CN104403638A - Preparation method for nanoparticle enhanced refrigerant - Google Patents
Preparation method for nanoparticle enhanced refrigerant Download PDFInfo
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- CN104403638A CN104403638A CN201410648019.7A CN201410648019A CN104403638A CN 104403638 A CN104403638 A CN 104403638A CN 201410648019 A CN201410648019 A CN 201410648019A CN 104403638 A CN104403638 A CN 104403638A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K5/08—Materials not undergoing a change of physical state when used
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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 refrigeration agent, particularly a kind of preparation method of nano particle reinforced type refrigeration agent.
Background technology
In refrigeration, air-conditioning or a heat transfer system, expect that lubricating oil and refrigeration agent can be contacting one another at least some part of this system, as at ASHRAE handbook: illustrated in HVAC system and equipment.Therefore, no matter this lubricant and refrigeration agent by separately or join in refrigeration, air-conditioning or a heat transfer system as the part in a pre-mix pack, still expect that they contact within the system and therefore must be compatible.Because crystal grain is superfine, be in the atom of defect center in crystal boundary and crystal grain and the quantum size effect itself had, small-size effect, surface effects and macro quanta tunnel effect etc. and make nano material in lubrication and friction, have special falling to rub antifriction and high compound ability.Nano-substance exists with the form of nano particle or nanometer film at friction surface; there is good lubricity and antifriction performance; the lubricant that interpolation nano material is made can improve lubricity and load-carrying properties significantly; improve the quality of product, be particularly suitable for the lubrication occasion of severe condition.Since the nineties in 20th century, researchist starts exploration and nano material technology is applied to enhancement of heat transfer field, studies efficient heat transfer cooling technology of new generation.Nineteen ninety-five, the people such as the Choi of Argonne National Laboratory of the U.S. propose a brand-new concept-nano-fluid first.Nano-fluid refers to that a metal or non pinetallic nano powder are distributed in water, alcohol, wet goods tradition heat transferring medium, be prepared into novel heat exchange medium that is even, stable, high heat conduction, this is the research that nanotechnology is applied to the novelty of this traditional field of Thermal Power Engineering.Nano-fluid has huge potential application foreground in fields such as the energy, chemical industry, automobile, building, microelectronics, information, thus becomes the study hotspot in many fields such as material, physics, chemistry, thermal conduction study.
As (the Yong member of Imperial Academy, Bi Shengshan, Shi Lin .HFC134a/TiO such as the Yong members of Imperial Academy
2nanoparticle working medium system is applied to the experimental study [J] of refrigerator. Journal of Chemical Industry and Engineering, 2006 (5): 141-145.) nano particle added to HFC134a/ mineral refrigeration oil/nano-TiO in refrigeration oil
2working medium system is applied in home freezer, finds that its performance perameter is slightly better than HFC134a/ Esters oil system.
And for example China Patent Publication No. CN102295917A discloses a kind of preparation method of nano particle reinforced type refrigerant hydrate phase change cold-storage working substance, utilize the solublization of compound surfactant, refrigeration agent is soluble in water, obtained thermodynamically stable refrigeration agent microemulsion, then by nanoparticle dispersion in refrigeration agent microemulsion, obtained nano particle reinforced refrigerant hydrate phase change cold-storage working substance.By nanoparticle stable dispersion is carried out heat and mass transfer enhancement in refrigeration agent microemulsion system, augmenting response interface, induction nonhomogen-ous nucleation, thus the induction time and the condensate depression that significantly reduce hydrate generation, reach short brilliant effect effectively.This technique uses ultrasonic wave dispersion, and scale operation should not realize.
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, tensio-active agent is soluble in water, the aqueous solution of obtained tensio-active agent, then refrigeration agent is added drop-wise in the aqueous solution of tensio-active agent, stirs until solution is become from muddiness bright.According to the solubleness in water and in refrigeration agent of tensio-active agent, can be soluble in water by tensio-active agent, also can be dissolved in refrigeration agent.This system does not need to apply stirring, disturbance and outfield can make aqueous phase and refrigeration agent fully mix mutually, refrigeration agent with micelle or (with) form of micro emulsion is scattered in aqueous phase, or aqueous phase with micelle or (with) form of micro emulsion be scattered in refrigeration agent mutually in, the droplet size of disperse phase is 100 nanometers and following.But this kind of method, to add tensio-active agent, has influence on the mass-transfer performance of refrigeration agent.
For another example Chinese patent notification number CN1240805C discloses a kind of static fast generation process for refrigerant gas hydrate, this inventive method is as follows: adopt wire through aqueous solution of anionic surfactant and refrigeration agent two-phase interface and contact with container wall, the moment that wire againsts wall moves, make refrigerant gas hydrate at the contact position rapid crystallization nucleation of wire with wall, after this refrigerant gas hydrate generates fast under the effect of tensio-active agent, and whole hydration reaction is carried out always in static water.
Existing method all will utilize mechanical stirring and perturbation action that cooling agent is mixed, or add tensio-active agent and form microemulsion, nanoparticles etc. are difficult to all be distributed in two-phase system, even if extraneous stirring also successively must be applied when adding additive or circulates impel two-phase mixtures, the presence or absence of this external force and continuity all make the degree of mixing of two-phase be a greater impact, thus have impact on the heat transfer property of refrigeration agent.In addition, external mechanical shearing force, electromagnetic field and ultrasonic wave etc. also greatly increases facility investment and energy consumption.
Summary of the invention
The technical problem to be solved in the present invention is the defect overcoming prior art, provides that a kind of technique is simple, cost is low, the preparation method of nano particle reinforced type refrigeration agent that environmental protection, product heat transfer property are excellent.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions: a kind of preparation method of nano particle reinforced type refrigeration agent, comprises the following steps:
A () by weight, nano oxidized for 5-15 part sub-nickel is distributed in 1000 parts of ethanol, add 1-10 part vinylformic acid hexafluoro butyl ester, 0.1-1 part benzoyl peroxide, 0.1-5 part polyvinyl alcohol, 0.1-1 part Sodium dodecylbenzene sulfonate again, at 60-80 DEG C of reaction 6-15 hour, obtain the nano oxidized sub-nickel fine suspension through surface aggregate;
The b nano oxidized sub-nickel fine suspension and 2 through surface aggregate that step (a) obtains by (), 3,3,3-tetrafluoeopropene, 1,1, to be that 1:8000-50000:10-50000:0.1-0.5 liquid phase is blended with mass ratio obtain nano particle reinforced type refrigerant product for 1,3-tetrafluoeopropene, 1-ethyl-3-methylimidazole diethyl phosphoric acid salt.
Further:
Nano oxidized sub-nickel shot footpath described in step (1) is preferably 10-100nm.
Blended described in step (2) refer to first at temperature-45 ~-60 DEG C with liquid state pre-mixing 10-35h, then join in the glass reactor of high-throughput microchannel, be mixed to get nano particle reinforced type refrigerant product with 10-100Kg/h flow velocity.
The preparation method of nano particle reinforced type refrigeration agent of the present invention, passes through nano oxidized sub-nickel and the process of vinylformic acid hexafluoro butyl ester surface aggregate, becomes lipophilicity from wetting ability, then with 2,3,3,3-tetrafluoeopropene (HFO-1234yf), 1,1,1,3-tetrafluoeopropene (HFO-1234ze), 1-ethyl-3-methylimidazole diethyl phosphoric acid salt with certain proportioning premix, then joins in the glass reactor of high-throughput microchannel, through being mixed to get product fully.
The raw material adopted in the present invention all can commercially availablely obtain, as the nano oxidized sub-nickel product that nano oxidized sub-nickel can select Changsha Ya Guang chemical metallization company limited to produce; Vinylformic acid hexafluoro butyl ester (C
7h
6f
6o
2) can select
nanjing Kang Manlin chemical industry Industrial Co., Ltd.the vinylformic acid hexafluoro butyl ester product produced; 2,3,3,3-tetrafluoeopropene (HFO-1234yf, CH
2=CFCF
3) product that Juhua Group Co. can be selected to produce; 1,1,1,3-tetrafluoeopropene (HFO-1234ze, CF
3cH=CHF) product Juhua Group Co. can being selected to produce; (molecular formula is 1-ethyl-3-methylimidazole diethyl phosphoric acid salt: { [Emim]
+[(EtO)
2(PO) O]
-) can select
shanghai Di Bai chemical Technology Co., Ltd.the product produced.
The chemical reaction system of micro passage reaction to be a kind of unit process interface yardstick the be microminiaturization of micron dimension.Because it has the features such as the regular microchannel of small size, large specific surface sum, it shows extraordinary ability in mass transfer, heat transfer etc., obviously be better than traditional reactor, microcosmic mixing is the mixing on molecular scale, and it has important impact to rapid reaction processes such as burning, polymerization, organic synthesis, precipitation, crystallizations.Its reason be Quickly react system need the local mixing of the short residence time and high strength with avoid on molecular scale from collection.GEN-1, GEN-2, GEN-3 type glass reactor that high-throughput microchannel glass reactor in the present invention can adopt Corning Incorporated to produce.
Compared with prior art, the present invention has following beneficial effect:
1, technique is simple, cost is low, the present invention adopts refrigerant mixture by after proportioning premix, join in the glass reactor of high-throughput microchannel again, through being mixed to get product fully, high-throughput microchannel glass reactor has the features such as the regular microchannel of small size, large specific surface sum, the local mixing with the short residence time and high strength with avoid on molecular scale from collection, various ingredients can be made to obtain high strength mixing, enhance the heat transfer property of product;
2, product heat transfer property is excellent, containing homodisperse nano oxidized sub-nickel in the refrigeration agent of preparation, nano oxidized sub-nickel passes through and the process of vinylformic acid hexafluoro butyl ester surface aggregate, lipophilicity is become from wetting ability, the thermal conductivity of liquid improves greatly, in nano oxidized sub-nickel particle and particle, particle and refrigeration agent, other components and the interaction between particle and wall and collision, also make refrigerant product heat transfer property be further enhanced; Simultaneously owing to introducing 1-ethyl-3-methylimidazole diethyl phosphoric acid salt in polymerization, add the refrigerating efficiency of refrigerant product, products obtained therefrom comparatively HFO-1234yf mono-working medium thermal conductivity increasing degree more than 0.8%;
3, environmental protection, nano particle reinforced type refrigeration agent global warming potential (GWP) prepared by the present invention is below 5.5, and ozone depletion potential (ODP) is 0.
Embodiment
Below in conjunction with specific embodiment, the present invention is further detailed, but the present invention is not limited to described embodiment.
Embodiment 1
Step (1): nano oxidized sub-nickel surface polymerization
By every part of 1g, polymerization proportioning is as follows:
By proportioning, nano oxidized sub-nickel is distributed in ethanol, then adds vinylformic acid hexafluoro butyl ester monomer, benzoyl peroxide, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, 70 DEG C of reactions 9 hours, namely obtain the nano oxidized sub-nickel fine suspension through surface aggregate.
Step (2): blended
The nano oxidized sub-nickel fine suspension through surface aggregate that 0.005Kg step (1) is prepared and 98.5Kg2, 3, 3, 3-tetrafluoeopropene (HFO-1234yf), 1.4942Kg 1, 1, 1, 3-tetrafluoeopropene (HFO-1234ze), 0.0008Kg 1-ethyl-3-methylimidazole diethyl phosphoric acid salt is in 500L stirring-type reactor, with liquid state pre-mixing 20h at temperature-55 DEG C, then (Corning Incorporated produces to join high-throughput microchannel glass reactor, GEN-1 type) in, in the glass reactor of high-throughput microchannel with 10Kg/h flow velocity through being fully mixed to get product, be numbered WN-1.
Embodiment 2
Step (1): nano oxidized sub-nickel surface polymerization
By every part of 1g, polymerization proportioning is as follows:
By proportioning, nano oxidized sub-nickel is distributed in ethanol, then adds vinylformic acid hexafluoro butyl ester monomer, benzoyl peroxide, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, 60 DEG C of reactions 15 hours, namely obtain the nano oxidized sub-nickel fine suspension through surface aggregate.
Step (2): blended
The nano oxidized sub-nickel fine suspension through surface aggregate 0.01Kg step (1) prepared and 500Kg HFO-1234yf, 499.985Kg HFO-1234ze, 0.005Kg 1-ethyl-3-methylimidazole diethyl phosphoric acid salt are at 2m
3in stirring-type reactor, with liquid state pre-mixing 10h at temperature-45 DEG C, then (Corning Incorporated produces to join high-throughput microchannel glass reactor, GEN-2 type) in, in the glass reactor of high-throughput microchannel with the flow velocity of 40Kg/h through being fully mixed to get product, be numbered WN-2..
Embodiment 3
Step (1): nano oxidized sub-nickel surface polymerization
By every part of 1g, polymerization proportioning is as follows:
By proportioning, nano oxidized sub-nickel is distributed in ethanol, then adds vinylformic acid hexafluoro butyl ester monomer, benzoyl peroxide, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, 80 DEG C of reactions 6 hours, namely obtain the nano oxidized sub-nickel fine suspension through surface aggregate.
Step (2): blended
The nano oxidized sub-nickel fine suspension through surface aggregate 0.1Kg step (1) prepared and 800Kg HFO-1234yf, 199.89Kg HFO-1234ze, 0.01Kg 1-ethyl-3-methylimidazole diethyl phosphoric acid salt are at 2m
3in stirring-type reactor, with liquid state pre-mixing 20h at temperature-60 DEG C, then (Corning Incorporated produces to join high-throughput microchannel glass reactor, GEN-3 type) in, in the glass reactor of high-throughput microchannel with flow velocity 100Kg/h through being fully mixed to get product, be numbered WN-3.
Embodiment 4
Preparation method is with embodiment 1, and difference is: add 0.5 part of polyvinyl alcohol in step (1), adds the HFO-1234yf of 87Kg in step (2), 12.9492Kg HFO-1234ze, the pre-mixing time is 30h, and flow velocity is 20Kg/h, and products obtained therefrom is numbered WN-4.
Embodiment 5
Preparation method is with embodiment 1, and difference is: add 1 part of polyvinyl alcohol in step (1), and step adds 97Kg HFO1234yf in (2), 2.9492Kg HFO1234ze, the pre-mixing time is 25h, and flow velocity is 30Kg/h, and products obtained therefrom is numbered WN-5.
Embodiment 6
Preparation method is with embodiment 1, and difference is: add 2 parts of polyvinyl alcohol in step (1), and step adds 99.8Kg HFO1234yf in (2), 0.1492Kg HFO1234ze, the pre-mixing time is 15h, and flow velocity is 50Kg/h, and products obtained therefrom is numbered WN-6.
Embodiment 7
Preparation method is with embodiment 1, and difference is: add 3 parts of polyvinyl alcohol in step (1), and step adds 99.9Kg HFO1234yf in (2), 0.0942Kg HFO1234ze, the pre-mixing time is 35h, and flow velocity is 60Kg/h, and products obtained therefrom is numbered WN-7.
Embodiment 8
Preparation method is with embodiment 1, and difference is: add 4 parts of polyvinyl alcohol in step (1), and step adds 99.94Kg HFO1234yf in (2), 0.0542Kg HFO1234ze, and flow velocity is 80Kg/h, and products obtained therefrom is numbered WN-8.
Comparative example 1
By 98.5Kg2,3,3,3-tetrafluoeopropene (HFO-1234yf), 1.4942Kg 1,1,1,3-tetrafluoeopropene (HFO-1234z e), 0.0008Kg 1-ethyl-3-methylimidazole diethyl phosphoric acid salt carries out pre-mixing in 500L stirring-type reactor, and the pre-mixing time is 20h, then (Corning Incorporated produces to join high-throughput microchannel glass reactor, GEN-1 type) in, in the glass reactor of high-throughput microchannel with 10Kg/h flow velocity through being fully mixed to get product, products obtained therefrom is numbered WN-9.
Comparative example 2
Preparation method is with embodiment 1, and difference is: do not add 1-ethyl-3-methylimidazole diethyl phosphoric acid salt in step (2), products obtained therefrom is numbered WN-10.
Product performance are tested:
Embodiment 1-8 and comparative example 1-2 products obtained therefrom comparatively HFO1234yf mono-working medium thermal conductivity increasing degree in table 1, wherein:
Thermal conductivity increasing degree=(nano refrigerant thermal conductivity-HFO1234yf thermal conductivity)/HFO1234yf thermal conductivity × 100%.
Thermal conductivity calculation formula adopts
zhang Zhi is towering" thermodynamic property of low GWP mixing medium and cycle performance research ",
university Of Tianjin's Master's thesis, 2012, P38 method detects.
Relational expression:
In formula, the unit of thermal conductivity is W/ (mK), Tb is normal boiling point, and Tc is critical temperature, and unit is all K, M is molar mass, and 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 (3)
1. a preparation method for nano particle reinforced type refrigeration agent, is characterized in that comprising the following steps:
A () by weight, nano oxidized for 5-15 part sub-nickel is distributed in 1000 parts of ethanol, add 1-10 part vinylformic acid hexafluoro butyl ester, 0.1-1 part benzoyl peroxide, 0.1-5 part polyvinyl alcohol, 0.1-1 part Sodium dodecylbenzene sulfonate again, at 60-80 DEG C of reaction 6-15 hour, obtain the nano oxidized sub-nickel fine suspension through surface aggregate;
The b nano oxidized sub-nickel fine suspension and 2 through surface aggregate that step (a) obtains by (), 3,3,3-tetrafluoeopropene, 1,1, to be that 1:8000-50000:10-50000:0.1-0.5 liquid phase is blended with mass ratio obtain nano particle reinforced type refrigerant product for 1,3-tetrafluoeopropene, 1-ethyl-3-methylimidazole diethyl phosphoric acid salt.
2. the preparation method of nano particle reinforced type refrigeration agent according to claim 1, is characterized in that the nano oxidized sub-nickel shot footpath described in step (1) is 10-100nm.
3. the preparation method of nano particle reinforced type refrigeration agent according to claim 1, to it is characterized in that described in step (2) blended refer to first at temperature-45 ~-60 DEG C with liquid state pre-mixing 10-35h, then join in the glass reactor of high-throughput microchannel, be mixed to get nano particle reinforced type refrigerant product with 10-100Kg/h flow velocity.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US11746273B2 (en) | 2019-09-20 | 2023-09-05 | Ht Materials Science (Ip) Limited | Heat transfer mixture |
| US11753570B2 (en) | 2019-09-20 | 2023-09-12 | Ht Materials Science (Ip) Limited | Heat transfer mixture |
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| US11746273B2 (en) | 2019-09-20 | 2023-09-05 | Ht Materials Science (Ip) Limited | Heat transfer mixture |
| US11753570B2 (en) | 2019-09-20 | 2023-09-12 | Ht Materials Science (Ip) Limited | Heat transfer mixture |
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