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Synthesis method of 2-ethylhexyl salicylate

A technology of isooctyl salicylate and a synthesis method, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as no literature reports, and achieves easy operation, simple steps, Highly active effect

Inactive Publication Date: 2012-12-26
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Thanks to SO 4 2- / TiO 2 Has good catalytic activity, recently found that if in its preparation process such as WO 3 Promoter can make its catalytic performance better, and the use of composite solid superacid SO 4 2- / TiO 2 -WO 3 The research on the catalytic synthesis of isooctyl salicylate has not been reported in the literature

Method used

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  • Synthesis method of 2-ethylhexyl salicylate

Examples

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preparation example Construction

[0023] 1) Preparation of tungstic acid: Stir continuously in sodium tungstate and add to 1mol / L sulfuric acid solution, age and filter; wash with deionized water, dry at 100°C to obtain H 2 WO 4 solid, ground into powder;

[0024] 2) Amorphous TiO 2 ·nH 2 Preparation of O: TiCl 4 Dissolve in deionized water with continuous stirring in an ice bath, add concentrated ammonia water dropwise for hydrolysis, age and filter; wash with deionized water until Cl-free - , and then dried at 110 °C to obtain amorphous TiO 2 ·nH 2 O, ground into powder;

[0025] 3) Solid superacid SO 4 2- / TiO 2 -WO 3 Preparation: Take the H prepared above 2 WO 4 Powder and Amorphous TiO 2 ·nH 2 O powder mixed in a certain proportion (H 2 WO 4 The mass fraction is 10%), impregnated with dilute sulfuric acid solution, filtered, baked at 110°C for 3 hours, and then calcined at higher than 500°C to obtain an acid catalyst.

Embodiment 1

[0028] Weigh 33g Na 2 WO 4 2H 2 O, add to 50mL 1mol / L sulfuric acid solution deionized water with constant stirring, filter after aging. After washing with deionized water and drying at 100 °C, a yellow solid H 2 WO 4 , ground into powder; at the same time, measure 25mL TiCl 4 Dissolve in deionized water with continuous stirring in an ice bath, dropwise add concentrated ammonia water to hydrolyze until the solution is alkaline, filter after aging; wash with deionized water until Cl-free - , and then dried at 110 °C to obtain amorphous TiO 2 ·nH 2 O, ground into powder; weigh 2g H 2 WO 4 and 18g amorphous TiO 2 ·nH 2 O powder, mixed evenly, impregnated with 1mol / L sulfuric acid solution for 3h, filtered and baked at 110°C for 3h, then roasted at higher than 500°C to obtain solid super acid SO 4 2- / TiO 2 -WO 3 catalyst.

[0029] Add (13.8g, 0.1mol) salicylic acid and (50mL, 0.3mol) isooctyl alcohol into a 100mL three-necked flask, stir well, then add 2g of homema...

Embodiment 2

[0033] Add (13.8g, 0.1mol) salicylic acid and (50mL, 0.3mol) isooctyl alcohol into a 100mL three-necked flask, stir well, then add the solid superacid SO which was filtered and dried in Example 1 4 2- / TiO 2 -WO 3 Catalyst, heated to reflux at 190°C, reacted for 5h, stopped heating, cooled to room temperature, and filtered out the catalyst. After the filtrate was washed with hot water at 65°C, it was washed with saturated NaHCO 3 Wash until neutral, then wash with hot water. Separate the ester layer with anhydrous MgSO 4 Dry, filter with suction, distill under reduced pressure, collect the fraction with a boiling point of 84~86°C, and recover the excess solvent; collect the fraction at 172~174°C / 1.0kPa to obtain 20.5g of isooctyl salicylate product, with a yield of 81.9% ( as salicylic acid).

[0034] of the compound 1 The HNMR data are as follows:

[0035] 1 HNMR(DMSO)δ: 0.833~0.928(m, 6H, CH 3 ), 1.279~1.447 (m, 8H, CH 2 ), 1.684~1.714(m, 1H, CH), 4.242~4.255(d, 2...

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Abstract

The invention relates to a synthesis method of 2-ethylhexyl salicylate. According to the method, 2-ethylhexyl salicylate is synthesized from salicylic acid and isooctanol in the presence of solid superacid SO4<2-> / TiO2-WO3 as a catalyst under the backflow condition at temperature of 190 DEG C. The synthesis method has the advantages that the yield of 2-ethylhexyl salicylate is higher than 80%, the purity of 2-ethylhexyl salicylate is higher than 98%(GC), the superacid catalyst can be easily separated from a reaction system without causing environmental pollution or equipment erosion and can be reused, and the application prospect is high.

Description

technical field [0001] The present invention relates to a kind of synthetic method of isooctyl salicylate, specifically refer to take salicylic acid and isooctyl alcohol as raw material, utilize solid superacid SO 4 2- / TiO 2 -WO 3 As a catalyst for the synthesis of isooctyl salicylate. Background technique [0002] The chemical formula of 2-hydroxybenzoic acid-2-ethyloctyl (isooctyl salicylate) is as follows: [0003] [0004] Isooctyl salicylate (also known as 2-ethylhexyl salicylate), also known as isooctyl salicylate. As an important daily chemical product, it is a colorless to light yellow transparent liquid with a slightly aromatic smell, and is commonly used in the formulations of perfumes, soaps, cosmetics and sunscreens. It is a UV absorber that absorbs light with a wavelength near 300nm. Although its own ultraviolet absorption rate is not high, it is still widely used in sunscreen products, such as sunscreen cosmetics, sunscreen ointment, sunscreen fabrics...

Claims

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Application Information

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IPC IPC(8): C07C69/84C07C67/08
Inventor 孙柏旺毛秋霞
Owner SOUTHEAST UNIV
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