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Process for producing dioctyl terephthalate by semi-continuous method

A dioctyl phthalate, semi-continuous technology, applied in the field of chemical production, can solve the problems of low equipment use efficiency, low equipment utilization rate, low product stability, etc., and achieves low raw material and energy consumption, improved automation, The effect of stable product quality

Pending Publication Date: 2020-11-20
JIANGSU ZHENGDAN CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) The control of the batch production process is relatively complex, including various control variables such as temperature and liquid level, and has strict requirements on production conditions;
[0007] (2) The intermittent production cycle is long, the energy consumption is large, and the equipment utilization efficiency is low;
[0008] (3) Batch type is only suitable for small-scale production, and the product stability is low
[0009] In the domestic research on the production method of dioctyl terephthalate, although continuous production is mentioned, the continuous production process involved is relatively cumbersome, including esterification, dealcoholization, neutralization and washing, air stripping, adsorption and filtration. , wastewater treatment and other multiple processes, many equipments are used, the equipment utilization rate is low, the energy consumption is large, the environmental pollution is relatively large, and it is not in line with the actual industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A semi-continuous process for producing dioctyl terephthalate, using terephthalic acid and isooctyl alcohol as raw materials, and tetrabutyl titanate as a catalyst, adopts a semi-continuous process to synthesize dioctyl terephthalate, The specific steps are as follows:

[0028] Batch production: raise the temperature of the preheated first esterification tank to 180°C, add terephthalic acid (PTA) and isooctyl alcohol in batches, the molar ratio of acid to alcohol is 1:3, the catalyst tetrabutyl titanate The amount of ester addition is 0.2% of the total mass of the raw materials, and it is slowly stirred for 3 hours. The mixture in the first esterification kettle is added in batches to the second esterification kettle, and the catalyst tetrabutyl titanate is added at the same time. The catalyst addition amount is 0.1% of the total mass of the raw material, continue to stir, and raise the temperature to 220°C, and react for 2h.

[0029] Continuous production: After the e...

Embodiment 2

[0032] The difference between this example and Example 1 is that it is batch production: the preheated first esterification tank is heated to 185°C, and terephthalic acid (PTA) and isooctyl alcohol, acid alcohol are added in batches The molar ratio of the catalyst is 1:3.5, the amount of catalyst tetrabutyl titanate is 0.25% of the total mass of the raw material, slowly stirred for 3.5h, and the mixture in the first esterification tank is added in batches to the second esterification tank At the same time, the catalyst tetrabutyl titanate was added, the amount of the catalyst added was 0.15% of the total mass of the raw materials, the stirring was continued, and the temperature was raised to 225° C., and the reaction was carried out for 2.5 hours.

[0033] Continuous production: After the esterification reaction is completed, the mixture enters the neutralizer, the temperature is controlled at 50°C, and the acidity value of the solution is measured. At the same time, 4% sodium ...

Embodiment 3

[0036] The difference between this example and Example 2 lies in the batch production: the preheated first esterification tank is heated to 190°C, and terephthalic acid (PTA) and isooctyl alcohol, acid alcohol are added in batches The molar ratio of the catalyst is 1:4.5, and the amount of catalyst tetrabutyl titanate added is 0.3% of the total mass of the raw material, slowly stirred for 4h, and the mixture in the first esterification tank is added in batches to the second esterification tank, At the same time, the catalyst tetrabutyl titanate was added, and the amount of catalyst added was 0.2% of the total mass of the raw materials. Stirring was continued, and the temperature was raised to 230° C. for 3 hours of reaction.

[0037] Continuous production: After the esterification reaction is completed, the mixture enters the neutralizer, the temperature is controlled at 55°C, the acidity value of the solution is measured, and at the same time, 4% sodium carbonate aqueous solut...

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PUM

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Abstract

The invention discloses a process for producing dioctyl terephthalate by a semi-continuous method in the technical field of chemical production. The method sequentially comprises the following steps:firstly, carrying out a batch-type esterification reaction in two esterification kettles: in a first esterification kettle, taking terephthalic acid and isooctyl alcohol as raw materials to carry outa mono-esterification reaction with a catalyst (tetrabutyl titanate), adding a mixture obtained after the reaction into a second esterification kettle in batches, and simultaneously adding the catalyst (tetrabutyl titanate) to carry out a dual-esterification reaction; and continuously neutralizing and washing the obtained mixture, removing alcohol, stripping, decolorizing and filtering to obtain dioctyl terephthalate. According to the invention, the automation degree, the product quality and the labor productivity are improved, and the time is saved. The process has the advantages of stable product quality, low labor intensity, high economic benefit and the like.

Description

technical field [0001] The invention relates to a process for producing dioctyl terephthalate, in particular to a process for producing dioctyl terephthalate using a semi-continuous method of terephthalic acid and isooctyl ester. It belongs to the technical field of chemical production. Background technique [0002] At present, there are more than a dozen categories of plasticizers in the world, with a total of more than 500 varieties, with a total annual output of more than 5 million tons, and more than 70% are phthalates, of which diisooctyl phthalate (DOP) has good performance, but due to the shortcomings of DOP polluting the environment and high toxicity, it has been banned from export by many EU countries, and the abuse of this plasticizer has also been banned in my country. [0003] Diisooctyl terephthalate (DOTP) plasticizer has good electrical and thermal properties, and can replace DOP in PVC plastic electrical wire sheaths, and can also be used in the production of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/48C07C67/54C07C67/56C07C67/58C07C69/82
CPCC07C67/08C07C67/48C07C67/54C07C67/56C07C67/58C07C69/82
Inventor 曹正国李江华王福陈佳佳荆晓平周伟林
Owner JIANGSU ZHENGDAN CHEM IND CO LTD
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