; the reaction temperature in the esterification reactors connected in series is controlled within 180-240°C, the flow rate of the material into the first esterification reactor is adjusted such that the acid value of the liquid material flowing out of the final fourth esterification reactor is lower than 0.50 mgKOH/g, and the material generated at the end of the reaction is conveyed to the dealcoholization reactor for further dealcoholization.
AO 18.06.1059 NL
Table 1 Change of acid value in the fourth esterification reactor over time
Time / h | 2 | 4 | 6 | 8 | 10 | 12 | 14 | 16 | 18 | 20 | 22 | 24 |
Acid value / mgKOH/g | 0.42 | 0.43 | 0.48 | 0.45 | 0.49 | 0.48 | 0.5 | 0.47 | 0.46 | 0.44 | 0.5 | 0.46 |
Embodiment 2
Fallen PTA and 98% iso-octyl alcohol with a mass ratio of 1:2.6 are added into the preheating and dehydrating reactor, stirred mechanically and heated through heat transfer oil, with the temperature in the reactor not lower than 160°C during mechanical stirring, to realize material preheating and dehydration; the reaction material which is preheated and dehydrated is conveyed from the preheating and dehydrating reactor to the first esterification reactor in the esterification system through a pump (or high potential difference), the catalyst metering pump at the top of the reactor is turned on, and mechanical stirring and heating are started for reaction; with continuous input of the reaction material, when reaching the material outlet at the upper part of the first esterification reactor, the reaction material in the reactor overflows naturally through the pipe or is conveyed to the second esterification reactor through the pump for further reaction at certain flow rate; along with the reaction progress, similarly, when reaching the material outlet at the upper part of the second esterification reactor, the reaction material in the reactor overflows naturally through the pipe or is conveyed to the third esterification reactor through the pump for further reaction, and so on; the reaction material finally flows into the final fifth esterification reactor; the reaction temperature in the esterification reactors connected in series is controlled within 180-240°C, the flow rate of the material into the first esterification reactor is adjusted such that the acid value of the liquid material flowing out of the final fifth esterification reactor is lower than 0.50 mgKOH/g, and the material generated at the end of the reaction is conveyed to the dealcoholization reactor for further dealcoholization.
AO 18.06.1059 NL
Table 2 Change of acid value in the fifth esterification reactor over time
Time 1 h | 2 | 4 | 6 | 8 | 10 | 12 | 14 | 16 | 18 | 20 | 22 | 24 |
Acid value / mgKOH/ g | 0.4 7 | 0.4 7 | 0.4 8 | 0.5 0 | 0.4 9 | 0.4 8 | 0.4 2 | 0.4 1 | 0.4 3 | 0.4 4 | 0.4 2 | 0.4 6 |
Embodiment 3
Alkali dissolved PTA and 98% iso-octyl alcohol with a mass ratio of 1:3.2 are added into the preheating and dehydrating reactor, stirred mechanically and heated through heat transfer oil, with the temperature in the reactor not lower than 160°C during mechanical stirring, to realize material preheating and dehydration; the reaction material which is preheated and dehydrated is conveyed from the preheating and dehydrating reactor to the first esterification reactor in the esterification system through a pump (or high potential difference), the catalyst metering pump at the top of the reactor is turned on, and mechanical stirring and heating are started for reaction; with continuous input of the reaction material, when reaching the material outlet at the upper part of the first esterification reactor, the reaction material in the reactor overflows naturally through the pipe or is conveyed to the second esterification reactor through the pump for further reaction at certain flow rate; along with the reaction progress, similarly, when reaching the material outlet at the upper part of the second esterification reactor, the reaction material in the reactor overflows naturally through the pipe or is conveyed to the third esterification reactor through the pump for further reaction, and so on; the reaction material finally flows into the final sixth esterification reactor; the reaction temperature in the esterification reactors connected in series is controlled within 180-240°C, the flow rate of the material into the first esterification reactor is adjusted such that the acid value of the liquid material flowing out of the final sixth esterification reactor is lower than 0.50 mgKOH/g, and the material generated at the end of the reaction is conveyed to the dealcoholization reactor for further dealcoholization.
AO 18.06.1059 NL
Table 3 Change of acid value in the sixth esterification reactor over time
Time / h | 2 | 4 | 6 | 8 | 10 | 12 | 14 | 16 | 18 | 20 | 22 | 24 |
Acid value / mgKOH/ g | 0.4 5 | 0.4 4 | 0.4 7 | 0.4 7 | 0.4 7 | 0.4 4 | 0. 5 | 0.4 9 | 0.4 6 | 0.5 0 | 0.5 0 | 0.4 8 |
Embodiment 4
PTA and 98% iso-octyl alcohol with a mass ratio of 1:2.4 are added into the preheating and dehydrating reactor, stirred mechanically and heated through heat transfer oil, with the temperature in the reactor not lower than 160°C during mechanical stirring, to realize material preheating and dehydration; the reaction material which is preheated and dehydrated is conveyed from the preheating and dehydrating reactor to the first esterification reactor in the esterification system through a pump (or high potential difference), the catalyst metering pump at the top of the reactor is turned on, and mechanical stirring and heating are started for reaction; with continuous input of the reaction material, when reaching the material outlet at the upper part of the first esterification reactor, the reaction material in the reactor overflows naturally through the pipe or is conveyed to the second esterification reactor through the pump for further reaction at certain flow rate; along with the reaction progress, similarly, when reaching the material outlet at the upper part of the second esterification reactor, the reaction material in the reactor overflows naturally through the pipe or is conveyed to the final third esterification reactor through the pump for further reaction; the reaction temperature in the esterification reactors connected in series is controlled within 180240°C, the flow rate of the material into the first esterification reactor is adjusted such that the acid value of the liquid material flowing out of the final third esterification reactor is lower than 0.50 mgKOH/g, and the material generated at the end of the reaction is conveyed to the dealcoholization reactor for further dealcoholization.
AO 18.06.1059 NL
Time / h | 2 | 4 | 6 | 8 | 10 | 12 | 14 | 16 | 18 | 20 | 22 | 24 |
Acid value / mgKOH/ g | 0.4 8 | 0.4 5 | 0.4 7 | 0.4 5 | 0.4 9 | 0.4 7 | 0.5 0 | 0.4 7 | 0.4 8 | 0.4 9 | 0.4 2 | 0.5 0 |
AO 18.06.1059 NL
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EP4023629A4 (en) * | 2020-11-17 | 2022-12-21 | LG Chem, Ltd. | Method for preparing diester compound |
EP4029852A4 (en) * | 2020-11-17 | 2022-12-21 | LG Chem, Ltd. | Method for preparing diester-based material |
EP4032875A4 (en) * | 2020-11-17 | 2022-12-21 | LG Chem, Ltd. | Method for preparing diester compound |
US11605505B2 (en) | 2018-08-16 | 2023-03-14 | Samsung Electro-Mechanics Co., Ltd. | Multilayer ceramic electronic component |
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CN102503831A (en) * | 2011-11-07 | 2012-06-20 | 潍坊市元利化工有限公司 | Continuous esterification production method for plasticizer |
CN104496819B (en) * | 2014-12-17 | 2016-07-06 | 中国林业科学研究院林产化学工业研究所 | A kind of method that environment-friendly plasticizer is prepared in waste resource recycling |
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US11605505B2 (en) | 2018-08-16 | 2023-03-14 | Samsung Electro-Mechanics Co., Ltd. | Multilayer ceramic electronic component |
EP4023629A4 (en) * | 2020-11-17 | 2022-12-21 | LG Chem, Ltd. | Method for preparing diester compound |
EP4029852A4 (en) * | 2020-11-17 | 2022-12-21 | LG Chem, Ltd. | Method for preparing diester-based material |
EP4032875A4 (en) * | 2020-11-17 | 2022-12-21 | LG Chem, Ltd. | Method for preparing diester compound |
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