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Preparation method of hexyl n-caprylate

A technology of n-octanoic acid and hexyl ester, applied in the field of preparation of n-octanoic acid hexyl ester, can solve the problems of low yield of n-octanoic acid hexyl ester and high corrosion of equipment, and achieve the advantages of improving selectivity, increasing yield and reducing corrosiveness. Effect

Pending Publication Date: 2022-07-15
永华化学股份有限公司
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Problems solved by technology

But the yield of n-octanoic acid hexyl of above-mentioned preparation method is relatively low, generally lower than 60%; Due to the use of protonic acid simultaneously, the corrosivity to equipment is higher

Method used

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  • Preparation method of hexyl n-caprylate
  • Preparation method of hexyl n-caprylate
  • Preparation method of hexyl n-caprylate

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preparation example Construction

[0023] The invention provides a preparation method of hexyl n-octanoate, comprising:

[0024] After mixing n-octanoic acid, n-hexanol and tetrabutyl titanate, esterification reaction was performed to obtain hexyl n-octanoate.

[0025] In the present invention, n-octanoic acid and n-hexanol are preferably mixed and heated, and then tetrabutyl titanate is added to carry out an esterification reaction to obtain hexyl n-octanoate.

[0026] In the present invention, the ratio of the substance amounts of the n-octanoic acid and n-hexanol is preferably 1:(1.5-5), more preferably 1:(2-3). The present invention limits the amount of n-hexanol to be more than that of n-octanoic acid, so on the one hand, the reaction of n-octanoic acid is guaranteed to be complete; .

[0027] In the present invention, the temperature reached by the heating is preferably 110 to 130°C, and more preferably 120°C. In the present invention, the temperature to which the heating is performed is the temperatur...

Embodiment 1

[0038] 1. Synthesis reaction

[0039] 1.1 Feeding: add 291.4g of n-octanoic acid and 417g of n-hexanol in a 4-port glass reactor of 5L; feed nitrogen into the reaction mass for 1 minute, and after being heated to 120° C., add a catalyst (mass concentration is 10% tetramethyl titanate). n-hexanol solution of butyl ester) 4g, continue to heat up to 180 ℃, keep warm until no water droplets are produced in the oil-water separator, sample and analyze the acidity value, stop heating when the acidity is less than 0.1%, and terminate the reaction. (The material ratio of n-octanoic acid and n-hexanol is 1:2, and the mass of tetrabutyl titanate accounts for 0.056% of the total weight of the starting materials n-octanoic acid and n-hexanol)

[0040] 2. Purification

[0041] 2.1 Negative pressure dealcoholization

[0042] After the reaction, the crude product is subjected to negative pressure distillation to remove unreacted n-hexanol, the vacuum degree is controlled between 0.2 and 0.5...

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Abstract

The invention relates to the technical field of organic synthesis, and provides a preparation method of hexyl n-octanoate, which comprises the following steps: mixing n-caprylic acid, n-hexanol and tetrabutyl titanate, and carrying out esterification reaction to obtain the hexyl n-octanoate. According to the invention, the tetrabutyl titanate is used as a catalyst for the reaction, so that the selectivity of the product hexyl n-octoate is improved, and the yield of the hexyl n-octoate is improved; meanwhile, as the catalyst tetrabutyl titanate is almost non-corrosive, the corrosion of the catalyst to equipment in the preparation process is reduced. Experimental results show that by means of the preparation method, the yield of the hexyl n-octoate can reach 80% or above.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of hexyl n-octanoate. Background technique [0002] Hexyl n-octanoate naturally exists in apples, strawberries, bananas, grapes and other fruits, and its appearance is colorless or slightly yellow clear liquid, extremely insoluble in water, soluble in organic solvents such as ethanol, ether, oil, etc. T2760-2014 The edible flavors allowed by the Chinese food additive standard are mainly used for the preparation of edible flavors and daily chemical flavors. [0003] The traditional synthesis method of hexyl n-octanoate is as follows: using n-octanoic acid and n-hexanol as raw materials, and protonic acids such as concentrated sulfuric acid as catalysts for preparation. However, the yield of hexyl n-octanoate in the above preparation method is relatively low, generally lower than 60%; at the same time, due to the use of protonic acid, the...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/24B01J31/02
CPCC07C67/08B01J31/0275C07C69/24
Inventor 张路家
Owner 永华化学股份有限公司
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