CN107737514A - A kind of fluorescence drier and preparation method thereof - Google Patents
A kind of fluorescence drier and preparation method thereof Download PDFInfo
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- CN107737514A CN107737514A CN201711030910.4A CN201711030910A CN107737514A CN 107737514 A CN107737514 A CN 107737514A CN 201711030910 A CN201711030910 A CN 201711030910A CN 107737514 A CN107737514 A CN 107737514A
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- drier
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
- B01D53/28—Selection of materials for use as drying agents
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- Oil, Petroleum & Natural Gas (AREA)
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- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention belongs to drier field, more particularly in the related drier of air-conditioning or the detection leakage of other refrigeration systems.A kind of fluorescence drier, the desiccant particle overlying are loaded with fluorescent dye.Preparation method, comprise the following steps：The desiccant particle of forming is selected, selects fluorescent dye solvent, and determine saturated extent of adsorption of the drier to solvent；Measure fluorescent dye to be dissolved in solvent, prepare the solution containing fluorescent dye of respective concentration, concentration of polymer solution is between 0.01 ‰ 20%；Desiccant particle is put into the above-mentioned solution containing fluorescent dye, it is filtered, the desiccant particle for being adsorbed with fluorescent dye is evaporated under reduced pressure 1h, obtains fluorescence drier.The present invention carries the novel drier of fluoroscopic examination, fluorescent dye can directly carry out dyestuff loading processing on drier production line, fluorescent dye is introduced into air-conditioning refrigeration system while desiccant container is loaded, has saved the cost of labor of air conditioner refrigerating manufacturer production line.
Description
Technical field
The invention belongs to drier field, more particularly in the related drying of air-conditioning or the detection leakage of other refrigeration systems
Agent.
Background technology
Present automobile all uses new R-134a refrigerants substantially, and this system is more more compact than former R-12 systems,
Coolant quantity is also relatively fewer, so refrigeration performance influence of the leakage of refrigerant on novel air conditioning system is bigger.And its leakage point is examined
Survey is more difficult compared with R12, because the PAG lubricating oil of R-134a systems does not have " oiliness ", in the past by inspection oil stain or wet point
Leak detection mode just become inadvisable.It is a kind of so that quick, accurate, clean, fluoroscopic leak test technology of the safety for advantage meets the tendency of and
It is raw, if in fluorescent dye addition system, then with black light light irradiation, the fluorescent dye on leakage point will send fluorescence with
Show that air-conditioning system has seepage.Fluorescent dye can also be retained in systems for a long time, play prevention effect.This technology initially in
Nineteen ninety-five is invented by U.S. TP Spectronics u s companys of parent company, and company is additionally filled in its automobile air-conditioner production line
Dry plate shape air-conditioning fluoroscopic leak test agent, for find search automotive air-conditioning system leakage.
The method that refrigeration system is introduced on fluorescent dye, earliest United States Patent (USP) US5149453 reports are directly by one
Quantitative fluorescent dye compound is added in lubricating oil or refrigerant system.So fluoroscopic leak test agent is arrived with system circulation
Up to leak source position.When refrigeration system is exposed under fluorescence, even the leak source of very little can be found.But this method is led
Cause has part during refrigerant or oil filling and remained in outside system, influences the judgement of leak source.
United States Patent (USP) US5440919 and US5681984 are proposed to be attached to fluoroscopic leak test agent on carrier and then added again
Enter into desiccant container, be eventually introduced refrigeration system, to reach the purpose of fluoroscopic leak test, but need to give birth in desiccant container
Increase by a step in producing line and manually launch fluoroscopic leak test agent absorber, additionally increase cost of labor.US5440919 also proposes to incite somebody to action
Desiccant container is manufactured on the preset fabric of fluorescent dye again and introduces refrigeration system, or in some cases by advance
Hybrid desiccant and fluorescent dye, then adhere to fluorescent dye on desiccant particle by heating melting, it is re-introduced into refrigeration system
System is feasible, but the method processing temperature is higher, typically more than 200 DEG C, and fluorescence in solid mixed process
Agent skewness problem is inevitable.
The content of the invention
The technical problem to be solved in the present invention is：Solve air-conditioning or other refrigeration systems detection leakage fluorescer is dosed not
Just the problem of, extra artificial dispensing process is numerous and diverse, there is provided a kind of fluorescence drier, drier carry fluorescent dye, and cost is low, throw
Add facility.
The present invention is that technical scheme is used by solving the above problems：A kind of fluorescence drier, is related to desiccant particle,
The desiccant particle overlying is loaded with fluorescent dye.
Preferably, the desiccant particle is selected from 3A, 4A, 5A, 13X, AH-7, AH-9, AH-11, Al2O3In one kind or
Two or more mixing.
Preferably, the one kind of the fluorescent dye in perylene, naphthalimide, cumarin, anthracene, thioxanthene alkane
Or two or more mixing.
A kind of preparation method of described fluorescence drier, comprises the following steps：
A) desiccant particle of forming is selected, selects fluorescent dye solvent, and determine saturated extent of adsorption of the drier to solvent；
B) measure fluorescent dye to be dissolved in solvent, prepare the solution containing fluorescent dye of respective concentration, concentration of polymer solution in
Between 0.01 ‰ -20%；
C) desiccant particle is put into the above-mentioned solution containing fluorescent dye, it is filtered, the drier of fluorescent dye will be adsorbed with
Particle is evaporated under reduced pressure 1h, obtains fluorescence drier.
Preferably, the temperature of the vacuum distillation is 50-100oC。
Preferably, the mass concentration of the solution containing fluorescent dye is 0.1 ‰ -10%.
Preferably, the one or more in arene, fat hydrocarbon, alicyclic hydrocarbon type and halogenated hydrocarbons.
Preferably, the solvent is selected from arene：Benzene,toluene,xylene；The fat hydrocarbon：It is pentane, hexane, pungent
Alkane；The alicyclic hydrocarbon type：Hexamethylene, cyclohexanone, toluene cyclohexanone；The halogenated hydrocarbons：In chlorobenzene, dichloro-benzenes, dichloromethane
One or more kinds of mixing.
Preferably, the solution is separated by filtration the solvent after the distillation of rear and vacuum decompression, recycles again.
The invention provides a kind of new novel drier for carrying fluoroscopic examination, fluorescent dye is on drier production line
Dyestuff loading processing can be directly carried out, and a kind of fluorescence drier and preparation method thereof also has following beneficial benefit：
1st, preparation method is simple, and processing procedure is simple, and each reaction condition is easy to realize；
2nd, fluorescent dye is dissolved using solvent, it is after refrigeration desiccant particles are separated by filtration with the solution of fluorescent dye and true
Solvent after sky vacuum distillation, can be recycled again, reduce the cost of production product；
3rd, fluorescent dye is introduced into air-conditioning refrigeration system while desiccant container is loaded, saves the life of air conditioner refrigerating producer
The cost of labor of producing line.
Embodiment
Below, by embodiment, the present invention will be described in more detail, but the present invention is not by any limit of these examples
It is fixed, not because each embodiment sequencing to the present invention caused by any restrictions.
Embodiment 1
The g of refrigeration drier AH-7 beads 10 is put into toluene solvant, determines that AH-7 is to the adsorbance of toluene by difference assay
5g.Perylene is dissolved in 5g toluene, is configured to the solution of mass concentration 0.5%, is then added thereto AH-7 beads, 2 points
Filtered after clock.60 DEG C of vacuum distillation 1h of AH-7 beads of fluoroscopic leak test agent will be adsorbed, finally give fluorescent dye containing perylene
Drier.
Embodiment 2
By drier Al2O3In the g of bead 20 input xylene solvents, Al is determined by difference assay2O3The adsorbance of paraxylene
For 6 g.Cumarin is dissolved in 6 g dimethylbenzene, 0.3% solution is configured to, then by Al2O3Bead is added thereto, after 5min
Filtering.The Al of fluoroscopic leak test agent will be adsorbed2O3100 DEG C of vacuum distillation 1h of bead, finally give the drying containing fluorescent coumarin dye
Agent.
Embodiment 3
Refrigeration drier AH-9 beads 20g is put into cyclohexane solvent, absorption of the AH-9 to hexamethylene is determined by difference assay
Measure as 5g.Anthracene is dissolved in 5g hexamethylenes, is configured to 0.2% solution, then AH-9 beads are added thereto, filtered after 2min.
1h are evaporated under reduced pressure by 60 DEG C again, finally give the drier of the fluorescent dye containing anthracene.
Embodiment 4
By drier Al2O3In bead 10g input dichloromethane solvents, Al is determined by difference assay2O3Absorption to dichloromethane
Measure as 5g.Naphthalimide is dissolved in 5g dichloromethane, is configured to 0.1% solution, then by Al2O3Bead adds it
In, filtered after 2min.1h are evaporated under reduced pressure by 50 DEG C again, finally give the drier of the fluorescent dye containing naphthalimide.
Embodiment 5
Drier 5A beads 10g is put into toluene solvant, determines that 5A is 4g to the adsorbance of toluene by difference assay.By naphthalene two
Carboximide is dissolved in 4g toluene, is configured to 0.2% solution, is then added thereto 5A beads, is filtered after 2min.Pass through again
60 DEG C of vacuum distillation 1h, finally give the drier of the fluorescent dye containing naphthalimide.
Embodiment 6
To be freezed drier AH-7 and AH-9 bead（In mass ratio 3:7）In 100 g input toluene solvants, determined by difference assay
Hybrid desiccant is 30 g to the adsorbance of toluene.Perylene is dissolved in 30 g toluene, is configured to 0.1% solution, then
AH-7 beads are added thereto, filtered after 5min.Again by 60 DEG C of vacuum distillation 1h, fluorescent dye containing perylene is finally given
Mixed type dry drying prescription.
Embodiment 7
By drier Al2O3With 4A beads（In mass ratio 1:1）In 10g input pentane solvents, determine that mixing is dry by difference assay
Drying prescription is 3g to the adsorbance of pentane.By naphthalimide and cumarin according to mass ratio 1:1 is dissolved in 3g pentanes, is configured to
Drier, is then added thereto by 0.3% solution, is filtered after 2min.Again by 50 DEG C of vacuum distillation 1h, finally give containing naphthalene
The mixed type dry drying prescription of dicarboximide and cumarin mixing fluorescent dye.
Embodiment 8
Refrigeration drier AH-11 beads 10g is put into xylene solvent, the suction of AH-11 paraxylene is determined by difference assay
Attached amount is 4g.By anthracene and cumarin according to mass ratio 1:2 are dissolved in 4g dimethylbenzene, are configured to 0.3% solution, then by AH-11
Bead is added thereto, and is filtered after 2min.Again by 100 DEG C of vacuum distillation 1h, finally give containing anthracene and cumarin mixing fluorescence dye
The drier of material.
Embodiment 9
By drier Al2O3In bead 20g input solvents, Al is determined by difference assay2O3Mixing to chlorobenzene and dichloromethane is molten
Agent（Volume ratio is 1:2）Adsorbance is 10g.Cumarin is dissolved in 10g in the mixed solvents, is configured to 0.15% solution, then will
Drier Al2O3Bead is added thereto, and is filtered after 2min.Again by 100 DEG C of vacuum distillation 1h, finally give containing coumarin fluorescent
The drier of dyestuff.
Embodiment 10
Will refrigeration drier AH-9 and AH-7（In mass ratio 1:1）In bead 20g input solvents, determine that mixing is dry by difference assay
Drying prescription is to chlorobenzene and the mixed solvent of dichloromethane（Volume ratio is 1:2）Adsorbance is 10g.It is molten that cumarin is dissolved in 10g mixing
In agent, 0.18% solution is configured to, then drier bead is added thereto, filtered after 2min.Steamed again by 100 DEG C of decompressions
1h is evaporated, finally gives the mixed type dry drying prescription containing fluorescent coumarin dye.
After the obtained drier containing fluorescent dye of above-described embodiment 1-10 is carried out into non-woven bag encapsulation respectively, add empty
Modulate after running a period of time in cooling system, the pad using uviol lamp to system（Suspicious leak）It is irradiated, so as to
The fluorescence of lower transmitting is excited to judge the position of leakage point in ultraviolet according to fluorescent dye.In refrigeration systems, with refrigeration
The fluorescent dye being loaded on drying machine is covered in the dilution dissolving that circulates of agent and lubricating oil liquid, reaches identification concentration, during detection
Precisely efficiently detect leak source, Detection accuracy is up to 100%.
Claims (9)
1. a kind of fluorescence drier, is related to desiccant particle, it is characterised in that：The desiccant particle overlying is loaded with fluorescence dye
Material.
A kind of 2. fluorescence drier according to claim 1, it is characterised in that：The desiccant particle be selected from 3A, 4A,
5A, 13X, AH-7, AH-9, AH-11, Al2O3One or both of it is mixed above.
A kind of 3. fluorescence drier according to claim 1, it is characterised in that：The fluorescent dye be selected from perylene,
One or both of naphthalimide, cumarin, anthracene, thioxanthene alkane are mixed above.
A kind of 4. preparation method of any described fluorescence drier of claim 1-3, it is characterised in that：Comprise the following steps：
The desiccant particle of forming is selected, selects fluorescent dye solvent, and determine saturated extent of adsorption of the drier to solvent；
Measure fluorescent dye to be dissolved in solvent, prepare the solution containing fluorescent dye of respective concentration, concentration of polymer solution in
Between 0.01 ‰ -20%；
Desiccant particle is put into the above-mentioned solution containing fluorescent dye, it is filtered, the drier of fluorescent dye will be adsorbed with
Grain is evaporated under reduced pressure 1h, obtains fluorescence drier.
A kind of 5. preparation method of fluorescence drier according to claim 4, it is characterised in that：The temperature of the vacuum distillation
Spend for 50-100oC。
A kind of 6. preparation method of fluorescence drier according to claim 4, it is characterised in that：It is described containing fluorescent dye
The mass concentration of solution is 0.01 ‰ -20%.
A kind of 7. preparation method of fluorescence drier according to claim 4, it is characterised in that：It is described to be selected from aromatic hydrocarbon
One or more in class, fat hydrocarbon, alicyclic hydrocarbon type and halogenated hydrocarbons.
A kind of 8. preparation method of fluorescence drier according to claim 7, it is characterised in that：The solvent is selected from fragrance
Hydro carbons：Benzene,toluene,xylene；The fat hydrocarbon：Pentane, hexane, octane；The alicyclic hydrocarbon type：Hexamethylene, cyclohexanone, first
Phenylcyclohexanone；The halogenated hydrocarbons：One or both of chlorobenzene, dichloro-benzenes, dichloromethane are mixed above.
9. according to a kind of preparation method of any described fluorescence drier of claim 4-8, it is characterised in that：The solution
The solvent being separated by filtration after the distillation of rear and vacuum decompression, is recycled again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711030910.4A CN107737514A (en) | 2017-10-30 | 2017-10-30 | A kind of fluorescence drier and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711030910.4A CN107737514A (en) | 2017-10-30 | 2017-10-30 | A kind of fluorescence drier and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107737514A true CN107737514A (en) | 2018-02-27 |
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| CN201711030910.4A Pending CN107737514A (en) | 2017-10-30 | 2017-10-30 | A kind of fluorescence drier and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022102026A1 (en) * | 2020-11-11 | 2022-05-19 | 三菱電機株式会社 | Refrigeration cycle device |
| WO2022118467A1 (en) * | 2020-12-04 | 2022-06-09 | 三菱電機株式会社 | Refrigeration cycle device |
| CN117861475A (en) * | 2024-03-12 | 2024-04-12 | 河北华油天然气有限责任公司 | Low-temperature-resistant gas leakage detecting agent and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5149453A (en) * | 1985-02-25 | 1992-09-22 | H. B. Fuller Automotive Products, Inc. | Method for detecting leakage in a refrigeration system |
| US5440919A (en) * | 1994-08-29 | 1995-08-15 | Spectronics Corporation | Method of introducing leak detection dye into an air conditioning or refrigeration system |
| US5681984A (en) * | 1996-07-22 | 1997-10-28 | Bright Solutions, Inc. | Leak detection in heating, ventilating, refrigeration, and air conditioning systems utilizing adsorptive materials |
| WO2005113807A2 (en) * | 2004-05-05 | 2005-12-01 | Spectronics Corporation | Enhanced leak detection dye carrier |
| CN101672556A (en) * | 2009-09-19 | 2010-03-17 | 浙江三花汽车控制系统有限公司 | Liquid storage drying device with fluorescer |
-
2017
- 2017-10-30 CN CN201711030910.4A patent/CN107737514A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5149453A (en) * | 1985-02-25 | 1992-09-22 | H. B. Fuller Automotive Products, Inc. | Method for detecting leakage in a refrigeration system |
| US5440919A (en) * | 1994-08-29 | 1995-08-15 | Spectronics Corporation | Method of introducing leak detection dye into an air conditioning or refrigeration system |
| US5681984A (en) * | 1996-07-22 | 1997-10-28 | Bright Solutions, Inc. | Leak detection in heating, ventilating, refrigeration, and air conditioning systems utilizing adsorptive materials |
| WO2005113807A2 (en) * | 2004-05-05 | 2005-12-01 | Spectronics Corporation | Enhanced leak detection dye carrier |
| CN101672556A (en) * | 2009-09-19 | 2010-03-17 | 浙江三花汽车控制系统有限公司 | Liquid storage drying device with fluorescer |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022102026A1 (en) * | 2020-11-11 | 2022-05-19 | 三菱電機株式会社 | Refrigeration cycle device |
| WO2022118467A1 (en) * | 2020-12-04 | 2022-06-09 | 三菱電機株式会社 | Refrigeration cycle device |
| CN117861475A (en) * | 2024-03-12 | 2024-04-12 | 河北华油天然气有限责任公司 | Low-temperature-resistant gas leakage detecting agent and preparation method thereof |
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