CN104511179A - High-purity quartz spring filling-material rectifying tower and method for preparing high-purity rectification reagent by using same - Google Patents
High-purity quartz spring filling-material rectifying tower and method for preparing high-purity rectification reagent by using same Download PDFInfo
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Abstract
The invention relates to rectifying operation equipment and a production method for a high-purity or ultra-clean high-purity reagent, and concretely relates to a high-purity quartz spring filling-material rectifying tower and a method for preparing a high-purity rectification reagent by using the same. A large-diameter tower section is utilized and is filled with a quartz glass spring, and the high-purity quartz glass spring filling material is applied to the high-purity quartz glass rectifying tower. Because the high-purity quartz spring filling material on a sieve plate increases the gas-liquid contact surface, the mass transfer effect is substantially improved, the theoretical plate number reaches 8-10, the average resolution is improved by 20% or more compared with that of a sieve plate tower, and the plate efficiency is improved by about 50%. The high-purity quartz spring filling-material rectifying tower is a multifunctional tower, the rectifying tower is capable of removing low-boiling-point and high-boiling-point impurities in raw materials at the same time during continuous rectification, and reaching the effect, which is realized through two-tower combination, of removing low-boiling-point and high-boiling-point impurities through once rectification, and enabling the target product to be purified.
Description
Technical field
The present invention relates to a kind of high-purity or ultra-clean and high pure chemical reagent distillation operation equipment and production method, be specially high purity quartz spring stuffing rectification column and prepare the method for high-purity distillation reagent.
Background technology
Domestic early stage high purity reagent and ultra-clean and high pure chemical reagent rectifying mainly use high purity quartz Webster still.Webster (Vigreux column) still, also known as thorn shape still, it is a glass tube with the centripetal thorn of array, and often group has three root thorns, arrange in the shape of a spiral between each group, its advantage does not need filler, and in distillation process, liquid is seldom detained in post, and easy dress is easily washed, shortcoming is that separative efficiency is not high, the general theory number of plates is about 2.0 ~ 3.0, is only applicable to the two component rectifying that boiling point difference is larger, and such as high-purity sulphuric acid removes the rectifying of moisture and low-boiling-point substance impurity in producing.Because Webster rectifying column separative efficiency is low, the highly purified requirement of most of ultra-clean and high pure chemical reagent can not be met, therefore the high purity quartz turhogrid orifice column that progressively separated efficiency is relatively high replaced.
High purity quartz turhogrid orifice column is made up of sieve-plate tower bar and electrical heating tower reactor and pendulum phegma control device etc., theoretical cam curve is about 4.0-6.0, dual-flow tray tower can be divided into batch fractionating and continuous rectification two kinds by its mode of operation: one is batch fractionating turhogrid orifice column, its structure is simple, plate face utilizes fully, without liquid level drop, distribution of gas is even, but need liquid layer on higher gas speed ability retaining plate, operating flexibility is little, still lower with packed tower phase specific efficiency, it is non-steady state operation, for keeping distillate composition constant, namely distillate composition keeps constant, corresponding reflux ratio must be made constantly to increase, another kind pauses transformation to batch fractionating turhogrid orifice column, using the top probe tube of tower reactor as charge pipe, increase by a high-boiling components impurity exhaust conduit bottom tower reactor, become the continuous rectification turhogrid orifice column of tool rectifying section, its architectural feature is that target product cuts out continuously at tower top, material liquid adds continuously on tower reactor top, high-boiling components impurity cuts out continuously bottom tower reactor, it is except possessing batch fractionating turhogrid orifice column Partial Feature, distillation operation also can be made to carry out continuously, but it deposits wretched insufficiency: 1, in continuous rectification process, because it does not have the function removing low-boiling-point substance, therefore easily cause the low-boiling-point substance impurity content in tower top target product higher, usually high-purity or ultra-clean and high pure chemical reagent can not be met to the requirement of high product purity.2, raw material and high-boiling components coexist tower reactor turnover, in the high-boiling components that tower bottom can be caused to cut out low-boiling-point substance and target product content rise.3, because glass tower bar adopts overall blowing gas refining welding procedure, thus the diameter of rectifying column bar and be not highly easy to do large, general tower shank diameter≤80mm, therefore this rectifying column is only applicable to laboratory scale use.4, on tower bar sieve plate, no-arbitrary pricing rectification efficiency is low.5, only there is rectifying section and do not possess stripping section, cannot steady state operation be realized.
Summary of the invention
The object of the invention is to for above technical problem, provide a kind of and realize the high purity quartz spring stuffing rectification column that industrialized high-purity or ultra-clean and high pure chemical reagent distillation operation uses and the method preparing high-purity distillation reagent thereof.
Concrete technical scheme of the present invention is as follows:
A kind of high purity quartz, spring stuffing rectification column, by rectifying tower reactor, flat mouth packed tower saves, reinforced shower nozzle flat mouth tower joint, save under flat mouth reducing tower cap, flat mouth reducing tower cap saves, coiled tube condenser, coiled pipe cooler, gas-liquid separator forms, it is characterized in that: the upper end of rectifying tower reactor arranges flat mouth packed tower joint, the bottom of rectifying tower reactor arranges high-boiling components pipe valve, the upper end of flat mouth packed tower joint arranges reinforced shower nozzle flat mouth tower joint, on reinforced shower nozzle flat mouth tower joint, flat mouth packed tower joint is set, saves under the top that flat mouth packed tower saves arranges flat mouth reducing tower cap, flat mouth reducing tower cap saves, flat mouth reducing tower cap saves the top by pipeline terminal pad trumpet cooler, the bottom of coiled tube condenser connects gas-liquid separator, the upper end by capacity of returns control valve terminal pad chimney cooler is saved under flat mouth reducing tower cap, the lower end of coiled pipe cooler connects gas-liquid separator, establish packing support sieve plate in flat mouth packed tower joint, reinforced shower nozzle flat mouth Ta Jienei establishes reinforced shower nozzle, packing support sieve plate, flat mouth reducing tower cap saves, save under flat mouth reducing tower cap by built-in coiled reflux condenser, pipe cap formula rises gas catch tray, pipe dish downflow weir distributor, electromagnetism pendulum counter flow controller forms, tower reactor, tower saves, tower cap, pipeline, valve takes Flange joint, and full tower is except quartz parcel electromagnetism pendulum, the pure teflon gasket of varicosity (tower joint pad tool liquid re-distributor function), flange, outside bolt, rectifying tower reactor, flat mouth packed tower saves, reinforced shower nozzle flat mouth tower joint, save under flat mouth reducing tower cap, flat mouth reducing tower cap saves, coiled tube condenser, coiled pipe cooler, the material of gas-liquid separator is 99.998% pure quartz glass or high purity quartz,
The mixing spring filler that the filler of high purity quartz, spring stuffing rectification column is made up of by a certain percentage the pure quartz glass spring of different screw diameter, quartz glass spring diameter is 8mm, is highly 10 to 30mm); Quartz glass spring diameter is 12 mm, is highly 10 to 30mm; Quartz glass spring diameter is 16 mm, highly for 10-30mm; 1:2:3(volume ratio pressed by above-mentioned spring) composition mixing spring filler, high purity quartz spring helical length h=10-30mm, spring string diameter=0.2-0.6 mm;
The gasket seal that high purity quartz, spring stuffing rectification column tower reactor, Ta Jiefa connect is the pure teflon gasket of varicosity of δ=5, internal diameter due to this pad is less than tower joint internal diameter (little 12-20 mm) and pad inner circle is die-cut into zigzag, makes the pure teflon gasket of varicosity have again a liquid re-distributor function.
Flat mouth packed tower joint, reinforced shower nozzle flat mouth tower joint are connected to form by flange seal, tower bar (tower joint) diameter > 100mm, the rectifying being applicable to the high-purity or ultra-clean and high pure chemical reagent of boiling point ﹤ 250 DEG C is produced, the such as rectifying of alcohols, halogenated hydrocarbons, aromatic hydrocarbon; Or be made by overall blowing gas refining welding procedure, whole tower bar without sealing surface, diameter≤100mm, the rectifying being applicable to the high-purity of boiling point >=250 DEG C or ultra-clean and high pure chemical reagent is produced, the rectifying of such as sulfuric acid, suitability for industrialized production can in parallelly use, to increase its output.
The thermal source of rectifying tower reactor is electrical heating or heat-conducting oil heating or steam heated, and rectifying tower reactor is pure quartz glass chuck still or steel lining tetrafluoro rectifying still.
It prepares the method for high-purity distillation reagent to utilize high purity quartz, spring stuffing rectification column, comprises the following steps:
Step 1: material liquid, with by shower nozzle, stripping section tower joint, is added to continuously in rectifying tower reactor, adds thermal rectification;
Step 2: in continuous rectification process, tower top low-boiling-point substance impurity, by coiled tube condenser, gas-liquid separator, low-boiling-point substance pipe, valve, is cut out continuously;
Step 3: tower top target product is by electromagnetism pendulum counter flow controller, coiled pipe cooler, gas-liquid separator, production tube, valve, be cut out continuously, the refluxer that this process flat mouth reducing tower cap saves, rise gas catch tray by pipe cap formula to enter in electromagnetism pendulum counter flow controller and carry out secondary distribution, a part enters pipe dish downflow weir distributor and is back to equably in tower, a part cuts out as finished product by capacity of returns control valve, now electromagnetism pendulum is in opening, the size of reflux ratio passes through temperature and the flow of cooling water in control panel tubular type reflux condenser, the opening degree of capacity of returns control valve is regulated to realize,
Step 4: high-boiling components impurity by high-boiling components pipe valve, is cut out continuously at the bottom of rectifying tower reactor.
High purity quartz of the present invention, spring stuffing rectification column, for production that is high-purity or ultra-clean and high pure chemical reagent, overcome the deficiency of high purity quartz Webster still and high purity quartz turhogrid orifice column rectifying device, this tower also possesses stripping section except having rectifying section, steady state operation can be realized, and first pure quartz glass spring filler is used in pure quartz glass rectifying column, because the high purity quartz spring filler on sieve plate adds vapour-liquid contact surface, thus considerably improve mass transfer effect, its theoretical cam curve is made to reach 8-10, 20 more than % are improved than the average divided degree of sieve-plate tower, plate efficiency improves about 50%.
High purity quartz, spring stuffing rectification column are multipurpose towers, can to remove in raw material in continuous rectification low simultaneously boils and high-boiling components impurity for it, a rectifying just can reach two tower couplings and remove low boiling or the rectification effect of high-boiling components impurity, makes target product obtain purifying.High purity quartz, spring stuffing rectification column are practical, when low-boiling-point substance in raw material is only one-component and is target product, make electromagnetism pendulum be in closed condition, get tower top low-boiling-point substance cut and be product during operation.High purity quartz, spring stuffing rectification column also can carry out batch fractionating, after during operation, rectifying tower reactor is once fed in raw material, electromagnetism pendulum is made to be in opening, by temperature and the flow of cooling water in control panel tubular type reflux condenser, regulate the opening degree of capacity of returns control valve, control the size of capacity of returns, constant to ensure target product composition.
High purity quartz, spring stuffing rectification column employ the encapsulant of the pure teflon gasket of varicosity as tower reactor and Ta Jie and pipeline, valve.The pure polytetrafluoroethylene (PTFE) of varicosity integrates the physicochemical property of the pure polytetrafluoroethylene (PTFE) excellence of rigidity and the sealing material of rubber excellent seal performance, its application makes tower bar (tower joint) diameter be increased to 200mm or more, achieves the industrial applications of pure quartz glass rectifying column.The pure teflon gasket of varicosity is made up of pure polytetrafluoroethylene (PTFE), the expansion PTFE of multidirectional fibre structure, and special processing technology makes material identical in the tensile strength of all directions.Solve cold flow creep problem with the pad of this materials processing, pad parameter is improved greatly, and the pure polytetrafluoroethylene (PTFE) of varicosity compares with the pure polytetrafluoroethylene (PTFE) of rigidity and has the following advantages:
1, after its compression, material does not broaden substantially, and creep resistance is significantly better than the pure polytetrafluoroethylene (PTFE) of rigidity and filled polytetrafluoroethylene pad.2, easily cutting and punching press.3, make up flange face that is irregular and that damage, this is less than rigidity tetrafluoro.4, be applicable to pressure-sensitive joint face (being the desirable seal material of the frangible seal faces such as glass, plastics, pottery and distressed metal sealing surface), this is also less than rigidity tetrafluoro.
Varicosity pure teflon gasket application in addition, also overcomes the stripping of rubber sheet gasketing and filled polytetrafluoroethylene pad and cast to the pollution of ultra-clean and high pure chemical reagent.
Data display is as far back as the market scale of world's electronic chemical product in 2007 just more than 35,000,000,000 dollars, and domestic manufacture of solar cells in 2010 consumes various liquid ultra-clean and high pure chemical reagent or reagent more than 15.6 ten thousand tons.Show according to latest digital: for Chongqing City, the Chongqing IT industry after upgrading in 2011 is expected to reach 1,000,000,000,000 output values.Account for microelectronic industry output value 3-5% by ultra-clean and high pure chemical reagent to calculate, only the ultra-clean and high pure chemical reagent output value in Chongqing will reach 300 ~ 50,000,000,000 yuan, therefore in " 13 " planning, ultra-clean and high pure chemical reagent has the wide market demand.Moreover, along with the develop rapidly of domestic microelectric technique, particularly extensive and super large-scale integration (VLSI) or ULSI (ULSI) Micrometer-Nanometer Processing Technology is constantly updated, also more and more higher to the quality requirement of ultra-clean and high pure chemical reagent (Process Chemi-cals), study for this reason and a kind ofly realize the high-purity of suitability for industrialized production or ultra-clean and high pure chemical reagent rectifying device is imperative.
Accompanying drawing explanation
Fig. 1 is the structural representation of high purity quartz, spring stuffing rectification column.
Fig. 2 is the reinforced shower head structure schematic diagram of shower nozzle flat mouth Ta Jienei.
Fig. 3 is the planar structure schematic diagram of reinforced shower nozzle.
Fig. 4 is the structural representation establishing packing support sieve plate in flat mouth packed tower joint.
Fig. 5 is the structural representation of flat mouth packed tower joint.
Fig. 6 is the structural representation of reinforced shower nozzle flat mouth tower joint.
Fig. 7 is the structural representation that flat mouth reducing tower cap saves.
Fig. 8 is the structural representation saved under flat mouth reducing tower cap.
Fig. 9 is the structural representation of coiled tube condenser.
Figure 10 is the structural representation of gas-liquid separator.
Figure 11 is the structural representation of existing batch fractionating technology.
Figure 12 is the structural representation of existing continuous rectification technology.
Wherein, 1---rectifying tower reactor, 2---flat mouth packed tower saves, 3---reinforced shower nozzle flat mouth tower joint, 4---save under flat mouth reducing tower cap, 5---flat mouth reducing tower cap saves, 6---coiled pipe cooler, 7---coiled tube condenser, 8---gas-liquid separator, 9---capacity of returns control valve, 10---finished product pipe valve, 11---low-boiling-point substance pipe valve, 12---high-boiling components pipe valve, 13---packing support sieve plate, 14---sieve plate hole, 15---reinforced shower nozzle, 16---thermometer boss, 17---coiled reflux cooler, 18---coil pipe downflow weir distributor, 19---return duct, 20---electromagnetism pendulum, 21---electromagnetism pendulum during closed condition, 22---production tube, 23---electromagnetism pendulum controls return channel, 24---electromagnet, 25---short-selling pipe, 26---lime set inlet tube, 27---pipe cap formula rises gas catch tray, 28---gas-liquid entrance, 29---, 30---liquid outlet tube
Detailed description of the invention
Below in conjunction with specific embodiment, this patent is described further.
A kind of high purity quartz, spring stuffing rectification column, by rectifying tower reactor, flat mouth packed tower saves, reinforced shower nozzle flat mouth tower joint, save under flat mouth reducing tower cap, flat mouth reducing tower cap saves, coiled tube condenser, coiled pipe cooler, gas-liquid separator forms, the upper end of rectifying tower reactor arranges flat mouth packed tower joint, the bottom of rectifying tower reactor arranges high-boiling components pipe valve, the upper end of flat mouth packed tower joint arranges reinforced shower nozzle flat mouth tower joint, on reinforced shower nozzle flat mouth tower joint, flat mouth packed tower joint is set, saves under the top that flat mouth packed tower saves arranges flat mouth reducing tower cap, flat mouth reducing tower cap saves, flat mouth reducing tower cap saves the top by pipeline terminal pad trumpet cooler, the bottom of coiled tube condenser connects gas-liquid separator, the upper end by capacity of returns control valve terminal pad chimney cooler is saved under flat mouth reducing tower cap, the lower end of coiled pipe cooler connects gas-liquid separator, establish packing support sieve plate in flat mouth packed tower joint, reinforced shower nozzle flat mouth Ta Jienei establishes reinforced shower nozzle, packing support sieve plate, flat mouth reducing tower cap saves, save under flat mouth reducing tower cap by built-in coiled reflux condenser, pipe cap formula rises gas catch tray, pipe dish downflow weir distributor, electromagnetism pendulum counter flow controller forms, tower reactor, tower saves, tower cap, pipeline, valve takes Flange joint, and full tower is except quartz parcel electromagnetism pendulum, the pure teflon gasket of varicosity (tower joint pad tool liquid re-distributor function), flange, outside bolt, rectifying tower reactor, flat mouth packed tower saves, reinforced shower nozzle flat mouth tower joint, save under flat mouth reducing tower cap, flat mouth reducing tower cap saves, coiled tube condenser, coiled pipe cooler, the material of gas-liquid separator is 99.998% pure quartz glass or high purity quartz,
The mixing spring filler that the filler of high purity quartz, spring stuffing rectification column is made up of by a certain percentage the pure quartz glass spring of different screw diameter, quartz glass spring diameter is 8mm, is highly 10 to 30mm); Quartz glass spring diameter is 12 mm, is highly 10 to 30mm; Quartz glass spring diameter is 16 mm, highly for 10-30mm; 1:2:3(volume ratio pressed by above-mentioned spring) composition mixing spring filler, high purity quartz spring helical length h=10-30mm, spring string diameter=0.2-0.6 mm;
The gasket seal that described high purity quartz, spring stuffing rectification column tower reactor, Ta Jiefa connect is the pure teflon gasket of varicosity of δ=5, internal diameter due to this pad is less than tower joint internal diameter (little 12-20 mm) and pad inner circle is die-cut into zigzag, makes the pure teflon gasket of varicosity have again a liquid re-distributor function.
Described flat mouth packed tower joint, reinforced shower nozzle flat mouth tower joint are connected to form by flange seal, tower bar (tower joint) diameter > 100mm, the rectifying being applicable to the high-purity or ultra-clean and high pure chemical reagent of boiling point ﹤ 250 DEG C is produced, the such as rectifying of alcohols, halogenated hydrocarbons, aromatic hydrocarbon; Or be made by overall blowing gas refining welding procedure, whole tower bar without sealing surface, diameter≤100mm, the rectifying being applicable to the high-purity of boiling point >=250 DEG C or ultra-clean and high pure chemical reagent is produced, the rectifying of such as sulfuric acid, suitability for industrialized production can in parallelly use, to increase its output.
The thermal source of described rectifying tower reactor is electrical heating or heat-conducting oil heating or steam heated, and rectifying tower reactor is pure quartz glass chuck still or steel lining tetrafluoro rectifying still.
It prepares the method for high-purity distillation reagent to utilize high purity quartz, spring stuffing rectification column, comprises the following steps:
Step 1: material liquid, with by shower nozzle, stripping section tower joint, is added to continuously in rectifying tower reactor, adds thermal rectification;
Step 2: in continuous rectification process, tower top low-boiling-point substance impurity, by coiled tube condenser, gas-liquid separator, low-boiling-point substance pipe, valve, is cut out continuously;
Step 3: tower top target product is by electromagnetism pendulum counter flow controller, coiled pipe cooler, gas-liquid separator, production tube, valve, be cut out continuously, the refluxer that this process flat mouth reducing tower cap saves, rise gas catch tray by pipe cap formula to enter in electromagnetism pendulum counter flow controller and carry out secondary distribution, a part enters pipe dish downflow weir distributor and is back to equably in tower, a part cuts out as finished product by capacity of returns control valve, now electromagnetism pendulum is in opening, the size of reflux ratio passes through temperature and the flow of cooling water in control panel tubular type reflux condenser, the opening degree of capacity of returns control valve is regulated to realize,
Step 4: high-boiling components impurity by high-boiling components pipe valve, is cut out continuously at the bottom of rectifying tower reactor.
For 150L high purity quartz, the invention will be further described for spring stuffing rectification column.
150L high purity quartz, spring stuffing rectification column is by rectifying tower reactor, flat mouth packed tower saves, reinforced shower nozzle flat mouth tower joint, on flat mouth reducing tower cap, lower joint, coiled tube condenser, cooler, the compositions such as gas-liquid separator, wherein establish packing support sieve plate in flat mouth packed tower joint, reinforced shower nozzle flat mouth Ta Jienei establishes reinforced shower nozzle, packing support sieve plate, on flat mouth reducing tower cap, lower joint is by built-in coiled reflux condenser, pipe cap formula rises gas catch tray, pipe dish downflow weir distributor, electromagnetism pendulum counter flow controller forms, tower reactor, tower saves, tower cap, pipeline, valve takes Flange joint, full tower is except quartz parcel electromagnetism pendulum, the pure teflon gasket of varicosity (tower joint pad tool liquid re-distributor function), flange, outside bolt, process by 99.998% pure quartz glass or glass sand.
Describe high purity quartz, spring stuffing rectification column the mixing spring filler that is made up of by a certain percentage the pure quartz glass spring of different screw diameter of filler, 8mm(h=10-30mm), 12 mm(h=10-30mm), 16 mm(h=10-30mm) spring by 1:2:3(volume ratio) huddle composition mixing spring filler, high purity quartz spring helical length h=10-30mm, spring string diameter=0.2-0.6 mm.
The gasket seal that described high purity quartz, spring stuffing rectification column tower reactor, Ta Jiefa connect is the pure teflon gasket of varicosity of δ=5, internal diameter due to this pad is less than tower joint internal diameter (little 12-20 mm) and pad inner circle is die-cut into zigzag, makes the pure teflon gasket of varicosity have again a liquid re-distributor function.
Described high purity quartz, spring stuffing rectification column have two kinds: a kind of is flange form, tower bar is saved by some towers and is connected to form by flange seal, tower bar (tower joint) diameter > 100mm, the rectifying being applicable to the high-purity or ultra-clean and high pure chemical reagent of boiling point ﹤ 250 DEG C is produced, the such as rectifying of alcohols, halogenated hydrocarbons, aromatic hydrocarbon; One is tower rod-type, and it uses overall blowing gas refining welding procedure to be made, and whole tower bar is without sealing surface, diameter≤100mm, the rectifying being applicable to the high-purity of boiling point >=250 DEG C or ultra-clean and high pure chemical reagent is produced, the rectifying of such as sulfuric acid, suitability for industrialized production can in parallelly use, to increase its output.
The thermal source of described high purity quartz, spring stuffing rectification column, according to the character of institute's rectifying target product, can select electrical heating, heat-conducting oil heating, steam heated.Rectifying tower reactor can also be pure quartz glass chuck still or steel lining tetrafluoro rectifying still.
The high purity reagent rectificating method of described high purity quartz, spring stuffing rectification column is:
Step 1: material liquid is saved by shower nozzle, stripping section tower with certain flow, is added in rectifying tower reactor continuously, by electrical heating rectifying (or other heat source rectifying);
Step 2: in continuous rectification process, tower top low-boiling-point substance impurity, by coiled tube condenser, gas-liquid separator, low-boiling-point substance pipe, valve, is cut out continuously;
Step 3: tower top target product is by electromagnetism pendulum counter flow controller, coiled pipe cooler, gas-liquid separator, production tube, valve, be cut out continuously, the refluxer that this process flat mouth reducing tower cap saves, rise gas catch tray by pipe cap formula to enter in electromagnetism pendulum counter flow controller and carry out secondary distribution, a part enters pipe dish downflow weir distributor and is back to equably in tower, a part cuts out as finished product by capacity of returns control valve, now electromagnetism pendulum is in opening, the size of reflux ratio passes through temperature and the flow of cooling water in control panel tubular type reflux condenser, the opening degree of capacity of returns control valve is regulated to realize,
Step 4: high-boiling components impurity by high-boiling components pipe valve, is cut out continuously at the bottom of rectifying tower reactor.
The high purity quartz of the present invention, spring stuffing rectification column, for production that is high-purity or ultra-clean and high pure chemical reagent, overcome the deficiency of high purity quartz Webster still and high purity quartz turhogrid orifice column rectifying device, this tower also possesses stripping section except having rectifying section, steady state operation can be realized, and first pure quartz glass spring filler is used in pure quartz glass rectifying column, because the high purity quartz spring filler on sieve plate adds vapour-liquid contact surface, thus considerably improve mass transfer effect, its theoretical cam curve is made to reach 8-10, 20 more than % are improved than the average divided degree of sieve-plate tower, plate efficiency improves about 50%.
High purity quartz, spring stuffing rectification column are multipurpose towers, can to remove in raw material in continuous rectification low simultaneously boils and high-boiling components impurity for it, a rectifying just can reach two tower couplings and remove low boiling or the rectification effect of high-boiling components impurity, makes target product obtain purifying.High purity quartz, spring stuffing rectification column are practical, when low-boiling-point substance in raw material is only one-component and is target product, make electromagnetism pendulum be in closed condition, get tower top low-boiling-point substance cut and be product during operation.High purity quartz, spring stuffing rectification column also can carry out batch fractionating, after during operation, rectifying tower reactor is once fed in raw material, electromagnetism pendulum is made to be in opening, by temperature and the flow of cooling water in control panel tubular type reflux condenser, regulate the opening degree of capacity of returns control valve, control the size of capacity of returns, constant to ensure target product composition.
High purity quartz, spring stuffing rectification column employ the encapsulant of the pure teflon gasket of varicosity as tower reactor and Ta Jie and pipeline, valve.The pure polytetrafluoroethylene (PTFE) of varicosity integrates the physicochemical property of the pure polytetrafluoroethylene (PTFE) excellence of rigidity and the sealing material of rubber excellent seal performance, its application makes tower bar (tower joint) diameter be increased to 200mm or more, achieves the industrial applications of pure quartz glass rectifying column.The pure teflon gasket of varicosity is made up of pure polytetrafluoroethylene (PTFE), the expansion PTFE of multidirectional fibre structure, and special processing technology makes material identical in the tensile strength of all directions.
Claims (5)
1. a high purity quartz, spring stuffing rectification column, by rectifying tower reactor, flat mouth packed tower saves, reinforced shower nozzle flat mouth tower joint, save under flat mouth reducing tower cap, flat mouth reducing tower cap saves, coiled tube condenser, coiled pipe cooler, gas-liquid separator forms, it is characterized in that: the upper end of rectifying tower reactor arranges flat mouth packed tower joint, the bottom of rectifying tower reactor arranges high-boiling components pipe valve, the upper end of flat mouth packed tower joint arranges reinforced shower nozzle flat mouth tower joint, on reinforced shower nozzle flat mouth tower joint, flat mouth packed tower joint is set, saves under the top that flat mouth packed tower saves arranges flat mouth reducing tower cap, flat mouth reducing tower cap saves, flat mouth reducing tower cap saves the top by pipeline terminal pad trumpet cooler, the bottom of coiled tube condenser connects gas-liquid separator, the upper end by capacity of returns control valve terminal pad chimney cooler is saved under flat mouth reducing tower cap, the lower end of coiled pipe cooler connects gas-liquid separator, establish packing support sieve plate in flat mouth packed tower joint, reinforced shower nozzle flat mouth Ta Jienei establishes reinforced shower nozzle, packing support sieve plate, flat mouth reducing tower cap saves, save under flat mouth reducing tower cap by built-in coiled reflux condenser, pipe cap formula rises gas catch tray, pipe dish downflow weir distributor, electromagnetism pendulum counter flow controller forms, rectifying tower reactor, flat mouth packed tower saves, reinforced shower nozzle flat mouth tower joint, save under flat mouth reducing tower cap, flat mouth reducing tower cap saves, coiled tube condenser, coiled pipe cooler, the material of gas-liquid separator is 99.998% pure quartz glass or high purity quartz, high purity quartz, the filler of spring stuffing rectification column is mixed by spiral pure quartz glass spring, and quartz glass spring diameter is 8mm, be highly 10 to 30mm and quartz glass spring diameter be 12 mm, be highly 10 to 30mm and quartz glass spring diameter be 16 mm, be highly 10-30mm, 1:2:3(volume ratio pressed by above-mentioned spring) composition mixing spring filler, high purity quartz spring helical length h=10-30mm, spring string diameter=0.2-0.6 mm.
2. a kind of high purity quartz according to claim 1, spring stuffing rectification column, it is characterized in that: the gasket seal that described high purity quartz, spring stuffing rectification column tower reactor, Ta Jiefa connect is the pure teflon gasket of varicosity of δ=5, the internal diameter of this pad is less than tower joint internal diameter (little 12-20 mm) and pad inner circle is die-cut into zigzag.
3. a kind of high purity quartz according to claim 1, spring stuffing rectification column, it is characterized in that: described flat mouth packed tower joint, reinforced shower nozzle flat mouth tower joint are connected to form by flange seal, tower bar (tower joint) diameter > 100mm, the rectifying being applicable to the high-purity or ultra-clean and high pure chemical reagent of boiling point ﹤ 250 DEG C is produced; Described flat mouth packed tower joint, reinforced shower nozzle flat mouth tower joint or is made by overall blowing gas refining welding procedure, whole tower bar is without sealing surface, and diameter≤100mm, is applicable to the rectifying production of the high-purity of boiling point >=250 DEG C or ultra-clean and high pure chemical reagent.
4. a kind of high purity quartz according to claim 1, spring stuffing rectification column, is characterized in that: the thermal source of described rectifying tower reactor is electrical heating or heat-conducting oil heating or steam heated, and rectifying tower reactor is pure quartz glass chuck still or steel lining tetrafluoro rectifying still.
5. it prepares the method for high-purity distillation reagent to utilize high purity quartz, spring stuffing rectification column, it is characterized in that comprising the following steps:
Step 1: material liquid, with by shower nozzle, stripping section tower joint, is added to continuously in rectifying tower reactor, adds thermal rectification;
Step 2: in continuous rectification process, tower top low-boiling-point substance impurity, by coiled tube condenser, gas-liquid separator, low-boiling-point substance pipe, valve, is cut out continuously;
Step 3: tower top target product is by electromagnetism pendulum counter flow controller, coiled pipe cooler, gas-liquid separator, production tube, valve, be cut out continuously, the refluxer that this process flat mouth reducing tower cap saves, rise gas catch tray by pipe cap formula to enter in electromagnetism pendulum counter flow controller and carry out secondary distribution, a part enters pipe dish downflow weir distributor and is back to equably in tower, a part cuts out as finished product by capacity of returns control valve, now electromagnetism pendulum is in opening, the size of reflux ratio passes through temperature and the flow of cooling water in control panel tubular type reflux condenser, the opening degree of capacity of returns control valve is regulated to realize,
Step 4: high-boiling components impurity by high-boiling components pipe valve, is cut out continuously at the bottom of rectifying tower reactor.
Priority Applications (1)
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104841247A (en) * | 2015-04-17 | 2015-08-19 | 泰州润达环保科技有限公司 | Denitrating tower structure |
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| CN102430255A (en) * | 2011-09-21 | 2012-05-02 | 新疆美克化工股份有限公司 | Rectification tower of 1,4-butanediol raffinate recovery system |
| CN203598512U (en) * | 2013-09-29 | 2014-05-21 | 四川西陇化工有限公司 | High-purity quartz and spring packing fractionating column |
| CN204275535U (en) * | 2014-09-09 | 2015-04-22 | 上海博荟化工有限公司 | A kind of rectifying column |
| EP2574606B1 (en) * | 2006-03-01 | 2016-09-28 | Grupo Petrotemex, S.A. De C.V. | Polycarboxylic acid production system employing cooled mother liquor from oxidative digestion as feed to impurity purge system |
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| EP2574606B1 (en) * | 2006-03-01 | 2016-09-28 | Grupo Petrotemex, S.A. De C.V. | Polycarboxylic acid production system employing cooled mother liquor from oxidative digestion as feed to impurity purge system |
| CN102430255A (en) * | 2011-09-21 | 2012-05-02 | 新疆美克化工股份有限公司 | Rectification tower of 1,4-butanediol raffinate recovery system |
| CN203598512U (en) * | 2013-09-29 | 2014-05-21 | 四川西陇化工有限公司 | High-purity quartz and spring packing fractionating column |
| CN204275535U (en) * | 2014-09-09 | 2015-04-22 | 上海博荟化工有限公司 | A kind of rectifying column |
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| CN104841247A (en) * | 2015-04-17 | 2015-08-19 | 泰州润达环保科技有限公司 | Denitrating tower structure |
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