CN101967426A - Preparation process and system for ultrasonic reinforced supercritical CO2 extraction of tussah pupa oil - Google Patents

Preparation process and system for ultrasonic reinforced supercritical CO2 extraction of tussah pupa oil Download PDF

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CN101967426A
CN101967426A CN 201010510729 CN201010510729A CN101967426A CN 101967426 A CN101967426 A CN 101967426A CN 201010510729 CN201010510729 CN 201010510729 CN 201010510729 A CN201010510729 A CN 201010510729A CN 101967426 A CN101967426 A CN 101967426A
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tussah
extraction
pupal fat
supercritical
ultrasound
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王朝臣
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Abstract

The invention relates to a preparation process for ultrasonic reinforced supercritical CO2 extraction of tussah pupa oil. The process comprises the following steps of: (1) pre-treating raw materials, namely sorting, cleaning, sterilizing and freeze-drying tussah pupas and crushing the tussah pupas into tussah pupa powder by adopting a high-speed crusher; (2) putting the tussah pupa powder obtained in the step (1) into an extraction kettle, opening a CO2 gas bottle when the temperature reaches 40 to 50 DEG C to blow gas, adjusting the flow when the extraction pressure reaches 18 to 25MPa, and extracting the tussah pupa oil for 60 to 120 minutes at constant temperature under constant pressure; (3) emitting ultrasonic wave to the supercritical CO2 fluid in the extraction kettle by adopting a built-in insertion ultrasonic reinforcing mode in the step (2) to reinforce the tussah pupa oil extraction process; and (4) collecting the tussah pupa oil at the outlet of a separation kettle. The preparation process can remarkably improve the production efficiency, save the production cost and reduce the production energy consumption, and has large-scale industrialized application prospect. The invention also relates to an ultrasonic reinforced supercritical CO2 extraction system for the tussah pupa oil. The system has the predominant advantages of reasonable design, convenience for control, high production efficiency, low energy consumption and the like.

Description

Tussah pupal fat ultrasound-enhanced supercritical CO 2The preparation technology and the system of extraction
Technical field
The present invention relates to functional foodstuff preparation technology, particularly a kind of tussah pupal fat ultrasound-enhanced supercritical CO 2The preparation technology and the system of extraction.
Background technology
21 century, insect will become the third-largest protein source that is only second to microorganism and cell biological.The insect functional foodstuff is the focus of 21 century world's food circle development, and its trophicity, functional the consistent of domestic and international expert that obtained are approved.Insect heat is about to begin.
Tussah is the very high spun silk insect of a kind of economic worth, belongs to Arthropoda, Insecta, lepidopteran, Saturniidae, pass through ovum, larva, pupa, and four period of metamorphosis of adult are a kind of holometabolous insects.The insect of Saturniidae can be rated as the giant in the insect world, and the individuality that it is very large is more suitable for edible and processing.
Cocoon chrysalis belongs to food, medicine homology insect, and its edibility and health-care treatment are proved.Dried cocoon chrysalis amount of total fat is about about 31%, contains abundant unsaturated fatty acids, and oleic acid, linolenic and linoleic have vision protection, increase intelligence, delay senility, effect such as blood fat reducing.Tussah pupal fat health-care effect is of high nutritive value well, has very high utility value.At present the research of tussah pupal fat is still sentenced the starting stage, traditional milling process, solvent-extraction process prepare the tussah pupal fat can not effectively solve the problem of functional substance sex change, if can work out intensive processing technology, will widen purposes, form industrialization, promote the sustainable development of tussah industry, promptly carry forward the national treasure Chinese medicine masses that benefit the society again.
Breeding silkworms is purpose with the filature of cocooing always, and the consumption of tussah, is functionally seldom utilized by people, studies very few.In recent years, along with the exploitation of chemical fibre, the occupation rate of silk in textile industry descends year by year.The tussah producing region is all in the mountain area, and silkworm raiser's income descends year by year, and the tussah industry is atrophy year by year.How developing the tussah resource is a great problem that tussah producing region peasant faces, and is worth us to think deeply again.
Problems such as cocoon chrysalis is the characteristic resources of China, exists the deep processing degree low at present, and industrialization level is not high, resources advantage is not converted into product advantage and economic advantages.The tussah pupal fat has good trophicity, functional, still is in the starting stage both at home and abroad, does not add modern advanced complete processing.About the complete processing of tussah pupal fat, domestic have only supercritical CO 2The simple research of extraction (SCE), its effect is also bad, and extraction yield and cost are undesirable, there is no other people research at present.
Supercutical fluid is supercritical CO especially 2(SC-CO 2) have quality product height, environmentally friendly, nontoxic, characteristics such as do not burn, be widely used at aspects such as material, chemical industry, medicine, food.But SC-CO 2Problems such as the time that exists in extraction process is long, pressure is high, extraction temperature is higher have limited its extensive commercial application.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of tussah pupal fat ultrasound-enhanced supercritical CO is provided 2The preparation technology of extraction has the production efficiency height, saves and produce the advantage that rises this and reduce production energy consumption.
The present invention solves its technical problem and is achieved through the following technical solutions:
A kind of tussah pupal fat ultrasound-enhanced supercritical CO 2The preparation technology of extraction, it is characterized in that: this preparation technology's step is:
(1). raw materials pretreatment: cocoon chrysalis adopts high speed disintegrator to be ground into the cocoon chrysalis powder through sorting, cleaning, sterilization, lyophilize;
(2). step (1) gained cocoon chrysalis powder is put into extraction kettle, when temperature reaches 40-50 ℃, open CO 2Gas cylinder is supplied gas, and when extracting pressure reaches 18-25MPa, regulates flow, at constant temperature and pressure extraction tussah pupal fat 60-120min;
(3). in step (2) process, adopt the ultrasound-enhanced mode of built-in insert, the supercritical CO in extraction kettle 2Fluid emission ultrasonic wave is strengthened tussah pupal fat extraction process;
(4). collect the tussah pupal fat from the separating still exit.
And described cocoon chrysalis powder is 90~110 orders.
And described ultrasonic frequency is 16kHz~24kHz, and power density is 80W/L~120W/L, the ultrasound wave irradiation mode be the intermittent time/the continuous irradiation time is 4s/4s~8s/8s.
The present invention also provides a kind of tussah pupal fat ultrasound-enhanced supercritical CO 2Extracting system, it has reasonable in design, is convenient to control, production efficiency height, outstanding advantage such as energy consumption is low.
A kind of tussah pupal fat ultrasound-enhanced supercritical CO 2Extracting system is characterized in that: by the CO that connects successively by pipeline 2Gas cylinder, cleaner, storage tank, mixing tank, high-pressure pump, extraction kettle, separating still constitute the transmitting terminal of the ultrasonic convertor of plug-in mounting in extraction kettle.
Advantage of the present invention and beneficial effect are:
1. the present invention is applied to advanced person's ultrasound-enhanced technology in the complete processing of tussah pupal fat, with supercritical CO 2Extraction (SCE) cocoon chrysalis oil phase ratio, ultrasound-enhanced supercritical CO 2Extraction (USCE) tussah pupal fat can obviously reduce the temperature of SCE tussah pupal fat, shortens the extraction time, reduces extracting pressure, improves the extraction yield of tussah pupal fat.
2. tussah pupal fat ultrasound-enhanced supercritical CO of the present invention 2Extraction (USCE) preparation technology can significantly improve production efficiency, saves production cost and reduce production energy consumption, has the heavy industrialization Application Prospect.
3. tussah pupal fat ultrasound-enhanced supercritical CO of the present invention 2Outstanding advantages such as extraction (USCE) preparation system by ultrasonic tr-ansducer is installed, thereby can significantly improve tussah pupal fat extraction yield in supercritical extraction reactor, have reasonable in design, is convenient to control, and efficient height, energy consumption are low.
Description of drawings
Fig. 1 is the schema of tussah pupal fat ultrasound-enhanced supercritical CO2 extracting system of the present invention;
Fig. 2 is the experimental result broken line graph of extraction temperature to the influence of SCE and USCE tussah pupal fat yield;
Fig. 3 extracts the experimental result broken line graph of time to the influence of SCE and USCE tussah pupal fat yield;
Fig. 4 extracting pressure is to the experimental result broken line graph of the influence of SCE and USCE tussah pupal fat yield;
Fig. 5 cocoon chrysalis powder fineness is to the experimental result broken line graph of the influence of SCE and USCE tussah pupal fat yield.
Embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
A kind of tussah pupal fat ultrasound-enhanced supercritical CO 2The preparation technology of extraction, it is characterized in that: this preparation technology's step is:
(1). raw materials pretreatment: produce tussah with Dandong City, Liaoning Province and belong to tussah kind cocoon chrysalis, kind is " Chinese People's Anti-Japanese Military and Political College ", and cocoon chrysalis adopts high speed disintegrator to be ground into 90~110 order cocoon chrysalis powder through sorting, cleaning, sterilization, lyophilize.
(2). step (1) gained cocoon chrysalis powder is put into extraction kettle, when temperature reaches 40-50 ℃, open CO 2Gas cylinder is supplied gas, and when extracting pressure reaches 18-25MPa, regulates flow, at constant temperature and pressure extraction tussah pupal fat 60-120min.
(3). in step (2) process, adopt the ultrasound-enhanced mode of built-in insert, the supercritical CO in extraction kettle 2Fluid emission ultrasonic wave is strengthened tussah pupal fat extraction process, and ultrasonic frequency is 16kHz~24kHz, and power density is 80W/L~120W/L, the ultrasound wave irradiation mode be the intermittent time/the continuous irradiation time is 4s/4s~8s/8s; Optimal conditions is: ultrasonic frequency is 20kHz, and power density is 100W/L, the ultrasound wave irradiation mode be the intermittent time/the continuous irradiation time is 6s/6s.
(4). collect the tussah pupal fat from the separating still exit.
A kind of tussah pupal fat ultrasound-enhanced supercritical CO 2Extracting system is by the CO that connects successively by pipeline 2Gas cylinder 1, cleaner 2, storage tank 3, mixing tank 5, high-pressure pump 7, extraction kettle 8, separating still 10 constitutes, and separating still adopts two.The transmitting terminal of the ultrasonic convertor 9 of plug-in mounting in extraction kettle.At CO 2The exit end of gas cylinder, storage tank, high-pressure pump all is equipped with control valve, and tensimeter 4 all is installed on storage tank, extraction kettle, separating still.The separating still export pipeline all is equipped with control valve.Electric heater unit is installed in the storage tank.Terminal separating still is connected with cleaner by pipeline, makes CO 2Gas backstreaming is equipped with under meter 6 on the pipeline.
Below to ultrasound-enhanced supercritical CO 2Extraction (USCE) and supercritical CO 2The comparison that experimentizes of the extraction yield of extraction (SCE) cocoon chrysalis oil making technology.
Tussah pupal fat extraction yield method of calculation
The supercentrifuge centrifugal condition is: 8000 rev/mins, 20 minutes, remove impurity, moisture etc., and the gained extract is the tussah pupal fat.Tussah pupal fat extraction yield calculation formula is:
V = A B × 100 %
In the formula: V is the extraction yield; A is the cocoon chrysalis weight of oil of extraction after centrifugal; B is an extraction kettle dress sample cocoon chrysalis grain weight amount.
Experimental result
1. extraction temperature is to the influence of tussah pupal fat extraction yield
In the extraction time is that 90min, extracting pressure are that 20MPa, fineness are under the 100 purpose conditions SCE and USCE tussah pupal fat to be experimentized, and the results are shown in Figure 2.Extraction temperature is to the favourable aspect of the influence of SCE: along with the rising of temperature, the chance that contacts with solvent increases, and molecular thermalmotion speeds up, and the rising of temperature makes CO 2Viscosity reduce, spread coefficient increases, mass transfer velocity is accelerated; Extraction temperature is to the unfavorable aspect of SCE: temperature raises and causes CO 2Density reduce, the solubleness of solute is descended, cause the decline of percentage extraction.The too high sex change that can influence functional substance in the tussah pupal fat of temperature, so temperature is unsuitable too high, for SCE, the suitable extraction temperature of tussah pupal fat is 50 ℃.
For USCE, add ultrasonic field the extraction yield of tussah pupal fat is obviously raise, under lower extraction temperature, still can obtain higher extraction yield.Ultrasonicly can produce the mechanical wave effect, especially this effect shows more obviously near critical temperature, effect that can reinforcing mass transfer, and ultrasonic when in medium, propagating, and ultrasonic vibrational energy constantly is absorbed and is converted into heat energy, makes SC-CO 2The mass transfer temperature raise, speed up, the result shows that the optimal temperature of USCE tussah pupal fat is 45 ℃.
2 extraction times are to the influence of tussah pupal fat extraction yield
In extraction temperature is that 45 ℃, extracting pressure are that 20MPa, fineness are under the 100 purpose conditions SCE and USCE tussah pupal fat to be experimentized, and the results are shown in Figure 3.Along with the prolongation of extraction time, effect of extracting is become better and better.The extraction rate curve of initial stage USCE tussah pupal fat is higher than SCE, along with both difference of prolongation of time reaches unanimity.When the time surpassed 90min, the extraction rate curvilinear trend of USCE tussah pupal fat tended towards stability.Therefore, the optimum extraction time of USCE is 90min.
3. extracting pressure is to the influence of tussah pupal fat extraction yield
In extraction temperature is that 45 ℃, extraction time are that 90min, fineness are under the 100 purpose conditions SCE and USCE tussah pupal fat to be experimentized, and the results are shown in Figure 4.As seen from Figure 4, for SCE and USCE, the extraction yield of tussah pupal fat all increases with the rising of pressure, but the trend that USCE rises below 20MPa is faster.For SCE, the extraction yield of tussah pupal fat raises with pressure and is the near-linear rising, illustrates that pressure is remarkable to the influence of tussah pupal fat percentage extraction in 30MPa; For USCE, extracting pressure is in 15MPa the time, and the extraction yield of tussah pupal fat is similar to SCE to the relation of pressure, but reaches 20MPa when above when pressure, and slope of a curve is on a declining curve, illustrates that this moment, pressure reduced the influence degree of percentage extraction.Therefore, the best extracting pressure of USCE is 20MPa.
4. the cocoon chrysalis powder fineness is to the influence of tussah pupal fat extraction yield
In extraction temperature is that 45 ℃, extraction time are that 90min, extracting pressure are under the condition of 20MPa SCE and USCE tussah pupal fat to be experimentized, and the results are shown in Figure 5.As seen from Figure 5, along with the increase of fineness, effect of extracting is become better and better; When fineness surpassed 100 orders, trend tended towards stability.It is not obvious that the extraction rate curve of USCE is compared SCE, and the extraction rate of SCE when 100 orders are following rises obviously, and Fig. 5 shows that the optimum fineness of USCE is 100 orders.
Experimental result shows that extraction has strengthening effect to ultrasonic wave to SCE.With SCE cocoon chrysalis oil phase ratio, USCE tussah pupal fat can obviously reduce the temperature of SCE tussah pupal fat, shortens the extraction time, reduces extracting pressure, improves the extraction yield of tussah pupal fat.By orthogonal experiment, obtain the optimum process condition of USCE tussah pupal fat: temperature is 45 ℃, and the time is 90min, and pressure is 20MPa, and degree of grinding is 100 orders.Tussah pupal fat extraction yield can reach 28.92% under best USCE processing condition.Add ultrasonic energy and significantly improve the yield of SCE tussah pupal fat, enhance productivity, save production cost and reduce production energy consumption.Along with going deep into of research, USCE tussah pupal fat has the heavy industrialization Application Prospect.

Claims (4)

1. tussah pupal fat ultrasound-enhanced supercritical CO 2The preparation technology of extraction, it is characterized in that: this preparation technology's step is:
(1). raw materials pretreatment: cocoon chrysalis adopts high speed disintegrator to be ground into the cocoon chrysalis powder through sorting, cleaning, sterilization, lyophilize;
(2). step (1) gained cocoon chrysalis powder is put into extraction kettle, when temperature reaches 40-50 ℃, open CO 2Gas cylinder is supplied gas, and when extracting pressure reaches 18-25MPa, regulates flow, at constant temperature and pressure extraction tussah pupal fat 60-120min;
(3). in step (2) process, adopt the ultrasound-enhanced mode of built-in insert, the supercritical CO in extraction kettle 2Fluid emission ultrasonic wave is strengthened tussah pupal fat extraction process;
(4). collect the tussah pupal fat from the separating still exit.
2. tussah pupal fat ultrasound-enhanced supercritical CO according to claim 1 2The preparation technology of extraction, it is characterized in that: described cocoon chrysalis powder is 90~110 orders.
3. tussah pupal fat ultrasound-enhanced supercritical CO according to claim 1 2The extraction preparation technology, it is characterized in that: described ultrasonic frequency is 16kHz~24kHz, power density is 80W/L~120W/L, the ultrasound wave irradiation mode be the intermittent time/the continuous irradiation time is 4s/4s~8s/8s.
4. tussah pupal fat ultrasound-enhanced supercritical CO 2Extracting system is characterized in that: by the CO that connects successively by pipeline 2Gas cylinder, cleaner, storage tank, mixing tank, high-pressure pump, extraction kettle, separating still constitute the transmitting terminal of the ultrasonic convertor of plug-in mounting in extraction kettle.
CN 201010510729 2010-10-15 2010-10-15 Preparation process and system for ultrasonic reinforced supercritical CO2 extraction of tussah pupa oil Pending CN101967426A (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN103436356A (en) * 2013-07-22 2013-12-11 苏州三和开泰花线织造有限公司 Supercritical CO2 extraction technology of silkworm chrysalis oil
CN104629892A (en) * 2015-01-27 2015-05-20 湖南富农蚕桑生物科技有限公司 Method for separating odorless silkworm pupa oil and silkworm pupa protein from silkworm pupa
CN105087149A (en) * 2014-05-16 2015-11-25 十堰天翔茧丝生化有限公司 Comprehensive utilization method of silkworm chrysalis

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CN103436356A (en) * 2013-07-22 2013-12-11 苏州三和开泰花线织造有限公司 Supercritical CO2 extraction technology of silkworm chrysalis oil
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CN104629892A (en) * 2015-01-27 2015-05-20 湖南富农蚕桑生物科技有限公司 Method for separating odorless silkworm pupa oil and silkworm pupa protein from silkworm pupa

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Application publication date: 20110209