CN101525283A - Zone melting purification device and method of purifying phenylformic acid by adopting same - Google Patents
Zone melting purification device and method of purifying phenylformic acid by adopting same Download PDFInfo
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- CN101525283A CN101525283A CN200910129342A CN200910129342A CN101525283A CN 101525283 A CN101525283 A CN 101525283A CN 200910129342 A CN200910129342 A CN 200910129342A CN 200910129342 A CN200910129342 A CN 200910129342A CN 101525283 A CN101525283 A CN 101525283A
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Abstract
The invention belongs to the technical field of material purification and relates to a zone melting purification device and a method for purifying phenylformic acid by adopting the same, wherein, the zone melting purification device comprises a long-cylindrical sample tube used for containing a sample to be purified, a support component which comprises a base and a bracket fixed on the base and used for supporting and fixing the sample tube, at least one heating furnace which is sleeved on the sample tube and can move up and down along the sample tube, a temperature controller used for adjusting the temperature of the heating furnace, a driving component which is connected with the heating furnace and drives the heating furnace to move up and down along the sample tube, and the zone melting purification device further comprises an angle adjuster which is used for adjusting the inclination of the sample tube. By adopting the device for purifying the phenylformic acid, the up-down movement and the temperature of a furnace body of the heating furnace can be accurately and automatically controlled without the need of monitoring the whole purifying process by persons, and the invention has high automation degree and high purification efficiency with the phenylformic acid purity of 99.999 percent (mol ratio).
Description
Technical field
The invention belongs to material purification techniques field, more specifically, relate to a kind of zone melting purification device and benzoic method of this device purification of employing of using the liquid-solid equilibrium principle.
Background technology
Zone melting is according to the liquid-solid equilibrium principle, utilizes fusion-solidification process to remove the method for impurity.Zone melting is mainly used in the ultrapure purifications of material such as metal, semiconductor material, organic crystal compound.Along with science and technology development, zone melting has been penetrated into emerging fields such as chemical industry, medicine, standard reagent, single crystal growth, raw material of optical fibre, eutectic composites, becomes a kind of widespread use, general effective important purification techniques.
The principle of zone melting as shown in Figure 1, when the tabetisol when the solid chemical compound of fusing point is arranged because impurity is different with distribution coefficient in the liquid phase in solid phase, make in this solid chemical compound impurity the tabetisol by after redistributed.In actually operating, by pipe being adorned fusible material local heating, make it produce zone melting, and along with heating region continuous circulation of permanent low speed on operative orientation is moved, make impurity in the material constantly produce zone precipitation or classification floating life, concentrate in the end of pipe dress material at last and remove, repeat the tabetisol course, just can obtain highly purified material, reach highly purified purpose.
Country's combustion heat benchmark comprises benchmark calorimeter, high-purity benzene formic acid purifying plant, primary standard material phenylformic acid composition, shows the hierarchical relationship of national combustion heat benchmark as Fig. 2.Country's combustion heat benchmark is China's combustion heat value transmission and the measurement instrument of the highest ranking of tracing to the source, and can trace to the source to voltage, resistance, time fundamental physical quantity with the benzoic combustion heat value of country-level reference material of benchmark calorimeter measurement.Is that standard heat of combustion value with primary standard material phenylformic acid (high-purity benzene formic acid) is that carrier carries out in the transmission of China's combustion heat value with tracing to the source.Determine that with relative measurement method the national grade ii standard material phenylformic acid of combustion heat value is directly used in the calorimetric calibration of combustion heat surveying instrument oxygen bomb in the fields such as the electric power enterprise of coal trade settlement, thermal power generation, defence and military scientific research, the material energy with primary standard material phenylformic acid.
The benzoic purity requirement of one-level heat reference material is more than 99.99% (mol ratio), and the pure reagent purity of phenylformic acid general analysis is 99.5%, can reach 99.9% through recrystallization, distillation purification purity, general method of purification can't improve benzoic purity again.In order to obtain the primary standard material phenylformic acid that purity is 99.99% (mol ratio), usually adopt the zone melting method phenylformic acid of purifying, existing zone melting purification device, moving up and down with temperature of process furnace controlled and can not accurately automatically be controlled, must the time be carved with the people and monitor whole purification process, thereby consumption people consuming time, level of automation is not high, thus purification efficiency is not high.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the purpose of this invention is to provide a kind of zone melting purification device controlled and that precision is high of operating.
Another object of the present invention provides a kind of employing zone melting purification device of the present invention benzoic method of purifying.
To achieve these goals, according to an aspect of the present invention, the invention provides a kind of zone melting purification device, this device comprises,
Sample hose, it is an elongated cylindrical, is used for splendid attire sample to be purified;
Support component, it comprises base and the support that is fixed on the base, is used for supporting and the fixed sample pipe;
At least one process furnace, it is placed on the sample hose, and can move up and down along sample hose;
Temperature controller is used to regulate the furnace body temperature of process furnace; With
Drive disk assembly is connected with process furnace, and the drive process furnace moves up and down along sample hose.
Be described in more detail below zone melting purification device of the present invention.
Described sample hose, it is an elongated cylindrical, is used for splendid attire sample to be purified.As preferably, this sample hose material is selected acidproof hard glass, because the glass chemistry stable in properties, and can sample not polluted, and be easy to observe the melting zone situation, and heat conductance is little, and it is fast to conduct heat, and thermosteresis is less, helps the melting zone and produces.When sample to be purified was phenylformic acid, the internal diameter of preferred sample hose was 2.5～2.7cm, and length is 29～31cm.
Described support component comprises base and the support that is fixed on the base, is used for supporting and the fixed sample pipe.For example, at least one end of the upper and lower ends of described sample hose is fixed on the support.
Described process furnace can be for one or more, and are preferably two process furnace, and two process furnace are connected.Each process furnace is the cylindrical furnace of hollow, and hollow space is used to pass sample hose; Be the diagonal angle state in the body of heater four heater air flow pressure switch rods evenly are set, for the well heater that guarantees process furnace conducts heat fast and sample is heated evenly, body of heater employing aluminum alloy materials; Inlay bar-shaped 100 Ω platinum-resistance thermometers in the body of heater and measure furnace body temperature; Body of heater arranged outside tetrafluoroethylene thermal insulation layer is to reduce calorific loss.
When preferred two process furnace, the height of two process furnace is identical, the height that is spaced apart a process furnace between the process furnace, i.e. and the design of the width in a tabetisol can improve purification efficiency.
Described temperature controller, each process furnace disposes temperature controller separately, is used to regulate and control the furnace body temperature of process furnace.The AL-519 type Artificial intelligence industry regulator that temperature controller can select for use Xiamen space electric automation Science and Technology Ltd. to produce is regulated, is controlled furnace body temperature by the heater voltage of control process furnace, and temperature control precision is at 0.1 ℃.
In actual applications, adopt two process furnace usually, can improve purification efficiency.But because the working order of two process furnace is inequality, for example: if the process furnace travel direction is from the top down, the process furnace of walking below will be heated to sample temperature of fusion formation melting zone from room temperature, and the power that needs will be greatly.Along with following process furnace leaves gradually, the sample melting zone begins to form the solid state crystallization body, and the process furnace heated sample that the influence of the surplus temperature of sample and heat be easier upwards above conduction makes melts once more that to form the needed heating power in melting zone relative smaller.Therefore, the power of two process furnace or furnace body temperature are set can not be the same, should with two independently temperature controller control the heating power of two process furnace respectively, in purification process, can observe two melting zones and two intermediary sample xln zones, melting zone (solid-state areas) so significantly.If two process furnace come controlled temperature with the heating power of same temperature controller control heater, can only form a sample melting zone, this point is verified by experiment.
Usually, when sample to be purified is phenylformic acid, preferred two process furnace, the spacing between the height of process furnace and the described adjacent process furnace is 4～4.5cm.Benzoic temperature of fusion is 122～123 ℃, and general furnace body temperature is controlled at about 130～135 ℃, and heating power is 50～100 watts, if the process furnace travel direction is from the top down, stove was about 2～3 ℃ under last stove setting furnace body temperature was lower than, otherwise opposite.
Described drive disk assembly, it comprises synchronous machine, gear drive, worm gear and endless screw speed changer, driving chain and guide deflection sheave, described synchronous machine is connected with gear drive, described gear drive is connected with worm gear and endless screw speed changer, described worm gear and endless screw speed changer connects a rotation axis, on the described rotation axis transmitting gear is set, the two ends of described driving chain are connected with the lower end of the upper end of topmost process furnace and bottom process furnace respectively, described driving chain is walked around guide deflection sheave and the transmitting gear on the support respectively, and described guide deflection sheave is arranged on the top and bottom of support.
As preferably, described synchronous machine slows down through gear drive and worm gear and endless screw speed changer, calculates reduction ratio by linear velocity, and linear velocity is 3.5～5cm/h, and preferred 4cm/h.For example, drawing final reduction ratio according to rotating speed of motor design step down gear is 320: 1, and promptly the process furnace translational speed is 4cm/h.
As preferably, zone melting purification device of the present invention may further include one and regulates the angle demodulator of sample hose obliquity.Described angle demodulator comprises: two strongbacks and the locating shaft that are relatively arranged on the base both sides respectively, described base is fixed on the locating shaft, the two ends of described locating shaft are connected with two strongback bearings respectively, base can be rotated with locating shaft, described base and strongback are provided with fanning strip on corresponding at least one side, a plurality of pilot holes are set on the described fanning strip, the curved setting on fanning strip of described a plurality of pilot hole, the latch that can pass strongback and match with pilot hole is set on the described strongback, and described latch is positioned at the top of locating shaft.
According to a further aspect in the invention, provide a kind of employing aforementioned region fusion of the present invention purifying plant benzoic method of purifying, this method comprises the steps:
(1) it is in the sample hose of 2.5～2.7cm that phenylformic acid powder that will be to be purified is inserted end sealing internal diameter, is filled to apart from about the opening part 5cm, seals with sealing film, fixes sample hose by aforementioned region fusion purifying plant of the present invention;
(2) process furnace is moved to the bottom of sample hose;
(3) power-on, start synchronous machine, process furnace is moved up along sample hose, and translational speed is controlled at 3.5～5cm/h, preferred 4cm/h, the furnace body temperature of setting process furnace is at 130～135 ℃, the sample melting zone generates situation in the observation sample pipe, and along with the formation in sample melting zone, the formation of xln, sample subsides in the sample hose, open upper end open then, insert sample again;
(4) carry out repeatedly step (3) repeatedly, until the sample xln apart from sample hose upper end open 5～10cm place;
(5) then, directly process furnace is moved to the top of sample hose;
(6) power-on, start synchronous machine, process furnace is moved down along sample hose, speed control is at 3.5～5cm/h, preferred 4cm/h, and the furnace body temperature of setting process furnace is at 130～135 ℃, observes in the sample hose that is in the process furnace position sample and all is molten state and forms one or more melting zones;
(7) when process furnace moves to the bottom of sample hose, repeating step (5) and step (6) repeatedly obviously are sundown in the lower end of sample hose, promptly finish purification; With
(8) after purification is finished, sample hose is taken off, intercept middle two/part, promptly obtain the phenylformic acid of needed purification.
As preferably, adopt two process furnace, furnace body temperature is controlled at about 130～135 ℃, heating power is 50～100 watts, and when the process furnace travel direction be from bottom to top the time, last stove is set furnace body temperature and is higher than down about 2～3 ℃ in stove; When the process furnace travel direction is from the top down the time, last stove is set furnace body temperature and is lower than down about 2～3 ℃ in stove.
Select two or more process furnace to consider,, just be equal to a process furnace and move twice along the sample hose total length, so saved the time with 4cm/h when two process furnace move once along the sample hose total length with 4cm/h simultaneously from time factor.And during two process furnace, the height that is spaced apart a process furnace between the process furnace, the i.e. design of the width in a tabetisol, be in order in short as far as possible distance, to form the purpose that two melting zones reach twice purification, make the sample of sample hose middle portion obtain the purification number of times of as much, so that guarantee smart benzoic quality and the quantum of output of purifying, improve purification efficiency.
Compared with prior art, beneficial effect of the present invention is:
1, the present invention can adopt a plurality of especially double furnaces to heat synchronously, and the width that is spaced apart a process furnace of the process furnace i.e. width in a tabetisol designs, and quality and raising purification efficiency can guarantee to purify.
2, can slow down by synchronous machine and wheel box, make the translational speed of process furnace accurately be controlled at 4cm/h, satisfy the needs of phenylformic acid zone melting purification.
3, the angle of inclination of sample hose can help regulating according to the experiment situation sectional area in sample melted district by angle demodulator free adjustment in the scope of 20～90 degree among the present invention, reduces inner tensions, prevents that sample hose from bursting.
4, double furnace is carried out temperature control respectively by the two-way temperature regulator, thereby make the temperature difference of two process furnace.Can be according to the factors such as angle of inclination of laboratory environment temperature and sample hose by observing the controlled temperature that benzoic molten state is set process furnace respectively.Benzoic temperature of fusion is 122～123 ℃, and general temperature is controlled at about 130～135 ℃, 50～100 watts of heating powers, along the process furnace travel direction, move the design temperature of process furnace the preceding be higher than move after 2～3 ℃ of the design temperatures of process furnace.
5, the sample hose material is selected acidproof hard glass.The glass chemistry stable in properties can not pollute, be easy to observe the melting zone situation to sample, and heat conductance is little, the fast thermosteresis of conducting heat is less, helps the melting zone and produces.
6, zone melting purification device of the present invention is not only unidirectional moves the purification be used for sample, and two-way when mobile when process furnace, and impurity is evenly distributed in the sample, realizes adulterated purpose.
Description of drawings
Fig. 1 is the zone melting principle schematic.
Fig. 2 shows the hierarchical relationship of national combustion heat benchmark.
Fig. 3 is the structural representation of zone melting purification device embodiment one of the present invention.
Fig. 4 is the one-piece construction synoptic diagram of zone melting purification device embodiment two of the present invention.
Fig. 5 is the right side view of Fig. 4.
Fig. 6 is the angle demodulator synoptic diagram of zone melting purification device of the present invention.
Fig. 7 is the structural representation of the fanning strip in the zone melting purification device of the present invention.
Fig. 8 is the structural representation of the vertical section of the process furnace of zone melting purification device of the present invention.
Fig. 9 is the structural representation of the cross section of the process furnace of zone melting purification device of the present invention.
Description of reference numerals
The 1-sample hose
101-base 102-support
The 103-crossbeam
201-synchronous machine 202-gear drive
203-worm gear and endless screw speed changer 204-reduction box
The 205-first transmitting gear 206-second transmitting gear
The 207-first guide deflection sheave 208-second guide deflection sheave
210-the 4th guide deflection sheave 211-first driving chain
The 212-second driving chain 213-rotation axis
214-the 5th guide deflection sheave 215-the 6th guide deflection sheave
216-the 8th guide deflection sheave
The 301-first process furnace 302-second process furnace
303-well heater 304-two-way temperature controller
305-rigid connector 306-thermometer
307-thermal insulation layer 308-first temperature control instrument
309-second temperature control instrument
401-locating shaft 402-first strongback
The 403-second strongback 404-fanning strip
405-pilot hole 406-latch
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail, but not as a limitation of the invention.
Embodiment one
Zone melting purification apparatus structure synoptic diagram as shown in Figure 3, comprise sample hose 1, support component (not shown), process furnace and drive disk assembly, described sample hose 1 is an elongated cylindrical, be used for the sample that splendid attire is purified, described drive disk assembly comprises synchronous machine 201, reduction box 204, first driving chain 211 and second driving chain 212, synchronous machine 201 drives after reduction box 204 slows down and is placed in reduction box 204 same last first transmitting gears 205 of axle and 206 rotations of second transmitting gear, thereby drives two driving chains 211 and 212 transmissions.
Process furnace is for the sample in the sample hose provides thermal source, makes it produce the tabetisol, so process furnace also can be replaced by the other forms of product of thermal source that can provide.Process furnace in the present embodiment is first process furnace 301, because first process furnace 301 is connected in the two ends of first driving chain 211 and second driving chain 212 simultaneously, therefore, can move up and down with driving chain.Linear velocity after the translational speed of first process furnace 301 and motor slow down is identical.
Support component in the present embodiment does not illustrate, and support component is used for support fixation sample hose 1, is used for fixing a plurality of guide deflection sheaves yet, and a plurality of guide deflection sheaves are respectively applied for the guiding of first driving chain 211 and second driving chain 212.
Embodiment two
As Fig. 4, shown in Figure 5, zone melting purification device of the present invention comprises: be used for the purified sample hose 1 of sample of splendid attire; Be used to support support component with fixed sample pipe 1; Be placed on the sample hose 1, and the process furnace that can move up and down along sample hose 1; Be connected with process furnace and drive the drive disk assembly that process furnace moves.
The material of sample hose 1 is selected acidproof hard glass.The glass chemistry stable in properties can not pollute sample, be easy to observe the melting zone situation, and heat conductance is little, heat transfer is fast, thermosteresis is less, helps the melting zone and produces.
Support component comprises base 101 and the support 102 that is fixed on the base, and the upper end of support 102 is provided with crossbeam 103, and crossbeam 103 middle parts have pilot hole, and sample hose 1 is arranged in pilot hole, so sample hose 1 is fixed on the support 102 by the pilot hole on the crossbeam 103.Certainly, crossbeam 103 also can be arranged on support 102 lower ends, or the top and bottom of support 102 all are provided with crossbeam 103, and is fixing simultaneously from upper/lower terminal to sample hose 1.In the present embodiment, on the top of support 102 first guide deflection sheave 207 is set respectively, second guide deflection sheave 208, the 3rd guide deflection sheave (not shown) and the 4th guide deflection sheave 210, the 5th guide deflection sheave 214 is set in the bottom of support 102 simultaneously, the 6th guide deflection sheave 215, the 7th guide deflection sheave (not shown) and the 8th guide deflection sheave 216, first driving chain 211 is through first guide deflection sheave 207 and second guide deflection sheave 208 of support 102 upper ends, the 5th guide deflection sheave 214 of support 102 lower ends, the 6th guide deflection sheave 215 guiding, second driving chain 212 is through the 3rd guide deflection sheave (not shown) and the 4th guide deflection sheave 210 guiding, the 7th guide deflection sheave (not shown) of support 102 lower ends and the 8th guide deflection sheave 216 guiding.
Described process furnace is two, promptly is connected by rigid connector 305 between first process furnace 301 and second process furnace, 302, the first process furnace 301 and second process furnace 302.The height of two process furnace is identical with spacing between two process furnace, is 4～4.5cm.This design can improve purification efficiency.Certainly, what the quantity of process furnace also can be for except that two is more a plurality of, can make different selections as required in actual production and experiment.As Fig. 8, shown in Figure 9, two process furnace are the cylindrical furnace of hollow, and hollow space is used to wear sample hose 1, be the diagonal angle state in the body of heater four heater air flow pressure switch rods 303 evenly are set, body of heater arranged outside tetrafluoroethylene thermal insulation layer 307 is to reduce calorific loss.For the well heater 303 that guarantees process furnace conducts heat fast and sample is heated evenly, body of heater employing aluminum alloy materials.
Two process furnace can improve purification efficiency, but because the working order of first process furnace 301 and second process furnace 302 is inequality, for example: if the travel direction of two process furnace is from the top down, second process furnace of walking below 302 will be heated to sample temperature of fusion formation melting zone from room temperature, and the power that needs will be greatly.Along with leaving gradually of second process furnace 302, the sample melting zone begins to form the solid state crystallization body, and first process furnace, 301 heated sample that the influence of the surplus temperature of sample and heat be easier upwards above conduction makes melt once more that to form the needed heating power in melting zone relative smaller.The power of obvious two process furnace or temperature are set can not be the same, therefore in the body of heater of two process furnace, inlay bar-shaped 100 Ω platinum-resistance thermometers 306 respectively and measure furnace body temperatures, can be according to the factors such as angle of inclination of laboratory environment temperature and sample hose 1 by observing the controlled temperature that benzoic molten state is set process furnace respectively.As the phenylformic acid of purifying, according to benzoic temperature of fusion is 122～123 ℃, and general temperature is controlled at about 130～135 ℃, and the heating power of process furnace is controlled at 50～100 watts, two process furnace move from the top down, low about 2～3 ℃ of the temperature of first process furnace, 301 to the second process furnace 302.Therefore independently first temperature control instrument 308 and second temperature control instrument 309 are controlled the heating power of two process furnace respectively to use two in the present embodiment, two AL-519 type Artificial intelligence industry regulator adjustings that temperature control instrument all selects for use Xiamen space electric automation Science and Technology Ltd. to produce, by regulating, control the heater voltage controlled temperature of two process furnace, 0.1 ℃ of temperature control precision.For simplified construction, with two independently temperature control instrument be integrated into a two-way temperature regulator 304.In purification process, can observe two melting zones and two intermediary sample xln zones, melting zone (solid-state areas) so significantly.
Described drive disk assembly comprises synchronous machine 201, gear drive 202, worm gear and endless screw speed changer 203, first driving chain 211 and second transmission chain 212, synchronous machine 201 is connected with gear drive 202, gear drive 202 is connected with worm gear and endless screw speed changer 203, worm gear and endless screw speed changer 203 connects a rotation axis 213, first transmitting gear 205 and second transmitting gear 206 are set on the rotation axis 213, first driving chain 211 is walked around first transmitting gear 205 respectively, the 5th guide deflection sheave 214, first guide deflection sheave 207, second guide deflection sheave 208 and the 6th guide deflection sheave 215, the second driving chains 212 are walked around second transmitting gear 206 respectively, the 7th guide deflection sheave, the 3rd guide deflection sheave, the 4th guide deflection sheave 210 and the 8th guide deflection sheave 216.Certainly, the 6th guide deflection sheave 215 and the 8th guide deflection sheave 216 that are positioned at support 102 lower ends can omit, and directly promptly make power wheel by first transmitting gear 205 and second transmitting gear 206 and make guide deflection sheave again.Synchronous machine 201 slows down after speed change, and reduction ratio is 320: 1, linear velocity 4cm/h, and promptly the translational speed of two process furnace is 4cm/h.Can control the translational speed of process furnace by regulating synchronous machine and ratio of gear.
Certainly, as required, the quantity of driving chain can be one or more, moves up and down reposefully under the drive of driving chain as long as can guarantee process furnace.
Embodiment three, four
Long-pending in order to make sample hose 1 can be in different angles of inclination to strengthen sample in cross section, reduce the sample hose inner tensions and prevent that sample hose from bursting, present embodiment three, four with embodiment one, two difference only is, increased an angle demodulator as shown in Figure 6, comprise first strongback 402 that is relatively arranged on the base both sides respectively, second strongback 403 and locating shaft 401, base 101 is fixed on the locating shaft 401, the two ends of locating shaft 401 are connected with two strongback bearings respectively, base 101 can be rotated with locating shaft 401, on base 101 and first strongback, the 402 corresponding sides fanning strip 404 is set, as shown in Figure 7, seven pilot holes 405 are set on the fanning strip 404, seven pilot hole 405 curved settings on fanning strip 404, be provided with on first strongback 402 and can pass first strongback 402 and the localized latch 406 that can match with pilot hole 405, latch 406 is positioned at the top of locating shaft 401.
According to the experiment situation, regulate the sectional area in sample melted district when needs, when reducing inner tensions, sample hose 1 can be tilted, as long as removed base 101 and support 102, whole support component just rotates up with locating shaft 401, and the fanning strip 404 that is arranged on base 101 sides also moves with base 101, thereby the pilot hole 405 that matches with latch 406 is changed.For example when support component and sample hose 1 vertical the placement, latch 406 plugs and locatees with pilot hole topmost, and when fanning strip 404 rotated up, following pilot hole 405 was just pegged graft and the location with latch 406.The angle of inclination of sample hose 1 can prevent that sample hose 1 from bursting in 20～90 degree free adjustment like this.
Embodiment five
Utilize the embodiment of the invention two or four zone melting purification device to carry out benzoic purification, purification step is as follows:
(1) will need the phenylformic acid powder of purifying to insert (external diameter 3.0mm in the acidproof horminess glass tube that lower end closed, length are 70～80cm, internal diameter 2.6mm) in the sample hose 1, be filled to apart from about the opening part 5cm, seal with sealing film, fix sample hose 1 by aforementioned region fusion purifying plant of the present invention;
(2) two process furnace are moved to the bottom of sample hose 1;
(3) power-on, start synchronous machine, making process furnace is that 4cm/h moves up along sample hose 1 with the translational speed, the temperature of setting first process furnace 301 is 134 ℃, and the temperature of second process furnace 302 is 132 ℃, and the sample melting zone generates situation in the observation sample pipe, along with the formation in sample melting zone, the formation of xln, sample subsides in the sample hose, opens upper end open then, inserts sample again;
(4) carry out repeatedly step (3) repeatedly, until the sample xln apart from sample hose upper end open 5cm place;
(5) again two process furnace are moved to the top of sample hose;
(6) power-on, start synchronous machine, making two process furnace is 4cm/h with the translational speed, move down along sample hose 1, the temperature of setting first process furnace 301 is 132 ℃, and the temperature of second process furnace 302 is 134 ℃, observes the interior sample of the sample hose that is in the process furnace position and all is two melting zones of molten state formation, along with slowly moving of process furnace, the sample melted district also moves thereupon.Melting zone is water white liquid state, and process furnace leaves melting zone, and sample temperature reduces generation white crystals body, and the impurity in the sample moves to the direction that the liquid phase melting zone forms in liquid phase and solid phase intersection;
(7) repeating step (5) and step are (6) 8 times, obviously are sundown in the lower end of sample hose 1, promptly finish purification;
(8) after purification is finished, sample hose is taken off, intercept middle two/part, promptly obtain the phenylformic acid of needed purification, benzoic purity can reach more than 99.99%.
Certainly, what process furnace can be for beyond one or two as required is a plurality of, and the translational speed of process furnace also can be adjusted by synchronous machine and wheel box, and the travel direction of process furnace is realized by the forward and reverse of control synchronous machine.
Certainly, process furnace not only can only move towards a direction, promptly only is used for the purification of sample, also can make process furnace two-way mobile, promptly moves back and forth up and down, and then impurity can be evenly distributed in the sample, realizes adulterated purpose.
The analysis to measure result verification
With the benzoic purity of high purity after the coulometry measured zone fusion purification
Adopt the accurate coulometric titration of continuous current to measure the high-purity benzoic purity of purifying in the research with this purifying plant.The accurate coulometric titration measuring apparatus of this continuous current is national standard reagent purity testing standard apparatus.
1) measuring principle
Coulometric titration reference measurement device is to carry out certain electrode reaction quantitatively by measuring measured matter, or the product of measured matter and a certain electrode reaction carries out the electric weight (coulomb) that chemical reaction consumed, the method for carrying out quantitative analysis according to Faraday's law quantitatively.This method has the highest metering quality, and is for referencial use without any need for the standard of same amount, belongs to the reference measurement method.
By accurate measurement electric current (I), time (t) and sample quality fundamental physical quantities such as (m), and by molar mass (M), the Faraday's number physics constant such as (F) of material, according to Faraday's law of electrolysis, calculate the amount of chemical substance of measured matter and the characteristic purity value of measured matter, this method is internationally recognized direct pedestal method.Value directly upwards can be traceable to international SI units by this standard apparatus, in the stoichiometry system, have the highest metrology characteristic.
Its mathematic(al) representation is:
In the formula:
The purity of P-measured matter (%);
The electrolytic electric current of I-(A);
The quality (g) of m-measured matter weighing
T-electrolysis m restrains measured matter actual institute time-consuming (s)
The electron transfer number of n-electrode reaction;
F-Faraday's number (As/mol);
The molar mass of M-measured matter (g/mol).
2) measuring result
The phenylformic acid purity result who measures after purifying with the accurate coulometric titration of continuous current country reference measurement device is 99.999% (mol/mol), and the single measurement standard deviation is 0.026% (n=8).Take off data such as table one.
Table one:
Claims (10)
1, a kind of zone melting purification device is characterized in that, this device comprises:
Sample hose, it is an elongated cylindrical, is used for splendid attire sample to be purified;
Support component, it comprises base and the support that is fixed on the base, is used for supporting and the fixed sample pipe;
At least one process furnace, it is placed on the sample hose, and can move up and down along sample hose;
Temperature controller, the temperature that is used to regulate process furnace; With
Drive disk assembly is connected with process furnace, and the drive process furnace moves up and down along sample hose.
2, zone melting purification device according to claim 1 is characterized in that, described process furnace is two; Each process furnace is the cylindrical furnace of hollow, and hollow space is used to pass sample hose; Be the diagonal angle state in the body of heater four heater air flow pressure switch rods evenly are set, body of heater adopts aluminum alloy materials; Inlay bar-shaped 100 Ω platinum-resistance thermometers in the body of heater and measure furnace body temperature; With body of heater arranged outside tetrafluoroethylene thermal insulation layer.
3, zone melting purification device according to claim 2, it is characterized in that the height of described two process furnace is identical, the height that is spaced apart a process furnace between two process furnace, and each process furnace disposes temperature controller separately, is used to regulate and control the furnace body temperature of each process furnace.
4, zone melting purification device according to claim 1, it is characterized in that, described drive disk assembly, it comprises synchronous machine, gear drive, worm gear and endless screw speed changer, driving chain and guide deflection sheave, described synchronous machine is connected with gear drive, described gear drive is connected with worm gear and endless screw speed changer, described worm gear and endless screw speed changer connects a rotation axis, on the described rotation axis transmitting gear is set, the two ends of described driving chain are connected with the lower end of the upper end of topmost process furnace and bottom process furnace respectively, described driving chain is walked around guide deflection sheave and the transmitting gear on the support respectively, and described guide deflection sheave is arranged on the top and bottom of support.
5, zone melting purification device according to claim 4, it is characterized in that the linear velocity of described synchronous machine after gear drive and worm gear and endless screw speed changer deceleration is 3.5～5cm/h, and is preferably 4cm/h, be that the process furnace translational speed is 3.5～5cm/h, and be preferably 4cm/h.
6, according to each described zone melting purification device among the claim 1-5, it is characterized in that, this device comprises that further one regulates the angle demodulator of sample hose obliquity, described angle demodulator comprises: two strongbacks and the locating shaft that are relatively arranged on the base both sides respectively, described base is fixed on the locating shaft, the two ends of described locating shaft are connected with two strongback bearings respectively, base can be rotated with locating shaft, described base and strongback are provided with fanning strip on corresponding at least one side, a plurality of pilot holes are set on the described fanning strip, the curved setting on fanning strip of described a plurality of pilot hole, the latch that can pass strongback and match with pilot hole is set on the described strongback, and described latch is positioned at the top of locating shaft.
7, zone melting purification device according to claim 1 is characterized in that, this device is used to the phenylformic acid of purifying, wherein,
The internal diameter of described sample hose is 2.5～2.7cm;
Described process furnace is two, and these two process furnace are connected; Each process furnace is the cylindrical furnace of hollow, and hollow space is used to pass sample hose; Be the diagonal angle state in the body of heater four heater air flow pressure switch rods evenly are set, body of heater adopts aluminum alloy materials; Inlay bar-shaped 100 Ω platinum-resistance thermometers in the body of heater and measure furnace body temperature; Body of heater arranged outside tetrafluoroethylene thermal insulation layer; The height of process furnace and the spacing between the process furnace are 4～4.5cm; Described temperature controller, each process furnace disposes temperature controller separately, is used to regulate and control the furnace body temperature of process furnace;
Described drive disk assembly, it comprises synchronous machine, gear drive, worm gear and endless screw speed changer, driving chain and guide deflection sheave, described synchronous machine is connected with gear drive, described gear drive is connected with worm gear and endless screw speed changer, described worm gear and endless screw speed changer connects a rotation axis, on the described rotation axis transmitting gear is set, the two ends of described driving chain are connected with the lower end of the upper end of topmost process furnace and bottom process furnace respectively, described driving chain is walked around guide deflection sheave and the transmitting gear on the support respectively, and described guide deflection sheave is arranged on the top and bottom of support; And the linear velocity of described synchronous machine after gear drive and worm gear and endless screw speed changer deceleration is 3.5～5cm/h, and is preferably 4cm/h, and promptly the process furnace translational speed is 3.5～5cm/h, and is preferably 4cm/h;
This device comprises that further one regulates the angle demodulator of sample hose obliquity, described angle demodulator comprises: two strongbacks and the locating shaft that are relatively arranged on the base both sides respectively, described base is fixed on the locating shaft, the two ends of described locating shaft are connected with two strongback bearings respectively, base can be rotated with locating shaft, described base and strongback are provided with fanning strip on corresponding at least one side, a plurality of pilot holes are set on the described fanning strip, the curved setting on fanning strip of described a plurality of pilot hole, the latch that can pass strongback and match with pilot hole is set on the described strongback, and described latch is positioned at the top of locating shaft.
8, the described zone melting purification device of a kind of employing claim 7 benzoic method of purifying, this method comprises the steps:
(1) phenylformic acid powder that will be to be purified is inserted in the sample hose of end sealing, is filled to apart from about the opening part 5cm, seals with sealing film, and fixes sample hose;
(2) process furnace is moved to the bottom of sample hose;
(3) power-on, start synchronous machine, process furnace is moved up along sample hose, and translational speed is controlled at 3.5～5cm/h, preferred 4cm/h, the furnace body temperature of setting process furnace is at 130～135 ℃, the sample melting zone generates situation in the observation sample pipe, and along with the formation in sample melting zone, the formation of xln, sample subsides in the sample hose, open upper end open then, insert sample again;
(4) carry out repeatedly step (3) repeatedly, until the sample xln apart from sample hose upper end open 5～10cm place;
(5) then, directly process furnace is moved to the top of sample hose;
(6) power-on, start synchronous machine, process furnace is moved down along sample hose, speed control is at 3.5～5cm/h, preferred 4cm/h, and the furnace body temperature of setting process furnace is at 130～135 ℃, observes in the sample hose that is in the process furnace position sample and all is molten state and forms one or more melting zones;
(7) when process furnace moves to the bottom of sample hose, repeating step (5) and step (6) repeatedly when the lower end at sample hose obviously is sundown, are promptly finished purification; With
(8) after purification is finished, sample hose is taken off, intercept middle two/part, promptly obtain the phenylformic acid of needed purification.
9, the benzoic method of purification according to claim 8 is characterized in that, repeating step (5) and step are (6) 8 times in the described step (7).
10, according to Claim 8 or the benzoic method of 9 described purifications, it is characterized in that the furnace body temperature of described process furnace is controlled at 130～135 ℃, heating power is 50～100 watts; The process furnace travel direction is from the top down in described step (6), and stove was 2～3 ℃ under last stove setting furnace body temperature was lower than; The process furnace travel direction is from bottom to top in described step (3), and stove was 2～3 ℃ under last stove setting furnace body temperature was higher than.
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| CN103813483A (en) * | 2014-01-24 | 2014-05-21 | 百川化工(如皋)有限公司 | Method for melting trimellitic anhydride and used device |
| CN104974062A (en) * | 2015-06-30 | 2015-10-14 | 成都理工大学 | TDI purification process of zone melting method |
| CN106478409A (en) * | 2015-11-25 | 2017-03-08 | 衡阳屹顺化工有限公司 | A kind of benzoic acid purification system |
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| CN1228286C (en) * | 2003-01-07 | 2005-11-23 | 西北工业大学 | Melting purification equipment in organic compound field and its purification method |
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| CN103813483A (en) * | 2014-01-24 | 2014-05-21 | 百川化工(如皋)有限公司 | Method for melting trimellitic anhydride and used device |
| CN103813483B (en) * | 2014-01-24 | 2015-12-30 | 百川化工(如皋)有限公司 | A kind of method of melting trimellitic anhydride and equipment therefor |
| CN104974062A (en) * | 2015-06-30 | 2015-10-14 | 成都理工大学 | TDI purification process of zone melting method |
| CN106478409A (en) * | 2015-11-25 | 2017-03-08 | 衡阳屹顺化工有限公司 | A kind of benzoic acid purification system |
| CN108677027A (en) * | 2018-07-31 | 2018-10-19 | 核工业理化工程研究院 | A kind of multi-stage evaporator and multistage evaporation method for alkali metal purification |
| CN108677027B (en) * | 2018-07-31 | 2024-01-05 | 核工业理化工程研究院 | Multistage evaporator for alkali metal purification and multistage evaporation method |
| CN111413294A (en) * | 2020-03-31 | 2020-07-14 | 西北农林科技大学 | Method for rapidly detecting wax in sunflower seed oil |
| CN111413294B (en) * | 2020-03-31 | 2023-03-28 | 西北农林科技大学 | Method for rapidly detecting wax in sunflower seed oil |
| CN112979487A (en) * | 2021-02-25 | 2021-06-18 | 上海市计量测试技术研究院 | Purification method of acetanilide purity standard substance |
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