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Process for preparing terpilenol

A technology of terpineol and turpentine, which is applied in the preparation of hydroxyl addition and organic chemistry, can solve the problems of cumbersome preparation of strongly acidic styrene-based cation exchange resin catalysts, high corrosiveness of acid catalysts, and low effective utilization rate, and achieve The effect of high product yield, simple post-processing steps and simplified production process

Inactive Publication Date: 2014-05-14
GUANGDONG SENYU FOREST CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] CN1482113A discloses a kind of turpentine mainly containing α-pinene as raw material, with low-carbon alcohol or ketone as solvent, adopts modified strongly acidic styrene series cation exchange resin as catalyst, and carries out catalytic hydration reaction through fixed bed reactor , a method for synthesizing L-α-terpineol in one step, in which the preparation of a strongly acidic styrene-based cation-exchange resin catalyst is very cumbersome
[0009] CN102992960A discloses a kind of preparation method of terpineol, uses α-pinene as raw material, one-step method directly synthesizes terpineol, adds industrial α-pinene, water, 98% sulfuric acid, and puts it in the reaction tank, Carry out hydration reaction at 70-80°C to produce crude terpineol, and then obtain terpineol product through fractionation; but its acid catalyst is highly corrosive to equipment, the reaction temperature is high, the risk is high, the effective utilization rate is low, and the recovery amount Big, not conducive to environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Raw material ratio is:

[0033]Turpentine with a pinene content of 60% 10kg

[0034] 35% phosphoric acid 1kg

[0035] O-15 type Pingping plus 0. 1kg;

[0036] The production process steps of terpineol are as follows: after feeding into the reactor according to the above formula, the temperature is raised to 60°C under stirring, the temperature is controlled and reacted for 5 hours, and the reaction is stopped; Wash with 5kg of water; after washing, let stand for stratification, recycle the water layer, add 0.1kg of hydrochloric acid with a mass fraction of 33% to the organic layer and stir for 1h, then add sodium carbonate to adjust the pH to 7.1, stand for stratification, Separate the water layer and solid, and then distill the remaining material (vacuum degree 0.098MPa), collect the fraction at 130-140°C, which is the product of terpineol. The yield of terpineol was 67.2%, and the purity of terpineol determined by HPLC was 98.2%. The product complies with the requ...

Embodiment 2

[0039] Raw material ratio is:

[0040] Turpentine with a pinene content of 76% 1kg

[0041] 40% phosphoric acid 0.12kg

[0042] O-10 type Pingping plus 0.01kg;

[0043] The production process steps of terpineol are as follows: after feeding into the reactor according to the above formula, the temperature is raised to 65° C. under stirring, the temperature is controlled for 6 hours, and the reaction is stopped; Wash with 0.5kg of water; after washing, let it stand for stratification, and recycle the water layer, add 0.01kg of hydrochloric acid with a mass fraction of 33% to the organic layer and stir for 1 hour, then add sodium carbonate to adjust the pH to 7.5, and let it stand for stratification , separate the water layer and solid, and then distill the remaining material (vacuum degree 0.098MPa), collect the fraction at 130-140°C, which is the terpineol product. The yield of terpineol was 67.8%, and the purity of terpineol determined by hplc was 98.4%. The product compli...

Embodiment 3

[0046] Raw material ratio is:

[0047] Turpentine with a pinene content of 95% 10kg

[0048] 45% phosphoric acid 1kg

[0049] 1631 0.05kg;

[0050] The production process steps of terpineol are as follows: after feeding into the reactor according to the above formula, the temperature is raised to 70° C. under stirring, the temperature is controlled for 4 hours, and the reaction is stopped; Wash with 5kg of water; after washing, let stand for stratification, and recycle the water layer, add 0.1kg of hydrochloric acid with a mass fraction of 33% to the organic layer and stir for 1 hour, then add sodium carbonate to adjust the pH to 7.9, stand for stratification, Separate the water layer and solid, and then distill the remaining material (vacuum degree 0.098MPa), collect the fraction at 130-140°C, which is the product of terpineol. The yield of terpineol was 71.8%, and the purity of terpineol determined by HPLC was 99.3%. The product complies with the requirements stipulated ...

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Abstract

The invention discloses a process for preparing terpilenol. The terpilenol can be synthesized by taking turpentine as a raw material and 35-45% in parts by weight of phosphoric acid as a catalyst in one step, and the content of dipentene in the turpentine can be increased to 12-20%. The invention further provides phosphoric acid loaded mesoporous gamma aluminum trioxide as a catalyst for further improving the yield. According to the technical scheme, the production process is simplified, the working intensity is alleviated, the danger and the production cost in production are alleviated, and an obtained product is high in yield and high in purity.

Description

technical field [0001] The invention relates to a production process of terpineol, in particular to a process for producing terpineol by a one-step reaction method. Background technique [0002] Terpineol, also known as terpineol, is a monocyclic monoterpene alcohol compound with the molecular formula C 10 h 18 O, with a molar molecular mass of 154.25, is insoluble in water, soluble in organic solvents such as ethanol, and slightly soluble in water and glycerin. Usually, terpineol products are a mixture of various isomers mainly composed of α-terpineol, β-terpineol, and γ-terpineol. Terpineol has a lilac aroma and is a green and environmentally friendly fine chemical product with a wide range of uses. It is often used as an industrial solvent, bactericide, cleaning agent, mineral flotation agent, blending essence, etc. In addition, terpineol is also It can be used in industries such as medicine, household and daily cleaning agents, inks, instruments, and telecommunication...

Claims

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Application Information

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IPC IPC(8): C07C33/14C07C29/08
CPCC07C29/08C07C2601/16C07C33/14
Inventor 莫树华林海权黄波涛黄石坚黄浩
Owner GUANGDONG SENYU FOREST CHEM