A kind of isobornyl acetate synthetic catalyst and the synthetic method of isobornyl acetate

A kind of technology of isobornyl acetate and synthesis method, which is applied in the field of synthesis of isobornyl acetate, can solve the problems of low catalyst usage, low selectivity of target product, large amount of waste water, etc., and achieve broadening of sources, short reaction time, The effect of improving the utilization rate

Active Publication Date: 2020-04-03
云南森美达生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Before the 1970s, sulfuric acid was used as a catalyst in the industrial synthesis of isobornyl acetate from camphene, which would generate a large amount of waste water during subsequent product treatment and washing, so there was a big problem
However, there are generally disadvantages such as low catalyst usage and low selectivity of target products.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Step 1: Mix 10 grams of mordenite with 100 grams of 20% zinc acetate aqueous solution, heat to 90°C-100°C and stir for 5h-7h;

[0027] Step 2: filter the mixed solution after stirring, and roast and activate the obtained mordenite at 550° C. to 650° C. for 3 hours to 5 hours to obtain a mordenite-supported zinc acetate catalyst;

[0028] Step 3: Add 40g of raw material oil (containing 47.2% amphene), 10g of glacial acetic acid and 1g of mordenite-supported zinc acetate catalyst into the reaction flask, and stir and react at 50°C for 6h; the reaction liquid contains 1.2% of amphene by gas chromatography. %, camphene conversion rate 97.5%, isobornyl acetate 41.7%; isobornyl acetate selectivity is 90.7%;

[0029] Step 4: The reaction solution was filtered to recover the mordenite-supported zinc acetate catalyst, and the oil phase was distilled under reduced pressure to obtain a chromatographic content of isobornyl acetate of 98.7%.

Embodiment 2

[0031] Step 1: Mix 10 grams of mordenite with 50 grams of 30% copper acetate aqueous solution, heat to 90°C-100°C and stir for 5h-7h;

[0032] Step 2: filter the mixed solution after stirring, and roast and activate the obtained mordenite at 550° C. to 650° C. for 3 hours to 5 hours to obtain a mordenite-supported copper acetate catalyst;

[0033] Step 3: Add 40g of raw oil (containing 63.8% amphene), 12g of glacial acetic acid and 0.4g of mordenite-supported copper acetate catalyst into the reaction flask, and stir and react at 65°C for 4h; the reaction liquid is detected to contain amphene by gas chromatography 1.3%, camphene conversion rate 98.0%, isobornyl acetate 56.8%; isobornyl acetate selectivity 90.9%;

[0034] Step 4: The reaction solution was filtered to recover the mordenite-supported copper acetate catalyst, and the oil phase was distilled under reduced pressure to obtain a chromatographic content of isobornyl acetate of 99.2%.

Embodiment 3

[0036] Step 1: Mix 10 grams of mordenite with 70 grams of 25% cobalt acetate aqueous solution, heat to 90°C-100°C and stir for 5h-7h;

[0037] Step 2: filter the mixed solution after stirring, and roast and activate the obtained mordenite at 550° C. to 650° C. for 3 hours to 5 hours to obtain a mordenite-supported cobalt acetate catalyst;

[0038] Step 3: Add 40g of raw oil (containing 80.3% amphene), 16g of glacial acetic acid and 0.8g of mordenite-supported cobalt acetate catalyst into the reaction flask, and stir and react at 60°C for 5h; the reaction liquid is detected to contain amphene by gas chromatography 1.4%, camphene conversion rate 98.3%, isobornyl acetate 71.9%; isobornyl acetate selectivity 91.1%;

[0039] Step 4: The reaction solution was filtered to recover the mordenite-supported cobalt acetate catalyst, and the oil phase was distilled under reduced pressure to obtain a chromatographic content of isobornyl acetate of 99.3%.

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PUM

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Abstract

The invention discloses a catalyst for synthesizing isobornyl acetate, and is characterized in that a preparation method of the catalyst comprises the following steps: step 1, mixing mordenite with a Lewis acid water solution, heating the mixed solution to 90DEG C-100DEG C and stirring the mixed solution for 5h-7h; and step 2, filtering the stirred mixed solution, calcining the obtained mordenite at 550DEG C-650DEG C for activating the mordenite for 3h-5h to obtain a Lewis acid-loaded mordenite catalyst. The invention also provides a synthetic method of isobornyl acetate, and the isobornyl acetate is synthesized by adopting the catalyst. By adopting the scheme of the invention, the isobornyl acetate is synthesized under the catalysis of the catalyst disclosed by the invention, the conversion rate of the raw material oil camphene is as high as above 97%, the selectivity on the isobornyl acetate is above 91%, and the utilization ratio of the raw material oil is greatly improved; and the synthetic method of isobornyl acetate has the advantages of simple operation, environment friendliness, low production cost and the like.

Description

technical field [0001] The invention relates to a method for synthesizing isobornyl acetate, in particular to a catalyst for synthesizing isobornyl acetate and a method for synthesizing isobornyl acetate. Background technique [0002] Isobornyl acetate, also known as white ethyl ester, hexyl acetate, English aliases isobornyl acetate, Acetic acid isobornyl ester, isomethyl lonone (CAS NO 125-12-2), is an important chemical intermediate, mainly used for synthesis Camphor, essence and spices, etc. Isobornyl acetate is used as a fragrance because of its fragrance and pine leaf odor. It is used in cosmetics, soaps, indoor disinfectants, indoor air fresheners, indoor spray essences, bath essences, and raw materials for talcum powder. As a fine chemical intermediate, isobornyl acetate is irreplaceable in downstream industries, with a high annual growth rate of market demand and good economic benefits. [0003] Before the 1970s, sulfuric acid was used as a catalyst in the industr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/24B01J37/08B01J31/26C07C67/04C07C69/14
CPCB01J29/24B01J31/26B01J37/08C07C67/04C07C69/14Y02P20/584
Inventor 崔军涛梁兴华汪锦航邱安彬李强
Owner 云南森美达生物科技股份有限公司
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