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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 above 200°C, the cost of separation is relatively high

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

Embodiment 1

[0028] In a 250ml round bottom flask equipped with a condensing reflux tube, add 10.12g (0.078mol) 2-amino-5-chloropyridine, commercially available octadecyl mixed acid (caprylic acid / capric acid=52.8 / 47.3) 10.03g and 200ml of methanol was heated to reflux for 1h with stirring, and cooled to room temperature. After 2 days, white crystals were obtained, filtered (the filtrate was retained), recrystallized from methanol and filtered to obtain white crystals, washed 3 times with methanol (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 50 ml of 1N hydrochloric acid. A layered liquid was obtained, and the organic layer was octanoic acid (the aqueous phase was retained, and 2-amino-5-chloropyridine was recovered). After washing with 20ml saturated brine, anhydrous Na 2 SO 4 After drying, 4.9...

Embodiment 2

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

[0036] 13 CNMR (125MHz, CDCl3, TMS): δ=179.47, 34.26, 31.31, 29.07, 28.88, 24.87, 22.45, 14.12.

[0...

Embodiment 3

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

[0041] 13 CNMR (125MHz, CDCl3, TMS): δ=179.59, 34.38, 31.66, ...

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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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