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Preparation method of dodecanol benzoate

A technology of dodecyl alcohol ester and benzoic acid, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of difficult separation of catalysts, easy carbonization of reaction liquids, and deep color of products, and achieves a solution to the problem. It is not easy to separate from the product, easy to industrialize production, light color effect

Inactive Publication Date: 2014-03-05
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of using sulfuric acid as a catalyst include corrosion of equipment, easy carbonization of the reaction solution, deep color of the product, difficulty in separating the catalyst, and large amount of waste water.

Method used

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  • Preparation method of dodecanol benzoate
  • Preparation method of dodecanol benzoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Preparation of zirconia nanotube-supported zirconium sulfate catalyst

[0021] Prepare a mixed solvent with formamide and glycerol at a volume ratio of 1:1, and then add NH 4 F and H 2 O, prepared with 1%NH 4 F and 1%H 2 A mixed solution of O, the mixed solution is used as the electrolyte, the zirconium sheet (purity greater than 97%) is used as the anode, the platinum sheet (99.99% purity) is used as the cathode, the distance between the electrodes is 2 cm, anodized at room temperature for 3 hours at a voltage of 50V, Oxide is formed on the surface of the zirconium sheet. After the reaction, the oxide is peeled off from the zirconium sheet, washed with water, dried, and annealed at 500° C. for 1 hour to obtain a zirconia nanotube carrier. Dissolve 1.86g of zirconium sulfate in 5g of aqueous solution containing 0.03% sulfuric acid, then add 1.0g of zirconia nanotube support, ultrasonically impregnate for 1 hour, dry, and bake at 400°C for 1 hour to prepare the c...

Embodiment 2

[0026] (1) Preparation of catalyst

[0027] The catalyst was prepared according to the steps of Example 1(1).

[0028] (2) Preparation of Lauryl Benzoate

[0029] Add 18.4g of dodecyl alcohol and 11.5g of benzoic acid into the reactor, add 0.6g of catalyst, heat up to 180°C for 3.5 hours, cool, filter and recover the catalyst to obtain the product dodecyl benzoate, the conversion rate of benzoic acid is 97.4 %.

Embodiment 3

[0031] (1) Preparation of catalyst

[0032] The catalyst was prepared according to the steps of Example 1(1).

[0033] (2) Preparation of Lauryl Benzoate

[0034] Add 18.4g of dodecyl alcohol and 11.5g of benzoic acid into the reactor, add 0.6g of catalyst, heat up to 200°C for 2.5 hours, cool, filter and recover the catalyst to obtain the product dodecyl benzoate, the conversion rate of benzoic acid is 97.5 %.

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Abstract

The invention relates to a preparation method of dodecanol benzoate, which comprises the following step: adding dodecanol and benzoic acid into a reactor; and then adding catalyst, controlling the mass ratio of the dodecanol to the benzoic acid to the catalyst to 18.4 to 11.5 to 0.6; and then heating up to 180-200 degrees centigrade to react for 2.5-3.5 hours; then cooling, filtering and recycling the catalyst to obtain the product dodecanol benzoate, wherein the catalyst is zirconium sulfate catalyst loaded by zirconium oxide nanotube. According to the preparation method, the zirconium sulfate catalyst loaded by the zirconium oxide nanotube is used as the catalyst; the zirconium sulfate catalyst loaded by the zirconium oxide nanotube is solid acid catalyst, thus overcoming the defects of device corrosion, easy carbonization of reaction solution and dark color of the product caused by using sulfuric acid as the catalyst. The dodecanol benzoate prepared by the invention is clear, transparent, light in color and high in quality and the conversation rate can be 96% or higher.

Description

Technical field: [0001] The invention belongs to the field of cosmetics, and relates to a preparation method of lauryl benzoate. technical background: [0002] Lauryl benzoate is a kind of oil with excellent performance. It is safe, non-toxic, non-irritating, not easy to rancidity, strong solubility, resistant to temperature changes, has affinity and permeability to the skin, and has antioxidant properties , Widely used in the production of cosmetics, can be used in moisturizing cream, lipstick, mascara, massage oil, nail polish, milk and so on. [0003] Lauryl benzoate is mainly prepared by the esterification reaction of benzoic acid and dodecyl alcohol, and sulfuric acid is generally used as a catalyst, such as the report in "Surfactant Industry" (1995, 2: 48-49). The main disadvantages of using sulfuric acid as a catalyst include corrosion of equipment, easy carbonization of the reaction solution, deep color of the product, difficulty in separating the catalyst, and larg...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/78C07C67/08B01J27/053
CPCY02P20/584
Inventor 王西新赵建玲侯晓蕊白丽云唐成春
Owner HEBEI UNIV OF TECH