CN102989193B - Method for purifying organic mixture in static melt crystallization - Google Patents
Method for purifying organic mixture in static melt crystallization Download PDFInfo
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Abstract
The invention relates to a method for purifying an organic mixture in static melt crystallization. By the aid of the method, the melt crystallization is conducted to the organic mixture in the magnetic filed environment. The method comprises steps of melting the organic mixture in a melt crystallizer, adding the magnetic filed in the surrounding of the melt crystallizer, adding the magnetic carrier to the organic liquid mixture, cooling crystallization, and enabling a solid product to attach to the carrier to grow gradually. When the melt crystallization operation reaches to the destination, the strength, the direction, the location, the range or the time of the magnetic field is adjusted, the crystallization is enriched, the liquid and the solid are obtained after being separated, the liquid and the carrier are obtained after the solid is heated and melted, and the carrier can be recycled after being taken out. The liquid-solid separation problem of the melt crystallization product is solved, and when the solid-liquid separation of the melt crystallization product fails through the centrifugation action or the filtration operation, the melt crystallization operation of the organic mixture system can be achieved. The method has the advantages of being low in energy consumption and capable of reusing the carrier.
Description
Technical field
The present invention relates to separation technology field, relate in particular to the method for static fusion-crystallization purification organic mixture in a kind of magnetic field environment.
Background technology
Fusion-crystallization technology is a kind of technology of utilizing the fusing point difference of each component in organic mixture to carry out separation, purifying, concentrating organic mixture, in the refining purification of chemical intermediate, medicine intermediate or biochemical product, is widely used.The organic mixture that fusion-crystallization is processed: at normal temperatures or be liquid after heating, the organic mixture being formed by a plurality of components of dissolving each other, each component fusing point has certain difference.
CN102350271A has invented a kind of melt crystallization separating device, can be widely used in organic separation.The melting crystallizer that CN102423542A provides can be widely used in the obvious isomer of all fusing point differences, the organic separation of homologue.Above-mentioned two patents have all solved existing melting crystallizer complex structure, volume is large and operation easier is large problem, and apparatus structure is simple, volume is little and easy to operate, adopt the separation of scraper accelerating solid, have reduced organic mixture loss.CN102627531A has invented a kind of water fusion-crystallization production needle-like 2, the method for 5-xylenol, and after its crystallization, system obtains 2,5-xylenol after centrifuge preliminary hydro-extraction and the dehydration of revolution vacuum desiccator two-stage.This invention can make to produce safer, reduces production costs.CN102198937A has invented a kind of method of static multistage melting crystallization method for preparing electronic grade phosphoric acid, adopts repeatedly the method for melting → purifying → row partial mother liquid, and the method is simple to operate, and energy consumption is low, and operating condition is gentle, and product purity is higher.
In static fusion-crystallization process, organic mixture liquid temp is reduced gradually, the component that fusing point is high and solubility is little is separated out with solid-state, forms crystal seed (also can directly add crystal seed in liquid); Continue to control the temperature of material, until constantly there is solid to adhere to the crystal of growing up to certain size on crystal seed, now, form solid-liquid suspensions.For static fusion-crystallization process, under the prerequisite without outfield intensifying, now the solid particle in suspension is subject to the effect of gravity and two power of buoyancy simultaneously.According to the size and Orientation of the component sum of two power vertical direction, organic mixture system can be divided into two kinds: the first, the direction of the component sum in two power vertical direction is downward, and solid particle starts to sink, until be enriched in reactor bottom; The second, the component sum in two power vertical direction is zero, the solid particle being suspended in liquid can transfixion.
For above-mentioned the second system, realize one of the problem to be solved that is effectively separated into of crystallization terminal solid-liquid product constantly.For some specific systems, because liquid viscosity is large, cannot realize by filtration effective separation of solid-liquid product; For other specific systems, because the solid product particle forming is less and density is less, cannot realize by centrifugal method effective separation of solid-liquid product.The present invention is directed to above-mentioned the second system, a kind of method that realizes fusion-crystallization operation in magnetic field environment is provided, fusion-crystallization operation with forward direction crystallizer in additional untouchable power---magnetic force, in crystallization operation process, the solid particle of formation is subject to the effect (magnetic force, gravity and buoyancy) of three power simultaneously.Crystallization terminal constantly, by regulating magnetic field intensity, scope, direction, position or changing the stress balance state of crystalline solid action time, realize the directed movement of crystalline solid and be enriched in the appointed area of melting crystallizer, thereby realize effective separation of solid-liquid product.The present invention is applicable to realize component by fusion-crystallization and purifies, but cannot obtain by conventional lock out operation the organic mixture of target product.
Summary of the invention
The object of the invention is to solve the separation problem of the solid-liquid product of fusion-crystallization terminal, the method of static fusion-crystallization purification organic mixture in a kind of magnetic field environment is provided, makes to rely on single fusion-crystallization technology to be difficult to realize the separated special organic mixture of purification and be achieved the separation of purifying.
For reaching this object, the present invention by the following technical solutions:
A method for static fusion-crystallization purification organic mixture, described method is carried out fusion-crystallization operation to organic mixture in magnetic field environment.
Specifically, said method comprising the steps of:
(1) organic mixture is placed in to melting crystallizer, it is melted completely, form liquid I;
(2), to melting crystallizer externally-applied magnetic field, make liquid I be placed in magnetic field completely;
(3) in liquid I, add magnetic carrier, it is uniformly dispersed, form carrier-liquid suspension system II;
(4) described suspension system II is carried out to decrease temperature crystalline operation, on magnetic carrier surface, form crystallization, form crystalline solid, in melting crystallizer, form suspension system III;
(5) by flux control, make crystalline solid enrichment in melting crystallizer, form system IV;
(6) described system IV is carried out to Separation of Solid and Liquid, obtain the product liquid V of solid product VI and purification.
The method of the invention is optionally carried out:
(7) by described solid product VI heating, melting forms product liquid VII and carrier;
(8) product liquid VII is separated with carrier, the carrier obtaining is reused.
Through above-mentioned steps, organic mixture is separated into product liquid V and product liquid VII, and in two kinds of product liquids, the content of target components has obvious variation compared with constituent content in organic mixture, can realize the purification of organic mixture.
The method of the invention, by melting crystallizer externally-applied magnetic field, be take magnetic retention particulate vector as crystal seed, and the solid product that crystallization process produces is attached on carrier and grows up gradually.When fusion-crystallization operation reaches terminal, by regulating action intensity, position, direction, scope or the time in magnetic field, the solid product particle that makes to be wrapped in carrier is enriched in the appointed area of crystallizer.Separation of Solid and Liquid obtains solid, after solid heat fused, magnetic carrier is taken out for recycling.The concrete operations such as heating of the present invention, fusing, cooling, fusion-crystallization, externally-applied magnetic field and modulation magnetic field, Separation of Solid and Liquid, all can be carried out according to the common practise of this area by those skilled in the art.
Organic mixture of the present invention includes but are not limited to the mixture that fine chemicals, chemicals, plant extracts organic mixture medicine, medicine intermediate, disinfectant, synthetic perfume, leather chemicals reagent, Western medicine, dyestuff intermediate, standard liquid, waste cooking oil, animal fat, vegetable fat or coating etc. are comprised of organic matter.
Under the prerequisite not changing in organic mixture physicochemical properties, the fusing mode of described step (1) can adopt any mode of heating known in those skilled in the art.The present invention can be selected from a kind of in Direct Contact Heating, liquid bath heating, heating using microwave or infrared heating, further a kind of in preferably electrical heating, heating water bath, oil bath heating or infrared heating.
Under the prerequisite not changing in organic mixture physicochemical properties, the rate of heat addition is unrestricted, carries out reasonable control and can realize the object of the invention in practical operation, can be constant speed heating, also can speed change heating.
Under the prerequisite not changing in organic mixture physicochemical properties, melt the required maximum temperature reaching and be close to or higher than in organic mixture the fusing point fusing point of high component.The maximum temperature that " being close to or higher than " of the present invention refers to when heating is at fusing point near the fusing point of high component, can make organic mixture melt completely, to guarantee being melted to the moment that adds magnetic carrier formation suspension system II after organic mixture moves to melting crystallizer, without solid organic matters (comprising the sightless micro-solid particle of naked eyes), separate out.Those skilled in the art can general knowledge and the experience according to oneself select this temperature when practical operation, for example, in organic mixture fusing point the fusing point of high component be 75 ℃, the highlyest in practical operation be heated to 76 ℃ of left and right and can make organic mixture melt completely.
Till the maximum temperature of step of the present invention (1) fusing continues to organic mixture and melts form liquid completely.Under the prerequisite not changing in organic mixture physicochemical properties, maximum temperature duration of described step (1) fusing is unrestricted, those skilled in the art rationally control in practical operation, and it is end time that the organic mixture of take melts formation liquid (not comprising the sightless micro-solid particle of naked eyes in liquid) completely.
Described melting crystallizer is the container of jacketed, and chuck is for circulation cycle heating or cooling liquid, as water, heat conduction wet goods.Its volume is unrestricted, according to producing actual needs, determines.Its shape includes but not limited to cylinder, cuboid and other suitable shapes, is preferably cylinder or cuboid.Modes of emplacement includes but not limited to vertical type, tilting or horizontal.The material of described melting crystallizer is nonmagnetic material and/or nonmetallic materials; Described nonmetallic materials are a kind of or at least combination of bi-material in glass, quartz, pottery, high molecular polymer or fiberglass; A kind of or at least combination of bi-material in the preferred lucite of described high molecular polymer, engineering plastics, resin or silica gel.Typical but non-limiting example comprises glass, pottery, fiberglass, engineering plastics, silica gel, quartzy and ceramic combination, the combination of fiberglass and lucite, the combination of resin and silica gel, the combination of engineering plastics, resin and silica gel etc.Allly in prior art bear temperature in operating temperature excursion of the present invention, can allow magnetic field to pass and can significantly not affect the combination of homogenous material well known in the art or the two kinds/two or more materials of magnetic field intensity, all can be used for implementing the present invention.
In described step (2), externally-applied magnetic field is the magnetic field that permanent magnet or galvanomagnetic-effect produce, and the magnetic field that can also adopt other modes well known in the art to produce, all can be used for implementing the present invention.
Magnetic fields position and scope are unrestricted, rationally determine and can reach the object of the invention.Described magnetic field is lasting magnetic field or pulsed magnetic field.
Magnetic field intensity can be constant, also can be that conversion occurs, the magnetic field intensity of whole fusion-crystallization process is determined as follows: suffered three power of buoyancy of the gravity that the magnetic force that magnetic fields produces on carrier, carrier are suffered and carrier component sum is in vertical direction zero, magnetic carrier is scattered in liquid I equably, to form carrier-liquid suspension system II.
Carrier not with the prerequisite of organic materials generation chemical reaction under, the described carrier of step of the present invention (3) is magnetisable material or modified magnetisable material.The magnetic material of all tools well known in the art, all can be used for the present invention.Described modification can be any modification to magnetisable material well known in the art, and chemical method is modified and Physical modification all can.
Preferably, described magnetisable material is a kind of or at least combination of bi-material in metal simple-substance, magnetic alloy or magnetic oxide, further preferable alloy simple substance; The preferred iron of described metal simple-substance, cobalt, nickel, lanthanide series metal simple substance, further preferred iron simple substance.
Preferably, described in, being modified to finishing, outside modification, interior finishing or middle part modifies.
Preferably, described in, be modified to surface finish, etching, coating or parcel; Surface parcel material therefor is plastics and/or pottery, described plastics preferably polytetrafluoroethylene.The combination of one or both of various surperficial lappings well known in the art/two or more materials, all can be used for the present invention.
Preferably, carrier be shaped as cube, spheroid, cylinder or irregularly shaped in a kind of combination of or at least two kinds of shapes; Preferably, described carrier is hollow or half hollow.At carrier, can be suspended in equably under the prerequisite in organic liquid, the shape of carrier is unrestricted, can be the regular shapes such as cube, spheroid, cylinder, also can be random form irregularly shaped, also can be regular shape and erose combination, can be also various shapes hollow, half hollow.
At carrier, can be suspended in equably under the prerequisite in liquid I, the size of carrier is unrestricted, can be single-size particle, can be also by the combination of the different size particle in certain particle size distribution.
At carrier, can be suspended in equably under the prerequisite in liquid I, in operating temperature range of the present invention, carrier material guarantees not and any component generation chemical reaction of organic mixture, and the physicochemical property of organic mixture can not change.
Described step (4) cooling method can be other fluid temperature reductions well known in the art that circulate in circulator bath cooling or chuck in chuck, also can be other cooling methods well known in the art such as wind cooling temperature lowering, be preferably the cooling of chuck fluid circulating or the wind cooling temperature lowering of melting crystallizer.Rate of temperature fall and outlet temperature determine according to the physicochemical properties of organic mixture, and take the content that can generate a certain component in solid and solid or certain several component and organic mixture has discernible macroscopical difference to control rate of temperature fall and the terminal of lowering the temperature as target.Can be temperature-reduction at constant speed, can be also speed change cooling, can be also to fall mild heat mixing carry out or hocket.The outlet temperature duration take solid particle in system grow up to the moment of the demand size terminal that is the duration constantly.
Described step (5) by regulate externally-applied magnetic field intensity, position, direction or time the chien shih crystalline solid magnetic force, gravity and three power of the buoyancy component sum in vertical direction that are subject to non-vanishing, make crystalline solid enrichment.The present invention can take at the uniform velocity to regulate, speed change regulates, magnetic field alternately has or not the regulative modes well known in the art such as adjusting, adjusting is to guarantee: the magnetic force that solid particle is subject to, gravity and three power of buoyancy component sum are in vertical direction non-vanishing, make crystalline solid move and in appointed area enrichment, be generally the bottom that is enriched in melting crystallizer along desired orientation.
The solid-liquid separating method of step of the present invention (6) can adopt solid-liquid separating method well known in the art, is preferably valve blowing, directly topples over, drainage or pumping.
Described step (7) is heated to solid product VI and melts completely.During heating terminal, solid product VI is melted to liquid completely, and carrier can wait routine operation mode to take out by filtration.The separate mode of described step (8) is for filtering or fishing for, and other separate modes that do not change the physicochemical property of liquid VII and carrier well known in the art, all can be used for the present invention.
A method for static fusion-crystallization purification organic mixture, described method specifically comprises the following steps:
(1) organic mixture is placed in to melting crystallizer, heating is melted it completely, forms liquid I, and after fusing, the volume of liquid material is advisable not overflow melting crystallizer;
(2) to melting crystallizer externally-applied magnetic field around, make the liquid I in melting crystallizer be placed in magnetic field completely;
(3) in liquid I, add magnetic carrier auxiliary stirring, carrier is uniformly dispersed under the effect in magnetic field, form uniform carrier-liquid suspension system II;
(4) step (3) gained suspension system II is carried out to decrease temperature crystalline operation, until solid product is attached on carrier and grows up to required size, form crystalline solid, in melting crystallizer, form suspension system III;
(5) regulate intensity, position, scope, direction or the time in magnetic field, make crystalline solid enrichment in melting crystallizer, form system IV;
(6) system IV step (5) being obtained is carried out Separation of Solid and Liquid, obtains the product liquid V of solid product VI and purification;
(7) solid product VI step (6) being obtained is placed in container, and heating container to solid product VI melting forms product liquid VII and carrier;
(8) liquid VII step (7) being obtained is separated with carrier, and the carrier obtaining is reused.
Compare with prior art scheme, the present invention has following beneficial effect:
The present invention carries out static fusion-crystallization operation in magnetic field environment, makes the fusion-crystallization operation of under common environment (without magnetic force) be difficult to realize to purify separated special organic mixture to be achieved to purify separated.
The inventive method solves emphatically the solid-liquid separation problem of fusion-crystallization product, is applicable to fusion-crystallization product and cannot realizes by centrifugally operated or filter operation the organic mixture system of Separation of Solid and Liquid.It is low that the inventive method has energy consumption, the reusable advantage of carrier.
Accompanying drawing explanation
Fig. 1 is the operational flowchart of the inventive method;
Fig. 2 is the vertical profile structural representation of melting crystallizer;
Fig. 3 is the cross-sectional structural representation of melting crystallizer;
Fig. 4 is carrier stress schematic diagram.
Below the present invention is described in more detail.But following example is only simple and easy example of the present invention, does not represent or limit the scope of the present invention, and protection scope of the present invention is as the criterion with claims.
The specific embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
A method for static fusion-crystallization purification organic mixture, said method comprising the steps of:
(1) organic mixture is at room temperature liquid or solid-state or solid-liquid mixed state, the material of getting certain volume is directly put in melting crystallizer, regulation and control temperature of charge (being generally heating operation), organic matter is melted completely, form liquid I, after fusing, the volume of liquid material is advisable not overflow melting crystallizer;
(2) to melting crystallizer externally-applied magnetic field around, make the liquid I in melting crystallizer be placed in magnetic field completely;
(3) in liquid I, add magnetic carrier, suitably auxiliary stirring operation is dispersed in crystallizer carrier under the effect in magnetic field, forms uniform carrier-liquid suspension system II;
(4) step (3) gained suspension system II is carried out to decrease temperature crystalline operation, with certain rate of temperature fall, cool the temperature to the temperature of appointment and keep certain hour in this temperature, until solid product is attached on carrier and grows up to required size, form suspension system III;
(5) regulate intensity, position, scope, direction or the time in magnetic field, the solid particle that makes to be wrapped in carrier moves to the direction of appointment, thereby realizes the position (being generally one end of crystallizer) that solid product is enriched in appointment, forms system IV;
(6) solid-liquid of system IV step (5) being obtained is separated, obtains product liquid V and solid product VI;
(7) solid product VI step (6) being obtained is placed in container, and heating container to solid organic matters melting forms product liquid VII and carrier;
(8) liquid VII step (7) being obtained is separated with carrier, and the carrier obtaining is for reusing.
Be below specific embodiments of the invention:
As shown in Figure 2, following examples are with height h=30cm, inner diameter d for melting crystallizer size
inthe crystallizer of=5cm is example (volume is 589ml), while adopting other size melting crystallizers, as long as carry out reasonable operation, can realize the object of the invention.Organic mixture to be purified is at room temperature solid-liquid admixture, and its character is as follows:
The concentration that requires A in purification organic mixture, makes its content be not less than 95%.
Embodiment 1
(1) organic mixture being shaken up, get 500ml and be placed in melting crystallizer, is the recirculated water of 70 ℃ to passing into temperature in melting crystallizer chuck, and constant temperature 60min, makes organic mixture be melted to liquid state completely, forms liquid I;
(2) to melting crystallizer externally-applied magnetic field around, liquid I in melting crystallizer is placed in magnetic field range completely, by electromagnetic induction, produces magnetic field, according to right-hand screw rule, determine magnetic line of force direction, make the suffered magneto motive direction of carrier upwards, continue to provide electric current and magnetic field;
(3) get ferric oxide particle (average grain diameter is 2mm, is shaped as hollow ball shape, and hollow parts spheroid average grain diameter is 1.85mm, and surface is not modified) 0.5g, as carrier; Carrier is scattered in melting crystallizer, under the effect in magnetic field, forms uniform carrier-liquid suspension system II;
(4) step (3) gained suspension system II is carried out to decrease temperature crystalline operation, recirculated water is lowered the temperature, make suspension system II with the rate of temperature fall cooling of 0.1 ℃/min, be down to 45 ℃, constant temperature 10h, in suspension system, organic solid product is separated out and is attached on carrier, forms suspension system III; Solid product contains component A, B and C simultaneously, and wherein the content of component A greatly reduces compared with the content in raw material, and the content of B component and C greatly increases compared with the content in raw material;
(5) in coil, stop passing into electric current, the crystalline solid that is wrapped in carrier is only subject to the effect of gravity and buoyancy, and downwards, move down its suffered making a concerted effort, thereby is enriched in the bottom of melting crystallizer, forms system IV;
(6) liquid in melting crystallizer is collected in container by valve blowing, obtains product liquid V, and its contained component comprises component A(96% left and right) and B component (3% left and right)+component C(1% left and right); Remaining solid product takes out and obtains solid product VI, and its contained component comprises that component A(content is less than 30%), remaining for B component and the two content sum of component C(be: the content of 100%-component A);
(7) solid product VI step (6) being obtained is placed in container, by the method for heating water bath, container is heated, the rate of heat addition with 5 ℃/min rises to 60 ℃, and at 60 ℃ of constant temperature 30min, makes the whole meltings of solid product VI form product liquid VII and carrier;
(8) adopt the carrier that the mode of fishing for obtains step (7) to take out, for reusing.
Embodiment 2
(1) organic mixture being shaken up, get 500ml and be placed in melting crystallizer, is the recirculated water of 70 ℃ to passing into temperature in melting crystallizer chuck, and constant temperature 60min, makes organic mixture be melted to liquid state completely, forms liquid I;
(2) to melting crystallizer additional hot-wire coil around, to coil, provide electric current, by electromagnetic induction, produce magnetic field, make the liquid I in melting crystallizer be placed in magnetic field range completely, according to right-hand screw rule, determine magnetic line of force direction, make the suffered magneto motive direction of carrier upwards, continue to provide electric current and magnetic field;
(3) get ferric oxide particle (average grain diameter is 2mm, is shaped as hollow ball shape, and hollow parts spheroid average grain diameter is 1mm rice, and surface is not modified) 0.5g, as carrier; Carrier is scattered in melting crystallizer, under the effect in magnetic field, forms uniform carrier-liquid suspension system II;
(4) step (3) gained suspension system II is carried out to decrease temperature crystalline operation, recirculated water is lowered the temperature, rate of temperature fall cooling 5min with 0.1 ℃/min, the alternate cycles pattern of the heating rate intensification 1min of 0.2 ℃/min is lowered the temperature, constant temperature 10h after being down to 45 ℃, in suspension system, organic solid product is separated out and is attached on carrier, forms suspension system III; Solid product contains component A, B and C simultaneously, and wherein the content of component A greatly reduces compared with the content in raw material, and the content of B component and C greatly increases compared with the content in raw material;
(5) size of current passing in coil is reduced to half, be wrapped in the stressed no longer balance of crystalline solid of carrier, downwards, move down its suffered making a concerted effort, thereby be enriched in the bottom of melting crystallizer, forms system IV;
(6) with pump, the liquid pumping in melting crystallizer is out collected in container, obtains product liquid V, its contained component comprises component A(96% left and right) and B component (3% left and right)+component C(1% left and right); Remaining solid product takes out and obtains solid product VI, and its contained component comprises that component A(content is less than 30%), remaining for B component and the two content sum of component C(be: the content of 100%-component A);
(7) solid product VI step (6) being obtained is placed in container, by electrically heated method, container is heated, the rate of heat addition with 5 ℃/min rises to 60 ℃, and at 60 ℃ of constant temperature 30min, makes the whole meltings of solid product VI form product liquid VII and carrier;
(8) adopt the carrier that filter type obtains step (7) to take out, for reusing.
Embodiment 3
(1) organic mixture being shaken up, get 500ml and be placed in melting crystallizer, is the recirculated water of 70 ℃ to passing into temperature in melting crystallizer chuck, and constant temperature 60min, makes organic mixture be melted to liquid state completely, forms liquid I;
(2) to melting crystallizer externally-applied magnetic field around, liquid I in melting crystallizer is placed in magnetic field range completely, by electromagnetic induction, produces magnetic field, according to right-hand screw rule, determine magnetic line of force direction, make the suffered magneto motive direction of carrier upwards, continue to provide electric current and magnetic field;
(3) get ferric oxide particle (average grain diameter is 2mm, is shaped as solid spherically, and surface is not modified) 0.5g, as carrier; Carrier is scattered in melting crystallizer, under the effect in magnetic field, forms uniform carrier-liquid suspension system II.
(4) step (3) gained suspension system II is carried out to decrease temperature crystalline operation, recirculated water is lowered the temperature, rate of temperature fall cooling 5min with 0.2 ℃/min, the alternate cycles pattern of the heating rate intensification 1min of 0.1 ℃/min is lowered the temperature, be down to 45 ℃, constant temperature 10h, in suspension system, organic solid product is separated out and is attached on carrier, forms suspension system III.Solid product contains component A, B and C simultaneously, and wherein the content of component A greatly reduces compared with the content in raw material, and the content of B component and C greatly increases compared with the content in raw material.
(5) by direct current, change the electric current passing in coil into alternating current, be wrapped in the stressed no longer balance of crystalline solid of carrier, resultant direction is downward, moves down, thereby is enriched in the bottom of melting crystallizer A, forms system IV;
(6) liquid in melting crystallizer is collected in container by valve blowing, obtains product liquid V, and its contained component comprises component A(96% left and right) and B component (3% left and right)+component C(1% left and right); Remaining solid product takes out and obtains solid product VI, and its contained component comprises that component A(content is less than 30%), remaining for B component and the two content sum of component C(be: the content of 100%-component A);
(7) solid product VI step (6) being obtained is placed in container, by the method for heating using microwave, container is heated, the rate of heat addition with 5 ℃/min rises to 60 ℃, and at 60 ℃ of constant temperature 30min, makes the whole meltings of solid product VI form product liquid VII and carrier;
(8) adopt the carrier that the mode of fishing for obtains step (7) to take out, for reusing.
Embodiment 4
(1) organic mixture being shaken up, get 500ml and be placed in melting crystallizer, is the recirculated water of 70 ℃ to leading to temperature in melting crystallizer chuck, and constant temperature 60min, makes organic mixing be melted to liquid state completely, forms liquid I;
(2) to melting crystallizer externally-applied magnetic field around, hot-wire coil, to coil, provide electric current, by electromagnetic induction, produce magnetic field, make the liquid I in melting crystallizer be placed in magnetic field range completely, according to right-hand screw rule, determine magnetic line of force direction, make the suffered magneto motive direction of carrier upwards, continue to provide electric current and magnetic field;
(3) get ferric oxide particle (average grain diameter is 3mm, is shaped as the hollow cubic bodily form, and hollow parts cube average grain diameter is 2.7mm, and surface is not modified) 5g, as carrier; Carrier is scattered in melting crystallizer, under the effect in magnetic field, forms uniform carrier-liquid suspension system II;
(4) step (3) gained suspension system II is carried out to decrease temperature crystalline operation, recirculated water is lowered the temperature, with the rate of temperature fall cooling of 0.1 ℃/min, be down to 45 ℃, constant temperature 10h, in suspension system, organic solid product is separated out and is attached on carrier, forms suspension system III.Solid product contains component A, B and C simultaneously, and wherein the content of component A greatly reduces compared with the content in raw material, and the content of B component and C greatly increases compared with the content in raw material.
(5) change current direction in coil, be wrapped in suffered the making a concerted effort downwards of crystalline solid of carrier, Particle Acceleration moves down, thereby is enriched in the bottom of melting crystallizer, forms system IV;
(6) liquid in melting crystallizer is collected in container by valve blowing, obtains product liquid V, and its contained component comprises component A(96% left and right) and B component (3% left and right)+component C(1% left and right); Remaining solid product takes out and obtains solid product VI, and its contained component comprises that component A(content is less than 30%), remaining for B component and the two content sum of component C(be: the content of 100%-component A);
(7) solid product VI step (6) being obtained is placed in container, by electrically heated method, container is heated, the rate of heat addition with 5 ℃/min rises to 60 ℃, and at 60 ℃ of constant temperature 30min, makes the whole meltings of solid product VI form product liquid VII and carrier;
(8) adopt the carrier that filter type obtains step (7) to take out, for reusing.
Embodiment 5
(1) organic mixture being shaken up, get 500ml and be placed in melting crystallizer, is the recirculated water of 70 ℃ to leading to temperature in melting crystallizer chuck, and constant temperature 60min, makes organic mixture be melted to liquid state completely, forms liquid I;
(2) to melting crystallizer externally-applied magnetic field around, liquid I in melting crystallizer is placed in magnetic field range completely, by electromagnetic induction, produces magnetic field, according to right-hand screw rule, determine magnetic line of force direction, make the suffered magneto motive direction of carrier upwards, continue to provide electric current and magnetic field;
(3) get ferric oxide particle (average grain diameter is 3mm, is shaped as the hollow cubic bodily form, and hollow parts cube average grain diameter is 1mm, and surface is not modified) 5g, as carrier; Carrier is scattered in melting crystallizer, under the effect in magnetic field, forms uniform carrier-liquid suspension system II;
(4) step (3) gained suspension system II is carried out to decrease temperature crystalline operation, recirculated water is lowered the temperature, rate of temperature fall cooling 5min with 0.1 ℃/min, the alternate cycles pattern of the heating rate intensification 1min of 0.2 ℃/min is lowered the temperature, be down to 45 ℃, constant temperature 10h, in suspension system, organic solid product is separated out and is attached on carrier, forms suspension system III.Solid product contains component A, B and C simultaneously, and wherein the content of component A greatly reduces compared with the content in raw material, and the content of B component and C greatly increases compared with the content in raw material.
(5) tilt coil is 60 °, and be wrapped in magnetic force size that the crystalline solid of carrier is subject to and become original half, stressed no longer balance, it is made a concerted effort downwards, and particle moves down, thereby is enriched in the bottom of melting crystallizer, forms system IV;
(6) liquid in melting crystallizer is collected in container by drainage, obtains product liquid V, and its contained component comprises component A(96% left and right) and B component (3% left and right)+component C(1% left and right); Remaining solid product takes out and obtains solid product VI, and its contained component comprises that component A(content is less than 30%), remaining for B component and the two content sum of component C(be: the content of 100%-component A);
(7) solid product VI step (6) being obtained is placed in container, by the method for infrared heating, container is heated, the rate of heat addition with 5 ℃/min rises to 60 ℃, and at 60 ℃ of constant temperature 30min, makes the whole meltings of solid product VI form product liquid VII and carrier;
(8) adopt the carrier that the mode of fishing for obtains step (7) to take out, for reusing.
Embodiment 6
(1) organic mixture being shaken up, get 500ml and be placed in melting crystallizer, is the recirculated water of 70 ℃ to leading to temperature in melting crystallizer chuck, and constant temperature 60min, makes organic mixture be melted to liquid state completely, forms liquid I;
(2) to melting crystallizer externally-applied magnetic field around, hot-wire coil, to coil, provide electric current, by electromagnetic induction, produce magnetic field, make the liquid I in melting crystallizer be placed in magnetic field range completely, according to right-hand screw rule, determine magnetic line of force direction, make the suffered magneto motive direction of carrier upwards, continue to provide electric current and magnetic field;
(3) get ferric oxide particle (average grain diameter is 1mm, is shaped as solid elliposoidal, and surface is through etching) 1g, as carrier; Carrier is scattered in melting crystallizer, under the effect in magnetic field, forms uniform carrier-liquid suspension system II.
(4) step (3) gained suspension system II is carried out to decrease temperature crystalline operation, recirculated water is lowered the temperature, with the rate of temperature fall cooling of 0.1 ℃/min, be down to 45 ℃, constant temperature 10h, in suspension system, organic solid product is separated out and is attached on carrier, forms suspension system III.Solid product contains component A, B and C simultaneously, and wherein the content of component A greatly reduces compared with the content in raw material, and the content of B component and C greatly increases compared with the content in raw material.
(5) electric current in coil is diminished gradually to zero, be wrapped in the stressed no longer balance of crystalline solid of carrier, it is made a concerted effort downwards, and particle moves down, thereby is enriched in the bottom of melting crystallizer, forms system IV;
(6) liquid in melting crystallizer is collected in container by directly toppling over, and obtains product liquid V, and its contained component comprises component A(96% left and right) and B component (3% left and right)+component C(1% left and right); Remaining solid product takes out and obtains solid product VI, and its contained component comprises that component A(content is less than 30%), remaining for B component and the two content sum of component C(be: the content of 100%-component A);
(7) solid product VI step (6) being obtained is placed in container, by the method for heating water bath, container is heated, the rate of heat addition with 5 ℃/min rises to 60 ℃, and at 60 ℃ of constant temperature 30min, makes the whole meltings of solid product VI form product liquid VII and carrier;
(8) adopt the carrier that filter type obtains step (7) to take out, for reusing.
Through the inventive method, organic mixture is separated into product liquid V and product liquid VII, in two kinds of product liquids, the content of target components A is respectively 96% and be less than 30%, in two kinds of product liquids, the content of component A is compared with the content in raw material, all there is obvious change, but the amount of product liquid VII is compared with the amount much less of product liquid V, so, realize the purification of component A in organic mixture.
Applicant's statement, the present invention illustrates method of purification of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned purification step, does not mean that the present invention must rely on above-mentioned purification step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to the selection of the interpolation of the equivalence replacement of the selected organic mixture of the present invention and auxiliary element, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (32)
1. a method for static fusion-crystallization purification organic mixture, is characterized in that, described method is carried out fusion-crystallization operation to organic mixture in magnetic field environment;
Said method comprising the steps of:
(1) organic mixture is placed in to melting crystallizer, it is melted completely, form liquid I;
(2), to melting crystallizer externally-applied magnetic field, make liquid I be placed in magnetic field completely;
(3) in liquid I, add magnetic carrier, it is uniformly dispersed, form carrier-liquid suspension system II;
(4) described suspension system II is carried out to decrease temperature crystalline operation, on magnetic carrier surface, form crystallization, form crystalline solid, in melting crystallizer, form suspension system III;
(5) by flux control, make crystalline solid enrichment in melting crystallizer, form system IV;
(6) described system IV is carried out to Separation of Solid and Liquid, obtain the product liquid V of solid product VI and purification.
2. the method for claim 1, is characterized in that, described method is optionally carried out:
(7) by described solid product VI heating, melting forms product liquid VII and carrier;
(8) product liquid VII is separated with carrier, the carrier obtaining is reused.
3. method as claimed in claim 1 or 2, it is characterized in that, described organic mixture comprises fine chemicals, chemicals, plant extracts organic mixture medicine, medicine intermediate, disinfectant, synthetic perfume, leather chemicals reagent, Western medicine, dyestuff intermediate, standard liquid, waste cooking oil, animal fat, vegetable fat or coating.
4. method as claimed in claim 1 or 2, is characterized in that, the fusing mode of described step (1) is a kind of in Direct Contact Heating, liquid bath heating, heating using microwave or infrared heating.
5. method as claimed in claim 4, is characterized in that, the fusing mode of described step (1) is a kind of in electrical heating, heating water bath, oil bath heating or infrared heating.
6. method as claimed in claim 1 or 2, is characterized in that, described step (1) be molten into constant speed heating or speed change heating.
7. method as claimed in claim 1 or 2, is characterized in that, the required maximum temperature reaching of fusing of described step (1) is close to or higher than in organic mixture the fusing point fusing point of high component.
8. method as claimed in claim 1 or 2, is characterized in that, till the maximum temperature of described step (1) fusing continues to organic mixture and melts form liquid completely.
9. method as claimed in claim 1 or 2, is characterized in that, the container that described melting crystallizer is jacketed, and described chuck is for circulation cycle heating or cooling liquid.
10. method as claimed in claim 1 or 2, is characterized in that, described melting crystallizer be shaped as cylinder or cuboid; Modes of emplacement is vertical type, tilting or horizontal.
11. methods as claimed in claim 1 or 2, is characterized in that, the material of described melting crystallizer is nonmagnetic material and/or nonmetallic materials; Described nonmetallic materials are a kind of or at least combination of bi-material in glass, quartz, pottery, high molecular polymer or fiberglass.
12. methods as claimed in claim 11, is characterized in that, described high molecular polymer is a kind of or at least combination of bi-material in lucite, engineering plastics, resin or silica gel.
13. methods as claimed in claim 1 or 2, is characterized in that, in described step (2), externally-applied magnetic field is the magnetic field that permanent magnet or galvanomagnetic-effect produce.
14. methods as claimed in claim 1 or 2, is characterized in that, described magnetic field is lasting magnetic field or pulsed magnetic field.
15. methods as claimed in claim 1 or 2, it is characterized in that, suffered three power of buoyancy of the gravity that the magnetic force that magnetic fields produces on carrier in fusion-crystallization process, carrier are suffered and carrier component in vertical direction be combined into zero, magnetic carrier is scattered in liquid I equably, to form carrier-liquid suspension system II.
16. methods as claimed in claim 1 or 2, is characterized in that, the described magnetic carrier of step (3) is magnetisable material or modified magnetisable material.
17. methods as claimed in claim 16, is characterized in that, described magnetisable material is a kind of or at least combination of bi-material in metal simple-substance, magnetic alloy or magnetic oxide.
18. methods as claimed in claim 17, is characterized in that, described magnetisable material is metal simple-substance.
19. methods as claimed in claim 18, is characterized in that, described metal simple-substance is iron, cobalt, nickel, lanthanide series metal simple substance.
20. methods as claimed in claim 19, is characterized in that, described metal simple-substance is iron simple substance.
21. methods as claimed in claim 16, is characterized in that, described in be modified to finishing, outside modification, interior finishing or middle part is modified.
22. methods as claimed in claim 21, is characterized in that, described finishing is polishing, etching, coating or parcel; Surface parcel material therefor is plastics and/or pottery.
23. methods as claimed in claim 22, is characterized in that, described plastics are polytetrafluoroethylene (PTFE).
24. methods as claimed in claim 1 or 2, is characterized in that, carrier be shaped as cube, spheroid, cylinder or irregularly shaped in a kind of combination of or at least two kinds of shapes.
25. methods as claimed in claim 1 or 2, is characterized in that, described carrier is hollow or half hollow.
26. methods as claimed in claim 9, is characterized in that, the cooling of chuck fluid circulating or wind cooling temperature lowering that the cooling method of described step (4) is melting crystallizer.
27. methods as claimed in claim 26, is characterized in that, described cooling is temperature-reduction at constant speed, speed change cooling or falls mild heat mixing and carry out or the cooling that hockets.
28. methods as claimed in claim 1 or 2, it is characterized in that, described step (5) by regulate externally-applied magnetic field intensity, position, direction or time the chien shih crystalline solid magnetic force, gravity and three power of the buoyancy component sum in vertical direction that are subject to non-vanishing, make crystalline solid enrichment.
29. methods as claimed in claim 2, is characterized in that, the solid-liquid separating method of described step (6) is valve blowing, directly topple over, drainage or pumping.
30. methods as claimed in claim 2, is characterized in that, described step (7) is heated to solid product VI and melts completely.
31. methods as claimed in claim 2, is characterized in that, the separate mode of described step (8) is for filtering or fishing for.
32. methods as claimed in claim 1 or 2, is characterized in that, said method comprising the steps of:
(1) organic mixture is placed in to melting crystallizer, heating is melted it completely, forms liquid I, and after fusing, the volume of liquid material is advisable not overflow melting crystallizer;
(2) to melting crystallizer externally-applied magnetic field around, make the liquid I in melting crystallizer be placed in magnetic field completely;
(3) in liquid I, add magnetic carrier auxiliary stirring, carrier is uniformly dispersed under the effect in magnetic field, form uniform carrier-liquid suspension system II;
(4) step (3) gained suspension system II is carried out to decrease temperature crystalline operation, until solid product is attached on carrier and grows up to required size, form crystalline solid, in melting crystallizer, form suspension system III;
(5) regulate intensity, position, scope, direction or the time in magnetic field, make crystalline solid enrichment in melting crystallizer, form system IV;
(6) system IV step (5) being obtained is carried out Separation of Solid and Liquid, obtains the product liquid V of solid product VI and purification;
(7) solid product VI step (6) being obtained is placed in container, and heating container to solid product VI melting forms product liquid VII and carrier;
(8) liquid VII step (7) being obtained is separated with carrier, and the carrier obtaining is reused.
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