CN108285776B - Application method of hydrocarbon refrigeration additive with warning, leakage detecting and explosion suppression functions - Google Patents
Application method of hydrocarbon refrigeration additive with warning, leakage detecting and explosion suppression functions Download PDFInfo
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M133/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen
- C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
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- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
- G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/221—Six-membered rings containing nitrogen and carbon only
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Abstract
The invention discloses an application method of a hydrocarbon refrigerant additive with warning, leak detection and explosion suppression functions, which is characterized in that the additive is an oil-soluble compound, is added into refrigerating machine oil and enters a refrigerating system along with the refrigerating machine oil; the odor threshold is low, and the odor alarm has an alarm function after the refrigerant leaks; bright yellow green light can be emitted under natural conditions, the leakage position can be accurately displayed, and the leakage detection efficiency is improved; meanwhile, the device has the function of inhibiting the explosion of the hydrocarbon refrigerant, and improves the intrinsic safety of the refrigerant. The invention has the advantages of sensitivity, accuracy, rapidness and safety, and the system solves the urgent requirements of warning, leak point tracking and safety after the leakage of the hydrocarbon refrigerant.
Description
Technical Field
The invention relates to a refrigerant additive, in particular to an application method of a hydrocarbon refrigeration additive with warning, leakage detecting and explosion suppression functions.
Background
Hydrocarbon refrigerants refer to single compounds or multi-component mixtures composed of lower paraffins, the most common hydrocarbon refrigerants being propane, isobutane, n-butane or mixtures thereof. The hydrocarbon refrigerant does not damage the ozone layer, has no greenhouse effect, has the advantages of nature, environmental protection, high efficiency, energy conservation, high refrigeration quality, money and quantity saving, high oil mixing rate, wide application and the like, and is the refrigerant with the most application prospect. However, the hydrocarbon refrigerant has been widely accepted for a long time and is difficult to popularize and apply mainly because it is colorless and odorless, is not easy to detect after leakage, has a relatively low ignition point, and forms an explosive gas mixture with air after accumulating in the air to reach a lower concentration limit.
At present, the means for improving the use safety of the hydrocarbon refrigerant mainly include the following:
(1) the warning odorant is added into the system, so that people can easily detect the leakage of the refrigerant, and the warning or alarm function is realized. Chinese patents CN200510029292, CN200480033507, CN200480038014, CN200680042084, CN200810094429, CN200910214514 and CN201010154844 respectively adopt hydrogen sulfide, ethanethiol, alkyl sulfide, acrylic ester and the like as warning odors, so that the warning effect is improved. But the hydrogen sulfide has poor stability and corrodes pipelines; ethanethiol, alkyl thioether, acrylate, etc. have high toxicity and are easy to decompose and lose efficacy. The Chinese patent CN201210276788 adopts thiophene derivatives and pyridine as warning gases, has a good warning effect and good stability and system compatibility, but the added warning agent has a single purpose, only reminds a user of the warning effect, and has no influence on improving the leak detection efficiency and the intrinsic safety of the refrigerant.
(2) And an explosion inhibitor is added into the system to reduce the explosion probability. Chinese patents CN200710036014, CN200710056679 and CN91108302 adopt a large amount of carbon dioxide refrigerant as inert filler to inhibit explosion reaction. The difference between the density and the volatility of the high-content two components is large, so that the service life of the compressor is shortened; chinese patents CN200710068821, CN200710304784, CN200810115669, CN200810094555, CN200810097393, CN200810231911, CN200910018489, CN200910102217, CN200910260825, CN201010205315, CN201010141092, CN201010128616, CN02126637 and CN201210064427 adopt fluorine-containing halothane refrigerant as explosion suppressant, but the dosage is large and the cost is high. The Chinese patent CN 201410508003 adopts alkyl lead and iron pentacarbonyl as explosion suppression agents, the explosion suppression effect is obvious, but the system mixing uniformity is poor, and a leakage position cannot be quickly found during leakage.
(3) And a tracer is added into the system, so that the leak detection efficiency is improved. Chinese patent CN200480033507 proposes a detectable refrigerant composition and its application, which uses hydrofluorocarbon, fluoroether, hydrocarbon alcohol, hydrocarbon amine, nitrogen oxide, ammonia and other compounds as tracer, and these substances are colorless and odorless or have extremely low olfactory threshold, and need to be detected by means of special devices such as chemical/electro-active array detector, ultrasonic detector and so on, and cannot be visually detected. The fluorescent leak detection technology is used for finding and searching the leakage of the automobile air conditioning system, relevant information is not found in Chinese patents, and the world patents WO 20111320 and WO 2005049761 and the U.S. patents US 6248890, US 6165384, US 4758366 and US 6248890 adopt a compound with fluorescent property as a fluorescent tracer to be applied to the refrigerant leak detection. However, the fluorescent agent is limited by the molecular design level of the fluorescent agent, the existing fluorescent agent can emit fluorescence only under the irradiation of an ultraviolet lamp, and the ultraviolet lamp is opened under the condition of refrigerant leakage to have certain potential safety hazard. Therefore, this technique is suitable only for fluorine-containing refrigerant systems having no explosive characteristics such as R22 and R134 a. Fluorescent agents that match hydrocarbon refrigerants have not been reported.
It follows that the addition of either a warning agent, an explosion suppressant, or a tracer, in part, solves the problem in some way. Although the multi-component compounding can possibly achieve a better comprehensive effect, the application of the multi-component compounding is limited by the problems of poor compatibility among the components, excessive addition amount and the like. More importantly, the existing additives are directly mixed with the refrigerant. Since most additives are in liquid or solid form (CO)2、NH3Except) mixing-selling-charging with gaseous hydrocarbon refrigerant inevitably has the defect of different product performance of each batch due to density difference.
Therefore, the prior art is in need of improvement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a single-component additive for hydrocarbon refrigerant, which has the functions of warning, detecting leakage and suppressing explosion. The additive has good oil solubility, and can enter a refrigeration system together with the refrigerator oil; the odor threshold is extremely low, and the odor alarm has an alarm function after the refrigerant leaks; the molecule contains a fluorescent chromophoric group, so that bright yellow green light can be emitted under natural light, the leakage position can be accurately displayed, and the leakage detection efficiency is improved; the explosion suppression group can effectively suppress the explosion tendency of the hydrocarbon refrigerant and improve the intrinsic safety of the refrigerant. It is suitable for various refrigerating equipments such as air conditioner, refrigerator and freezer.
The principle of the invention is as follows: a small amount of oil-soluble additive is dissolved in the refrigerator oil and enters a refrigerating system together. In the running process of the refrigeration equipment, the refrigerant is mixed with the hydrocarbon refrigerant to be homogeneous, and the normal running of a refrigeration system is not influenced. When the system leaks, the additive has obvious peculiar smell and can play a role in warning; the peak value of the absorption wavelength of the additive is 320-475 nm, so that the energy required by fluorescence generation can be obtained from natural light; the emission wavelength is 450-650 nm, and the most sensitive to human being can be emittedYellow green fluorescence is sensed, and the observation is convenient. Therefore, if leakage exists, the leakage position can be directly observed by naked eyes; meanwhile, under dangerous environments (such as electric sparks, open flames and the like), the additive can be decomposed to generate a large amount of inhibitor free radicals (CF)2，NH2) By activated radicals (CH) generated with hydrocarbon refrigerants3OH, HCO, etc.) to remove the activated free radicals needed by explosion reaction, thereby achieving the explosion suppression effect.
In order to solve the technical problems, the embodiment of the invention provides a single-component additive for hydrocarbon refrigerants, which has the functions of warning, detecting leakage and suppressing explosion, and adopts the following technical scheme:
a monocomponent additive with warning, leakage detecting and explosion suppressing functions for hydrocarbon refrigerant features that its parent structure is 1, 8-naphthoylimine, the N atom is linked with haloalkane group, and the naphthalene ring at No. 3 or No. 4 is linked with mercapto or sulfenyl.
The further preferable scheme of the invention is as follows: the alkyl halide is low-carbon chain alkyl halide (C atom number is less than 4), and has a chemical formula of-CF2I、-CHFCF3、-CF2CF3、-CH2CF2CF3、-CHFCF2CF3、-CF2CF2CF3、-CHFCF2CHF2or-CHFCF3CH2F, in-CF2I is preferably; the sulfenyl belongs to low-carbon chain sulfenyl (the number of C atoms is less than 4), and the chemical formula is-SCH3、-SCH2CH3or-SCH2CH2CH3to-SCH3Preferably, it is used.
Compared with the prior art, the single-component additive for the hydrocarbon refrigerant, which has the functions of warning, leak detection and explosion suppression, has the following advantages. Firstly, the additive is dissolved in the refrigerator oil and enters a refrigerating system, but is not premixed with a hydrocarbon refrigerant and then refilled, so that the defect that the product performance of each batch is different due to density difference of components is avoided; secondly, single group diversity 'warning, leak detection and explosion suppression' functions are integrated, so that the problems of poor compatibility among various single-function additives, overlarge addition amount and the like are solved; thirdly, the smell is special, the smell of common substances in the surrounding environment (such as gas, sewer and rotten taste of food) is obviously distinguished, the olfactory discrimination is high, the leakage can be still obviously detected even if the leakage is diluted by 100 times in the air, and the warning effect of preventing the leakage is obvious; fourthly, the most sensitive yellow-green fluorescence of human can be observed by naked eyes without professional instruments, so that the observation is convenient; fifthly, the explosion suppression performance is good, the chemical reaction is directly interfered under the condition of quasi-explosion by utilizing the chemical explosion suppression principle, and the explosion suppression agent has the characteristics of small using amount and good effect; sixth, the storage stability is high. The additive has the advantages that the system components of the additive do not change obviously after 360-day accelerated aging test under the constant temperature condition of 100 ℃, the additive still has obvious functional characteristics, and can meet the requirement of long-term recycling; seventh, corrosion resistance is good. The additive has good compatibility with (copper, iron or aluminum material) pipelines, does not generate corrosivity, and is beneficial to long-term use of refrigeration equipment.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
According to the single-component additive for the hydrocarbon refrigerant with the functions of warning, leak detection and explosion suppression, in the specific implementation, the hydrocarbon refrigerant is represented by propane, the quality (calculated by 100%) of matched refrigerating machine oil is determined according to the mass ratio of the common refrigerant to the refrigerating machine oil on the market, and then the adding amount of the additive is determined. Wherein: the additive is self-made, and the purity is more than or equal to 99%. The addition amount of the additive (based on the total mass of the refrigerating machine oil) is 5-20%. Propane is a commercial chemical raw material, the purity of an effective component is more than or equal to 99.6 percent, and the water content is less than or equal to 0.002 percent; the refrigerator oil is a commercial product, and the water content is less than or equal to 0.05 percent.
Selecting a certain air conditioner capable of normally operating as an implementation object. The air-conditioning pipe is externally connected with a flow controllable regulating valve for simulating refrigerant leakage. The method comprises the steps of completely removing original refrigerant and refrigeration oil in the air conditioner, filling a corresponding amount of propane according to the power of the air conditioner, and injecting the refrigeration oil with different additive contents into a system from a low-pressure port of the air conditioner according to the mass ratio of the propane to the refrigeration oil of 2: 1. After filling, electrifying and running for 20 min to uniformly mix all the components.
The warning evaluation method of the additive comprises the following steps: in the semi-closed area without wind and open fire, an adjusting valve externally connected with an air conditioning pipe is opened, and the gas flow is fixed to be 100 ml/min. After 2 min, 5 independent testers standing 5 m from the regulating valve evaluated the olfactory sensation of the refrigerant containing the additive. The odor intensity of the finished product of the hydrocarbon refrigerant can be evaluated, namely the warning capability of the additive is respectively set to be 1 grade (very weak), 2 grade (weak), 3 grade (general), 4 grade (stronger) and 5 grade (strong).
The leak detection evaluation method of the additive comprises the following steps: in the semi-closed area without wind, naked flame and strong light, an adjusting valve externally connected with an air-conditioning pipe is opened, and the gas flow is fixed to be 100 ml/min. After 2 min, 5 independent testers standing 1m from the regulating valve observed whether fluorescence was produced at the outlet of the regulating valve. Evaluation of the fluorescence intensity allows the leak detection ability of the additive to be determined, and the level 1 (very weak), the level 2 (weak), the level 3 (normal), the level 4 (strong), and the level 5 (strong) are set.
The explosion suppression evaluation method of the additive comprises the following steps: discharging hydrocarbon refrigerant through an adjusting valve, uniformly mixing the refrigerant with air according to a mass ratio of 1:5, and filling the mixture into a stainless steel explosion-proof steel ball which is vacuumized in advance until the system pressure is 0.1 MPa. Wherein the size of the explosion chamber is phi x h =300 mm x 300 mm, and the volume is about 20L; the discharging firing pin is of a pin-pin structure, is made of brass, has a curvature radius of 0.5-1 mm, a discharging gap of 2 mm, a discharging loop resistance value of 0 omega, and an ignition voltage of 8 kV. The wall of the explosion tank is provided with a pressure sensor which is connected with a recorder. And measuring the pressure in the steel ball 30 min after the electric spark ignition. The measured pressure value (absolute pressure) can determine the explosion condition of the gas in the steel ball, thereby measuring the explosion suppression effect of the additive.
Example 1: the additive is 6-methylthio-2-difluoroiodomethyl-1H-benzisoquinoline-1, 3(2H) -diketone with a molecular structural formula
. The additive amount of the water-soluble polymer in the refrigerator oil(based on the total mass of the refrigerating machine oil) is 5%. The finished refrigerant prepared by the additive is evaluated as 2-grade (weak) in alarm strength after leakage, 3-grade (general) in leakage detection capability and 0.9MPa in pressure value after ignition (partial explosion of the refrigerant).
Example 2: the additive is 5-mercapto-2-pentafluoroethyl-1H-benzisoquinoline-1, 3(2H) -diketone with a molecular structural formula
. The amount thereof added to the refrigerator oil was 20% by mass based on the total mass of the refrigerator oil. The finished refrigerant prepared by the additive of the invention is evaluated as 5-grade (strong) in alarm strength after leakage, 5-grade (strong) in leakage detection capability and 0.1MPa in pressure value after ignition (the refrigerant is not exploded).
Example 3: the additive is 6-propylthio-2- (2,2,3,3, 3-pentafluoropropane) -1H-benzisoquinoline-1, 3(2H) -diketone with a molecular structural formula
. The amount thereof added to the refrigerator oil was 10% by mass based on the total mass of the refrigerator oil. The alarm strength of the finished refrigerant prepared by the additive is evaluated to be 3 grade (general), the leakage detection capability is evaluated to be 4 grade (stronger), and the pressure value after ignition is 0.3MPa (a small part of the refrigerant is exploded).
Example 4: the additive is 5-ethylthio-2- (1,2,2, 3-trifluoropropyl) -1H benzisoquinoline-1, 3(2H) -diketone with a molecular structural formula
. The amount of the additive in the refrigerator oil (based on the total mass of the refrigerator oil) was 15%. The finished refrigerant prepared by the additive is evaluated as 4-grade (stronger) in alarm strength after leakage, 5-grade (stronger) in leakage detection capability and 0.1MPa in pressure value after ignition (the refrigerant is not exploded).
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (6)
1. An application method of a hydrocarbon refrigeration additive with warning, leak detection and explosion suppression functions is characterized in that: before use, the additive is dissolved in the refrigerator oil and is added into the refrigeration equipment together with the refrigerator oil; the additive accounts for 5-20% of the total weight of the refrigerator oil, wherein the matrix structure of the additive is 1, 8-naphthalimide, and a halogenated alkane group (R) is connected to a nitrogen atom1) Having a mercapto or mercapto group (R) attached to the naphthalene ring2) The expression of the parent structure is as follows:
2. haloalkane hydrocarbon group (R) according to claim 11) Characterized in that the alkyl halide R1Belongs to low carbon chain halogenated alkane, and the number of C atoms is less than 4.
3. Haloalkane group (R) according to claim 1 or 21) Characterized in that the chemical formula is-CF2I、-CHFCF3、-CF2CF3、-CH2CF2CF3、-CHFCF2CF3、-CF2CF2CF3、-CH(CF3)2、-CHFCF2CHF2or-CHFCF3CH2F。
4. The mercapto or mercapto (R) compound according to claim 12) Characterised in that the mercapto or mercapto group (R)2) At the 5-or 6-position of the naphthalene ring.
5. The hydrocarbylthio (R) of claim 1 or 42) Characterised in that the hydrocarbon thio group (R)2) Belongs to low carbon chain hydrocarbon sulfenyl, and the number of C atoms is less than 4.
6. The hydrocarbylthio (R) of claim 1 or 42) Characterized in that the chemical formula is-SCH3、-SCH2CH3or-SCH2CH2CH3。
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| CN201610328131.1A CN105969313B (en) | 2016-05-17 | 2016-05-17 | A kind of carbon-hydrogen refrigerant one pack system additive |
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| CN110848876B (en) * | 2018-08-21 | 2021-07-02 | 奥克斯空调股份有限公司 | Refrigerant leakage detection method and system and air conditioner |
| CN110940045B (en) * | 2018-09-21 | 2021-04-27 | 奥克斯空调股份有限公司 | Air conditioner refrigerant leakage detection method and air conditioner |
| CN110940043B (en) * | 2018-09-21 | 2021-05-18 | 奥克斯空调股份有限公司 | Air conditioner refrigerant leakage detection method and air conditioner |
| CN112378602B (en) * | 2020-11-30 | 2023-05-16 | 中国第一汽车股份有限公司 | Pure electric vehicle air conditioner pipeline split charging pipeline detection equipment and control method thereof |
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| CN102775964A (en) * | 2012-08-06 | 2012-11-14 | 江苏福瑞至环保新材料有限责任公司 | Hydrocarbon refrigerant with warning smell |
| CN105189423A (en) * | 2013-03-13 | 2015-12-23 | 阿科玛股份有限公司 | Methods for purifying and stabilizing hydrofluoroolefins and hydrochlorofluoroolefins |
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| CN108285776A (en) | 2018-07-17 |
| CN105969313B (en) | 2018-02-06 |
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