Method for separating caprylic acid from mixture of caprylic acid and capric acid

A separation method and mixture technology, applied in the field of separation of caprylic acid, can solve the problems of high cost, and achieve the effects of facilitating industrial scale-up, low implementation cost and good repeatability

Inactive Publication Date: 2009-03-11
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the boiling point of octadecanoic acid is ab

Method used

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  • Method for separating caprylic acid from mixture of caprylic acid and capric acid
  • Method for separating caprylic acid from mixture of caprylic acid and capric acid

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0027] Example 1

[0028] In a 250ml round bottom flask equipped with a condenser reflux tube, 10.12g (0.078mol) 2-amino-5-chloropyridine, 10.03g of commercially available octyldecanoic acid (octanoic acid / decanoic acid=52.8 / 47.3) and 200ml methanol, heated to reflux with stirring for 1h, and cooled to room temperature. White crystals were obtained after 2 days, filtered (the filtrate was retained), recrystallized from methanol and filtered to obtain white crystals, washed with methanol 3 times (3×50ml), and dried naturally in the air.

[0029] 13 CNMR (125MHz, CDCl3, TMS): δ=179.53, 159.52, 152.63, 123.55, 111.34, 38.23, 31.52, 29.12, 28.89, 24.84, 22.81, 14.12. m.p.=37°C.

[0030] The above white crystals were dissolved in 50ml of 1N hydrochloric acid. The layered liquid is obtained, and the organic layer is octanoic acid (the aqueous phase is retained, and 2-amino-5-chloropyridine is recovered). After washing with 20ml saturated brine, anhydrous Na 2 SO 4 After drying, 4.92 g o...

Example Embodiment

[0034] Example 2

[0035] In a 500ml round bottom flask equipped with a condensing reflux tube, add 10.5g (0.11mol) 2-aminopyridine, 10.1g of commercially available octanodecanoic acid (52.8 / 47.3) and 100ml ethanol, and heat to reflux for 1h under stirring. , Cool to room temperature. White crystals were obtained after 1 day, filtered (the filtrate was retained), and white crystals were obtained by filtration after recrystallization from methanol, washed with methanol 3 times (3×50ml), and dried naturally in the air. The white crystals were dissolved in 50 ml of 1N hydrochloric acid to obtain a layered solution. The organic layer is octanoic acid (the aqueous phase is retained, and 2-aminopyridine is recovered). After washing with 200ml saturated brine, anhydrous Na 2 SO 4 After drying, 4.7 g of caprylic acid was obtained, with a yield of 88.1%, and its purity determined by liquid chromatography was 96.5%.

[0036] 13 CNMR (125MHz, CDCl3, TMS): δ=179.47, 34.26, 31.31, 29.07, 28.88...

Example Embodiment

[0039] Example 3

[0040]In a 1000ml round bottom flask equipped with a condenser reflux tube, 42.7g (0.45mol) 2-hydroxypyridine, 50.0g of commercially available octanodecanoic acid (52.8 / 47.3) and 500ml methanol were added respectively, and heated to reflux for 1h under stirring. , Cool to room temperature. White crystals were obtained after 2 days, filtered (the filtrate was retained), recrystallized from methanol and filtered to obtain white crystals, washed with methanol 3 times (3×50ml), and dried naturally in the air. The above white crystals were dissolved in 500 ml of 1N hydrochloric acid. A layered solution is obtained, and the organic layer is octanoic acid (the aqueous phase is retained, and the 2-hydroxypyridine is recovered). After washing with 100ml saturated brine, anhydrous Na 2 SO 4 After drying, 24.7 g of liquid caprylic acid was obtained, with a yield of 94.2%, and its purity was 95.3% by liquid chromatography.

[0041] 13 CNMR (125MHz, CDCl3, TMS): δ=179.59, 34...

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Abstract

The invention discloses a method for separating octanoic acid from a mixture of octanoic acid and decanoic acid. The separating method is as follows: in a resolution solvent, substitute pyridine fully reacts with the mixture of the octanoic acid and the decanoic acid at reflux temperature, and a compound crystal is separated out after cooling; after being recrystallized, the compound crystal crude product obtained after filtration is hydrolyzed by diluted hydrochloric acid the concentration of which is 2 percent to 10 percent, and is separated to obtain an aqueous layer A and an organic layer A which is washed and dried to obtain the monomer octanoic acid. Compared with the prior art, the method has the advantage of higher resolution efficiency. Due to the high selectivity of molecular recognition, the yield of the monomer octanoic acid can be between 80 and 95 percent and the purity can be between 95 percent and 99 percent only by crystallizing once. Besides, the method has simple operation, good repeatability and low implementation cost, and is advantageous to industrial expansion.

Description

(1) Technical field [0001] The invention relates to a method for separating caprylic acid from caprylic acid mixture. (2) Background technology [0002] As an important industrial raw material, the production and separation process of fatty acid has a long history. Over the years, most of the processes for separating fatty acids have been limited to relatively simple separation: that is, to separate saturated fatty acids from unsaturated fatty acids. The solid acid and liquid acid obtained after separation are still a mixture, which greatly limits the application of fatty acids. range, greatly reducing its application value. If a suitable method can be used to further separate the above-mentioned separated products into high-purity monomeric fatty acids, the use value of fatty acids can be greatly improved, and the development prospect is very promising. [0003] Monomer caprylic acid and capric acid are extremely important industrial raw materials in the manufacture of pr...

Claims

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Application Information

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IPC IPC(8): C07C53/126C07C51/487
Inventor 金志敏舒展陈伟良李王宗金卓军
Owner ZHEJIANG UNIV OF TECH
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