CN100479898C - Triple-frequency ultrasonic extraction device and using method thereof - Google Patents

Triple-frequency ultrasonic extraction device and using method thereof Download PDF

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Publication number
CN100479898C
CN100479898C CNB2006101240031A CN200610124003A CN100479898C CN 100479898 C CN100479898 C CN 100479898C CN B2006101240031 A CNB2006101240031 A CN B2006101240031A CN 200610124003 A CN200610124003 A CN 200610124003A CN 100479898 C CN100479898 C CN 100479898C
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frequency
ultrasonic
probes
triple
face
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CN1994510A (en
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丘泰球
杨日福
范晓丹
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

The invention relates to a three-frequency ultrasonic extractor, which comprise ultrasonic extracting pot, ultrasonic wave generator, condenser, cooler, and oil-water separator, wherein the upper part of extracting pot has foam picker via tube connected to the condenser, cooler, and oil-water separator; the bottom of separator via tube is connected to the extracting pot; the middle of pot has six-face cylinder vibrator; the wire is through the stainless steel tube to connect the ultrasonic wave generator; the pot is round, whose upper part has material inlet and lower part has slag outlet, side part has electromagnetic valve and circulate pump. The invention also discloses relative application. Compared with single-frequency ultrasonic extracting technique, it has high efficiency, low temperature demand and short extracting time.

Description

Triple-frequency ultrasonic extraction device and using method thereof
Technical field
The present invention relates to a kind of extraction element, particularly a kind of triple-frequency ultrasonic extraction device and using method thereof.
Background technology
Because Chinese medicine has advantages such as special efficacy, safety aspect treatment, thereby be subjected to the world and attract attention, but ingredient complexity in the Chinese medicine, to the extraction of its active ingredient, be not only the primary link of Chinese medicine preparation, also be the prerequisite of Chinese medicine performance drug effect, therefore, the extraction of active ingredient is most important.Yet in the thousands of how tame herbal pharmaceutical enterprise of China, the leading technology of Chinese medicine extracts active ingredients is still continued to use and is soaked two kinds of extraction method and hot extractions.Exist extraction time long but soak extraction method, the recovery rate deficiency, efficient is low, if adopt hot extraction, then exist the multiple effective component can Yin Gaowen and destroyed, the high and dangerous disadvantage such as big of energy consumption, simultaneously, it is big that traditional handicraft has quantity of solvent, solvent recovery energy consumption height, and environmental pollution is serious.Therefore greatly waste Chinese material medicine resource and the pharmacological effect that has reduced Chinese medicine, restricted the development of herbal pharmaceutical engineering.
In order to address these problems, people attempt to adopt supercritical CO 2Extractive technique, supercritical extraction technique (SFE) is though the tool plurality of advantages, but be confined to lipophilicity, the less material extraction of molecular weight, technology high starting point, equipment complexity, invest relatively largely, the medicinal material treating capacity is little, is more difficult to get at general traditional Chinese medicine enterprise and applies.People have also developed microwave extraction method, but the depth of microwave penetration limited (with its wavelength at the same order of magnitude), simultaneously, non-polar solven does not absorb microwave energy, and has safety issue in operation and the use, makes this method restricted application.The research of relevant ultrasound assisted extraction technique is the domestic and international focus of research, studies show that in a large number, compares with conventional extracting method, have extraction efficiency height, extraction time short, extract that temperature is low, plurality of advantages such as wide adaptability and energy efficient.But the mode of single-frequency irradiation is mainly adopted in the research of extraction aspect at present, and extraction process exists " dead angle ", lack of homogeneity.
In the existing at home ultrasonic extraction device, all adopt a plurality of ultrasonic transduction heads of single-frequency to be installed on outer wall or oscillator places in the middle of the tank body.For the utility model patent of " 02212915.4 " a kind of ultrasonic wave extractor is disclosed as the patent No., charge door, drain hole, air inlet, gas vent are arranged on the tank body of extractor, be provided with the material division board in the tank body cavity, in the tank body cavity, be provided with supersonic generator.
The patent No. is equipped with ultrasonic head for the utility model patent of " 01267013.8 " discloses a kind of ultrasonic wave extractor at the bottom of jar, ultrasonic head also is housed in the side of tank body, and the ultrasonic head that is equipped with is equipped with protective cover.
The patent No. discloses a kind of ultrasonic wave extraction element for the utility model patent of " 200520001353.X ", comprise ultrasonic extractor, secondary settlement jar that ultrasonic probe is housed and feed liquid circulation line and the circulating pump that is connected extractor and settling tank, the ultrasonication probe is housed at ultrasonic extractor top, directly contact plant and extract, the ultrasonic power probe is housed outside the extractor sidewall, in the jar bottom filter septum is housed, under the dividing plate air jet system is arranged, make by fumarole uniform on the air jet system to be extracted material come-up, and liquid stream forms the turbulent flow endless form.Operation material non-blind area under action of ultrasonic waves in jar.
The patent No. discloses a kind of ultrasonic wave extractor for the utility model patent of " 200520022995.8 ", it comprises at least one combined ultrasonic transducer, described combined ultrasonic transducer is the immersion ultrasonic transducer, the cavity and the ultrasonic transducer unit that comprise a hollow, described ultrasonic transducer unit is fixed on the corresponding position of both ends of the surface inboard of cavity, with cavity resonance, be the ultrasonic wave of the three-dimensional ring of new ultrasonic vibration source thereby produce with cavity.
If same energy dissipation in a more wide field rather than concentrated energy dissipation efficiency can be more better on a probe, in order to obtain higher efficiency, in the existing at home ultrasonic extraction device, all adopt a plurality of ultrasonic transduction heads of single-frequency to be installed on outer wall or oscillator places in the middle of the tank body.More than these designs all can consider to be provided with probe quantity more, but the quantity of popping one's head in is restricted by the intensity of power, does not all consider from supersonic frequency.
Summary of the invention
In order to solve the deficiencies in the prior art part, primary and foremost purpose of the present invention is to provide a kind of triple-frequency ultrasonic extraction device.This triple-frequency ultrasonic extraction device will provide a kind of effective means for the modernization of Chinese medicine, promote the technological transformation of China's traditional Chinese medicine industry and the update of equipment, quicken the Chinese medicine industry to the high-tech industry development, promote comprehensive lifting of traditional Chinese medicine enterprise technology, quality, benefit level, improve Chinese medicine in competitiveness international, the domestic market.
Another object of the present invention is to provide the using method of above-mentioned triple-frequency ultrasonic extraction device.
The objective of the invention is to realize: a kind of triple-frequency ultrasonic extraction device by following technical proposals, comprise the ultrasonic wave extractor, supersonic generator, condenser, cooler and oil water separator etc., described ultrasonic wave extractor top is provided with mist eliminator, mist eliminator is connected with oil water separator with the condenser cooler successively by pipeline, the bottom of oil water separator is connected in the ultrasonic wave extractor by pipeline, the centre of ultrasonic wave extractor is provided with six cylinder oscillators, fix six cylinder oscillators by stainless steel tube, lead-in wire passes from stainless steel tube and is connected to supersonic generator, the ultrasonic wave extractor is a round structure, top is equipped with charge door, and the bottom is a slag-drip opening; Sidepiece is provided with magnetic valve and circulating pump.
Described six cylinder oscillators can be installed 1~8 group of ultrasonic probe.Each face that described six cylinder oscillators are arbitrary group all has the ultrasonic probe of three different frequencies.Every group of each face all has the ultrasonic probe of three different frequencies, six totally 18 ultrasonic probes, power 1200W.If install 4 groups, each face has 12 ultrasonic probes, and six totally 72 ultrasonic probes, power can be up to 4800W, and the like.
The disposing way of the ultrasonic probe of three described arbitrary group different frequencies adopts the frequency of any adjacent ultrasonic probe to have nothing in common with each other, and the frequency same way as of opposite ultrasonic probe guarantees that three kinds of frequencies at utmost are coupled.
Described three different frequencies all are no more than 200kHz; Evenly differ 10~20kHz between described three different frequencies.
The disposing way of the ultrasonic probe of three different frequencies of arbitrary group of described six cylinder oscillators is as follows: the 1st face frequency of 3 probes from top to bottom is respectively: frequency a, frequency of b, frequency c; The 2nd face frequency of 3 probes from top to bottom is respectively: frequency of b, frequency c, frequency a; The 3rd face frequency of 3 probes from top to bottom is respectively: frequency c, frequency a, frequency of b; The 4th face frequency of 3 probes from top to bottom is respectively: frequency a, frequency of b, frequency c; The 5th face frequency of 3 probes from top to bottom is respectively: frequency of b, frequency c, frequency a; The 6th face frequency of 3 probes from top to bottom is respectively: frequency c, frequency a, frequency of b.
The using method of triple-frequency ultrasonic extraction device comprises the steps: to take by weighing medicinal material 50~100kg, puts into ultrasonic extractor, adds 8~16 times water, soaks 1~2 hour, and heat up (≤60 ℃) stir, and ultrasonication 0.5~2 hour stops ultrasonicly, gets liquid.
Operation principle of the present invention is as follows: it is ultrasonic that single-frequency is compared in the triple-frequency ultrasonic coupling, produces higher pressure and temperature during the cavitation bubble explosion, in addition, adopt three kinds of frequency ultrasonic probes to launch ultrasonic in opposite directions, can reduce the inhomogeneities of sound field, improve cavitation effect, thereby improve recovery rate.
Triple-frequency ultrasonic extraction device of the present invention, with the ultrasonic wave extractor is that main part and slave part constitute multiplex's skill, multipurpose closed-loop system jointly, main part comprises ultrasonic generator, six cylinder oscillators, compressed air stirring, Steam Heating, temperature regulating and controlling system, pressure regulation control switch, parts such as liquid level control switch, extractor are that round structure passes through solenoid control; Slave part comprises that mist eliminator, condenser, cooler, oil water separator and circulating pump etc. can form multiplex (MUX) skill, multipurpose closed-loop system.Main body of the present invention is six cylinder oscillators, and each face has a plurality of ultrasonic probes, divides several groups, every group of power 1200W, if install 4 groups, power can be up to 4800W, and the like.Every group of each face has three ultrasonic probes, 1 of the ultrasonic probe of its medium frequency a, 1 of the ultrasonic probe of frequency of b, 1 of the ultrasonic probe of frequency c, six totally 18 ultrasonic probes, the characteristics of ornaments are that the frequency of any probe and its opposite all is identical, and the frequency of three adjacent probes all has nothing in common with each other arbitrarily, because therefore two probes of the opposite of six posts distance on same horizontal plane guarantees that three kinds of frequencies at utmost are coupled farthest.Can high liquid level and low liquid level extract, control each group respectively by liquid-level switch and open, effectively protect ultrasonic probe and save experimentation cost.Also be equipped with compressed air and stir, guarantee the uniformity of extracting.Hermetically sealed explosion-proof, can make water, ethanol, benzinum etc. extract solvent, satisfy the needs that various active drug compositions extract.
The present invention compared with prior art has following advantage and beneficial effect:
Triple-frequency ultrasonic extraction device of the present invention makes the multiple frequency ultrasonic extractive technique be applied to industrialization production and is achieved.Compare with the ultrasonic extraction of single-frequency, the good uniformity of extraction, extraction yield improves, and is lower to the requirement of temperature, and the extraction time shortens, and required solvent further reduces.Main body of the present invention is six cylinder oscillators, and each face has a plurality of ultrasonic probes, divides several groups, and every group of each face has three ultrasonic probes.The ultrasonic probe of three kinds of frequencies is put employing " frequency of any adjacent ultrasonic probe has nothing in common with each other, and opposite ultrasonic probe frequency is identical " mode, guarantees that three kinds of frequencies at utmost are coupled.Can high liquid level and low liquid level extract, control each group respectively with liquid-level switch and open, effectively protect ultrasonic probe and save experimentation cost.The present invention combines the ultrasonic probe of several lower supersonic frequencies, not only other devices of power density ratio are little, and better processing effect, show in relevant development test, three sonications frequently have higher efficiency can reach 75~78% (higher 4~8 times than single-frequency or double frequency), and the cavitation yield is wanted high last 1.5~20 times.In addition, introduce gas at device and stir, not only make material even, and can produce better cavitation effect.
Description of drawings
Fig. 1 is the triple-frequency ultrasonic extraction device structural representation.
Fig. 2 is a triple-frequency ultrasonic oscillator schematic diagram.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1
Complete set of equipments of the present invention is that main part and slave part constitute multiplex's skill, multipurpose closed system jointly with the ultrasonic wave extractor, main part comprises ultrasonic generator, six cylinder oscillators, compressed air stirs, parts such as Steam Heating, and configuration temperature regulating and controlling system, pressure regulation control switch, liquid level control switch etc.Slave part comprises compositions such as mist eliminator, condenser, cooler, oil water separator and circulating pump.
Be illustrated in figure 1 as triple-frequency ultrasonic extraction device of the present invention, comprise ultrasonic wave extractor 1, supersonic generator 2, condenser 6, cooler 7 and oil water separator 9 etc., described ultrasonic wave extractor 1 top is provided with mist eliminator 4, mist eliminator 4 is connected with oil water separator 9 with condenser 6 coolers 7 successively by pipeline, the bottom of oil water separator 9 is connected in the ultrasonic wave extractor 1 by pipeline, the centre of ultrasonic wave extractor 1 is provided with six cylinder oscillators 3, fix six cylinder oscillators 3 by stainless steel tube 22, lead-in wire 21 passes from stainless steel tube 22 and is connected to supersonic generator 2, ultrasonic wave extractor 1 is a round structure, top is equipped with charge door 14, and the bottom is a slag-drip opening 15; Sidepiece is provided with magnetic valve 16 and circulating pump 13.
Ultrasonic wave extractor 1 is a round structure, and charge door 14 is installed on top, adds material and uses flange seal, and the bottom is a slag-drip opening 15, by magnetic valve 16 controls; Six cylinder oscillators 3 are installed in the middle of the ultrasonic wave extractor 1, stainless steel tube 21 is fixed on extractor 1 top, support whole six cylinder oscillators 3, lead-in wire 21 passes from stainless steel tube 22 and is connected to supersonic generator 2, liquid level control switch is installed in the ultrasonic wave extractor 1, thereby can control the ultrasonic probe group that supersonic generator 2 is controlled six cylinder oscillators 3, make things convenient for two position to extract; Ultrasonic wave extractor 1 used vapour heats materials inside.Water vapour enters the liquid in the interlayer heating tank of ultrasonic wave extractor 1 from steam inlet 12; Be provided with compressed air in the tank body and stir, ultrasonic wave extractor bottom is led to compressed air in compressed air inlet 11, up stirs from tank base solution; The foam that produces in the high pressure dregs of a decoction is collected by mist eliminator 4, and mist eliminator 4 can be opened cleaning by flange after each extraction was finished; The steam that evaporation produces in the liquid in the extractor up flows and runs into condenser 6 and cooler 7, and cooling water flows into the back from cooling water inlet 8 and flows out from coolant outlet 5; Make steam cool off the liquid inflow oil water separator 9 that congeals into through condenser 6 and cooler 7, there is steam vent 17 oil water separator 9 upper ends, side has oil collect port 18, leaves standstill the back layering, and the upper strata is an oil, lower floor is a water, open the switch of oil water separator 9 bottoms, allow water be back to ultrasonic wave extractor 1, keep the liquid volume in the extractor, after extraction is finished in the oil water separator 9 remaining oil water mixed liquid body collect in the container by discharge outlet 10 so that further separate.
Ultrasonic wave extractor 1 usefulness compressed air stirs, and guarantees the uniformity of extracting.Available cycles pump 13 forces to extract the pot liquid circulation.Control high liquid level and the extraction of low liquid level with liquid-level switch, effectively protect ultrasonic probe and save experimentation cost.
Be illustrated in figure 2 as six cylinder triple-frequency ultrasonic oscillators.Six cylinder oscillators 3 are installed in the middle of the tank body.Stainless steel tube 22 is fixed on ultrasonic wave extractor 1 top, supports whole six cylinder oscillators 3, and lead-in wire 21 passes from stainless steel tube 22 and is connected to supersonic generator 2.The ultrasonic probe of 4 groups of different frequencies is set on six cylinder oscillators 3, and arbitrary group of each face all is provided with frequency a ultrasonic probe 23; Frequency of b ultrasonic probe 24; Frequency c ultrasonic probe 25.The disposing way of the ultrasonic probe of arbitrary group of three different frequencies of six cylinder oscillators is as follows: the 1st face frequency of 3 probes from top to bottom is respectively: frequency a, frequency of b, frequency c; The 2nd face frequency of 3 probes from top to bottom is respectively: frequency of b, frequency c, frequency a; The 3rd face frequency of 3 probes from top to bottom is respectively: frequency c, frequency a, frequency of b; The 4th face frequency of 3 probes from top to bottom is respectively: frequency a, frequency of b, frequency c; The 5th face frequency of 3 probes from top to bottom is respectively: frequency of b, frequency c, frequency a; The 6th face frequency of 3 probes from top to bottom is respectively: frequency c, frequency a, frequency of b.
If increasing ultrasonic probe is 8 groups, hyperacoustic power can reach 9600W, and the volume of ultrasonic wave extractor is also corresponding will to increase 1 times.
Embodiment 2
Adopt the extraction of triple-frequency ultrasonic extraction device to carry out according to the following procedure: take by weighing Exocarpium Citri Grandis medicinal material coarse powder 50kg, put into ultrasonic extractor, add 800kg water, soaked 1 hour, be warming up to 60 ℃, stirring, ultrasonication 0.5 hour stops ultrasonicly, gets liquid.
Embodiment 3
Adopt the extraction of triple-frequency ultrasonic extraction device to carry out according to the following procedure: take by weighing Ligusticum wallichii medicinal material coarse powder 75kg, put into ultrasonic extractor, add 800kg water, soaked 1 hour, be warming up to 60 ℃, stirring, ultrasonication 1 hour stops ultrasonicly, gets liquid.
Embodiment 4
Adopt the extraction of triple-frequency ultrasonic extraction device to carry out according to the following procedure: take by weighing Exocarpium Citri Grandis medicinal material coarse powder 100kg, put into ultrasonic extractor, add 800kg water, soaked 1 hour, be warming up to 60 ℃, stirring, ultrasonication 2 hours stops ultrasonicly, gets liquid.
Comparing embodiment: use triple-frequency ultrasonic extraction device and carry out ultrasonic extraction and decocting method extraction contrast
Ultrasonic extraction aurantiin from Exocarpium Citri Grandis: take by weighing 50 kilograms of Exocarpium Citri Grandis medicinal material coarse powder, put into ultrasonic extractor, add 800 kilograms water, soaked 1 hour, and be warming up to 60 ℃, ultrasonication is after 0.5 hour, stop ultrasonicly, get 50ml and cross 80 mesh sieves, the filtrate sample analysis.Clout liquid continued ultrasonic 0.5 hour, stopped ultrasonicly, and extract is crossed 80 mesh sieves, and the filtrate metering is also analyzed.
Take by weighing 50 kilograms of Exocarpium Citri Grandis medicinal material coarse powder, put into ultrasonic extractor, add 800 kilograms water, soaked 1 hour.Be warming up to 100 ℃, boiled soup 2 hours, extract is crossed 60~100 mesh sieves, emits filtrate metering and analysis.
The result shows that ultrasonic 30min just can extract about 70% composition.But the prolongation of time can not increase too many effect, is not too big so extract the quantitative changeization of 60min.Simultaneously, the decocting cooking method of comparing needs 100 ℃ just can carry out, and ultrasonic needed temperature is very low, has been maximum temperature at 60 ℃, can avoid like this destroying being subjected to heat-labile composition in the medicinal material.The low temperature of ultrasonic extraction and rapidly and efficiently can shorten the production cycle improves the quality of product inherence, cuts down the consumption of energy, and helps the production of enterprise.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spiritual essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (6)

1, a kind of triple-frequency ultrasonic extraction device, comprise the ultrasonic wave extractor, supersonic generator, condenser, cooler and oil water separator, it is characterized in that: described ultrasonic wave extractor top is provided with mist eliminator, mist eliminator by pipeline successively with condenser, cooler is connected with oil water separator, the bottom of oil water separator is connected in the ultrasonic wave extractor by pipeline, the centre of ultrasonic wave extractor is provided with six cylinder oscillators, fix six cylinder oscillators by stainless steel tube, lead-in wire passes from stainless steel tube and is connected to supersonic generator, described ultrasonic wave extractor is a round structure, top is equipped with charge door, and the bottom is a slag-drip opening; Sidepiece is provided with magnetic valve and circulating pump; Described six cylinder oscillators are installed 1~8 group of ultrasonic probe; Each face of arbitrary group of ultrasonic probe of described six cylinder oscillators all has the ultrasonic probe of three different frequencies, six totally 18 ultrasonic probes.
3, a kind of triple-frequency ultrasonic extraction device according to claim 1 is characterized in that: the disposing way of the ultrasonic probe of described three different frequencies adopts the frequency of any adjacent ultrasonic probe to have nothing in common with each other, the frequency same way as of opposite ultrasonic probe.
4, a kind of triple-frequency ultrasonic extraction device according to claim 1 is characterized in that: described three different frequencies all are no more than 200kHz.
5, a kind of triple-frequency ultrasonic extraction device according to claim 1 is characterized in that: all evenly differ 10~20kHz between the different frequency of the ultrasonic probe of described three different frequencies.
6, a kind of triple-frequency ultrasonic extraction device according to claim 1, it is characterized in that: the disposing way of arbitrary group of ultrasonic probe of described six cylinder oscillators is as follows: the 1st face frequency of 3 probes from top to bottom is respectively: frequency a, frequency of b, frequency c; The 2nd face frequency of 3 probes from top to bottom is respectively: frequency of b, frequency c, frequency a; The 3rd face frequency of 3 probes from top to bottom is respectively: frequency c, frequency a, frequency of b; The 4th face frequency of 3 probes from top to bottom is respectively: frequency a, frequency of b, frequency c; The 5th face frequency of 3 probes from top to bottom is respectively: frequency of b, frequency c, frequency a; The 6th face frequency of 3 probes from top to bottom is respectively: frequency c, frequency a, frequency of b.
7, the using method of the described triple-frequency ultrasonic extraction device of a kind of claim 1, it is characterized in that comprising the steps: to take by weighing medicinal material 50~100kg, put into ultrasonic extractor, the water that adds 8~16 times soaked 1~2 hour, heated up, stir, ultrasonication 0.5~2 hour stops ultrasonicly, gets liquid.
CNB2006101240031A 2006-12-01 2006-12-01 Triple-frequency ultrasonic extraction device and using method thereof Expired - Fee Related CN100479898C (en)

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CN103990295A (en) * 2014-05-30 2014-08-20 陕西师范大学 Complex-frequency ultrasonic cavitation medicine extraction device
CN106943769A (en) * 2017-04-19 2017-07-14 都江堰市马蒂斯生物科技有限公司 A kind of Kiwi berry high concentration extractor
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CN103990295A (en) * 2014-05-30 2014-08-20 陕西师范大学 Complex-frequency ultrasonic cavitation medicine extraction device
CN103990295B (en) * 2014-05-30 2015-12-30 陕西师范大学 A kind of multiple-frequency supersonic cavitation medicament extracting device
CN106943769A (en) * 2017-04-19 2017-07-14 都江堰市马蒂斯生物科技有限公司 A kind of Kiwi berry high concentration extractor
CN109438582A (en) * 2018-10-16 2019-03-08 宝应县有机食品质量监督检验中心 The method of multi-mode ultrasonic wave assisted extraction arrowhead starch

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