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Method for preparing diisobutyl phthalate

A technology of diisobutyl phthalate and phthalic anhydride, which is applied in the field of synthesizing diisobutyl phthalate, can solve the problems of high sewage treatment operation cost, shortened equipment life cycle, and increased production cost, etc. , achieve the effect of less waste water discharge, easy recycling and application, and reduce waste water discharge

Active Publication Date: 2019-10-15
ZHEJIANG JIANYE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of high-concentration organic wastewater has caused great difficulties to wastewater treatment, and the operating cost of sewage treatment is very high.
In addition, concentrated sulfuric acid has a serious corrosion effect on production equipment, which shortens the service life of equipment and increases production costs.

Method used

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  • Method for preparing diisobutyl phthalate
  • Method for preparing diisobutyl phthalate
  • Method for preparing diisobutyl phthalate

Examples

Experimental program
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Effect test

example 1

[0044] Example 1, the preparation of the magnetic nanoparticle-loaded acidic ionic liquid as catalyst:

[0045] 1) Obtain SiO2 2 @Fe 3 o 4 magnetic nanoparticles;

[0046] 2), [SO 3 H-pMIM-CPMS][HSO 4 ] acidic ionic liquid;

[0047] 3), magnetic nanoparticles loaded acidic ionic liquid

[0048] In 500ml of anhydrous toluene, add 30.0g of ferric oxide particles wrapped in silicon dioxide (SiO 2 @Fe 3 o 4 magnetic nanoparticles) and 15.0g [SO 3 H-pMIM-CPMS][HSO 4 ] Acidic ionic liquid, refluxed under nitrogen protection for 24h. Collect it with a magnet, wash it thoroughly with isopropyl ether (about 100-200 ml), and dry it under vacuum at 60° C. for 10 h; obtain an acidic ionic liquid loaded with magnetic nanoparticles.

[0049] Its structural formula is as follows:

[0050]

Embodiment 1

[0052] Embodiment 1, the method for preparing dibutylisobutyl phthalate:

[0053] S1. Add 148.1g (1mol) of phthalic anhydride, 275ml (3mol) of isobutanol, and 7.4g of catalyst into a 500ml three-necked flask. Heat (approximately 120-150° C.) for reflux dehydration, react for 4 hours, and cool the reaction solution to room temperature.

[0054] S2. Filter the reaction liquid after cooling S1 to room temperature, add 1.5 g of calcium oxide to the obtained filtrate I, and stir at room temperature for 1 h. Filtrate to obtain filtrate II and filter cake respectively, and the filter cake is washed with a small amount (about 15 ml) of isobutanol.

[0055] The washing liquid and the filtrate II were combined and dealcoholized under reduced pressure (heating under a pressure of less than 10 kPa to achieve isobutanol removal) to obtain 276.9 g of diisobutyl phthalate. The purity by gas phase analysis was 99.9%, and the yield was 99.5%.

[0056] The filter cake obtained by filtration ...

Embodiment 2

[0057] Embodiment 2, the method for preparing dibutylisobutyl phthalate:

[0058] S1. Add 148.1 g of phthalic anhydride, 184 ml (2 mol) of isobutanol, and 7.4 g of catalyst into a 500 ml three-necked flask. Heat (approximately 120-150° C.) for reflux dehydration, react for 4 hours, and cool the reaction solution to room temperature.

[0059] S2, is equal to S2 of embodiment 1.

[0060] 267.7 g of diisobutyl phthalate was obtained, the gas phase analysis purity was 99.4%, and the yield was 96.2%.

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Abstract

The invention discloses a method for preparing diisobutyl phthalate. The method comprises the following steps: 1, preparing a magnetic nanoparticle-supported acidic ionic liquid used as a catalyst; and 2, preparing the diisobutyl phthalate: carrying out refluxing dehydration condensation on phthalic anhydride and isobutanol under the catalysis of the magnetic nanoparticle-supported acidic ionic liquid for 3-6 h to obtain a diisobutyl phthalate reaction solution, cooling the reaction solution to room temperature, filtering the cooled reaction solution, adsorbing the obtained filtrate I by a solid alkali, performing filtration to obtain a filtrate II and a filter cake respectively, and carrying out reduced pressure dealcoholysis on the filtrate II to obtain the diisobutyl phthalate. The magnetic nanoparticle-supported acidic ionic liquid is used as the catalyst to achieve catalytic synthesis of the diisobutyl phthalate, so the method has the characteristics of high catalysis efficiency,easiness in recovery and reuse of the catalyst, simple process and less waste water discharge.

Description

technical field [0001] The invention relates to the field of plasticizer preparation, in particular to a method for synthesizing diisobutyl phthalate by using an acidic ionic liquid supported by magnetic nanoparticles as a catalyst. Background technique [0002] Diisobutyl phthalate is a good plasticizer, which has a strong dissolving ability for various resins. It is mainly used in the processing of polyvinyl chloride, which can make the product soft; it can be used as vinyl acetate, Plasticizer for alkyd resins, ethyl cellulose and neoprene; also used in the manufacture of paints, adhesives, artificial leather, printing inks, safety glass, dyes, pesticides, solvents for fragrances, and fabric lubricants. It has a wide range of uses and a large demand, and is currently the most commonly used plasticizer. [0003] The production of diisobutyl phthalate generally uses sulfuric acid as a traditional production process as a catalyst in China. This method has fast reaction spee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08B01J31/02B01J31/28C07C69/80
CPCC07C67/08B01J31/28B01J31/0295B01J2231/49C07C69/80
Inventor 陈钢冯烈陈云斌曹冬冬陈慧珍吴军
Owner ZHEJIANG JIANYE CHEM
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