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Preparation method of Kunlun musk

A kunlun musk and vacuuming technology, which is applied in the direction of organic chemistry, can solve the problems that affect the final product quality of kunlun musk, greatly affect the product refining and purification, and affect the effect of depolymerization reaction, so as to achieve good catalytic effect, improve product quality, The effect of reducing energy consumption

Pending Publication Date: 2020-08-07
绵阳三香汇生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The second type of method is relatively complicated in the use of chemical reagents and involves the flammable and explosive substance sodium alkoxide, so the operation risk is high, and it is basically no longer used in industry at present.
[0010] However, in the current technology, this type of method still has the following problems: 1. The temperature of the polycondensation reaction is high, usually at 180-200 ° C, and side reactions are prone to occur; 2. The degree of polymerization is not controlled in the polycondensation reaction, or it is controlled too much Relatively rough, affecting the effect of subsequent depolymerization reactions, and ultimately affecting product quality; 3. The depolymerization reaction catalyst components are complex, and most of the depolymerization catalysts reported in current literature and patents are composite depolymerization catalysts, composed of aluminum carbonate, p-toluenesulfonic acid , silicotungstomolybdenum acid, anhydrous copper sulfate and water, etc., the composition is complex, which has a great influence on the subsequent refining and purification of the product; 4. The depolymerization temperature is high, usually at 250-300 °C, and the depolymerization temperature in the later stage is even It will rise to 300~325℃
Obtaining the aroma of Kunlun musk product like this has burnt smell, which seriously affects the quality of Kunlun musk final product

Method used

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  • Preparation method of Kunlun musk
  • Preparation method of Kunlun musk

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] 1. Feeding

[0046] First put 360kg of ethylene glycol into the polycondensation reactor; then add 1200kg of tridecanedioic acid from the manhole of the reactor, and then add 450kg of ethylene glycol; vacuumize to 100mmHg, and return to normal pressure with nitrogen.

[0047] 2. Polycondensation reaction

[0048]Turn on the cooling water of the condenser and raise the temperature to 120°C without stirring; continue to heat until there is reflux, and then start stirring again, at this time the temperature of the kettle is about 138°C; it takes 3 hours to raise the temperature of the kettle from 138°C to 170°C , the top temperature is 120°C, about 225kg of water is distilled out, and the water is collected as waste water and enters the collection tank; then the vacuum is evacuated to 200mmHg at a speed of 3mmHg / min, and the temperature of the kettle is kept at 170°C during the process, and the top temperature is about 128°C. About 330kg of water / ethylene glycol is distil...

Embodiment 2

[0060] 1. Feeding

[0061] First put 210kg of ethylene glycol into the polycondensation reactor; then add 1200kg of tridecanedioic acid from the manhole of the reactor, and then add 450kg of ethylene glycol; vacuumize to 100mmHg, and return to normal pressure with nitrogen.

[0062] 2. Polycondensation reaction

[0063] Turn on the cooling water of the condenser and raise the temperature to 120°C without stirring; continue to heat until there is reflux, and then start stirring again, at this time the temperature of the kettle is about 138°C; it takes 3 hours to raise the temperature of the kettle from 138°C to 170°C , the top temperature is 120°C, about 225kg of water is distilled out, and the water is collected as waste water and enters the collection tank; then the vacuum is evacuated to 200mmHg at a speed of 3mmHg / min, and the temperature of the kettle is kept at 170°C during the process, and the top temperature is about 128°C. About 200kg of water / ethylene glycol is disti...

Embodiment 3

[0075] 1. Feeding

[0076] First put 360kg of ethylene glycol into the polycondensation reactor; then add 1200kg of tridecanedioic acid from the manhole of the reactor, and then add 450kg of ethylene glycol; vacuumize to 100mmHg, and return to normal pressure with nitrogen.

[0077] 2. Polycondensation reaction

[0078] Turn on the cooling water of the condenser and raise the temperature to 120°C without stirring; continue to heat until there is reflux, and then start stirring again, at this time the temperature of the kettle is about 138°C; it takes 3 hours to raise the temperature of the kettle from 138°C to 180°C , the top temperature is 125°C, about 230kg of water is distilled out, and the water is collected as waste water and enters the collection tank; then the vacuum is evacuated to 200mmHg at a speed of 3mmHg / min, and the temperature of the kettle is kept at 180°C during the process, and the top temperature is about 130°C. About 330kg of water / ethylene glycol is disti...

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Abstract

The invention discloses a preparation method of Kunlun musk, which includes steps of with alpha,omega-tridecanedioic acid and ethylene glycol as raw materials, preparing the Kunlun musk through low-temperature polycondensation reaction and low-temperature depolymerization reaction. The condensation polymerization reaction only needs 170 DEG C, wherein titanium isopropoxide is used as a depolymerization catalyst with cooperation of an entrainer ethylene glycol, so that the depolymerization reaction temperature only needs 220-240 DEG C, which is greatly reduced than that inthe prior art. Compared with a traditional Kunlun musk preparation method, the method has the advantages that the yield is high, conditions are mild, the purity of the obtained Kunlun musk product is larger than or equal to 99%, the fragrance is purer, bad offensive odor such as burnt smell is avoided, and the quality is better.

Description

technical field [0001] The invention relates to the field of kunlun musk production technology, in particular to a preparation method of kunlun musk. Background technique [0002] Musk, known as the king of spices, is the best in the spice family with its pure, rich and long-lasting fragrance. At present, the world's annual output of synthetic musk fragrances has exceeded 10,000 tons, of which 3,000 to 4,000 tons are high-grade macrocyclic musks. [0003] Among them, Kunlun musk (n-tridecanedioic acid cycloethylene ester) is the main species of macrocyclic musk, which has a strong fragrance-fixing effect and good diffusivity. Among the essences of high-end perfumes or high-end cosmetics, Kunlun musk is only Need to add 1% amount, you will receive obvious effect. [0004] Kunlun musk is widely used as a blending spice, and can be used in cologne, cosmetics, shampoo, detergent, etc. Because it is stable in alkali, it can also be used in soap essence. [0005] At present, ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D321/00
CPCC07D321/00
Inventor 不公告发明人
Owner 绵阳三香汇生物科技有限公司
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