CN106268493B - Dynamic liquid gas distribution device and gas distribution method thereof - Google Patents
Dynamic liquid gas distribution device and gas distribution method thereof Download PDFInfo
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- CN106268493B CN106268493B CN201610685797.2A CN201610685797A CN106268493B CN 106268493 B CN106268493 B CN 106268493B CN 201610685797 A CN201610685797 A CN 201610685797A CN 106268493 B CN106268493 B CN 106268493B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/80—Forming a predetermined ratio of the substances to be mixed
- B01F35/88—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise
- B01F35/882—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise using measuring chambers, e.g. volumetric pumps, for feeding the substances
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/10—Mixing gases with gases
- B01F23/12—Mixing gases with gases with vaporisation of a liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/10—Mixing gases with gases
- B01F23/19—Mixing systems, i.e. flow charts or diagrams; Arrangements, e.g. comprising controlling means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/23—Mixing of laboratory samples e.g. in preparation of analysing or testing properties of materials
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Abstract
The invention provides a dynamic liquid gas distribution device, which comprises a central controller, a source gas, two mass flowmeters (respectively used for controlling carrier gas and diluent gas), a microfluid sample introduction device, a liquid evaporation device, a gas mixing tank and a drying tank, wherein the central controller is used for controlling the carrier gas and the diluent gas; the source gas is simultaneously connected into two gas paths, one gas path is used as carrier gas (used for carrying evaporated liquid), the other gas path is used as diluent gas, the flow rates of the two gas paths are controlled by a mass flow meter, and one-way stop valves are arranged to prevent gas backflow; liquid to be evaporated is loaded in the micro-fluid sample feeding device, and the liquid is pushed into the liquid evaporation device at a fixed speed through a peristaltic pump or a micro-injection pump; the liquid evaporation device can control the temperature; the gas mixing tank is used for mixing gas; the drying tank is used for placing molecular sieves or other selectively filtered substances by a customer; the central controller controls and adjusts the flow rate of the mass flow meter, the pushing speed of the microfluid sample introduction device, the evaporation temperature of the liquid evaporation device and/or the fan rotating speed of the gas mixing tank; the liquid evaporating device consists of porous molecular sieve and heating plate and is connected to the carrier gas path and the microfluid sample feeder, and the molecular sieve can filter and heat the liquid to evaporate, so as to ensure the smooth drainage of the liquid and complete evaporation of the heated liquid to produce continuous gas.
Description
Technical Field
The invention relates to a liquid dynamic gas distribution device and a gas distribution method thereof, in particular to a trace liquid dynamic gas distribution device with a porous molecular sieve and a gas distribution method thereof.
Background
At present, a gas distribution instrument is an instrument for proportioning and mixing two or more gases (mostly two gases in the market) according to a certain proportion and outputting a gas with a set concentration. Two or more than two kinds of gases are often allocated in the mechanisms of environment, health monitoring, scientific research, teaching, metering and the like, and along with the development of science and technology, the requirements of people on gas distribution instruments are higher and higher. At present, two gas distribution instruments are commonly used in the market, one is a three-way electromagnetic valve control type, and the other is a mass flow meter control type.
The gas distribution instrument controlled by the three-way electromagnetic valve mainly uses a single chip microcomputer to control the on-off of a high-speed three-way electromagnetic valve connected with two paths of gas according to the proportioning requirement of the required gas so as to adjust the sampling amount of each path of gas and finally obtain the gas with set concentration, for example, the high-precision gas distribution instrument with the patent number of CN 2825085Y. The electromagnetic valve type gas distribution instrument has the advantages of wide gas application range, simple operation and relatively low price. The conventional gas can be used as it is without special setting or conversion. The gas type and the concentration to be prepared do not need to be taught before the instrument leaves the factory. However, it can only be used for distributing two gases; the gas distribution precision is low (more than 1%).
The mass flow meter type gas distribution instrument mainly uses the mass flow meter to control the flow of each path of gas so as to realize the preparation of gases with different types and concentrations. For example, a dynamic gas distribution system for standard gas with publication number CN 102258958A provides a dynamic gas distribution system for producing a range of standard gas mixtures. The system comprises: providing a diffusion tube containing a target species in a temperature-controlled diffusion cell; enabling carrier gas with a preset flow to flow through a diffusion cell containing a target substance, and enabling the carrier gas to carry the target substance to flow out of the diffusion cell; the carrier gas containing the target substance flowing out is branched into at least two carrier gas branch gas flows, wherein one carrier gas branch gas flow is communicated with the mixing chamber, and at least one of gas paths of the two carrier gas branch gas flows is provided with a flow controller; adjusting the flow controller to vary the flow of the carrier gas subsidiary stream into the mixing chamber; a predetermined flow rate of a diluent gas is flowed into the mixing chamber and mixed in the mixing chamber with the above-mentioned carrier gas branched gas flow flowed into the mixing chamber, thereby obtaining a standard gas mixture of a desired concentration of the target substance.
The gas distribution instrument is quite mature for gas source gas distribution, but the gas distribution instrument for dynamically distributing gas to a liquid gas source in the market is vacant, and the gas distribution instrument has large demand in laboratory research and industrial production due to the fact that the liquid gas source has the advantages of being multiple in types, small in using amount, low in price, free of steel cylinder storage, small in potential safety hazard and the like. At present, the device based on dynamic gas distribution of a liquid gas source mainly takes a diffusion tube as a main part, equipment with reliable performance is mainly monopolized by foreign companies, the price is high, different types of diffusion tubes are required to be replaced by different liquids, and consumable materials are also very high. Another device suitable for dynamic distribution of liquid is disclosed in publication No. CN102039096, in which a volatile liquid control device is used to effectively inject air into a gas generator, so as to convert volatile liquid in the gas generator into gas, and the conversion speed and conversion amount, and the inlet speed and inlet amount are effectively and automatically controlled, thereby realizing distribution of gas.
However, there are several problems with liquid distribution:
1) during gas distribution, continuous airflow needs to be generated, and particularly for organic liquid which can be completely volatilized at a certain temperature, a liquid evaporation device needs to be equipped to ensure that the organic liquid is completely volatilized.
2) The prepared liquid terminal concentration should cover a wide concentration range, such as ppt-ppm, so as to meet the requirements of scientific research and industrial production on gas standard gas.
3) The heated and volatilized liquid can be condensed or adsorbed when flowing through the pipeline, so that heat preservation is needed to prevent condensation, and a pipeline coating is needed to prevent gas adsorption.
Disclosure of Invention
Aiming at the problems, the invention provides a trace liquid dynamic gas distribution device with a porous molecular sieve and a gas distribution method thereof for the first time based on the existing liquid dynamic gas distribution device, which can generate continuous and stable dynamic gas flow and have wide gas distribution range and high precision.
The invention provides a dynamic liquid gas distribution device, which comprises a central controller, a source gas, two mass flowmeters (respectively used for controlling carrier gas and diluent gas), a microfluid sample introduction device, a liquid evaporation device, a gas mixing tank and a drying tank, wherein the central controller is used for controlling the carrier gas and the diluent gas; the source gas is simultaneously connected into two gas paths, one gas path is used as carrier gas (used for carrying evaporated liquid), the other gas path is used as diluent gas, the flow rates of the two gas paths are controlled by a mass flow meter, and one-way stop valves are arranged to prevent gas backflow; liquid to be evaporated is loaded in the micro-fluid sample feeding device, and the liquid is pushed into the liquid evaporation device at a fixed speed through a peristaltic pump or a micro-injection pump; the liquid evaporation device can control the temperature; the gas mixing tank is used for mixing gas; the drying tank is used for placing molecular sieves or other selectively filtered substances by a customer; the central controller controls and adjusts the flow rate of the mass flow meter, the pushing speed of the microfluid sample introduction device, the evaporation temperature of the liquid evaporation device and/or the fan rotating speed of the gas mixing tank; the liquid evaporating device consists of porous molecular sieve and heating plate and is connected to the carrier gas path and the microfluid sample feeder, and the molecular sieve can filter and heat the liquid to evaporate, so as to ensure the smooth drainage of the liquid and complete evaporation of the heated liquid to produce continuous gas.
Furthermore, the molecular sieve is arranged in a funnel-shaped device, liquid enters the molecular sieve, the bottom of the molecular sieve is provided with a heating plate, and the molecular sieve is contacted with high temperature to evaporate the liquid into gas which is discharged from the holes.
Further, the gas mixing tank may be temperature regulated and coated to ensure that the liquid does not condense and adsorb.
Further, the central controller automatically adjusts the flow rate of the mass flow meter according to the input target liquid concentration and the total flow rate; the central controller automatically adjusts the pushing speed of the microfluid sampling device according to the input type, characteristic parameters, concentration and total flow of the target liquid; the central controller automatically adjusts the evaporation temperature of the liquid evaporation device according to the type of the liquid; the central controller automatically or manually adjusts the fan speed of the gas mixing tank.
The invention also provides a dynamic liquid gas distribution method, which comprises the following steps: the method comprises the following steps of simultaneously connecting source gas into two gas paths, controlling the flow of each path of gas by using a mass flow meter, wherein one path of gas is used as carrier gas, the other path of gas is used as diluent gas, the carrier gas directly takes out evaporated gas, the diluent gas dilutes the gas taken out by the carrier gas again, the carrier gas can directly take out the gas and use when high-concentration target gas is needed, and the diluent gas is required to dilute again when low-concentration target gas is needed, so that the gas distribution concentration is adjustable in a wide range; a gas path through which the carrier gas flows is provided with a liquid evaporation device, and the liquid evaporation device can be heated to ensure that the liquid is completely evaporated, so that the gas distribution precision is ensured; the microfluid sample introduction device is loaded with liquid to be evaporated, and the liquid is pushed into the liquid evaporation device at a fixed speed through a peristaltic pump or a micro-injection pump and other devices; the liquid is carried away by the carrier gas and leaves the liquid evaporation device immediately after evaporation; finally, the two air flows are quickly and uniformly mixed in a gas mixing tank and then flow out; the central controller controls and adjusts the flow rate of the mass flow meter, the pushing speed of the microfluid sampling device and/or the evaporation temperature of the liquid evaporation device.
Drawings
FIG. 1: is a structural schematic diagram of the liquid dynamic air distribution device of the invention;
FIG. 2: is the structure schematic diagram of the molecular sieve of the liquid dynamic gas distribution device.
Detailed Description
Fig. 1 is a schematic structural diagram of a liquid dynamic air distribution device of the present invention: the liquid dynamic gas distribution device comprises a central controller, a source gas, a mass flow meter (carrier gas), a mass flow meter (diluent gas), a microfluid sample introduction device, a liquid evaporation device, a gas mixing tank, a drying tank and the like; the source gas is typically a gas, such as N2The synthetic air, Ar and the like are simultaneously connected into two gas paths, and the flow control is carried out through the gas mass flow meter respectively; liquid to be evaporated is loaded in the microfluid sample introduction device, and the liquid is pushed into the liquid evaporation device at a fixed speed through a peristaltic pump or an injection pump and the like; the liquid evaporation device can control the temperature, the smaller the volume is better, the liquid pushed by the microfluid sampling device is very small in volume, so that the liquid is expected to be directly evaporated in the air, if the liquid cannot be directly evaporated, the evaporation of the liquid is assisted by the liquid evaporation device, and the evaporated gas is immediately carried away from the liquid evaporation device by the carrier gas. In summary, the liquid evaporation device needs to ensure complete evaporation of the liquid; the gas mixing tank is used for mixing two gas flows of the two gas paths, and the part is not required in consideration of the possibility of condensation of liquid and the like and can be directly connected by a tee joint; the drying tank is used for placing molecular sieves or other selectively filtered substances by a customer, and the part belongs to an optional part and can be detached; the central controller controls and adjusts the carrier gas mass flow meter, the dilution gas mass flow meter, the pushing speed of the microfluid sampling device, the evaporation temperature of the liquid evaporation device and/or the fan rotating speed of the gas mixing tank. The gas mixing tank can adjust the temperature and determine that the liquid can not be condensed.
Preferably, the central controller automatically adjusts the flow rates of the mass flow meters of the carrier gas and the diluent gas according to the input type, characteristic parameters, concentration and total flow of the target liquid; the central controller calculates the required propelling speed according to the input target liquid type and characteristic parameters, and automatically adjusts the propelling speed of the microfluid sampling device; the central controller automatically adjusts the evaporation temperature of the liquid evaporation device according to the type of the liquid; the central controller automatically or manually adjusts the fan speed of the gas mixing tank.
Referring to fig. 2, the key of the apparatus is that during gas distribution, a continuous gas flow needs to be generated, and particularly for organic liquids which can be completely volatilized at a certain temperature, a liquid evaporation device needs to be equipped to ensure that the organic liquids are completely volatilized. Therefore, a porous molecular sieve device for infiltrating and filtering liquid is additionally arranged at the injection head of the liquid injection device. The molecular sieve is arranged in funnel-shaped equipment, liquid enters the molecular sieve, the bottom of the molecular sieve is provided with a heating plate, and the molecular sieve contacts high-temperature evaporation gas and is penetrated out from holes, so that the liquid is continuously injected and completely evaporated.
The invention also discloses a gas distribution method of the liquid dynamic gas distribution device, which comprises the following steps: simultaneously connecting source gas into two gas paths, wherein one gas path is used as carrier gas, and the other gas path is used as diluent gas and is controlled by a mass flow meter; a liquid evaporation device is arranged in the gas path through which the carrier gas flows; the liquid injection device is loaded with liquid to be evaporated, and the liquid is pushed into the liquid evaporation device at a fixed speed through a peristaltic pump or other devices; the liquid is carried away by the carrier gas and leaves the liquid evaporation device immediately after evaporation; finally, the carrier gas carries the evaporated gas and the diluent gas to flow into a gas mixing tank simultaneously to be uniformly mixed; the central controller controls and adjusts the carrier gas mass flow meter, the dilution gas mass flow meter, the pushing speed of the microfluid sampling device and/or the evaporation temperature of the liquid evaporation device.
A gas mixing tank is used for mixing carrier gas and diluent gas, considering that liquid can be condensed or adsorbed, the part needs to be subjected to heat preservation treatment and adopts an anti-adsorption coating, if the gas is easy to mix, the gas mixing tank is not needed, and the three-way connection can be directly adopted; the drying tank is used for placing molecular sieves or other selectively filtered substances by a customer; the gas mixing tank can adjust the temperature and determine that the liquid can not be condensed.
Preferably, the central controller automatically adjusts the flow rates of the carrier gas and the diluent gas according to the input target liquid concentration and the total flow rate; the central controller automatically adjusts the pushing speed of the microfluid sampling device according to the input type, characteristic parameters, concentration and total flow of the target liquid; the central controller automatically adjusts the evaporation temperature of the liquid evaporation device according to the type of the liquid; the central controller automatically or manually adjusts the fan speed of the gas mixing tank.
Claims (6)
1. A liquid dynamic gas distribution device comprises a central controller, a source gas, two mass flowmeters, a microfluid sample introduction device, a liquid evaporation device, a gas mixing tank and a drying tank, wherein the two mass flowmeters are respectively used for controlling carrier gas and diluent gas; the source gas is simultaneously connected into two gas paths, one path is used as carrier gas and is used for carrying evaporated liquid, the other path is used as diluent gas, the flow rates of the two paths of gas are controlled by a mass flow meter, and one-way stop valves are arranged to prevent the gas from flowing back; liquid to be evaporated is loaded in the micro-fluid sample feeding device, and the liquid is pushed into the liquid evaporation device at a fixed speed through a peristaltic pump or a micro-injection pump; controlling the temperature of the liquid evaporation device; the gas mixing tank is used for mixing gas; the drying tank is used for placing the molecular sieve by a customer; the central controller controls and adjusts the flow rate of the mass flow meter, the pushing speed of the microfluid sample introduction device, the evaporation temperature of the liquid evaporation device and/or the fan rotating speed of the gas mixing tank; the liquid evaporating device is composed of porous molecular sieve and heating plate, and is connected with the carrier gas path and the microfluid sample introduction device, and is characterized in that the upper end of the liquid evaporating device is provided with a porous molecular sieve which is arranged in the funnel-shaped device and is simultaneously connected with the microfluid sample introduction device and the carrier gas path; the bottom is the hot plate, and the hot plate temperature regulation just contacts with the molecular sieve, utilizes heat-conduction, and the molecular sieve soaks the filtration and heats the evaporation with liquid, thereby makes liquid fully be heated and evaporate completely when guaranteeing that liquid drains smoothly thereby produce the gas of continuity.
2. The liquid dynamic gas distribution device of claim 1, wherein the flow of the carrier gas and the dilution gas is controlled by a mass flow meter, and a one-way stop valve is arranged, and the range of the mass flow meter is from 10sccm to 100slm according to the concentration and flow requirements of the gas distribution, so that the final gas distribution concentration range is from 1ppt to 10 ppt6ppm。
3. The liquid dynamic air distribution device of claim 1, wherein the micro-fluid sample injection device is mainly composed of a peristaltic pump or a micro-sample injection pump, the sample injection needle is connected with the liquid evaporation device, the completely sealed sample injection speed and time are directly controlled by the central controller, the sample injection speed is from pL/min to mL/min, and the control range is wide.
4. The liquid dynamic gas distribution device of claim 1, further comprising a gas mixing tank for mixing the two gas flows of the two gas paths, wherein the gas mixing tank is temperature regulated and coated to ensure that the liquid does not condense and adsorb.
5. The liquid dynamic gas distribution device of claim 1, wherein the central controller automatically adjusts the flow rate of the mass flow meter according to the input target liquid concentration and the total flow rate; the central controller automatically adjusts the pushing speed of the microfluid sampling device according to the input type, characteristic parameters, concentration and total flow of the target liquid; the central controller automatically adjusts the evaporation temperature of the liquid evaporation device according to the type of the liquid; the central controller automatically or manually adjusts the fan speed of the gas mixing tank.
6. The liquid dynamic gas distribution device of claim 1, wherein the drying tank is connected by a movable opening, the filter medium loaded in the drying tank is easy to replace, and the whole drying tank can be directly disassembled.
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| CN107497308A (en) * | 2017-08-07 | 2017-12-22 | 武汉辰龙精密仪器有限公司 | A kind of " liquid-gas " generating means |
| CN107744731A (en) * | 2017-11-22 | 2018-03-02 | 安徽理工大学 | A kind of air distributing device that experiment is fired for fuel gas, liquid vapour and dust |
| CN108593848A (en) * | 2018-04-25 | 2018-09-28 | 清华大学深圳研究生院 | A kind of normal concentration sample gas generation device and production method |
| CN108489794A (en) * | 2018-06-28 | 2018-09-04 | 中国科学技术大学 | A kind of sample dilution sampling device |
| CN109569338A (en) * | 2018-11-06 | 2019-04-05 | 中广核研究院有限公司 | A kind of vapoury multicomponent standard-gas generating device |
| CN109738529A (en) * | 2018-12-20 | 2019-05-10 | 山东玉皇化工有限公司 | The method that dynamic air-distributing demarcates low-boiling point liquid and admixture of gas |
| CN109708943B (en) * | 2019-02-28 | 2021-09-14 | 山东非金属材料研究所 | Preparation method of trichlorobromomethane gas standard substance in nitrogen |
| CN111122584A (en) * | 2019-12-20 | 2020-05-08 | 苏州阿洛斯环境发生器有限公司 | Fogging device and fogging method |
| CN112944213A (en) * | 2021-03-17 | 2021-06-11 | 重庆渝微电子技术研究院有限公司 | Dynamic gas-liquid distribution system and method |
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| JP2012086164A (en) * | 2010-10-20 | 2012-05-10 | Jfe Steel Corp | Device and method for producing mixed gas production |
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| GB2446409B (en) * | 2007-02-06 | 2011-05-04 | Secretary Trade Ind Brit | Fluid mixtures |
| CN101713712A (en) * | 2008-10-06 | 2010-05-26 | 中国科学院大连化学物理研究所 | Dynamic preparation device for standard gas of solid-phase or liquid-phase compounds and application thereof |
| CN102039096B (en) * | 2009-10-16 | 2012-10-24 | 北京均方谱元科技有限公司 | System and method for dynamically distributing gases of volatile liquid under room temperature and normal pressure |
| CN202052481U (en) * | 2010-04-30 | 2011-11-30 | 中国人民解放军总装备部后勤部防疫大队 | Hydrazine propellant standard gas generator |
| CN102258958B (en) * | 2011-05-27 | 2014-07-23 | 中国计量科学研究院 | Dynamic gas distributing system for standard gas |
| CN204107347U (en) * | 2014-10-21 | 2015-01-21 | 武汉钢铁(集团)公司 | The anti-NH of constant temperature 3the SCR method distributing instrument of corrosion |
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| JP2012086164A (en) * | 2010-10-20 | 2012-05-10 | Jfe Steel Corp | Device and method for producing mixed gas production |
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