CN101642724A - High-purity organic solvent preparing integrated device - Google Patents
High-purity organic solvent preparing integrated device Download PDFInfo
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- CN101642724A CN101642724A CN200910091739A CN200910091739A CN101642724A CN 101642724 A CN101642724 A CN 101642724A CN 200910091739 A CN200910091739 A CN 200910091739A CN 200910091739 A CN200910091739 A CN 200910091739A CN 101642724 A CN101642724 A CN 101642724A
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- organic solvent
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Abstract
The invention discloses a high-purity organic solvent preparing integrated device comprising an automatic liquid injection device, a precise temperature control heating device, a rectification columnand an automatic shunting collection device. The automatic liquid injection device adds a certain amount of to-be-processed liquid to a distillation flask in the precise temperature control heating device, and the automatic shunting collection device collects the acquired high-purity solvent through the precise temperature control heating and the rectification work of the rectification column, wherein the rectification column consists of a plurality of rectification column bodies arranged in parallel connection. The invention meets the demands of high flux and high efficiency in the rectification technology through arranging a plurality of rectification column bodies in parallel connection for rectification. The invention realizes automation in the liquid adding part, the adsorptive separation part, the rectification part, the cooling part and the fraction collecting part, thereby facilitating experiment operation, and a warning system is arranged in the integrated device; after the system completes the processing task, or blockage is generated in the system, the pressure is too high and the like, the system can automatically give an alarm.
Description
Technical field
The present invention relates to the high-purity organic solvent preparing integrated device that use in a kind of laboratory.
Background technology
At present, domesticly be not applicable to that also the laboratory produces the equipment of high-purity organic solvent in a large number, as highly purified n-hexane, it all relies on import.N-hexane is to be raw material with the petroleum by-product, the pure hexane of analysis that obtains by catalytic reaction and rectifying, but it is difficult to satisfy domestic scientific research reagent requirement.And the laboratory rectifying device all is subjected to the restriction of flux, and single rectifying also is difficult to remove the trace impurity of analyzing in the pure hexane.
Summary of the invention
At the problem that prior art exists, the object of the present invention is to provide collection rectifying, adsorption column separating and purifying technology and pressure, warning, temperature to be controlled in the high-purity organic solvent preparing integrated device of one.
For achieving the above object, a kind of high-purity organic solvent preparing integrated device of the present invention, comprise automatic fluid injection device, precise temperature control heater, rectifying column and shunt gathering-device automatically, the cucurbit of automatic fluid injection device in the precise temperature control heater adds a certain amount of pending liquid, rectifying operation through precise temperature control heating and rectifying column, automatically the shunting gathering-device is just collected required high neat solvent, and wherein rectifying column is made up of some rectifying column bodies that are arranged in parallel.
Further, described rectifying column also comprises outer tube and external block, the two ends of outer tube are provided with cover plate with holes, the end of described every rectifying column body is inserted on two cover plates in the corresponding through hole, all add mounting flange on two cover plates, by mounting flange external block, cover plate and described outer tube are fixedlyed connected, be enclosed with on the outer wall of outer tube and be used for high-efficiency insulated vacuum jacket.
Through a step, described automatic fluid injection device comprises liquid phase pump, solvent bottle, adsorbing separation post and electromagnetic valve II, wherein, the adsorbing separation post comprises splitter body and upper end block, splitter body lower end is provided with quartz sand sieve plate, insert adsorption stuffing on the sieve plate, the upper end block also is provided with quartz sand sieve plate, and the splitter body is fixedlyed connected by mounting flange with block.
Further, described precise temperature control heater comprises electrical heating cover, cucurbit and liquid level sensor, the electrical heating cover has the intelligent precise temperature controlling function, to keep the temperature constant of liquid to be distilled in the cucurbit, to be provided with in the cucurbit being used to monitor the liquid level sensor of liquid stock in it.
Further, described automatic shunting gathering-device comprises receiving flask I, receiving flask II, electromagnetic valve I, condenser and still head, condenser carries out highly effective refrigeration by double-deck serpentine condenser and outer wall condensation clip cover, still head adopts dnockout core formula commonly used, still head is used for linking with the upper port of described rectifying column, also be provided with the temperature sensor that is used to monitor vapor (steam) temperature in it, steam is reclaimed by receiving flask I, receiving flask II through after the condenser condenses.
Further, described receiving flask I and receiving flask II are arranged in parallel, and it controls separately unlatching respectively by electromagnetic valve I, and electromagnetic valve I is provided with the controller that is used to control its action.
Further, described high-purity organic solvent preparing integrated device also comprises control system, warning system.
Further, be provided with explosion-proof valve, temperature and pressure sensor in the described cucurbit, it is too high that this sensor monitors the interior temperature and pressure of described cucurbit, promptly send signal to described control system and warning system, warning system is reported to the police automatically, explosion-proof valve is opened simultaneously, reduces the pressure in the described cucurbit rapidly, and described control system is controlled described electrical heating cover and stopped heating.
The present invention is by adopting the novel distillation post, and under the situation that does not reduce theoretical pedal number, but high flux, the high efficiency rectification process of carrying out can satisfy the demand of retention analysis laboratory to organic solvent.The present invention is from liquid feeding, adsorbing separation, rectifying, cooling, fraction are collected each several part and have all been realized automation, Shi Yan operation easily, and be provided with warning system in the equipment, after system finishes Processing tasks, during situations such as perhaps stopping up appears in system, and pressure is excessive, system can report to the police automatically.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is a rectifying column cross section structure schematic diagram.
The specific embodiment
As shown in Figure 1 and Figure 2, a kind of high-purity organic solvent preparing integrated device of the present invention comprises automatic fluid injection device, precise temperature control heater, rectifying column, shunts gathering-device, control system and warning system automatically.
The automatic fluid injection device comprises liquid phase pump 12, solvent bottle 13, adsorbing separation post 14, electromagnetic valve II 15, and liquid phase pump 12 is used for the initial liquid of the needs distillation of solvent bottle is injected cucurbit 2.Electromagnetic valve II 15 is a two-way valve, fluid injection during unlatching, and closure when equipment carries out work is overflowed to prevent that steam from overflowing from input duct.Adsorbing separation post 14 comprises splitter body and upper end block, splitter body lower end is provided with quartz sand sieve plate, insert adsorption stuffing on the sieve plate, the upper end block also is provided with quartz sand sieve plate, the splitter body is fixedlyed connected by mounting flange with block, adsorbing separation post 14 is removed specific impurities by adsorbent, to satisfy the requirement of experimental solutions purity.
The precise temperature control heater comprises electrical heating cover 1, cucurbit 2, liquid level sensor 3.Electrical heating cover 1 has intelligent precise temperature control type function, can make the temperature constant of liquid to be distilled in the cucurbit 2.Liquid level sensor 3 is used to control reservoir quantity, and the situation that retains of liquid in the monitoring cucurbit 2 in still-process is in order to avoid the liquid evaporate to dryness causes danger.
Rectifying column 11 comprises outer tube 21, has been arranged in parallel some rectifying column bodies 22 in the outer tube 21.The two ends of outer tube 21 are provided with cover plate 19 with holes, and the end of every rectifying column body 22 all is inserted on two cover plates 19 in the corresponding through hole, and so that rectifying column body 22 is fixed, the material of cover plate 19 is a polytetrafluoroethylene (PTFE).All add mounting flange 20 on the outside of two cover plates 19, by mounting flange 20 external block 18, cover plate 19 are press-fited with outer tube 21 and fixedly connected.Parcel is provided with and is used for high-efficiency insulated vacuum jacket 23 on the outer wall of outer tube 21, is filled with the length of side * height in the rectifying column body 22 and is of a size of 2 * 2 stainless steel angle type filler.In the present embodiment, rectifying column body 22 has 7, and its diameter is 20mm, effectively uses length to be 900mm.In the practical application, the quantity of rectifying column body 22 and size can be determined according to experiment is required.
Automatically the shunting gathering-device comprises receiving flask I 5, receiving flask II 6, electromagnetic valve I 7, condenser 8 and still head 9.Condenser 8 carries out highly effective refrigeration by double-deck serpentine condenser and outer wall condensation clip cover, and still head adopts dnockout core formula commonly used, and still head 9 is used for linking with the upper port of rectifying column 11, also is provided with the temperature sensor 10 that is used to monitor vapor (steam) temperature in it.Being condensed into liquid in condenser 8 after, the steam of distillation can enter among receiving flask I 5, the receiving flask II 6 by electromagnetic valve I 7.Electromagnetic valve I 7 itself is furnished with controller, can control the time of its start, can be with different fraction collections in corresponding bottle.
Control system comprises control panel 16, temperature and pressure sensor in temperature sensor 10 and the cucurbit 2 is as temperature among the present invention and pressure-detecting device, its effect is the pressure and temperature situation in the equipment pipeline in the monitoring process, to guarantee equipment working stability, safety.
During work, should check at first whether each instrument and equipment is in place and whether power supply is connected.After inspection finishes, connect general supply.On control panel 16, configure two temperature values that need control, i.e. the temperature in the cucurbit 2 and the temperature of temperature sensor 10.Press " beginning " key then, electromagnetic valve II 15 energising actions, liquid phase pump 12 work, beginning fluid injection in cucurbit 2.
To come the liquid in the cucurbit 2 is carried out preheating with the temperature that is lower than operating temperature at liquid phase pump 12 electrical heating cover 1 in the process of cucurbit 2 fluid injections, when liquid level sensor 3 detects signal, show the requirement that reaches the fluid injection aequum, controller will send signal this moment, electromagnetic valve II 15 is disconnected, and liquid phase pump 12 quits work, and heater will heat with operating temperature, rectifying column 11 carries out rectifying work, and receiving flask II 6 is collecting liquid always in this process.
After heating a period of time, the temperature sensor in the cucurbit 2 detects signal, shows to reach the temperature that sets, and electrical heating cover 1 quits work.After temperature sensor 10 detected signal, electromagnetic valve I 7 was started working, and condensed liquid flows among the receiving flask I 5.Be provided with explosion-proof valve 4, temperature and pressure sensor in the cucurbit 2, sensor is monitored in the cucurbit 2 all the time in the entire work process temperature, pressure change, temperature and pressure is too high in this sensor monitors cucurbit 2, promptly send signal to control system and warning system, warning system is reported to the police automatically, explosion-proof valve 4 is opened simultaneously, reduces the pressure in the cucurbit 2 rapidly, and control system control electrical heating cover 1 stops heating.
The present invention is used for rectifying by some rectifying column bodies are arranged in parallel, and the contradiction in the solution prior art between the height of single rectifying column, caliber etc. and the treating capacity has realized high flux in the distillation technology, high efficiency requirement.And under the situation that does not reduce theoretical pedal number, but high flux, the high efficiency rectification process of carrying out can satisfy the demand of retention analysis laboratory to organic solvent.The present invention is from liquid feeding, adsorbing separation, rectifying, cooling, fraction are collected each several part and have all been realized automation, Shi Yan operation easily, and be provided with warning system in the equipment, after system finishes Processing tasks, during situations such as perhaps stopping up appears in system, and pressure is excessive, system can report to the police automatically.
Claims (8)
1, a kind of high-purity organic solvent preparing integrated device, it is characterized in that, this equipment comprises automatic fluid injection device, precise temperature control heater, rectifying column and shunts gathering-device automatically, the cucurbit of automatic fluid injection device in the precise temperature control heater adds a certain amount of pending liquid, rectifying operation through precise temperature control heating and rectifying column, automatically the shunting gathering-device is just collected required high neat solvent, and wherein rectifying column is made up of some rectifying column bodies that are arranged in parallel.
2, high-purity organic solvent preparing integrated device as claimed in claim 1, it is characterized in that, described rectifying column also comprises outer tube and external block, the two ends of outer tube are provided with cover plate with holes, the end of described every rectifying column body is inserted on two cover plates in the corresponding through hole, all add mounting flange on two cover plates, external block, cover plate and described outer tube are fixedlyed connected, be enclosed with on the outer wall of outer tube and be used for high-efficiency insulated vacuum jacket by mounting flange.
3, high-purity organic solvent preparing integrated device as claimed in claim 1, it is characterized in that, described automatic fluid injection device comprises liquid phase pump, solvent bottle, adsorbing separation post and electromagnetic valve II, wherein, the adsorbing separation post comprises splitter body and upper end block, and splitter body lower end is provided with quartz sand sieve plate, inserts adsorption stuffing on the sieve plate, the upper end block also is provided with quartz sand sieve plate, and the splitter body is fixedlyed connected by mounting flange with block.
4, high-purity organic solvent preparing integrated device as claimed in claim 1, it is characterized in that, described precise temperature control heater comprises electrical heating cover, cucurbit and liquid level sensor, the electrical heating cover has the intelligent precise temperature controlling function, to keep the temperature constant of liquid to be distilled in the cucurbit, to be provided with in the cucurbit being used to monitor the liquid level sensor of liquid stock in it.
5, high-purity organic solvent preparing integrated device as claimed in claim 1, it is characterized in that, described automatic shunting gathering-device comprises receiving flask I, receiving flask II, electromagnetic valve I, condenser and still head, condenser carries out highly effective refrigeration by double-deck serpentine condenser and outer wall condensation clip cover, still head adopts dnockout core formula commonly used, still head is used for linking with the upper port of described rectifying column, also be provided with the temperature sensor that is used to monitor vapor (steam) temperature in it, steam is reclaimed by receiving flask I, receiving flask II through after the condenser condenses.
6, high-purity organic solvent preparing integrated device as claimed in claim 5, it is characterized in that, described receiving flask I and receiving flask II are arranged in parallel, and it controls separately unlatching respectively by electromagnetic valve I, and electromagnetic valve I is provided with the controller that is used to control its action.
7, high-purity organic solvent preparing integrated device as claimed in claim 1 is characterized in that, described high-purity organic solvent preparing integrated device also comprises control system, warning system.
8, high-purity organic solvent preparing integrated device as claimed in claim 7, it is characterized in that, be provided with explosion-proof valve, temperature and pressure sensor in the described cucurbit, it is too high that this sensor monitors the interior temperature and pressure of described cucurbit, promptly send signal to described control system and warning system, warning system is reported to the police automatically, and explosion-proof valve is opened simultaneously, reduce the pressure in the described cucurbit rapidly, described control system is controlled described electrical heating cover and is stopped heating.
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| CN200910091739A CN101642724A (en) | 2009-08-25 | 2009-08-25 | High-purity organic solvent preparing integrated device |
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| CN200910091739A CN101642724A (en) | 2009-08-25 | 2009-08-25 | High-purity organic solvent preparing integrated device |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102357368A (en) * | 2011-10-28 | 2012-02-22 | 江苏省产品质量监督检验研究院 | Evaporation residue measuring device capable of recovering solvent and solvent recovering method |
| CN102441289A (en) * | 2012-02-02 | 2012-05-09 | 常州市常顺精细化学品有限公司科技研究所 | Cluster rectification device |
| CN103083997A (en) * | 2013-03-01 | 2013-05-08 | 成都广亚科技有限公司 | Solvent purifying device capable of regenerating in situ and treatment method and regeneration method thereof |
| CN107255706A (en) * | 2017-07-07 | 2017-10-17 | 四川西普石油物资装备有限公司 | Prevent occurring the method for rushing sample when crude oil from determining |
| CN108051470A (en) * | 2018-01-12 | 2018-05-18 | 苏州市苏测检测技术有限公司 | For the Rotary Evaporators of food science literature |
| CN113350817A (en) * | 2021-05-28 | 2021-09-07 | 张成龙 | Evaporation kettle with regulation and control injection function |
| CN115054933A (en) * | 2022-06-23 | 2022-09-16 | 厦门海关技术中心 | Full-automatic distillation system for detecting harmful anions in mineral products and smelting slag |
-
2009
- 2009-08-25 CN CN200910091739A patent/CN101642724A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102357368A (en) * | 2011-10-28 | 2012-02-22 | 江苏省产品质量监督检验研究院 | Evaporation residue measuring device capable of recovering solvent and solvent recovering method |
| CN102357368B (en) * | 2011-10-28 | 2013-09-25 | 江苏省产品质量监督检验研究院 | Evaporation residue measuring device capable of recovering solvent and solvent recovering method |
| CN102441289A (en) * | 2012-02-02 | 2012-05-09 | 常州市常顺精细化学品有限公司科技研究所 | Cluster rectification device |
| CN102441289B (en) * | 2012-02-02 | 2013-12-18 | 常州市常顺精细化学品有限公司科技研究所 | Cluster rectification device |
| CN103083997A (en) * | 2013-03-01 | 2013-05-08 | 成都广亚科技有限公司 | Solvent purifying device capable of regenerating in situ and treatment method and regeneration method thereof |
| CN103083997B (en) * | 2013-03-01 | 2014-12-03 | 成都广亚科技有限公司 | Solvent purifying device capable of regenerating in situ and treatment method and regeneration method thereof |
| CN107255706A (en) * | 2017-07-07 | 2017-10-17 | 四川西普石油物资装备有限公司 | Prevent occurring the method for rushing sample when crude oil from determining |
| CN108051470A (en) * | 2018-01-12 | 2018-05-18 | 苏州市苏测检测技术有限公司 | For the Rotary Evaporators of food science literature |
| CN113350817A (en) * | 2021-05-28 | 2021-09-07 | 张成龙 | Evaporation kettle with regulation and control injection function |
| CN113350817B (en) * | 2021-05-28 | 2022-06-21 | 黄山市鼎利新材料有限公司 | Evaporation kettle with regulation and control injection function |
| CN115054933A (en) * | 2022-06-23 | 2022-09-16 | 厦门海关技术中心 | Full-automatic distillation system for detecting harmful anions in mineral products and smelting slag |
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Application publication date: 20100210 |