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Method for catalytic synthesis of nopol

A nopol alcohol and co-catalyst technology, which is applied in the field of spice preparation, can solve the problems of low utilization rate of paraformaldehyde, non-conservation and environmental protection, low yield of nopol alcohol, etc., to achieve selectivity and yield improvement, and production cost The effect of reducing and increasing the conversion rate

Inactive Publication Date: 2015-10-21
江西创赢香精香料科技协同创新有限公司
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Problems solved by technology

[0007] Although the above synthesis reaction about Nopol alcohol has achieved relatively ideal results, the utilization rate of paraformaldehyde is low, the yield of Nopol alcohol is still low, there are many by-products, high consumption, large pollution, and do not meet the requirements of saving and environmental protection. Require

Method used

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  • Method for catalytic synthesis of nopol

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Experimental program
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Effect test

Embodiment 1

[0025] Add 1000g of β-pinene, 200g of paraformaldehyde, and 7.5g of zinc chloride into a 2L reactor with a reflux condenser. The temperature was raised to 125°C, the stirring speed was 300 r / min, and the reaction was completed under normal pressure for 12 hours. Reduce the temperature of the material in the kettle to room temperature, filter after static precipitation, and obtain the crude product of Nopol alcohol, and rectify the crude product of Nopol alcohol to obtain a finished product with a content of more than 98%. In terms of paraformaldehyde, its selectivity is 89.6%, and the yield is 70.5%. .

Embodiment 2

[0027] Add 1000g of β-pinene, 200g of paraformaldehyde, and 7.5g of zinc chloride into a 2L reaction kettle. The temperature was raised to 125°C, the stirring speed was 300 r / min, and the pressure inside the kettle was 0.3 MPa. After 12 hours of reaction, the reaction was terminated. Lower the temperature of the material in the kettle to room temperature, and after the reaction solution is allowed to stand for stratification, the product is pressed out with nitrogen, and the crude product of Nopol alcohol is obtained by filtering after standing for the second time, and the crude product of Nopol alcohol is rectified to obtain a The finished product, in terms of paraformaldehyde, has a selectivity of 93.5% and a yield of 84.9%.

Embodiment 3

[0029] Add 1000g of β-pinene, 200g of paraformaldehyde, 7.5g of zinc chloride and 7.5g of aluminum trichloride into a 2L reaction kettle in sequence. The temperature was raised to 125° C., the stirring speed was 300 r / min, and the pressure inside the kettle was 0.3 MPa. After 10 hours of reaction, the reaction was terminated. Reduce the temperature of the material in the kettle to room temperature, and press out the product with nitrogen to obtain the crude product of Nopol alcohol. The crude product of Nopol alcohol is rectified to obtain a finished product with a content greater than 98%. In terms of paraformaldehyde, its selectivity is 96.7%, and the yield 92.5%.

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Abstract

The invention discloses a method for catalytic synthesis of nopol. The method comprises the steps of: using beta-pinene and paraform as raw materials, wherein the reaction is performed under the condition of closed pressure, using zinc chloride as a main catalyst, using stannic chloride, niobic acid and aluminum trichloride as an auxiliary catalyst, and performing catalyzing so as to prepare the nopol. The dosage of the catalyst is 0.3%-3% of the quality of beta-pinene, the dosage of the paraform is 5%-50% of the quality of the beta-pinene, the quality ratio of the main catalyst to the auxiliary catalyst is 10:1-1:1, the reacting temperature is 80-160 DEG C, the stirring speed is 100-300 r / min, the reacting time is 5-15h, and the intensity of pressure is 0.1-0.5MPa. Under the condition, according to paraform, the selectivity of the reaction is higher than 95%, the yield is higher than 90%, and the fragrance of the nopol product is good.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals and relates to a method for preparing spices. Background technique [0002] Nobutol has a soft woody aroma with camphor and mint notes, with a slightly linalool-like note. Nopol alcohol can be used in cosmetics and flavor formulations, mainly for the preparation of woody fragrance. Apart from this, it is also mainly used in the preparation of nopol acetate, a more widely used spice. [0003] In recent years, the establishment of high-purity β-pinene production from continuous distillation of turpentine has laid the foundation for the utilization of β-pinene. Nopol alcohol usually uses β-pinene and paraformaldehyde as raw materials, using Lewis acid or solid acid as a catalyst, and the hydroxymethylated product-nopol alcohol can be obtained through Prince condensation reaction. [0004] At present, most researches on the synthesis of Nopol alcohol focus on the selection of catalysts and r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/14C07C29/38
CPCC07C29/38C07C2602/42C07C33/14
Inventor 章志福任向荣俞忠华
Owner 江西创赢香精香料科技协同创新有限公司
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