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Preparation method of dioctyl phthalate based on acidic eutectic solvent

A technology of dioctyl phthalate and low eutectic solvent, which is applied in the field of preparation of dioctyl phthalate, can solve the problems of many side reactions, polluted environment by acidic waste water, difficult product separation, etc., and achieves improved yield. The effect of rate and purity

Active Publication Date: 2020-04-14
广州逸仙科技有限公司
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AI Technical Summary

Problems solved by technology

[0003] Traditional DOP synthesis usually uses concentrated sulfuric acid, p-toluenesulfonic acid or titanate as a homogeneous catalyst, and there are many problems such as many side reactions, acid waste water polluting the environment, and difficult product separation.

Method used

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  • Preparation method of dioctyl phthalate based on acidic eutectic solvent

Examples

Experimental program
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Effect test

preparation example Construction

[0038] see figure 1 , the preparation method specifically includes the following steps:

[0039] S1: Carry out monoesterification with phthalic anhydride and excess isooctyl alcohol as raw materials to obtain a mixture of monoester and isooctyl alcohol; the reaction temperature of monoesterification is 80~150°C, and the reaction time is 5~120 minutes.

[0040] S2: adding a deep eutectic solvent to the mixture obtained in step S1, performing first-stage esterification, and then standing and layering to obtain an upper organic phase and a lower aqueous phase;

[0041] S3: adding a deep eutectic solvent to the organic phase obtained in step S2, performing second-stage esterification, and then standing and stratifying to obtain an upper organic phase and a lower aqueous phase;

[0042] S4: adding a deep eutectic solvent to the organic phase obtained in step S3, performing third-stage esterification, and then standing and stratifying to obtain an upper organic phase and a lower aq...

Embodiment 1

[0056] according to figure 1 The flow chart in the test is carried out, 3 kg of phthalic anhydride and 6.59 kg of isooctyl alcohol are added to the pre-reactor PR, heated to 120 ° C, stirred and reacted for 20 min under normal pressure, and then the reaction liquid enters the first-stage esterification reactor R1 , while adding 1.92kg of 2-methylimidazole-benzenesulfonic acid as a deep eutectic solvent, stirring and reacting at 120°C and normal pressure for 7 h. After the reaction, the reaction liquid was added to the decanter D1 and allowed to stand for stratification, and the standing time was 3 h. After separating the upper layer (ester phase) obtained after the phase separation in the decanter D1, it enters the second-stage esterification reactor R2, and at the same time, 1.24 kg of imidazole-p-toluenesulfonic acid deep eutectic solvent is added, at 120 ° C And continue to stir the reaction under normal pressure for 7 h. After the reaction, the reaction solution was adde...

Embodiment 2

[0061] according to figure 1 The flow chart in the test is carried out, 3 kg of phthalic anhydride and 6.59 kg of isooctyl alcohol are added to the pre-reactor PR, heated to 120 ° C, stirred and reacted under normal pressure for 20 min, and then the reaction liquid enters the first-stage esterification reactor R1, At the same time, 2.40 kg of 2-methylimidazole-benzenesulfonic acid was added as a deep eutectic solvent, and the reaction was stirred at 120° C. and normal pressure for 6.5 h. After the reaction, the reaction liquid was added to the decanter D1 and allowed to stand for stratification, and the standing time was 3 h. After separating the upper layer (ester phase) obtained after the phase separation in the decanter D1, it enters the second-stage esterification reactor R2, and at the same time, 1.64 kg of imidazole-p-toluenesulfonic acid deep eutectic solvent is added, at 120 ° C And continue stirring reaction under normal pressure for 6.5 h. After the reaction, the r...

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Abstract

The invention relates to a preparation method of dioctyl phthalate based on an acidic eutectic solvent. The preparation method comprises the following steps: using phthalic anhydride and iso-octyl alcohol as raw materials, and carrying out esterification reactions in an eutectic solvent to generate dioctyl phthalate; wherein the eutectic solvent is composed of a hydrogen bond receptor and a hydrogen bond donor according to a molar ratio of 1: 1-8, the hydrogen bond receptor is imidazole or an imidazole derivative, and the hydrogen bond donor is sulfonic acid. The invention also relates to a synthesis system used in the preparation method. The preparation method provided by the invention has the advantages of high DOP yield and purity.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of dioctyl phthalate. Background technique [0002] Dioctyl phthalate (DOP) is the plasticizer species with the largest capacity, output and consumption among phthalates, and is currently the most widely used plasticizer with good comprehensive performance. Compared with other plasticizers, it has the advantages of high growth rate, wide adaptability, good chemical stability, easy access to raw materials, simple production process, and low cost. It is an ideal primary plasticizer. [0003] Traditional DOP synthesis usually uses concentrated sulfuric acid, p-toluenesulfonic acid or titanate as a homogeneous catalyst, which has many problems such as many side reactions, acid waste water pollution, and product separation difficulties. Therefore, improving the preparation method of DOP to enhance environmental protection, simplify the post-treatment process, and...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/80B01J31/02C07C67/58C07C67/48
CPCB01J31/0225B01J31/0244B01J2231/49C07C67/08C07C67/48C07C67/58C07C69/80
Inventor 叶银梅蔡文培林洁锋王娟
Owner 广州逸仙科技有限公司
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