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Litsea cubeba nucleolus deep-processing and comprehensive utilization process

A technology for deep processing of litsea cubeba seeds, which is applied in the field of deep processing and comprehensive utilization of litsea cubeba kernel kernels, can solve the problems of high catalyst cost, long reaction time, and high equipment requirements, and achieve short reaction time, high reaction conversion rate, The effect of comprehensive utilization of resources

Active Publication Date: 2008-12-24
YONGZHOU SAMSHIANG FLAVOURS & FRAGRANCES CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of liquid acid and alkali catalysts will produce a large amount of waste water discharge, causing environmental pollution; the separation of enzyme catalysis and heterogeneous catalysis products is relatively simple, but the reaction time is longer, and the catalyst cost is higher; the use of supercritical fluid technology, the reaction rate is fast, The yield is high, the separation and purification of the product is simple, and the adaptability to oil raw materials is good, but the method needs to be carried out under high temperature and high pressure, and the requirements for equipment are quite high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Get 410 grams of acid value 42mg / KOH as Litsea cubeba kernel, directly crush to 50-500 mesh, use 500 milliliters of 120# solvent gasoline (produced by Guangdong Maoming Petrochemical Refinery) as solvent to extract Litsea cubeba kernel by Soxhlet method 100 grams of oil; then 100 grams of Litsea cubeba kernel oil, 30 grams of methanol, 3 grams of anhydrous sodium sulfate and 1 gram of concentrated sulfuric acid are mixed and added to a stirring reactor for lipid-lowering reaction, and the reaction temperature is controlled at 70 ° C. The time is controlled at 1 hour; after the reaction stops, add 1.5 grams of anhydrous sodium carbonate to the mixed solution and continue to heat to 70 ° C, and stir for 1 hour to make the system neutral; and use vacuum distillation to recover methanol, and then raise the temperature to 130 ℃ decompression distillation to remove the water in the system, cooling, centrifugation and recovery of solid salt, the acid value was 1.7mg / KOH; then t...

Embodiment 2

[0033]Take 410 grams of acid value 42mg / KOH as Litsea cubeba kernel, directly crush to 50-500 mesh, use 500 milliliters of petroleum ether (boiling range 60-90°C) as solvent to extract Litsea cubeba kernel oil 100 by Soxhlet method gram; Then 100 grams of Litsea cubeba kernel oil, 50 grams of methanol, 5 grams of anhydrous sodium sulfate and 1 gram of concentrated sulfuric acid are mixed and added to the stirring reactor to carry out lipid-lowering reaction, the reaction temperature is controlled at 85 ° C, and the reaction time is controlled After 1.5 hours; after the reaction stopped, add 1.5 grams of anhydrous sodium carbonate to the mixture and continue heating to 70°C, and stir for 1 hour to make the system neutral; and recover methanol by vacuum distillation, and raise the temperature to 130°C after recovering methanol Remove the water in the system by distillation under reduced pressure, cool, and centrifuge to reclaim the solid salt, and the acid value is 1.6mg / KOH; the...

Embodiment 3

[0035] Get 410 grams of acid value 42mg / KOH as Litsea cubeba kernel, directly crush to 50-500 mesh, use 500 milliliters of 120# solvent gasoline as solvent to extract 100 grams of Litsea cubeba kernel oil by Soxhlet method; then 100 grams Litsea cubeba kernel oil, 30 grams of methanol, 3 grams of anhydrous sodium sulfate and 1 gram of concentrated sulfuric acid are mixed and added to the stirring reactor for lipid-lowering reaction. The reaction temperature is controlled at 80 ° C, and the reaction time is controlled at 2 hours; the reaction is stopped Add 1.5 grams of anhydrous sodium carbonate to the mixed solution and continue heating to 70°C, stir for 1 hour to make the system neutral; and recover methanol by vacuum distillation, raise the temperature to 130°C to remove the water in the system by vacuum distillation , cooling, centrifugation reclaims solid salt, records acid value and is 1.63mg / KOH; Then filtrate, methyl alcohol, phase transfer catalyst triethylbenzyl ammon...

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PUM

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Abstract

The invention provides a technique for deeply processing and comprehensively utilizing of a litsea cubeba kernel. In the invention, the litsea cubeba kernel is crushed and subject to heated reflux extraction in a Soxhlet extractor for 0.5 to 4 hours by taking a low boiling point nonlinear solvent as an extraction solvent, and the litsea cubeba kernel oil is obtained; the obtained litsea cubeba kernel oil, methanol, concentrated sulfuric acid and anhydrous sodium sulfate are mixed according to the ratio of 100:(between15 and 50):(between 1and 2):(between 3 and 5) and then put in a reaction kettle for degreaseing reaction, after the reaction, the mixed liquid are added with the anhydrous sodium sulfate to neutralize the sulphuric acid so as to obtain solid salt, by the reduced pressure distillation, the methanol is recovered and the moisture is dried, and the solid salt is removed by centrifugation; the obtained filtrate, the methanol, a phase transfer catalyst and sodium hydroxide are mixed according to the ratio of 100:(between15 and 50):(between 0.1 and 1):(between 0.5 and 2) and then put in the reactor reaction kettle for ester exchange reaction, after the reaction, the concentrated sulfuric acid are added to neutralize the sodium hydroxide, the obtained mixed liquid are kept stand and layered, the upper layer of coarse biodiesel is subject to the reduced pressure distillation to obtain the finished biodiesel, and the lower layer of the methanol and the glycerin are vaporized to recover the methanol for repeated use.

Description

[technical field] [0001] The invention relates to a new technology for deep processing and comprehensive utilization of litsea cubeba nucleolus. [Background technique] [0002] After the Litsea Cube Seeds are steam-distilled to prepare high-value-added Litsea Cube Seed Essential Oil, a large amount of Litsea Cube Seed Nucleolus remains, which seriously pollutes the environment. At present, a very small amount of litsea cubeb kernels are used to process litsea cubeba kernel oil, which can be used in daily chemical products instead of coconut oil after decolorization and degumification. However, due to the low added value and low conversion rate, there is no industrialization report at present, so a large number of litsea cubeba kernels are generally discarded as waste, resulting in a great waste of resources. There are many patented methods for preparing biodiesel from rapeseed oil, soybean oil, gutter oil and other oils, mainly including acid catalysis, alkali catalysis, en...

Claims

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Application Information

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IPC IPC(8): C11B1/10C11C3/00C11C3/10C10G3/00C07C31/04C07C31/22C05F5/00
CPCY02A40/20Y02E50/10Y02E50/30Y02P30/20Y02W30/40
Inventor 钟世安陈谦文蔡海清朱骏周明达蒋群丁荣李念
Owner YONGZHOU SAMSHIANG FLAVOURS & FRAGRANCES CORP
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