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Preparation method of novel terpinyl acetate

A new technology of terpineol acetate, which is applied in the field of preparation of new terpineol acetate, can solve the problems of slow reaction rate of terpineol acetate, influence on reaction effect, inability to heat up and cool down the reaction kettle, etc., achieving ingenious design and reasonable method , good quality effect

Inactive Publication Date: 2018-10-02
新洲(武平)林化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing terpineol acetate has a slow reaction rate and cannot quickly heat up and cool down the reactor, thereby affecting the reaction effect. For this reason, the present invention proposes a novel preparation method of terpineol acetate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of preparation method of novel terpineol acetate proposed by the present invention comprises the following steps,

[0020] S1, add terpineol and acetic anhydride to the high-efficiency reaction kettle at one time, add phosphoric acid under constant stirring, and after fully stirring, add SnCl at room temperature 4 ·5H 2 O, to be SnCl 4 ·5H 2 After O is completely dissolved, slowly heat up and react under stirring;

[0021] S2, after cooling the reaction solution to room temperature, add Na 2 CO 3 Neutralize H 3 PO 4 and SnCl 4 , by Na 2 CO 3 The neutralized reaction solution is directly distilled to evaporate most of the acetic acid;

[0022] S3, the liquid after distilling off the acetic acid was washed twice with 6% NaOH solution, then washed twice with saturated brine to remove residual acetic acid, and fractionated to obtain terpineol acetate product after being neutral.

[0023] In the present invention, the high-efficiency reaction kettle is mad...

Embodiment 2

[0028] A kind of preparation method of novel terpineol acetate proposed by the present invention comprises the following steps,

[0029] S1, add terpineol and acetic anhydride to the high-efficiency reaction kettle at one time, add phosphoric acid under constant stirring, and after fully stirring, add SnCl at room temperature 4 ·5H 2 O, to be SnCl 4 ·5H 2 After O is completely dissolved, slowly heat up and react under stirring;

[0030] S2, after cooling the reaction solution to room temperature, add Na 2 CO 3 Neutralize H 3 PO 4 and SnCl 4 , by Na 2 CO 3 The neutralized reaction solution is directly distilled to evaporate most of the acetic acid;

[0031] S3, the liquid after distilling off acetic acid is washed 3 times with 7% NaOH solution, and then washed 3 times with saturated brine to remove residual acetic acid, and fractionate after neutralization to obtain terpineol acetate product.

Embodiment 3

[0033] A kind of preparation method of novel terpineol acetate proposed by the present invention comprises the following steps,

[0034] S1, add terpineol and acetic anhydride to the high-efficiency reaction kettle at one time, add phosphoric acid under constant stirring, and after fully stirring, add SnCl at room temperature 4 ·5H 2 O, to be SnCl 4 ·5H 2 After O is completely dissolved, slowly heat up and react under stirring;

[0035] S2, after cooling the reaction solution to room temperature, add Na 2 CO 3 Neutralize H 3 PO 4 and SnCl 4 , by Na 2 CO 3 The neutralized reaction solution is directly distilled to evaporate most of the acetic acid;

[0036] S3, the liquid after evaporating acetic acid was washed 3 times with 8% NaOH solution, and then washed 3 times with saturated brine to remove residual acetic acid, and fractionated to obtain terpineol acetate product after being neutral.

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PUM

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Abstract

The invention discloses a preparation method of novel terpinyl acetate. The method comprises the steps as follows: S1, terpilenol and acetic anhydride are added to an efficient reactor once, phosphoric acid is added under the continuous stirring condition, sufficient and uniform stirring is performed, SnCl4.5H2O is added at the room temperature, and after the SnCl4.5H2O is completely dissolved, the obtained mixture is slowly heated and reacts under the stirring condition; S2, a reaction liquid is cooled to the room temperature, Na2CO3 is added to neutralize H3PO4 and SnCl4, the reaction liquidneutralized by Na2CO3 is directly distilled, and most acetic acid is distilled out; S3, the liquid with acetic acid distilled out is washed with a 6%-8% NaOH solution 2-4 times and then washed with asaturated saline solution 2-4 times, residual acetic acid is removed, fractionation is performed after the liquid is neutral, and a terpinyl acetate product is obtained. The design is ingenious, themethod is reasonable, and the obtained product is high in purity, good in quality and suitable for promotion.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of novel terpineol acetate. Background technique [0002] Terpineol acetate is the esterification product of terpineol. It has a delicate and sweet fragrance, like bergamot and lavender, and the fragrance lasts for a long time. This product is widely used in daily flavors such as lavender, spicy, and citrus flavors, as well as edible flavors such as white lemon, cherry, spicy, and meaty flavors. It plays a role in enhancing spicy flavors in seasoning essential oils. Raw material of oil, lavender oil, orange leaf oil, etc. [0003] Terpineol acetate is a food spice that is allowed to be used in my country's "Hygienic Standards for the Use of Food Additives". It is used to prepare fruit-type food flavors such as red bayberry, cherry, citrus, peach, and spices. The dosage in chewing gum is 14~260mg / kg; meat 1.7~40mg / kg; seasoning 15mg / kg; baked food...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/145B01J19/18B01J19/02
CPCC07C67/08B01J19/02B01J19/18B01J2219/00081C07C2601/16C07C69/145
Inventor 朱志文
Owner 新洲(武平)林化有限公司
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