CN107935846B - Device and method for continuously producing environment-friendly plasticizer - Google Patents
Device and method for continuously producing environment-friendly plasticizer Download PDFInfo
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- CN107935846B CN107935846B CN201711070334.6A CN201711070334A CN107935846B CN 107935846 B CN107935846 B CN 107935846B CN 201711070334 A CN201711070334 A CN 201711070334A CN 107935846 B CN107935846 B CN 107935846B
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Abstract
A device and a method for continuously producing environment-friendly plasticizer are disclosed, solid acid and liquid alcohol materials are added into a preheating dehydration kettle, stirred and heated until no water is removed, and the preheating and dehydration treatment of the materials are realized; conveying the preheated and dehydrated reaction materials from a preheating and dehydrating kettle to a multi-stage esterification reaction kettle connected in series through a pump or a high-level pressure difference, adding a catalyst into a first-stage esterification reaction kettle, stirring and heating to perform reaction; along with the continuous input of reaction materials, when the reaction materials in the esterification reaction kettle reach a discharge hole at the upper part of the kettle, the reaction materials are conveyed into a next-stage esterification reaction kettle for continuous reaction, the flow rate of the materials entering the esterification reaction kettle is regulated, and the reacted liquid materials are conveyed into a dealcoholization kettle for continuous dealcoholization. The device disclosed by the invention is reasonable in layout, simple in process, high in production efficiency and stable in operation, effectively improves the yield in unit time, and realizes the continuous and large-scale batch production of the environment-friendly plasticizer.
Description
Technical Field
The invention belongs to the technical field of preparation of environment-friendly plastic additives, and particularly relates to a method for continuously producing an environment-friendly plasticizer.
Background
The cable is known as the 'blood vessel' and 'nerve' of the national economy. The manufacturing industry of the electric wire and the electric cable is one of the largest matching industries in national economy, is the second major industry in the mechanical industry, is only next to the automobile industry, and the electric wire and the electric cable product are widely applied to the industries of energy, traffic, communication, automobiles, petrochemical industry and the like. With the improvement of the industrialized development degree of China, the improvement of the infrastructure and the improvement of the urbanization level, the cable industry is bound to develop to maturity and rapidity.
The environment-friendly plasticizer, namely di-isooctyl terephthalate (DOTP), is a fine chemical product with wide application and excellent performance, is mainly applied to PVC plastic products, and is a main additive for producing cable materials. Along with the rapid development of the cable industry, the demand of the cable industry is increasing day by day, and the cable industry has wide market prospect.
At present, the DOTP is produced industrially mainly by an intermittent method, which mainly has the following defects: 1) the intermittent production consumes longer time, and the product quality has large fluctuation and is not stable; 2) the process is backward and the labor intensity is high; 3) the intermittent esterification has high energy consumption and material consumption and low product yield; 4) the scale is small, the large-scale production cannot be realized, and the output of the plasticizer is limited. As the reaction adopts a large amount of recovered PTA material as a raw material, the particle size is not uniform, and the defects of poor compatibility, long reaction time consumption and the like of the solid-liquid esterification reaction are caused. The invention provides a novel method with stable process and high economic effect, and realizes continuous and large-scale production of the environment-friendly plasticizer.
Disclosure of Invention
The technical problem to be solved is as follows: the invention aims to provide a device and a method for continuously producing an environment-friendly plasticizer.
The technical scheme is as follows: a method for continuously producing an environment-friendly plasticizer comprises the following steps: (1) preheating and dehydrating materials: adding the solid acid and the liquid alcohol material into a preheating dehydration kettle according to the mass ratio of 1:2.4-1:3.2, stirring and heating, wherein the temperature in the kettle is more than 160 ℃ until no water is removed, and preheating and dehydrating the materials; (2) continuous esterification reaction: conveying the preheated and dehydrated reaction materials from a preheating dehydration kettle to a multi-stage esterification reaction kettle connected in series through a pump or a high-level pressure difference, adding a catalyst into a first-stage esterification reaction kettle, wherein the catalyst is tetrabutyl titanate, the addition amount of the tetrabutyl titanate is 0.1-0.5 wt% of the total reaction materials, and stirring and heating to 180-fold-material 240 ℃ for reaction; along with the continuous input of reaction materials, when the reaction materials in the esterification reaction kettle reach a discharge hole at the upper part of the kettle, the reaction materials naturally overflow through a pipeline or are conveyed into the next-stage esterification reaction kettle through a pump to continue reaction, the reaction temperature in each series esterification reaction kettle is controlled to be 180 DEG, the flow rate of the materials entering the esterification reaction kettle is regulated and controlled, the acid value of effluent liquid in the last esterification reaction kettle is smaller than 0.50mgKOH/g, and the liquid after the reaction is finished is conveyed into a dealcoholization kettle to be continuously dealcoholized.
The solid acid raw material in the step (1) is purified terephthalic acid, PTA pool material, PTA falling material or reclaimed material (commonly called PTA alkali dissolving material) in the alkali decrement process in the polyester fiber industry.
The number of the multistage esterification reaction kettles connected in series in the step (2) is at least two.
The esterification reaction in the step (2) is carried out in a plurality of fluidized bed reactors connected in series, and the number of the fluidized bed reactors connected in series is at least two.
The addition amount of the catalyst tetrabutyl titanate in the step (2) is 0.1-0.3 wt% of the total reaction materials.
A device for continuously producing environment-friendly plasticizer is sequentially connected with a preheating dehydration kettle, a multistage esterification reaction device and a dealcoholization kettle which are connected in series through pipelines; the preheating dehydration kettle is provided with a condenser and a wastewater receiving tank; the multi-stage esterification reaction device in series connection is composed of at least two stages of esterification reaction kettles in series connection or fluidized bed reactors in series connection, the first stage esterification reaction device is connected with the catalyst storage tank through a metering pump, and the last esterification reaction device is connected with the dealcoholization kettle through a pipeline.
The installation heights of all stages of devices in the multistage esterification reaction device are sequentially reduced, and reaction materials naturally overflow into the next adjacent stage of esterification reaction kettle.
The installation heights of all stages of devices in the multi-stage esterification reaction device are the same, and reaction materials are conveyed to the next adjacent stage of esterification reaction device through a pump.
The top of each stage of esterification reaction kettle is connected with a condenser and an alcohol-water separator, and the condensed isooctyl alcohol flows into the corresponding esterification reaction kettle from the alcohol-water separator through a pipeline.
The esterification reaction devices at all stages connected in series are connected into a condenser for uniform condensation and heat exchange, and condensed isooctyl alcohol is conveyed into esterification reaction kettles at all stages.
Has the advantages that: the invention provides a device and a method for continuously producing an environment-friendly plasticizer. The invention adopts the esterification reaction kettles or the fluidized bed reactors connected in series, realizes reaction continuity by natural overflow and pump delivery, has reasonable device layout, simple process, high production efficiency and stable operation, effectively improves the yield in unit time, and realizes the continuity and large-scale batch production of the environment-friendly plasticizer.
Drawings
FIG. 1 is a diagram of an apparatus for continuously producing an environmentally friendly plasticizer in which four esterification reaction kettles are connected in series, which is preferred in the present invention.
FIG. 2 is a diagram of an apparatus for continuously producing an environmentally friendly plasticizer in which six esterification reaction kettles are connected in series, which is preferred in the present invention.
In the figure, 1: preheating a dehydration kettle, 2: first esterification reaction kettle, 3: catalyst metering pump, 4: second esterification reaction kettle, 5: esterification reaction kettle No. three, 6: fourth esterification reaction kettle, 7: esterification reaction kettle No. five, 8: number six esterification reaction kettle, 9: and (4) dealcoholizing the mixture.
Fig. 1 is a diagram of an apparatus for continuously producing an environment-friendly plasticizer according to the present invention, in which four esterification reaction kettles are preferably connected in series, and as shown in fig. 1, the preheated and dehydrated reaction material is transferred from the preheating and dehydrating kettle to one esterification reaction kettle in an esterification system through a pump, the installation heights of the four esterification reaction kettles in the esterification system are sequentially reduced, and the reaction material flows into the next adjacent esterification reaction kettle in a natural overflow manner.
Fig. 2 is a diagram of an apparatus for continuously producing an environment-friendly plasticizer according to the present invention, in which six esterification reaction kettles are connected in series, and as shown in fig. 2, the reaction material after preheating and dewatering is transferred into the first esterification reaction kettle in the esterification system through a high head difference from the preheating and dewatering kettle, and the six esterification reaction kettles in the esterification system are installed at the same height, and the reaction material is transferred into the next adjacent esterification reaction kettle at a certain flow rate by a pump.
Detailed Description
The following examples are further illustrative of the present invention, but the present invention is not limited thereto.
Example 1
Adding PTA pool materials and 98% isooctyl alcohol in a mass ratio of 1:2.8 into a preheating dehydration kettle, starting mechanical stirring and heat conducting oil to heat, and keeping the temperature in the kettle to be not lower than 160 ℃ under the mechanical stirring to realize material preheating and dehydration treatment; conveying the preheated and dehydrated reaction materials from a preheating dehydration kettle into a first esterification reaction kettle in an esterification system through a pump (or a height difference), starting a catalyst metering pump at the top of the kettle, starting mechanical stirring and heating for reaction; along with the continuous introduction of reaction materials, when the reaction materials in the first esterification reaction kettle reach a discharge port at the upper part of the kettle, the reaction materials naturally overflow through a pipeline, or are conveyed into the second esterification reaction kettle according to a certain flow rate through a pump to continue the reaction, along with the reaction, the reaction materials in the second esterification reaction kettle naturally overflow through a pipeline, or are conveyed into the third esterification reaction kettle through a pump to continue the reaction, along with the reaction, the process is carried out by analogy of …, the reaction materials flow into the last fourth esterification reaction kettle, the reaction temperature in each series esterification reaction kettle is controlled to be 180-.
TABLE 1 change of acid value with time in esterification reaction vessel IV
Example 2
Adding PTA (pure terephthalic acid) falling material and 98% isooctanol in a mass ratio of 1:2.6 into a preheating dehydration kettle, starting mechanical stirring and heat conducting oil to heat, and keeping the temperature in the kettle to be not lower than 160 ℃ under the mechanical stirring to realize material preheating and dehydration treatment; conveying the preheated and dehydrated reaction materials from a preheating dehydration kettle into a first esterification reaction kettle in an esterification system through a pump (or a height difference), starting a catalyst metering pump at the top of the kettle, starting mechanical stirring and heating for reaction; along with the continuous feeding of the reaction materials, when the reaction materials in the first esterification reaction kettle reach a discharge port at the upper part of the kettle, the reaction materials naturally overflow through a pipeline, or are conveyed into the second esterification reaction kettle according to a certain flow rate through a pump to continue the reaction, along with the reaction, the reaction materials in the second esterification reaction kettle naturally overflow through a pipeline, or are conveyed into the third esterification reaction kettle through a pump to continue the reaction, along with the reaction, by analogy of …, the reaction materials flow into the last fifth esterification reaction kettle, the reaction temperature in each series esterification reaction kettle is controlled to be 180-.
TABLE 2 change of acid value with time in esterification reaction vessel No. five
Example 3
Adding PTA alkali soluble material and 98% isooctyl alcohol in a mass ratio of 1:3.2 into a preheating dehydration kettle, starting mechanical stirring and heat conducting oil to heat, and keeping the temperature in the kettle to be not lower than 160 ℃ under the mechanical stirring to realize material preheating and dehydration treatment; conveying the preheated and dehydrated reaction materials from a preheating dehydration kettle into a first esterification reaction kettle in an esterification system through a pump (or a height difference), starting a catalyst metering pump at the top of the kettle, starting mechanical stirring and heating for reaction; along with the continuous feeding of the reaction materials, when the reaction materials in the first esterification reaction kettle reach a discharge port at the upper part of the kettle, the reaction materials naturally overflow through a pipeline, or are conveyed into the second esterification reaction kettle according to a certain flow rate through a pump to continue the reaction, along with the reaction, the reaction materials in the second esterification reaction kettle naturally overflow through a pipeline, or are conveyed into the third esterification reaction kettle through a pump to continue the reaction, along with the reaction, by analogy of …, the reaction materials flow into the last sixth esterification reaction kettle, the reaction temperature in each series esterification reaction kettle is controlled to be 180-.
TABLE 3 change of acid value with time in esterification reaction vessel VI
Example 4
Adding purified terephthalic acid and 98% isooctyl alcohol in a mass ratio of 1:2.4 into a preheating dehydration kettle, starting mechanical stirring and heat conducting oil to heat, and keeping the temperature in the kettle to be not lower than 160 ℃ under the mechanical stirring to realize material preheating and dehydration; conveying the preheated and dehydrated reaction materials from a preheating dehydration kettle into a first esterification reaction kettle in an esterification system through a pump (or a height difference), starting a catalyst metering pump at the top of the kettle, starting mechanical stirring and heating for reaction; along with the continuous letting in of reaction material, when the reaction material in the esterification reaction cauldron reaches cauldron upper portion discharge gate, overflow through the pipeline nature, or carry the continuation reaction in the esterification reaction cauldron No. two according to certain flow through the pump, along with the reaction goes on, the same is said, when the reaction material in the esterification reaction cauldron No. two reaches cauldron upper portion discharge gate, overflow through the pipeline nature, or carry through the pump and continue the reaction in the last esterification reaction cauldron No. three, control reaction temperature 180 in each series esterification reaction cauldron and add 240 ℃, the flow that the regulation and control material got into the esterification reaction cauldron and advance, make thing liquid acid value be less than 0.50mgKOH/g in the last esterification reaction cauldron No. three, the material that the reaction ended is carried and is carried out continuous dealcoholization processing in the dealcoholization cauldron.
TABLE 4 change of acid value with time in esterification reaction vessel III
Claims (2)
1. A method for continuously producing an environment-friendly plasticizer is characterized by comprising the following steps: (1) preheating and dehydrating materials: adding the solid acid and the liquid alcohol material into a preheating dehydration kettle according to the mass ratio of 1:2.4-1:3.2, stirring and heating, wherein the temperature in the kettle is more than 160 ℃ until no water is removed, and preheating and dehydrating the materials; the solid acid is purified terephthalic acid, PTA water tank material, PTA falling material or reclaimed material in an alkali decrement process in the polyester fiber industry; (2) continuous esterification reaction: conveying the preheated and dehydrated reaction materials to a multistage esterification reaction kettle or a multistage fluidized bed reactor which are connected in series from a preheating dehydration kettle through a pump or a high-level pressure difference, wherein the number of the multistage esterification reaction kettle or the multistage fluidized bed reactor is at least two, adding a catalyst into a first-stage esterification reaction kettle or a multistage fluidized bed, wherein the catalyst is tetrabutyl titanate, the adding amount of the tetrabutyl titanate is 0.1-0.3 wt% of the total reaction materials, and stirring and heating to 180-phase 240 ℃ for reaction; along with the continuous input of reaction materials, when the reaction materials in the esterification reaction kettle reach a discharge hole at the upper part of the kettle, the reaction materials naturally overflow through a pipeline or are conveyed into the next-stage esterification reaction kettle through a pump to continue reaction, the reaction temperature in each series esterification reaction kettle is controlled to be 180 DEG, the flow rate of the materials entering the esterification reaction kettle is regulated and controlled, the acid value of effluent liquid in the last esterification reaction kettle is smaller than 0.50mgKOH/g, and the liquid after the reaction is finished is conveyed into a dealcoholization kettle to be continuously dealcoholized.
2. The device for continuously producing the environment-friendly plasticizer is characterized in that: the device is sequentially connected with a preheating dehydration kettle, a multistage esterification reaction device and a dealcoholization kettle which are connected in series through pipelines; the preheating dehydration kettle is provided with a condenser and a wastewater receiving tank; the multistage esterification reaction device in series connection consists of at least two stages of esterification reaction kettles in series connection or fluidized bed reactors in series connection, the first stage esterification reaction device is connected with the catalyst storage tank through a metering pump, and the last esterification reaction device is connected with the dealcoholization kettle through a pipeline; the installation heights of all stages of devices in the multistage esterification reaction device are sequentially reduced, and reaction materials naturally overflow to an adjacent next stage of esterification reaction kettle; or the installation heights of all stages of devices in the multi-stage esterification reaction device are the same, and the reaction materials are conveyed to the next adjacent stage of esterification reaction device through a pump; the top of each stage of esterification reaction kettle is connected with a condenser and an alcohol-water separator, and the condensed isooctyl alcohol flows into the corresponding esterification reaction kettle from the alcohol-water separator through a pipeline; and the esterification reaction devices at all stages connected in series are connected into a condenser for uniform condensation and heat exchange, and condensed isooctyl alcohol is conveyed into esterification reaction kettles at all stages.
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| CN201711070334.6A CN107935846B (en) | 2017-11-03 | 2017-11-03 | Device and method for continuously producing environment-friendly plasticizer |
| NL2021197A NL2021197B1 (en) | 2017-11-03 | 2018-06-28 | A device and method for continuously producing environment-friendly plasticizer |
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| KR102105057B1 (en) | 2018-08-16 | 2020-04-27 | 삼성전기주식회사 | Multi-layered ceramic electronic component |
| CN109107503A (en) * | 2018-09-19 | 2019-01-01 | 长园华盛(泰兴)锂电材料有限公司 | Tandem reaction equipment of vinylene carbonate and preparation method thereof |
| KR102488351B1 (en) * | 2019-07-04 | 2023-01-13 | 주식회사 엘지화학 | Method for manufacturing diester-based material |
| CN110302737A (en) * | 2019-07-29 | 2019-10-08 | 潍坊益华化工有限公司 | A kind of continuous esterification device and process |
| CN113457571A (en) * | 2020-03-30 | 2021-10-01 | 中石油吉林化工工程有限公司 | Polymerization inhibitor mechanism for MMA (methyl methacrylate) production device and polymerization inhibitor adding method |
| CN111732510A (en) * | 2020-07-03 | 2020-10-02 | 山东朗晖石油化学股份有限公司 | Continuous production equipment and process for DOTP plasticizer |
| CN111909037B (en) * | 2020-09-01 | 2023-04-18 | 潍坊弘润新材料有限公司 | Continuous production method of tetraisooctyl pyromellitate |
| KR20220067343A (en) * | 2020-11-17 | 2022-05-24 | 주식회사 엘지화학 | Method for preparing diester-based material |
| KR20220067385A (en) * | 2020-11-17 | 2022-05-24 | 주식회사 엘지화학 | Method for preparing diester compound |
| KR20220067352A (en) * | 2020-11-17 | 2022-05-24 | 주식회사 엘지화학 | Method for preparing diester-based material |
| KR20220067368A (en) * | 2020-11-17 | 2022-05-24 | 주식회사 엘지화학 | Method for preparing diester compound |
| CN112569621B (en) * | 2020-11-23 | 2021-12-03 | 湖北兴瑞硅材料有限公司 | Continuous dehydration device and dehydration process for dimethyl cyclosiloxane |
| CN112920094B (en) * | 2021-01-29 | 2024-10-18 | 江苏奥洁生物科技有限公司 | Method for regulating production load and improving yield of N-methyl sodium taurate |
| CN114933534B (en) * | 2022-04-28 | 2024-07-23 | 山东蓝帆化工有限公司 | Continuous esterification production process of diisooctyl terephthalate heterogeneous system |
| CN115010633B (en) * | 2022-07-11 | 2024-04-12 | 宁夏汉润生物科技有限公司 | Synthesis method and device of ring-closing compound |
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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 |
| CN104496819A (en) * | 2014-12-17 | 2015-04-08 | 中国林业科学研究院林产化学工业研究所 | Method for preparing environment-friendly plasticizer by recycling waste resources |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104496819A (en) * | 2014-12-17 | 2015-04-08 | 中国林业科学研究院林产化学工业研究所 | Method for preparing environment-friendly plasticizer by recycling waste resources |
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