CN104403638B - Preparation method for nanoparticle enhanced refrigerant - Google Patents
Preparation method for nanoparticle enhanced refrigerant Download PDFInfo
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- CN104403638B CN104403638B CN201410648019.7A CN201410648019A CN104403638B CN 104403638 B CN104403638 B CN 104403638B CN 201410648019 A CN201410648019 A CN 201410648019A CN 104403638 B CN104403638 B CN 104403638B
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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Abstract
The invention discloses a preparation method for a nanoparticle enhanced refrigerant. The method includes the steps of: in terms of weight part, dispersing 5-15 parts of nano-nickel protoxide into 1000 parts of ethanol, then adding 1-10 parts of hexafluorobutyl acrylate, 0.1-1 part of benzoyl peroxide, 0.1-5 parts of polyvinyl alcohol, and 0.1-1 part of sodium dodecyl benzene sulfonate, and carrying out reaction at 60-80DEG C for 6-15h to obtain a surface polymerized nano-nickel protoxide micro-suspension solution; and subjecting the obtained nano-nickel protoxide micro-suspension solution to liquid phase blending with 2, 3, 3, 3-tetrafluoropropene, 1, 1, 1, 3-tetrafluoropropene, and 1-ethyl-3-methylimidazole diethylphosphoric acid salt in a mass ratio of 1:8000-50000:10-50000:0.1-0.5, thus obtaining the nanoparticle enhanced refrigerant product. The method provided by the invention has the advantages of simple process, low cost and green and environmental protection, and the product has excellent heat transfer performance.
Description
Technical field
The present invention relates to the preparation method of cold-producing medium, particularly a kind of preparation method of nano particle reinforced type cold-producing medium.
Background technology
In refrigeration, air-conditioning or a heat transfer system, expect lubricating oil and cold-producing medium at least some portion of the system
Can be with contacting one another, such as in ASHRAE handbooks in point:It is illustrated in HVAC system and equipment.Therefore, no matter the lubricant
It is individually or as the part in a pre-mix pack to be added to a refrigeration, air-conditioning or heat to pass with cold-producing medium
In delivery system, still expect that they contact within the system and therefore must be compatible.Due to crystal grain it is superfine, in crystal boundary
With the atom of defect center in crystal grain and the quantum size effect, small-size effect, skin effect and the maroscopic quantity that itself have
Sub- tunnel-effect etc. makes nano material that there is special drop to rub antifriction and high compound ability in terms of lubrication with tribology.Nanometer thing
Matter in friction surface in the form of nano particle or nanometer film, with good greasy property and antifriction performance, receive by addition
Lubricant made by rice material can significantly increase greasy property and load-carrying properties, improve the quality of product, be particularly suitable for using
In the lubrication occasion of harsh conditions.Since the nineties in 20th century, researcher starts exploration and is applied to nano material technology by force
Change field of heat transfer, research efficient heat transfer cooling technology of new generation.Nineteen ninety-five, Choi of Argonne National Laboratories of the U.S. et al.
A brand-new concept-nano-fluid is proposed first.Nano-fluid refer to a metal or non pinetallic nano powder be distributed to water,
In the tradition heat transferring medium such as alcohol, oil, prepare uniformly, stable, the novel heat exchange medium of high heat conduction, this is that nanometer technology is applied to
The research of the novelty of Thermal Power Engineering this traditional field.Nano-fluid is in the energy, chemical industry, automobile, building, microelectronics, information
There is huge potential application foreground Deng field, so as to become the study hotspot in the crowd such as material, physics, chemistry, thermal conduction study field.
The such as Yong member of Imperial Academy (the Yong member of Imperial Academy, Bi Shengshan, Shi Lin .HFC134a/TiO2Nano-particle working medium system is applied to refrigerator
Experimental study [J]. Journal of Chemical Industry and Engineering, 2006 (5):HFC134a/ ore deposits 141-145.) being added to nano particle in refrigeration oil
Thing refrigeration oil/nano-TiO2Working medium system is applied in domestic refrigerator, it is found that its performance parameter is slightly better than HFC134a/ Esters oils
System.
And for example China Patent Publication No. CN102295917A discloses a kind of nano particle reinforced type refrigerant hydrate phase
Become the preparation method of cold-storage working substance, it is using the solubilization of compound surfactant, cold-producing medium is soluble in water, thermodynamics is obtained
Stable cold-producing medium microemulsion, is then scattered in nano-particle in cold-producing medium microemulsion, and nano particle reinforced refrigeration is obtained
Agent hydrate phase change cold-storage working substance.By the way that nano-particle is stably dispersed in into cold-producing medium microemulsion system come heat and mass transfer enhancement,
Increase reaction interface, induces nonhomogen-ous nucleation, so as to significantly reduce the induction time and degree of supercooling of hydrate generation, effectively
The brilliant effect of rush is reached.The technique is disperseed using ultrasonic wave, and large-scale production should not be realized.
And for example China Patent Publication No. CN101434833A discloses a kind of nano refrigerant hydrate phase change cold-storage working substance
And preparation method thereof, surfactant is soluble in water, the aqueous solution of surfactant is obtained, then cold-producing medium is added drop-wise into table
In the aqueous solution of face activating agent, stirring is until solution is changed into bright from muddiness.According to surfactant is in water and makes
Solubility in cryogen, can be soluble in water by surfactant, it is also possible in being dissolved in cold-producing medium.The system need not apply to stir
Mix, disturb and outfield by water phase is mutually sufficiently mixed uniformly with cold-producing medium, cold-producing medium with micelle or (and) in the form of micro emulsion
In being scattered in water phase, or water with micelle or (and) be scattered in cold-producing medium phase in the form of micro emulsion, the droplet size of dispersion phase
It is for 100 nanometers and following.But this kind of method has influence on the mass-transfer performance of cold-producing medium to add based on surfactant.
For another example Chinese patent notification number CN1240805C discloses a kind of refrigerant gas hydrate static state side of quickly generating
Method, the inventive method is as follows:Using wire through aqueous solution of anionic surfactant and cold-producing medium two-phase interface and with appearance
Wall face contacts, wire against wall moment movement, make refrigerant gas hydrate wire with wall contact
Locate rapid crystallization nucleation, hereafter refrigerant gas hydrate is quickly generated in the presence of surfactant, whole hydration reaction
Carry out in static water always.
Existing method is employed to mechanical agitation and perturbation action mixes refrigerant, or adds surfactant to be formed
Microemulsion, nano-particle etc. are difficult to be distributed in two-phase system, even if also must be continuous in the case where additive is added
It is continuously applied to extraneous stirring or circulates to promote the presence or absence of two-phase mixtures, this external force and continuity all to make the mixability of two-phase
It is a greater impact, so as to have impact on the heat transfer property of cold-producing medium.In addition, external mechanical shearing force, electromagnetic field and ultrasonic wave
Etc. also greatly increases equipment investment and energy consumption.
The content of the invention
The technical problem to be solved in the present invention is the defect for overcoming prior art, there is provided a kind of process is simple, low cost, green
Colour circle is protected, the preparation method of the nano particle reinforced type cold-producing medium that product heat transfer property is excellent.
In order to solve above-mentioned technical problem, the present invention is achieved by the following technical solutions:It is a kind of nano particle reinforced
The preparation method of type cold-producing medium, comprises the following steps:
A () by weight, the nano oxidized sub- nickel of 5-15 parts is distributed in 1000 parts of ethanol, add 1-10 part propylene
Sour hexafluoro butyl ester, 0.1-1 part benzoyl peroxides, 0.1-5 part polyvinyl alcohol, 0.1-1 part neopelexes, in 60-
80 DEG C of reaction 6-15 hours, obtain the nano oxidized sub- nickel fine suspension of Jing surface aggregates;
The nano oxidized sub- nickel fine suspension and 2,3,3,3- tetrafluoropropenes of b Jing surface aggregates that () obtains step (a),
1,1,1,3- tetrafluoropropenes, 1- ethyl-3-methylimidazole diethyl phosphate salt are with mass ratio as 1:8000-50000:10-
50000:The blending of 0.1-0.5 liquid phases obtains nano particle reinforced type refrigerant product.
Further:
Nano oxidized sub- nickel shot footpath described in step (1) is preferably 10-100nm.
Blending described in step (2) refers to that elder generation is pre-mixed 10-35h at temperature -45~-60 DEG C with liquid condition, then
In being added to high flux microchannel glass reactor, nano particle reinforced type cold-producing medium is mixed to get with 10-100Kg/h flow velocitys and is produced
Product.
The preparation method of the nano particle reinforced type cold-producing medium of the present invention, nano oxidized sub- nickel is passed through and acrylic acid hexafluoro
The process of butyl ester surface aggregate, from hydrophily lipophile is changed into, then with 2,3,3,3- tetrafluoropropenes (HFO-1234yf), and 1,3,3,
3- tetrafluoropropenes (HFO-1234ze), 1- ethyl-3-methylimidazole diethyl phosphate salt is premixed with certain proportioning, is then added to height
In the glass reactor of flux microchannel, product is mixed to get through sufficiently.
The commercially available acquirement of raw material employed in the present invention, such as nano oxidized sub- nickel can select Changsha Asia light chemical metallization
The nano oxidized sub- nickel product of Co., Ltd's production;Hexafluorobutyl acrylate (C7H6F6O2) can select the full woods chemical industry reality of Nanjing health
The hexafluorobutyl acrylate product of industry Co., Ltd production;2,3,3,3- tetrafluoropropene (HFO-1234yf, CH2=CFCF3) optional
The product produced with Juhua Group Co.;1,1,1,3- tetrafluoropropene (HFO-1234ze, CF3CH=CHF) can select hugeization collection
The product of company of group production;(molecular formula is 1- ethyl-3-methylimidazole diethyl phosphate salt:{[Emim]+[(EtO)2(PO)
O]-) can select the product that Shanghai Di Bai chemicals Technology Co., Ltd. produces.
Micro passage reaction is the chemical reaction system of the miniaturization that a kind of unit process interface yardstick is micron dimension.By
The features such as it has small size, bigger serface and regular microchannel, it shows extraordinary at aspects such as mass transfer, heat transfers
Ability, hence it is evident that better than traditional reactor, microcosmic mixing is mixing on molecular scale, it to burning, polymerization, organic synthesis,
The fast reaction processes such as precipitation, crystallization have important impact.Its reason is that fast reaction system needs the short time of staying
With the local mixing of high intensity with avoid on molecular scale from collection.High flux microchannel glass reactor in the present invention can be adopted
GEN-1, GEN-2, GEN-3 type glass reactor produced with Corning Incorporated.
Compared with prior art, the invention has the advantages that:
1st, process is simple, low cost, after the present invention is using refrigerant mixture is premixed by proportioning, are then added to high flux
In the glass reactor of microchannel, product is mixed to get through sufficiently, high flux microchannel glass reactor has small size, big
The features such as specific surface area and regular microchannel, the local mixing with the short time of staying and high intensity is avoiding molecular scale
On from collection, can make various ingredients obtain high intensity mixing, enhance the heat transfer property of product;
2nd, product heat transfer property is excellent, and homodisperse nano oxidized sub- nickel is contained in the cold-producing medium of preparation, nano oxidized
Sub- nickel is passed through and the process of hexafluorobutyl acrylate surface aggregate, and from hydrophily lipophile is changed into, and the thermal conductivity factor of liquid is carried significantly
Height, interaction in nano oxidized sub- nickel particle and particle, particle and cold-producing medium between other components and particle and wall and
Collision, also makes refrigerant product heat transfer property be further enhanced;Simultaneously because introducing 1- ethyl -3- methyl miaows in polymerization
Azoles diethyl phosphate salt, increased the refrigerating efficiency of refrigerant product, and products obtained therefrom is compared with HFO-1234yf either simplex matter thermal conductivity factors
Increasing degree is more than 0.8%;
3rd, environmental protection, the present invention prepare nano particle reinforced type cold-producing medium global warming potential (GWP) 5.5 with
Under, ozone depletion potential (ODP) is 0.
Specific embodiment
The present invention is further detailed below in conjunction with specific embodiment, but the invention is not limited in described reality
Apply example.
Embodiment 1
Step (1):Nano oxidized sub- nickel surface polymerization
Based on every part of 1g, polymerization proportioning is as follows:
Nano oxidized sub- nickel is distributed in ethanol by proportioning, adds hexafluorobutyl acrylate monomer, benzoyl peroxide first
Acyl, polyvinyl alcohol, neopelex, react 9 hours at 70 DEG C, that is, the nano oxidized sub- nickel for obtaining Jing surface aggregates is micro-
Suspension.
Step (2):Blending
The nano oxidized sub- nickel fine suspension of the Jing surface aggregates that 0.005Kg steps (1) are prepared and 98.5Kg2,
3,3,3- tetrafluoropropenes (HFO-1234yf), the tetrafluoropropenes (HFO-1234ze) of 1.4942Kg 1,3,3,3-, 0.0008Kg 1-
Ethyl-3-methylimidazole diethyl phosphate salt in 500L stirring-type reaction kettles, with liquid condition premixing at -55 DEG C of temperature
20h is micro- logical in high flux in being then added to high flux microchannel glass reactor (Corning Incorporated produces, GEN-1 types)
Product is obtained through being sufficiently mixed with 10Kg/h flow velocitys in road glass reactor, numbering is WN-1.
Embodiment 2
Step (1):Nano oxidized sub- nickel surface polymerization
Based on every part of 1g, polymerization proportioning is as follows:
Nano oxidized sub- nickel is distributed in ethanol by proportioning, adds hexafluorobutyl acrylate monomer, benzoyl peroxide first
Acyl, polyvinyl alcohol, neopelex, react 15 hours at 60 DEG C, that is, obtain the nano oxidized sub- nickel of Jing surface aggregates
Fine suspension.
Step (2):Blending
The nano oxidized sub- nickel fine suspension of the Jing surface aggregates that 0.01Kg steps (1) are prepared and 500Kg HFO-
1234yf, 499.985Kg HFO-1234ze, 0.005Kg 1- ethyl-3-methylimidazole diethyl phosphate salt is in 2m3Stirring-type
In reactor, 10h is pre-mixed with liquid condition at -45 DEG C of temperature, is then added to high flux microchannel glass reactor (beautiful
Corning Incorporated of state produces, GEN-2 types) in, with the flow velocity of 40Kg/h through fully mixed in the glass reactor of high flux microchannel
Conjunction obtains product, and numbering is WN-2..
Embodiment 3
Step (1):Nano oxidized sub- nickel surface polymerization
Based on every part of 1g, polymerization proportioning is as follows:
Nano oxidized sub- nickel is distributed in ethanol by proportioning, adds hexafluorobutyl acrylate monomer, benzoyl peroxide first
Acyl, polyvinyl alcohol, neopelex, react 6 hours at 80 DEG C, that is, the nano oxidized sub- nickel for obtaining Jing surface aggregates is micro-
Suspension.
Step (2):Blending
The nano oxidized sub- nickel fine suspension of the Jing surface aggregates that 0.1Kg steps (1) are prepared and 800Kg HFO-
1234yf, 199.89Kg HFO-1234ze, 0.01Kg 1- ethyl-3-methylimidazole diethyl phosphate salt is in 2m3Stirring-type is anti-
In answering kettle, 20h is pre-mixed with liquid condition at -60 DEG C of temperature, is then added to the high flux microchannel glass reactor (U.S.
Corning Incorporated produces, GEN-3 types) in, with flow velocity 100Kg/h through being sufficiently mixed in the glass reactor of high flux microchannel
To product, numbering is WN-3.
Embodiment 4
Preparation method is with embodiment 1, difference:Add in 0.5 part of polyvinyl alcohol, step (2) in step (1) and add
The HFO-1234ze of the HFO-1234yf of 87Kg, 12.9492Kg, the premixing time is 30h, and flow velocity is 20Kg/h, products obtained therefrom
Numbering is WN-4.
Embodiment 5
Preparation method is with embodiment 1, difference:Add in 1 part of polyvinyl alcohol, step (2) in step (1) and add
97Kg HFO1234yf, 2.9492Kg HFO1234ze, the premixing time is 25h, and flow velocity is 30Kg/h, and products obtained therefrom numbering is
WN-5。
Embodiment 6
Preparation method is with embodiment 1, difference:Add in 2 parts of polyvinyl alcohol, step (2) in step (1) and add
99.8Kg HFO1234yf, 0.1492Kg HFO1234ze, the premixing time is 15h, and flow velocity is 50Kg/h, and products obtained therefrom is numbered
For WN-6.
Embodiment 7
Preparation method is with embodiment 1, difference:Add in 3 parts of polyvinyl alcohol, step (2) in step (1) and add
99.9Kg HFO1234yf, 0.0942Kg HFO1234ze, the premixing time is 35h, and flow velocity is 60Kg/h, and products obtained therefrom is numbered
For WN-7.
Embodiment 8
Preparation method is with embodiment 1, difference:Add in 4 parts of polyvinyl alcohol, step (2) in step (1) and add
99.94Kg HFO1234yf, 0.0542Kg HFO1234ze, flow velocity is 80Kg/h, and products obtained therefrom numbering is WN-8.
Comparative example 1
By 98.5Kg2,3,3,3- tetrafluoropropenes (HFO-1234yf), the tetrafluoropropene (HFO- of 1.4942Kg 1,3,3,3-
1234ze), 0.0008Kg 1- ethyl-3-methylimidazoles diethyl phosphate salt is pre-mixed in 500L stirring-type reaction kettles,
The premixing time is 20h, in being then added to high flux microchannel glass reactor (Corning Incorporated produces, GEN-1 types),
Product is obtained through being sufficiently mixed with 10Kg/h flow velocitys in the glass reactor of high flux microchannel, products obtained therefrom numbering is WN-
9。
Comparative example 2
Preparation method is with embodiment 1, difference:1- ethyl-3-methylimidazole p diethylaminobenzoic acids are added without in step (2)
Ester salt, products obtained therefrom numbering is WN-10.
Properties of product are tested:
Embodiment 1-8 and comparative example 1-2 products obtained therefrom are shown in Table 1 compared with HFO1234yf either simplex matter thermal conductivity factor increasing degrees, its
In:
Thermal conductivity factor increasing degree=(nano refrigerant thermal conductivity factor-HFO1234yf thermal conductivity factors)/HFO1234yf leads
Hot coefficient × 100%.
Thermal conductivity factor computing formula adopts Zhang Zhi's towering " macroscopic property of low GWP mixed working fluids and cycle performance are studied ",
University Of Tianjin's Master's thesis, 2012, the detection of P38 methods.
Relational expression:
The unit of thermal conductivity factor is W/ (mK) in formula, and Tb is normal boiling point, and Tc is critical-temperature, and unit is all K, and M is
Molal weight, unit is g/mol, Tr=T/Tc, A*=0.494, α=0.0, β=0.5, γ=- 0.167.
Table 1:Embodiment 1-8 and comparative example 1-2 products obtained therefrom Performance comparision
Claims (2)
1. a kind of preparation method of nano particle reinforced type cold-producing medium, it is characterised in that comprise the following steps:
A () by weight, the nano oxidized sub- nickel of 5-15 parts is distributed in 1000 parts of ethanol, add 1-10 parts acrylic acid six
Fluorine butyl ester, 0.1-1 part benzoyl peroxides, 0.1-5 part polyvinyl alcohol, 0.1-1 part neopelexes, at 60-80 DEG C
Reaction 6-15 hours, obtain the nano oxidized sub- nickel fine suspension of Jing surface aggregates;
The nano oxidized sub- nickel fine suspension of b Jing surface aggregates that () obtains step (a) and 2,3,3,3- tetrafluoropropenes, 1,3,
3,3- tetrafluoropropenes, 1- ethyl-3-methylimidazole diethyl phosphate salt are with mass ratio as 1:8000-50000:10-50000:
0.1-0.5 liquid phases are pre-mixed 10-35h at temperature -45~-60 DEG C with liquid condition, are then added to high flux microchannel glass
In glass reactor, nano particle reinforced type refrigerant product is obtained with the blending of 10-100Kg/h flow velocitys.
2. the preparation method of nano particle reinforced type cold-producing medium according to claim 1, it is characterised in that step (1) is described
Nano oxidized sub- nickel shot footpath be 10-100nm.
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