Method for catalyzing synthesizing diisooctyl azelate through load type heteropolyacid

A technology of diisooctyl azelate and heteropolyacid, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve problems such as poor product quality, complicated post-processing, environmental pollution, etc. Achieve the effects of improving esterification efficiency, shortening reaction time, and good demulsification

Inactive Publication Date: 2012-12-19
SICHUAN SIPO CHEMICAL CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0003] At present, the production methods of diisooctyl azelate include transesterification, direct esterification, and reduced-pressure esterification. These methods use protonic acid, super solid acid, oxide or inorganic salt as catalysts, and use azelaic acid as catalyst. It is prepared by esterification reaction of acid and isooctyl alcohol, and there are problems such as complicated post-processing, poor product quality, dark color, serious equipment corrosion, many side reactions, and environmental pollution.

Method used

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  • Method for catalyzing synthesizing diisooctyl azelate through load type heteropolyacid

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Effect test

Embodiment 1

[0018] A method for the catalytic synthesis of diisooctyl azelate by a loaded heteropolyacid, comprising the following steps:

[0019] Under the protection of high-purity nitrogen, mix 100kg of azelaic acid and 260kg of isooctyl alcohol, add 1.0kg of phosphotungstic acid loaded on silica, react at 170°C for 2 hours, then raise the temperature to 200°C for 4 hours to obtain azelaic acid The crude product of diisooctyl ester; the crude product of diisooctyl azelate is passed through a 500-mesh filter plate to remove the catalyst; the filtrate is heated to 170°C, the vacuum degree of the system is kept at 50Pa, and molecular distillation is carried out under reduced pressure for 50 minutes to finally obtain Isooctyl ester finished product. Its performance indicators are shown in Table 1.

Embodiment 2

[0021] Under the protection of high-purity nitrogen, mix 100kg of azelaic acid and 240kg of isooctyl alcohol, add 1.5kg of phosphomolybdic acid loaded on silica, react for 1 hour at 180°C, and react for 3 hours at 210°C to obtain azelaic acid The crude product of diisooctyl ester; the crude product of diisooctyl azelate is passed through a 400-mesh filter plate to remove the catalyst; the filtrate is heated to 185°C, the vacuum degree of the system is kept at 65Pa, and molecular distillation under reduced pressure is carried out for 60 minutes to finally obtain Isooctyl ester finished product. Its performance indicators are shown in Table 1.

Embodiment 3

[0023] Under the protection of high-purity nitrogen, mix 100kg of azelaic acid and 240kg of isooctyl alcohol, add 1.8kg of phosphomolybdic acid loaded on titanium dioxide, react at 160°C for 3 hours, and raise the temperature to 230°C for 1 hour to obtain azelaic acid diiso The crude product of octyl ester; the crude product of diisooctyl azelate is passed through a 600-mesh filter to remove the catalyst; the filtrate is heated to 200°C, the vacuum degree of the system is kept at 65Pa, and molecular distillation is carried out under reduced pressure for 60 minutes to finally obtain diisooctyl azelate Ester products. Its performance indicators are shown in Table 1.

[0024] Table 1 Diisooctyl azelate Performance Index

[0025]

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Abstract

The invention discloses a preparation method for producing diisooctyl azelate with load type heteropolyacid served as a catalyst, which is simple in technology, low in cost, and environment-friendly, and has good product quality. The technical scheme is that the method comprises the steps as follows: getting azelaic acid and isooctyl alcohol as the raw materials under the protection of high-purity nitrogen; getting the load type heteropolyacid as a catalyst; carrying out an esterification reaction at a certain temperature, so as to obtain a rough diisooctyl azelate product; processing the rough product by filtering and molecular distillation, and refining, thus obtaining the finished product of the diisooctyl azelate. The method disclosed by the invention is simple in technology, has a mild reaction temperature, good quality of the product, and has no pollution to the environment, and meanwhile, the yield of the product is up to 96%.

Description

technical field [0001] The invention relates to a preparation method of diisooctyl azelate, in particular to a method for preparing and synthesizing diisooctyl azelate by using a loaded heteropolyacid as a catalyst. Background technique [0002] Diisooctyl azelate is an excellent cold-resistant plasticizer, which has good compatibility with polyvinyl chloride, polystyrene, polyvinyl acetate, etc. It has low viscosity, high boiling point, high growth rate effect, low volatility and migration, excellent heat resistance, light resistance, oil resistance, electrical insulation, and is suitable for artificial leather, film, sheet, wire and cable sheathing, etc. , can give the product good low temperature performance. [0003] At present, the production methods of diisooctyl azelate include transesterification, direct esterification, and reduced-pressure esterification. These methods use protonic acid, super solid acid, oxide or inorganic salt as catalysts, and use azelaic acid a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/48C07C67/08
Inventor 冯自伟李哲先王娜苏军
Owner SICHUAN SIPO CHEMICAL CO LTD
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