CN101892123A - Ultrasonic-assisted extraction method for tung oil - Google Patents

Abstract

The invention discloses an ultrasonic-assisted extraction method for tung oil, and relates to a method for extracting the tung oil. The method comprises the following steps of: (1) preparing tung tree seeds; (2) crushing the tung tree seeds; (3) performing ultrasonic-assisted extraction; (4) processing oil cake once according to the step (3) to obtain filtrate and combining the filtrate and the filtrate obtained in the step (3); and (5) performing reduced pressure distillation on the tung oil. The method has a simple process and can rapidly and efficiently extract the tung oil from the oil tree fruits in an energy saving way, and the obtained tung oil has the advantages of high yield, bright color and high stability, so the method solves the problems of low efficiency and energy consumption of deep processing technology, dark color of the tung oil, unstable properties, easy conversion from alpha-eleostearic acid into beta-eleostearic acid, high protein loss in the oil cake and the like in the tung tree processing of China; and the method provides guarantee for the deep processing of the tung oil, promotes the development of the tung tree industry of China and is suitable for the extraction of all tung oil.

Description

A kind of method of ultrasonic-assisted extraction tung oil

Technical field

The present invention relates to extract the method for tung oil, relate in particular to a kind of method of ultrasonic-assisted extraction tung oil.Being specifically related to a kind of is raw material with the tung oil tree fruit, extracts the greasy technology of tung oil, belongs to agriculture and forestry product and adopts the post-treatment technical field, and tung oil is mainly used in industries such as building, chemical industry, electronics and the energy.

Background technology

Tung oil is special product of China, and China is maximum in the world tung oil producing country and export State, enjoys a very good reputation in the world always.Tung oil is a kind of good siccative oil, because various fields such as that special chemical structure makes it is synthetic in coating manufacturing, resin, resin modified and tackiness agent preparation have a wide range of applications.At present, the preparation method of tung oil is the extracting method of continuing to use edible oil basically, is mainly milling process and lixiviation process.Milling process obtains a mao tung oil by the shelling of paulownia seed, pulverizing, steaming being fried, squeezing, and filters then and obtains product.By high temperature squeezing and baking seed, polymerization easily takes place in three conjugated double bonds in the tung oil main component eleostearic acid, thereby cause in the reduction of waste, tung oil quality of oil sources and the oil meal that protein component is destroyed etc., the tung oil colourity of gained is dark, impurity and water-content height.There is shortcoming such as carry that speed oil is slow, oil yield is low, length consuming time, solvent consumption are big in conventional lixiviation process.The limitation of ordinary method makes that the extraction cost of tung oil is too high, and the quality instability needs further refining.

Ultrasonic wave is meant that frequency is 2 * 10 ⁴～10 ⁹The sound wave of Hz.Because it is short and beam strong and be easy to by focusing on concentrated energy that ultrasonic wave has wavelength, so the effect between it and medium can be divided into 3 kinds of calorifics mechanism, mechanics of machinery mechanism and cavitation mechanism.Extract grease by the intensified by ultrasonic wave that adopts certain frequency, power, the result shows that under the essentially identical condition of oil extracting rate, ultrasound-enhanced extraction can reduce the extraction temperature, shortens extraction time, save solvent load, and can improve greasy quality.

Ultrasonic extraction technology has been applied in the preparation of vegetative grease, but up to the present, does not also have the using ultrasound ripple to extract the ripe normalization technique of tung oil.

Summary of the invention

The objective of the invention is to overcome the shortcoming and defect that prior art exists, a kind of method of ultrasonic-assisted extraction tung oil is provided,, optimize extraction process, realize efficient, the quick and economic extraction of tung oil promptly by ultrasonic wave auxiliary extraction tung oil.

The object of the present invention is achieved like this:

Comprise the underpressure distillation of fragmentation, ultrasonic wave auxiliary extraction and the tung oil of the producing of starting material tung oil tree seed, tung oil tree seed.

Specifically, the present invention includes the following step:

1. the tung oil tree seed produces

Selected sophisticated tung oil tree fruit obtains the tung oil tree seed by removal shell, kind skin;

2. the fragmentation of tung oil tree seed

The tung oil tree seed placed in 120 ℃ the loft drier and dried of poor quality ± 0.5% before and after the oven dry 1.5～2 hours; The cooling back is broken, obtains tung oil tree kind powder of seeds;

3. ultrasonic wave auxiliary extraction

Tung oil tree kind powder of seeds and ethyl acetate are pressed following mixed:

Tung oil tree kind powder of seeds: ethyl acetate=1g: 10ml;

Be sealed in the container, use ultrasonic wave continuous action 1.5～2 hours down at 40～50 ℃ then;

With the mixture suction filtration, remove the solid residue oil meal, collect filtrate;

4. 3. oil meal is carried out once according to step, obtain the 3. gained filtrate merging of filtrate and step;

5. the underpressure distillation of tung oil

Filtrate by Rotary Evaporators underpressure distillation under the negative pressure of 40 ℃ and 0.06～0.08Mp, is obtained tung oil.

Principle of work of the present invention is as follows:

Ultrasonic wave is meant that frequency is 2 * 10 ⁴～10 ⁹The sound wave of Hz, the vibration number height of its per second has exceeded the human auditory system upper limit (20000Hz).Ultrasonic wave has been widely used in industry fields such as medicine, electromechanics, light textile, chemical industry, food and the energy.Ultrasonic wave has the effect of ultrasound of a series of mechanics, calorifics, electromagnetism and chemistry, as mechanical effect, cavitation effect, heat effect and chemical effect etc.Wherein hyperacoustic cavitation effect has quickened the leaching of effective ingredients in plant, and its second-order effect such as mechanical vibration, emulsification, spreads, smashes the diffusion that also can quicken effective constituent with chemical effect etc. and discharge.In addition, ultrasonic wave also has additive effects such as turbulence effect, perturbation effect, interfacial effect and cavity effect.These effects make ultrasonic wave when the activeconstituents of extracting substance, not only can shorten extraction time, save solvent load, and can improve portioned product character.Therefore, utilize the ultrasonic-assisted extraction technology can be than more efficient, energy-conservation and from the tung oil tree fruit, extract tung oil apace.

Experiment showed, the present invention compared with prior art, have the following advantages and positively effect:

1, the ultrasonic wave auxiliary law is compared with milling process, and technology is simpler, less energy consumption, and the more transparent clarification of gained tung oil color, impurity is few, and acid number is little, and water-content is low, the α in the tung oil-eleostearic acid content height, extraction yield can improve 5～10%;

2, the ultrasonic wave auxiliary law is compared with ordinary organic solvents leaching method, and the cycle is short, and it is low to extract temperature, and solvent load is few, has reduced production cost.

3, technological process of the present invention is simple, can from the tung oil tree fruit, extract tung oil quick, efficient, energy-conservationly, the tung oil productive rate height of gained, bright, the good stability of color and luster, solved China tung oil tree processing deep processing technology poor efficiency, power consumption, the tung oil color and luster is dark, character is unstable, α-eleostearic acid easily changes in β-eleostearic acid, the oil meal problems such as the protein loss is big into;

4, give security for the deep processing of tung oil, promote the development of China's tung oil tree industry, be applicable to the extraction of all tung oil.

Embodiment

Describe in detail below in conjunction with embodiment:

1, extracts the experiment of tung oil method

1. selected sophisticated tung oil tree fruit obtains tung oil tree seed 6.04g by removal shell, kind skin;

2. will plant the tung oil tree seed and in 120 ℃ loft drier, dry 1.5～2 hours, of poor quality ± 0.5% before and after the oven dry.The cooling back is broken, obtains tung oil tree kind powder of seeds;

3. tung oil powder of seeds and ethyl acetate are placed triangular flask by the mixed of 1g: 10ml, be placed on 40 ℃ after the sealing down with ultrasonic wave continuous actions 1.5 hours; With the mixture suction filtration, remove the solid residue oil meal, collect filtrate;

4. 3. oil meal is carried out once according to step, obtain the 3. gained filtrate merging of filtrate and step;

5. with filtrate by Rotary Evaporators underpressure distillation under the negative pressure of 40 ℃ and 0.06～0.08Mp, obtain tung oil 3.92g.

2, to extracting the determination experiment of tung oil index

Physical and chemical indexs such as content to density, refractive power, saponification value, acid number and the moisture of extraction tung oil are measured, and the tung oil that extracts with milling process relatively, and its result is as shown in table 1.

Table 1 tung oil physico-chemical property test result

Table?1?The?phycochemical?properties?of?tung?oil

As seen from table, the nature difference of the tung oil that tung oil that the ultrasonic extraction method obtains and milling process obtain is little, in some properties, and ultrasonic extraction method even be better than milling process, for example outward appearance and acid number.

By gas chromatographic analysis, main lipid acid is made up of myristic acid, palmitinic acid, oleic acid, linolic acid, linolenic acid, eleostearic acid, arachidonic acid, mountain Yu acid and erucic acid etc. in the tung oil that extracts, account for 98.774% of all the components, and unsaturated fatty acids accounts for 97.77% of fatty acid total amount, and wherein eleostearic acid content accounts for 78.62% of total fatty acids total amount.

Claims (1)

1. the method for a ultrasonic-assisted extraction tung oil is characterized in that comprising the following steps:

1. the tung oil tree seed produces

Selected sophisticated tung oil tree fruit obtains the tung oil tree seed by removal shell, kind skin;

2. the fragmentation of tung oil tree seed

The tung oil tree seed placed in 120 ℃ the loft drier and dried of poor quality ± 0.5% before and after the oven dry 1.5～2 hours; The cooling back is broken, obtains tung oil tree kind powder of seeds;

3. ultrasonic wave auxiliary extraction

Tung oil tree kind powder of seeds and ethyl acetate are pressed following mixed:

Tung oil tree kind powder of seeds: ethyl acetate=1g: 10ml;

Be sealed in the container, use ultrasonic wave continuous action 1.5～2 hours down at 40～50 ℃ then;

With the mixture suction filtration, remove the solid residue oil meal, collect filtrate;

4. 3. oil meal is carried out once according to step, obtain the 3. gained filtrate merging of filtrate and step;

5. the underpressure distillation of tung oil

Filtrate by Rotary Evaporators underpressure distillation under the negative pressure of 40 ℃ and 0.06～0.08Mp, is obtained tung oil.