CN1161056A - Method of continuous extraction of crude wax and apparatus therefor - Google Patents

Method of continuous extraction of crude wax and apparatus therefor Download PDF

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Publication number
CN1161056A
CN1161056A CN 96190741 CN96190741A CN1161056A CN 1161056 A CN1161056 A CN 1161056A CN 96190741 CN96190741 CN 96190741 CN 96190741 A CN96190741 A CN 96190741A CN 1161056 A CN1161056 A CN 1161056A
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solid residue
extraction
mixture
organic solvent
ribbon
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福世一巳
藤村耕治
房野俊治
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Eneos Corp
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Nippon Petrochemicals Co Ltd
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Priority to CN 96190741 priority Critical patent/CN1161056A/en
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Abstract

This invention provides a method and an apparatus for continuously extracting a wax component contained in a solid residue with a solvent, in which method, the solid residue obtained from the juice of sugar cane is used as a raw material. To make the extraction time uniform and to obtain the wax at a high efficiency of extraction, the solid residue and an organic solvent for extraction are mixed under shear force and agitated in directions perpendicular to the flow direction. The mixing is conducted under an agitated flow condition so as to form a substantially plug flow in the flow direction.

Description

The continuous extration method of waxy stone and equipment used thereof
Technical field
The present invention relates to make the extracting process of waxy stone and implement the employed equipment of this method from sugarcane.
Background technology
From sugarcane production granulated sugar the time, extrude sugar cane juice by the stem of crushing sugar cane, this juice is boiled dry and obtained raw sugar.
The stem of crushing sugar cane and squeezing the juice of obtaining must be contained crust, the vascular bundle (path of plant absorbing nutriment and moisture) of chippy stem, fragment of stem flesh etc. except the granulated sugar composition, also contain wax and resinous principle.Therefore, in squeezing the juice, add flocculation agent, flocculating aids etc. as required, wax and resinous principle precipitation is also filtered, simultaneously also by filtering the removals such as fragment of the crust of chippy stem, vascular bundle, stem flesh.Produce raw sugar by hotting plate resulting filtrate, on the other hand, make waxy stone from filtration residue (filter cake is commonly referred to as " cachaza ").This filtration residue, paraffin removal and resinous principle, and outside the fragment of the crust of chippy stem, vascular bundle, stem flesh, also contain precipitation agent, earth etc., though also contain the moisture of 70-80 weight % usually, be solid matter in appearance.
In other words, owing to make the broken or pulverizing of sugarcane,, be the aggregate of aqueous crushed material or broken thing so the filter cake of this sugarcane strand juice is deformable solid as a whole by initial squeezing effect.And the crushing piece or the flinders that constitute aggregate be in irregular shape, and some be fibrous, owing to contain water thereby be to stir the aggregate that lumps together each other, is bulk again, demonstrates shape-holding property to a certain degree.Though say not to be viscoelastic body exactly, say in appearance or partly, be the aggregate that demonstrates similar viscoelastic body characteristic.
Japanese patent gazette spy opens and proposes in flat 6-122892 number filter cake not to be carried out drying, the method for carrying out continuous extraction by means of hydrophobic organic solvent in advance.In other words, Yi Bian be filter cake and hydrophobic organic solvent to be kneaded to carry out method of extraction on one side, can use the stirring heating transfer roller that has spiral, ribbon blade, splash bar etc. as its equipment used.And, stir (referring to this communique, page 4, the 5th hurdle, paragraph 0017) while can apply shearing force in order to make part be blocky filter cake and be dispersed into fragment.But, because process object is as the solvent of liquid and mixture as the filter cake of solid aggregate, so can not easily extract by the simple whipping devices of being put down in writing in the above-mentioned communique of carrying such as single shaft screw-type extruder.
In addition, the method from filter cake manufacturing wax of using vertical continuous extraction tower is disclosed in No. 2554073 communique of United States Patent (USP).In this method, in tower, only depend on the finger of rotation or agitating arm to stir filter cake on each column plate and extraction solvent carries out counter-current extraction.Though can think that the water that is contained in the filter cake is between the crushing piece that constitutes filter cake or the flinders or in its inner gap, such water especially can the obstruction solvent extraction under the occasion of hydrophobic solvent.Be difficult to prevent that by simple stirring the caused extraction of this water from hindering, and make the stirring aggravation, filter cake can become fragment and be dispersed in the solvent.Such dispersion state is unfavorable for conveying and processing thereafter, and might stop up and carry pipe arrangement etc., so be bad.
Here, experiment according to the inventor is distinguished, resulting filter cake carries out under the solvent-extracted occasion when those are handled squeezing the juice of sugarcane, initial stage in extraction mainly is that the wax composition is extracted morely, but the extraction time one is long, then becoming to grade from the xylogen of Caulis Sacchari sinensis fiber is extracted out easily, the xylogen composition with promptly use further separating of wax composition recrystallize operation etc. to separate means also to be not easy.Therefore, in order not contained the wax composition of xylogen composition, the residence time in the extraction equipment must be adjusted to suitable scope.
Though the batch-type solvent extration has the less advantage of the error of extraction time, uses batchwise operation, is difficult to a large amount of processing, be improper as the industrialization method for making in essence.
Like this, should handle in a large number, in fact do not produce the error of extraction time again when solvent extraction, existing method may not necessarily satisfy.
The present invention In view of the foregoing makes, its objective is provides a kind of extraction equipment of making waxy stone, it is to be raw material when carrying out solvent extraction at the solid residue of separating with squeezing the juice of sugarcane, can in fact not extract time error, and can make with high extraction efficiency.
Brief description of drawings
Fig. 1 is the simplified cross-sectional view of the example of double ribbon vane-type extraction equipment;
Fig. 2 is the simplified cross-sectional view of the example of two splash bar type extraction equipments; And
Fig. 3 is the front view and the sectional view of the example of aerofoil profile disk.
Disclosure of an invention
First invention of asking in this relates to the solvent method that institute's content of wax divides in the solvent extraction solid residue continuously, it is when the solid residue of separating from the squeezing the juice of sugarcane and organic extractant are applied shearing force, mixed, with the vertical direction of the moving phase of this mixture on fully stir, and streamwise forms the plunger tpe mobile basically and stirs and to extract under the flow state.
The application's second invention relates to a kind of horizontal continuous organic solvent extracting taking equipment of waxy stone, it is characterized in that comprising following (1) to (3) component part:
(1) opening is at sealed horizontal container one end, is used for supplying with continuously the solid residue separated from sugar cane crushing and the supplying opening of organic extraction solvent;
(2) be located at two groups of interior stirring conveying devices of said vesse, its agitating function all is to stir when solid residue and organic solvent are applied shearing force, though it is reciprocal that its conveying function is given the feed drive direction of mixture, then be to carry continuously to the other end in general from said vesse one end with regard to mixture; And
(3) opening is at the other end of sealed horizontal container, is used for extruding continuously the relief outlet of the mixture of above-mentioned solid residue and organic extractant.
The application's the 3rd invention is as the horizontal continuous organic solvent extracting taking equipment of the second described waxy stone of invention, it is characterized in that above-mentioned two groups of stirring conveying devices serve as that axle is rotated with the throughput direction of mixture all.
The application's the 4th invention is as the horizontal continuous organic solvent extracting taking equipment of the 3rd described waxy stone of invention, it is characterized in that having the structure that double ribbon vane-type is extruded type, it is given the conveyance drive force of direction opposite each other to mixture by two groups of ribbon blades.
The application's the 5th invention is the horizontal continuous organic solvent extracting taking equipment of waxy stone as described in the 4th invention, it is characterized in that above-mentioned two groups of ribbon blades are made up of major diameter ribbon blade and minor axis ribbon blade.
The 6th invention of the present invention is as the 3rd invention described waxy stone horizontal continuous organic solvent extracting taking equipment, it is characterized in that having any structure in two splash bar types, two collar plate shapes and two spiral types.
Explain the present invention below
When making granulated sugar, use earlier various squeezing machines, for example, extrude juice with the stem of roller squeezer crushing sugar canes such as the sugared machine of press for extracting juice with sugarcane.Also have plenty of and earlier sugarcane is pulverized.Though resulting squeezing the juice contained sugar, divide and resinous principle owing to contain wax, so be opaque liquid.Divide and resinous principle in order to remove wax in from then on squeezing the juice, add flocculation agent or flocculating aids etc. as required, the white lime that for example adds 2-10 weight % (usually about 5 weight %) makes it cohesion, uses appropriate means, for example filters out the solids component that is condensed with pressure filter etc.Here remain extruding dregs in pressure filter as residue, promptly contain wax in the filter cake in large quantities and divide and resinous principle.Except that pressure filter, filter or separation method such as centrifugation also can be removed wax etc. with semi-permeable membranes.
In the present invention, the so-called solid residue of separating from the squeezing the juice of sugarcane is meant above-mentioned squeezing the juice is taken the circumstances into consideration to add after the flocculation agent etc., with the solid residue that pressure filter or semi-permeable membranes filter or suitable for separation such as centrifugation is carried out resulting separation.Be typically filter cake.As mentioned above, solid residue normally paraffin removal divide or resinous principle outside, also contain the fragment of crust, vascular bundle, stem flesh of chippy stem and flocculation agent, flocculating aids, precipitation agent, earth etc., usually contain a lot of water in addition, for example contain 50-90 weight %, preferably contain 70-80 weight %, outward appearance is solid-state material.If use method of the present invention, then not carrying out drying specially can extract, but also can carry out drying with suitable dry means, moisture is reduced.
In extraction process, by mixed organic solvents in above-mentioned solid residue, when applying shearing force, stir, thus, from solid residue, use solvent extraction wax branch continuously.As extraction agent, for the wax in the dissolution extraction solid residue divides organic solvent as extraction agent.With regard to hydrophilic organic solvents such as alcohols or ketone, because the moisture that contains in a large number in the solid residue also is extracted simultaneously, solvent was not easy with separating of moisture thereafter, so preferably use hydrophobic organic solvent as extraction agent.
Can enumerate varsol as the excellent hydrophobic property organic solvent.Consider from aspects such as environmental pollution, securities, can enumerate for example C 5-C 9The non-aromatic varsol of scope, preferably C 5-C 9Liquid saturated hydrocarbons, for example cycloalkane or paraffinic, particularly C 6-C 9Isoparaffin or C 5-C 8N-paraffin or their mixture etc.
In extraction,, so as previously mentioned, earlier the wax branch is washed out, then just with the elution of xylogen composition because sugar-cane wax is dissolved in the general organic solvent than xylogen composition is easier.And under the occasion to the low organic solvent of the solvency power of these materials, in the elution process, the above-mentioned time difference increases more.On the other hand, under the occasion to the high organic solvent of the solvency power of wax or xylogen, the time till wax branch and the elution of xylogen composition can't produce very big difference.In other words, because the solvency power height, possible time of occurrence difference is little just the situation of wax branch with the elution of xylogen composition.Under this occasion, method of the present invention is difficult to effectively.From this point of view, in order to use method of the present invention, preferably use the lower organic solvent of solvency power, for example with hydrophobic organic solvents such as hydro carbons to wax branch or xylogen composition.
The use level of above-mentioned organic solvent is solid residue volumetrical 0.05-10 times, preferably 0.5-5 times of volume.0.05 times of the not enough solid residue of the volumetric quantity of solvent then extracts insufficient, on the other hand when surpassing 10 times of volumes, because the efficient of the solvent recuperation etc. of latter stage is reduced, so all be bad, the temperature of extraction can suitably be determined, though because of used solvent different, usually so long as be lower than the boiling point of the solvent working pressure under, just qualification specially.For example, can from the temperature range of normal temperature-100 ℃, select.
As concrete extracting process, be to adopt on one side solid residue is applied shearing force, on one side stir solids residue and above-mentioned hydrophobic organic solvent, extract continuously.
The solid residue that with the filter cake is representative is the aggregate of crushing piece and flinders, and exists in its gap and hinder wax and the contacted water of solvent.Therefore, by on one side solid residue being applied shearing force, on one side the mixture of stir solids residue and solvent, just can not make each fragment of above-mentioned aggregate discrete, and, even have under the occasion of water existence wax is fully contacted with solvent.Under occasion not to solid residue effect shearing force, even perhaps the effect but under the inadequate occasion, for example under the occasion by the simple stirring of suitable stirring velocity, owing to the water that is mingled with makes extraction insufficient, when low whipping speed is high in addition, each chip separation of aggregate, discrete, these all are bad.
For will be to solid residue while the mixture that applies shearing force, stir solids residue and solvent, the whipping appts that has suitable stirring function by employing can be realized.For example, can enumerate the double ribbon blade of rotation, two splash bars (forming on two axles of rotation a plurality of splash bars being set respectively), two disks (on two axles of rotation a plurality of disks being set respectively forms), two whipping apptss such as spiral.Under the occasion of whipping apptss such as spiral or ribbon, use uniaxial equipment, because the shearing force deficiency, so should not adopt.
Moreover these whipping apptss must have when stirring the function of the mixture of conveying solid substance residue and solvent continuously.In other words, can act on conveyance drive force continuously to said mixture, carry out the successive extracting operation with such whipping appts.Below, calling " stirring conveying device " with the whipping appts of carrying function.
Above-mentioned stirring conveying device can be located in the proper container.In order to prevent the volatilization of solvent, this container is preferably made closed structure.And, by above-mentioned conveying function the mixture of solid residue and solvent from an end of container to the other end continuously, along continuous straight runs is carried basically, carries out extracting operation betwixt.
As mentioned above, when the solid residue that obtains from squeezing the juice of sugarcane is extracted, extract longways, then to extract xylogen easily and become to grade and be difficult for the composition of separation and purification if cross.With regard to existing continuous extraction method, because the error of extraction time is quite big, be extracted out to a certain extent so the xylogen composition is inevitable, this causes purity drop.
Therefore, in order not produce the error of extraction time when the solvent extraction basically, in the method for the invention, with the vertical direction that flows on mix fully, streamwise forms the plunger tpe mobile basically and stirs under the flow state continuously contained wax branch in the solvent extraction solid residue simultaneously.
Form plunger tpe by streamwise and flow or stirring flow state akin with it, can be implemented in does not have error or the extraction of error minimal continuous fully on the extraction time.Though plunger tpe flow state completely preferably is as long as it is just passable to obtain the plunger tpe flow state basically.
With the vertical direction that flows on, it is necessary stirring fully.By this stirring, make solid residue contact mixing fully with organic solvent, extract with organic solvent.
For example, as said apparatus, adopt two groups of stirring conveying devices, the feed drive direction that the conveying function that each group is brought into play is set for respect to mixture is reciprocal.But, owing to mixture must be carried continuously towards certain orientation, so act in a certain direction as overall (each conveyance drive force sum) of conveyance drive force.Therefore, though the feed drive direction that two groups of devices are brought into play is opposite, its size (absolute value) will make that wherein a side is big slightly.For example, with regard to double ribbon blade or two whipping apptss such as spiral, can be opposite each other by the sense of rotation that makes two groups of ribbons or spiral, the methods such as rotation radius that perhaps change two ribbons realize.With regard to two splash bars, two whipping apptss such as disk, direction that can be by suitably changing splash bar or disk, the sense of rotation of turning axle wait and realize.
Here, described stirring conveying device all is rotated.In other words, the motion of the scraper plate of the ribbon of double ribbon blade or two spirals is rotations of spiral status, and having with the throughput direction is the speed of rotation component of axle.And with regard to two splash bars, two disks etc., be that throughput direction with mixture is the axle rotation.Therefore, each stirring conveying device has the highest linear velocity (terminal rotational line speed) at the circumference of rotator.
So, the average translational speed (m/ branch) of flow direction (direction of principal axis) that makes solid residue for A, make when the higher person is B in the terminal rotational line speed (m/ branch) of two groups of stirring conveying devices, the value of B/A should be got 0.5-50, is preferably the scope of 1-35.Under the occasion of less than 0.5, the translational speed of solid residue is too fast or rotate through slow or the two haves both at the same time, under such occasion, solid residue is just insufficient with contacting of solvent, is bad.Value at B/A surpasses under 50 the occasion in addition, the translational speed of solid residue is crossed slow or is rotated too fast or the two haves both at the same time, under such occasion, solid residue spreads all over the container inner wall side because of the centrifugal force of swivel arrangement, the result still is that solid residue is insufficient with contacting of solvent, so be bad.
As employed equipment in the inventive method, as long as can realize that along fully stirring with mobile vertical direction, streamwise forms the plunger tpe mobile basically and stirs flow state simultaneously, any equipment can adopt.
In other words, equipment as the inventive method, can enumerate a kind of horizontal continuous organic solvent extracting taking equipment that in horizontal extraction container, possesses the waxy stone of two groups of stirring conveying devices, in two groups of stirring conveying devices, its agitating function all is to stir when solid residue and organic solvent are applied shearing force, though it is reciprocal that its conveying function is given the feed drive direction of mixture, then be to carry continuously to the other end in general from an end of container with regard to mixture.
At each end of the flow direction of horizontal extraction equipment, opening respectively, they are respectively the relief outlets of the mixture after being used for supplying with the supplying opening of solid residue and organic solvent continuously and being used for discharging continuously extracting operation.
Specifically, for example, continuous extraction equipment by means of some equipment stir solids residue and organic solvent is arranged, these equipment be have respectively the double ribbon vane-type forcing machine of the major diameter formed by rightabout spiral and minor axis ribbon blade or have reverse rotation two groups of splash bar groups two splash bar type whipping devices or this splash bar group is changed into equipment of disk group etc.
Fig. 1 is the simplified cross-sectional view of the double ribbon vane-type extraction equipment example of expression.Drop into solid residue and organic solvent continuously from the inlet peristome 2 of double ribbon vane-type extraction equipment 1, for example fatty family varsol etc.Be contained in major diameter on the turning axle 3 and minor axis two ribbon blades 4a and 4b and form the spiral of direction opposite each other.The screw diameter of major diameter ribbon blade 4a is greater than the screw diameter of minor axis ribbon blade 4b.By making turning axle 3 rotation by electric motor 5, while make input solid residue and solvent be subjected to shearing force mixed, and mobile vertically, carry out solvent extraction therebetween continuously.After this, by suitable separation means (not shown), for example sieve, pressing machine, separating centrifuge etc. can obtain having dissolved the extraction liquid of waxy stone from removing solid residue through separating the exit opening portion 6 effusive extraction mixtures.By going out solvent, can obtain waxy stone by means such as evaporation appropriate separation from this extraction liquid.
In the equipment of described Fig. 1, the spiral of major diameter ribbon blade 4a is produced vertically the propulsive force (conveyance drive force) that (flow direction) carries out by rotation, produces flowing forward.On the other hand, minor axis ribbon blade 4b because the direction of spiral is opposite with major diameter ribbon blade 4a, so produce the propulsive force that retreats, produces backward mobile.In other words, by flowing that major diameter ribbon blade produces by the partly payment of flowing of minor axis ribbon blade generation.If,, with regard to flowing all, can flow towards Way out owing to make the propulsive force of the propulsive force of major diameter ribbon blade greater than minor axis ribbon blade though just do not carried out conveying by payment fully towards Way out.Here, the shape by suitably changing the ribbon blade or the spiral shell square of spiral can be distinguished the propulsive force that changes two groups of ribbon blades independently.
As mentioned above, the plunger tpe that generally speaking can form basically to Way out that just flows flows.Usually because the screw diameter of major diameter ribbon blade is big, so propulsive force is also big.Under the occasion with roughly the same pitch, the screw diameter that makes major diameter ribbon blade is 1 o'clock, and the screw diameter of minor axis ribbon blade is the scope of 0.1-0.9, is preferably the scope of 0.3-0.7.During this ratio less than 0.1, the effect of the mobile minor axis ribbon blade that payment major diameter ribbon blade causes is too little, and consequently the velocity flow profile of flow direction is excessive, is difficult to form plunger tpe and flows, so be bad.On the other hand, described ratio was greater than 0.9 o'clock, and the propulsive force of minor axis ribbon blade is excessive, was difficult to carry the extraction mixture towards Way out, so be bad.
As mentioned above, by the rotation of two groups of ribbon blades, radially realize mixing fully.
The rotation of two groups of ribbon blades, each other can along equidirectional, also can be in opposite direction.Example two spirals of Fig. 1 be oriented reverse direction, two ribbon blades rotate along equidirectional.When two ribbon blades were rotated in opposite direction, both spirals were oriented equidirectional.
No matter along under the occasion of equidirectional or rotation in opposite direction, the rotating speed of two ribbon blades can be set independently of one another.If the spiral that makes two ribbon blades adopts along the method for equidirectional with the same rotational speed rotation towards on the contrary, then physical construction is simple, cheap.
Rotating speed can be selected from the scope of 1-500r/min.
Fig. 2 is the simplified cross-sectional view of two splash bar type extraction equipment examples of expression.Be provided with in two splash bar type extraction equipments 11 inlet peristome 12, two turning axles 13, respectively be installed in a plurality of splash bars 14 on two turning axles, drive the electric motor 15 and the exit opening portion 16 of turning axle.
Though in Fig. 2, drive turning axle respectively, also available suitable transmission mechanism, by many turning axles of a motor drive by two electric motor.
Splash bar 14 alternately is arranged on two turning axles 13 as shown in FIG..Though two turning axles can preferably rotate along opposite directions usually along same direction rotation.Rotating speed can be selected from the scope of 1-500r/min.In addition, the number of splash bar can be most, is respectively 2-20 usually on each.The size of splash bar and interval thereof have no particular limits.
The shape of splash bar 14 can suitably be out of shape, so that can carry the solid residue that drops into and the mixture of organic solvent towards Way out.For example, as shown in Figure 2, with regard to the splash bar on the same axle, it is tilted every an opposite direction in edge, make it produce propulsive force, by those being made solid residue and solvent mixture make greater than the inclination that makes the splash bar that retreats towards the inclination of Way out progressive splash bar, then can making substantially flows moves towards Way out.In addition, if the length that makes the splash bar that advances is greater than the length that retreats splash bar, even then the big or small identical of inclination also can obtain same effect.
In two splash bar type extraction equipments shown in Fig. 2, disk can be set replace splash bars at different levels.
Under the occasion of collar plate shape, the disk of two turning axles when rotation, by its friction resistance, input solid residue and solvent when being subjected to shearing force along being stirred fully with the vertical direction of turning axle.On the other hand, because disk is to have tabular two dimensional structure,, with regard to flowing, forms plunger tpe basically and flow so concerning flow direction, show the effect in next door.As a result, velocity flow profile is little, can extract the little successive solvent extraction operation of time error in other words.
As under the occasion of disk, the angle that it is suitable that equipment integral tilts, for example 1-30 ° scope flows down by the effect by gravity, can guarantee axial flowing with simple disk.
In addition, fin can also be set on disk, apply propulsive force vertically.Fig. 3 is the front view and the side-view of aerofoil profile disk example.Aerofoil profile disk 17 is made of the disk that is provided with a plurality of fins 18.
Under the occasion of using two splash bar type extraction equipments shown in Figure 2,,, can obtain having dissolved the extraction liquid of waxy stone from removing solid residue through separating the exit opening portion 16 effusive mixtures if by equipment such as sieves.Isolate solvent by evaporation from this extraction liquid, can obtain waxy stone.
In any extraction equipment of Fig. 1 and Fig. 2, the extraction time can be set the extraction quantity that makes the xylogen composition for and reduce, and can select in the scope that 1-180 divides usually, preferably selects from the scope that 5-60 divides.In addition, under the occasion of using the such extrusion type extraction equipment of Fig. 1 or Fig. 2, average retention time (passing through the needed time of object being treated) is used as the extraction time.
Though the pressure during extraction can be used normal pressure, can use the pressure certainly of the vapour pressure that produces based on solvent, perhaps carry out suitable pressurization with being pressed into of rare gas element etc.Can shorten the extraction time by pressurizeing.Pressure during pressurization is different because of the compressive strength of equipment, is generally 5kg/cm 2Below.
The best mode that carries out an invention
Describe the present invention by the following examples in detail.
The the 1st and the 2nd embodiment
The resulting filter cake of squeezing the juice (solid state component 20 weight %) that filters sugarcane is supplied with double ribbon vane-type extraction equipment shown in Figure 1, with predetermined proportion (being shown in table 1) with Isosol (
Figure A9619074100131
ィ ソ ゾ-Le) 200 (trade(brand)name, Japan petroleum chemical company systems; C 6-C 9Different chain methane series varsol) as organic extractant, under the temperature shown in the table 1, carry out the extraction that wax divides.Utilize the indirect heating device suitably to heat.
The technical specification of device shown in Figure 1 is as follows:
Has the diameter of carrying the major diameter ribbon blade of effect towards Way out
17.0cm
Has the diameter of carrying the minor axis ribbon blade of effect towards Way in
9.0cm
Length from the inlet peristome to exit opening portion
53.2cm
Rotating speed (two ribbon blade in the same direction, with same rotating speed)
50r/min
As mentioned above, in equipment shown in Figure 1, two ribbon blades produce rightabout propulsive force respectively, and it carries effect to offset each other, preferentially form plunger tpe vertically by the conveying effect towards Way out and flow or akin with it stirring flow state.Moreover such flow state can be by when mixing, as observe inner the confirming of a plurality of whirlpools of then seeing.Continuous extraction the results are shown in table 1.
The the 1st and the 2nd embodiment changes extraction temperature and carries out, and the value of the ratio B/A of terminal rotational line speed (m/ branch) B of the average translational speed of the flow direction of its solid residue (axially) (m/ branch) A and stirring and e Foerderanlage is 2.7.
The 3rd embodiment
Identical with the 1st embodiment, filter cake is supplied with two splash bar type extraction equipments shown in Figure 2, with predetermined proportion (being shown in table 1) 1sosol200 is used as organic extractant, under the temperature shown in the table 1, carry out the extraction that wax divides.Utilize the indirect heating device to heat.The results are shown in table 1.
Comparative example
Except a ribbon vane-type extraction equipment (removing minor axis ribbon blade from equipment shown in Figure 1) is used as the extraction equipment, all the other are identical with the 1st embodiment, carry out the solvent extraction of filter cake with Isosol200.Under temperature shown in the table 1, carry out, utilize the indirect heating device to heat.
Because the device of this comparative example is uniaxial ribbon vane-type, so can not realize radially fully stirring and axially forming the plunger tpe mobile basically stirring flow state, therefore also produce stirring action vertically, can think that the extraction time upward produces error to a certain degree.It the results are shown in table 1.
Table 1
The example project Embodiment Comparative example 1
????1 ????2 ????3
Cooperate weight ratio Filter cake (1) Isosol200 ????10 ????8.2 ????10 ????8.2 ????10 ????8.2 ????10 ????8.2
Condition The extraction temperature (℃) find time (branch) ????28 ????30 ????45 ????30 ????45 ????30 ????46 ????30
Waxy stone percentage extraction (2) (%) ????65 ????91 ????85 ????30
The solids component of annotating in (1) filter cake is 20 weight % (all the other are water)
(2) solids component in the filter cake is to not containing trees such as xylogen with additive method
The analysis that the waxy stone of fat composition divides is calculated
Industrial applicibility
Effect of the present invention and practicality thereof are as follows:
(1) owing to form substantially flowing when streamwise is similar to the state that plunger type flows and carry out the extraction that wax divides, so the error of extraction time is very little, therefore seldom sneaks into the lignin difficult impurity that separates that becomes to grade.
(2) can be the high solid residue of the moisture content of from the squeezing the juice of sugarcane, separating intactly as raw material.
(3) equipment of the present invention, because mixing effect is good, thereby extraction efficiency is high.
(4) equipment of the present invention can move continuously, compares with existing equipment, and the consumption of solvent is few, and the volume of extraction equipment can reduce, and disposal ability is high.
(5) have two groups of ribbon blades of leaning on and realize reciprocal mobile continuous organic solvent extracting taking equipment double ribbon vane type extrusion type structure, waxy stone, blade shape by suitably changing the ribbon blade or the pitch of spiral etc. can easily change arbitrarily inner flow regime.
(6) the continuous organic solvent extracting taking equipment that has a waxy stone of two axle splash bar type structures can form plunger type flow regime almost completely.
(7) although the moisture solid residue take filter cake as representative, show in appearance or partly the behavior as accurate viscoelastic body, therefore differ widely in physical propertys such as viscosity, proportions with the extractant of liquid state at normal temperatures, if but adopt method and apparatus of the present invention, even solid residue is contacted effectively with solvent, realize good continuous extraction.

Claims (6)

1. with the solvent method that institute's content of wax divides in the solvent extraction solid residue continuously, it is characterized in that: it is when the solid residue of separating from the squeezing the juice of sugarcane and organic extractant are applied shearing force, mixed, with the vertical direction of the moving phase of this mixture on fully stir, and streamwise forms the plunger tpe mobile basically and stirs under the flow state and extract.
2. the horizontal continuous organic solvent extracting taking equipment of waxy stone is characterized in that comprising the component part of following (1) to (3):
(1) opening is at sealed horizontal container one end, is used for supplying with continuously the solid residue separated from the squeezing the juice of sugarcane and the supplying opening of organic extractant;
(2) be located at two groups of interior stirring conveying devices of said vesse, its agitating function all is that the mixture to solid residue and organic solvent stirs when applying shearing force, though it is reciprocal that its conveying function is given the feed drive direction of mixture, then be to carry continuously to the other end in general from said vesse one end with regard to mixture; And
(3) opening is at the other end of sealed horizontal container, is used for extruding continuously the relief outlet of the mixture of above-mentioned solid residue and organic extractant.
3. the horizontal continuous organic solvent extracting taking equipment of waxy stone as claimed in claim 2 is characterized in that: above-mentioned two groups of stirring conveying devices serve as that axle is rotated with the throughput direction of mixture all.
4. the horizontal continuous organic solvent extracting taking equipment of waxy stone as claimed in claim 3 is characterized in that: have the structure that double ribbon vane-type is extruded type, it is given the conveyance drive force of direction opposite each other to mixture by two groups of ribbon blades.
5. the horizontal continuous organic solvent extracting taking equipment of waxy stone as claimed in claim 4 is characterized in that: above-mentioned two groups of ribbon blades are made up of major diameter ribbon blade and minor axis ribbon blade.
6. the horizontal continuous organic solvent extracting taking equipment of waxy stone as claimed in claim 3 is characterized in that: have any structure in two splash bar types, two collar plate shapes and two spiral types.
CN 96190741 1995-06-13 1996-06-13 Method of continuous extraction of crude wax and apparatus therefor Pending CN1161056A (en)

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JP170347/95 1995-06-13
CN 96190741 CN1161056A (en) 1995-06-13 1996-06-13 Method of continuous extraction of crude wax and apparatus therefor

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CN100427172C (en) * 2005-03-04 2008-10-22 山东大学 Apparatus for continuous extracting and sterilizing solid materials under high and ultrahigh pressure
CN100542661C (en) * 2005-09-09 2009-09-23 鸿富锦精密工业(深圳)有限公司 Cylinder mixer
CN102215929A (en) * 2008-11-07 2011-10-12 株式会社K·E·M Method of highly efficiently extracting active ingredient from plant or mushroom
CN102455330A (en) * 2010-10-27 2012-05-16 中国科学院大连化学物理研究所 Head-space liquid-phase microextraction device based on semiconductor refrigeration technology
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CN113004973A (en) * 2020-12-11 2021-06-22 海南佳士乐实业有限公司 Spices extraction smart machine
US20210269738A1 (en) * 2019-08-20 2021-09-02 Scott E. Craig Extracting essential oils
CN114225739A (en) * 2021-12-19 2022-03-25 湖南安固仕新材料有限公司 Production process of putty paste with environment-friendly and crack resistance
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100427172C (en) * 2005-03-04 2008-10-22 山东大学 Apparatus for continuous extracting and sterilizing solid materials under high and ultrahigh pressure
CN100542661C (en) * 2005-09-09 2009-09-23 鸿富锦精密工业(深圳)有限公司 Cylinder mixer
CN102215929A (en) * 2008-11-07 2011-10-12 株式会社K·E·M Method of highly efficiently extracting active ingredient from plant or mushroom
CN102455330A (en) * 2010-10-27 2012-05-16 中国科学院大连化学物理研究所 Head-space liquid-phase microextraction device based on semiconductor refrigeration technology
CN102455330B (en) * 2010-10-27 2013-07-03 中国科学院大连化学物理研究所 Head-space liquid-phase microextraction device based on semiconductor refrigeration technology
CN105107227A (en) * 2015-08-31 2015-12-02 中国农业科学院农产品加工研究所 Self-unloading hot-pressing extraction device based on combined stirring
CN108215280A (en) * 2017-12-05 2018-06-29 安徽工程大学 A kind of flat turn oil extraction machine
CN109569343A (en) * 2018-11-30 2019-04-05 文林涛 Makeup production vacuum emulsification tank
US20210269738A1 (en) * 2019-08-20 2021-09-02 Scott E. Craig Extracting essential oils
US11718811B2 (en) * 2019-08-20 2023-08-08 Scott E. Craig Extracting essential oils
CN113004973A (en) * 2020-12-11 2021-06-22 海南佳士乐实业有限公司 Spices extraction smart machine
CN115245689A (en) * 2021-04-28 2022-10-28 中国石油化工股份有限公司 Countercurrent full-immersion type spiral extractor, material extraction system and material extraction method
CN115245689B (en) * 2021-04-28 2024-05-17 中国石油化工股份有限公司 Countercurrent full-immersion type spiral leacher, material leaching system and material leaching method
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