CN104592943A - Fluorine-containing iodo-hydrocarbon composition and preparation method thereof - Google Patents
Fluorine-containing iodo-hydrocarbon composition and preparation method thereof Download PDFInfo
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- CN104592943A CN104592943A CN201410820694.3A CN201410820694A CN104592943A CN 104592943 A CN104592943 A CN 104592943A CN 201410820694 A CN201410820694 A CN 201410820694A CN 104592943 A CN104592943 A CN 104592943A
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- C09K5/04—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa
- C09K5/041—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa for compression-type refrigeration systems
- C09K5/044—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa for compression-type refrigeration systems comprising halogenated compounds
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Abstract
The invention discloses a fluorine-containing iodo-hydrocarbon composition. The composition comprises the following components in parts by weight: 0.5-10 parts of a nano compatibilizer, 80-900 parts of 2,3,3,3-tetrafluoropropene, 10-300 parts of iodotrifluoromethane and 0.0008-0.01 part of 1-allyl-3-buthylimidazole nitrate ionic liquid. The invention also discloses a preparation method of the fluorine-containing iodo-hydrocarbon composition. The fluorine-containing iodo-hydrocarbon composition has the advantages of simple process, low cost, environment friendliness and good product properties.
Description
Technical field
The present invention relates to refrigerant art, be specifically related to a kind of fluorine-containing idohydrocarbon composition and method of making the same.
Background technology
In lubrication, add the lubricant that nano material makes can improve lubricity and load-carrying properties significantly, improve the quality of product, be particularly suitable for the lubrication occasion of severe condition, nano particle additive is utilized to improve thermodynamic property, heat transfer characteristic, the flow characteristics of refrigeration agent and refrigeration oil, thus reach parameters optimization, enhancement of heat transfer, improve oil soluble, improve compressor wear resistance, reduce the effects such as noise, will be improve one of the efficiency of refrigeration air conditioner heat pump equipment and the important innovations means of reliability.
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. CN101434833 A 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 be uniformly 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 refrigerant product.In addition, external mechanical shearing force, electromagnetic field and ultrasonic wave etc. also greatly increases facility investment and energy consumption and complex operation.
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, fluorine-containing idohydrocarbon composition and method of making the same 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 fluorine-containing idohydrocarbon composition, and by weight, it consists of:
By weight, described nanometer expanding material composition is preferably:
Described lubricant is preferably polyalkylene glycol or polyol ester class.
Described
antimony doped stannic oxide nano powderparticle diameter be preferably 1 ~ 10nm.
The present invention also provides the preparation method of described fluorine-containing idohydrocarbon composition, comprises the following steps:
(a) by weight, by 1-5 part
antimony doped stannic oxide nano powderbe distributed in 1000 parts of ethanol, then add chelate coordinate organic boron coupling agent 0.01-0.05 part, react 1-5h under normal temperature, then add 10-100 part lubricant, under normal temperature, react 2-10h, obtain nanometer expanding material, for subsequent use;
B () by weight, the nanometer expanding material that step (a) is prepared 0.5 ~ 10 part, 2,3,3,3-tetrafluoeopropene 80 ~ 900 parts, CF3I, 10 ~ 300 parts, 1-allyl group-3-butyl imidazole nitrate ion liquid 0.0008 ~ 0.01 part of mixture obtains fluorine-containing idohydrocarbon composition product.
Each component is preferably pressed proportioning first pre-mixing 10-30h under liquid phase by the mixture described in step (b), then joins in the glass reactor of high-throughput microchannel, is mixed to get fluorine-containing idohydrocarbon composition product with flow velocity 10-100Kg/h.
The present invention by nanometer expanding material and 2,3,3,3-tetrafluoeopropene (HFO1234yf), CF3I (CF
3i), 1-allyl group-3-butyl imidazole nitrate ion liquid with certain proportioning premix, then joins in the glass reactor of high-throughput microchannel, through being mixed to get product fully.HFO1234yf, CF
3i and 1-allyl group-3-butyl imidazole nitrate ion liquid has good solubleness and diffusivity.Add nanometer expanding material in composition, the nanosphere body of trace improves sliding, improves the consistency of each component in lubricating oil, makes lubricating oil more abundant with contacting of other component.
sb doped titanium dioxide tin (ATO) nano-powderthere is chemical resistant properties, acid and alkali-resistance, fast light, organic solvent-resistant, be not oxidized, the effect such as fire-retardant, high temperature resistant, corrosion-resistant, mechanical stability, effectively can reduce the flammable performance of HFO1234yf.
Described lubricant comprises naphthenic mineral oil, paraffinic mineral oil, ester oil, polyalkylene glycol, polyvinyl ether, alkylbenzene, polyester, one or more combinations polyolefinic.Preferred polyalkylene glycol (PAG) and polyol ester class (POE).
Raw material described in the present invention all can commercially availablely obtain, as
stibium doping stannic oxide (ATO) nano-powderhe'nan Wangwu Nano Technology Co., Ltd.'s product can be selected.Chelate coordinate organic boron coupling agent can select the SBW-III organic boron coupling agent product of Qingdao Siwei Chemical Co., Ltd..1-allyl group-3-butyl imidazole nitrate ion liquid [ABIm] [NO
3] [the ABIm] [NO that Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences can be selected to produce
3] ionic liquid product.2,3,3,3-tetrafluoeopropene (HFO1234yf, molecular formula: C
3h
2f
4) product that Juhua Group Co. can be selected to develop.The product that CF3I can select Juhua Group Co. to develop.
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.High-throughput microchannel glass reactor described in the present invention is commercially available prod, as the GEN-1 that Corning Incorporated can be adopted to produce, and GEN-2, GEN-3 type glass reactor.
Normal temperature of the present invention refers to 25 DEG C.
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, enormously simplify preparation technology;
2, product has good lubrication agent consistency and heat transfer property, adds nanometer expanding material and improve the consistency of composition in lubricating oil in component.Microballoon can be helped fully wetting in 2,3,3,3-tetrafluoeopropene.By increase refrigeration agent solvability in the lubricant.Cause the reduction of lubricant viscosity, and in compression refrigerating system, make lubricant effectively be back to constricted zone from non-constricted zone.In condenser zone, the minimizing of lubricant quantity also will improve the heat trnasfer of refrigeration agent, and therefore improve refrigeration capacity and the efficiency of system, and separation temperature is below-1 DEG C;
3, product refrigerating efficiency is high, owing to introducing 1-allyl group-3-butyl imidazole nitrate ion liquid in component, adds refrigerating efficiency, improves solubleness and the diffusivity of refrigeration agent.2,6-nonadienol can suppress the degraded trend of CF3I.
4, environmental protection, the refrigerant composition global warming potential (GWP) of preparation of the present invention is below 14, and ozone depletion potential (ODP) is 0.
Embodiment
Raw material described in the present invention all can commercially availablely obtain, wherein part material and description of equipment as follows:
stibium doping stannic oxide (ATO) nano-powder: He'nan Wangwu Nano Technology Co., Ltd.'s product, particle diameter is 1 ~ 10nm.
SBW-III organic boron coupling agent: the SBW-III organic boron coupling agent product of Qingdao Siwei Chemical Co., Ltd..
1-allyl group-3-butyl imidazole nitrate ion liquid [ABIm] [NO
3]: [ABIm] [NO that Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences produces
3] ionic liquid product.
2,3,3,3-tetrafluoeopropene (HFO1234yf, molecular formula: C
3h
2f
4): the product of Juhua Group Co.'s development.
CF3I: the product of Juhua Group Co.'s development.
High-throughput microchannel glass reactor: GEN-1, GEN-2, GEN-3 type glass reactor that Corning Incorporated produces.
Below in conjunction with specific embodiment, the present invention is further detailed, but the present invention is not limited to described embodiment.
Embodiment 1:
The preparation of step (1) nanometer expanding material, by every part of 1Kg, charge ratio is as follows:
Preparation method is:
By proportioning, in stirring-type reactor, by 3 parts
stibium doping stannic oxide (ATO) nano-powderbe distributed in 1000 parts of ethanol, add 0.03 part of SBW-III organic boron coupling agent again, 5h is reacted under normal temperature (25 DEG C), then add 50 parts of polyalkylene glycol (PAG) lubricants, 2 part 2,6-nonadienol, react 2h under normal temperature (25 DEG C), namely obtain nanometer expanding material, for subsequent use.
Preparation method is: by proportioning, the nanometer expanding material that 0.5 part of step (1) is prepared and 80 part 2,3,3,3-tetrafluoeopropene (HFO1234yf), 50 parts of CF3Is, 0.0008 part of 1-allyl group-3-butyl imidazole nitrate ion liquid in stirring-type reactor under liquid phase pre-mixing 10h, then (Corning Incorporated produces to join high-throughput microchannel glass reactor, GEN-1 type glass reactor) in, with flow velocity 10Kg/h flow velocity through being mixed to get product fully.Be numbered WN-1
Embodiment 2
The preparation of step (1) nanometer expanding material, by every part of 1Kg, charge ratio is as follows:
Preparation method is: by proportioning, in stirring-type reactor, by 1 part
stibium doping stannic oxide (ATO) nano powder bodybe distributed to
1000in part ethanol, then add
sBW-III organic boron coupling agent 0.01part, react 4h under normal temperature (25 DEG C), then add
polyol ester class (POE) lubricant 10part, 2,6-nonadienol 1 part, react 4h under normal temperature (25 DEG C), namely obtain nanometer expanding material.
Step (2) mixture, by every part of 1Kg, charge ratio is as follows:
Preparation method is: by proportioning, the nanometer expanding material that 1 part of step (1) is prepared and 700 part 2,3,3,3-tetrafluoeopropene (HFO1234yf), 300 parts of CF3Is, 0.005 part of 1-allyl group-3-butyl imidazole nitrate ion liquid in stirring-type reactor under liquid phase pre-mixing 20h, then (Corning Incorporated produces to join high-throughput microchannel glass reactor, GEN-2 type glass reactor) in, with flow velocity 50Kg/h flow velocity through being mixed to get product fully.Be numbered WN-2.
Embodiment 3
The preparation of step (1) nanometer expanding material, by every part of 1Kg, charge ratio is as follows:
Preparation method is: by proportioning, in stirring-type reactor, by 5 parts
stibium doping stannic oxide (ATO) nano powderbody is distributed in 1000 parts of ethanol, add SBW-III organic boron coupling agent 0.05 part again, 3h is reacted under normal temperature (25 DEG C), then polyalkylene glycol (PAG) lubricant 100 parts, 2 is added, 6-nonadienol 5 parts, react 6h under normal temperature (25 DEG C), namely obtain nanometer expanding material.
Step (2) mixture, by every part of 1Kg, charge ratio is as follows:
Preparation method is: by proportioning, the nanometer expanding material that 10 parts of steps (1) are prepared and 900 part 2,3,3,3-tetrafluoeopropene (HFO1234yf), 100 parts of CF3Is, 0.01 part of 1-allyl group-3-butyl imidazole nitrate ion liquid in stirring-type reactor under liquid phase pre-mixing 30h, then (Corning Incorporated produces to join high-throughput microchannel glass reactor, GEN-3 type glass reactor) in, with flow velocity 100Kg/h flow velocity through being mixed to get product fully.Be numbered WN-3.
Embodiment 4
The preparation of step (1) nanometer expanding material, by every part of 1Kg, charge ratio is as follows:
Preparation method is:
By proportioning, in stirring-type reactor, by 2 parts
stibium doping stannic oxide (ATO) nano-powderbe distributed in 1000 parts of ethanol, add 0.04 part of SBW-III organic boron coupling agent again, 1h is reacted under normal temperature (25 DEG C), then 30 parts of polyalkylene glycol (PAG) lubricants, 2 are added, 6-nonadienol 3 parts, react 8h under normal temperature (25 DEG C), namely obtain nanometer expanding material, for subsequent use.
Step (2) mixture, by every part of 1Kg, charge ratio is as follows:
Preparation method is: by proportioning, the nanometer expanding material that 4.5 parts of steps (1) are prepared and 150 part 2,3,3,3-tetrafluoeopropene (HFO1234yf), 10 parts of CF3Is, 0.003 part of 1-allyl group-3-butyl imidazole nitrate ion liquid in stirring-type reactor under liquid phase pre-mixing 15h, then (Corning Incorporated produces to join high-throughput microchannel glass reactor, GEN-1 type glass reactor) in, with flow velocity 30Kg/h flow velocity through being mixed to get product fully.Be numbered WN-4.
Embodiment 5
The preparation of step (1) nanometer expanding material, by every part of 1Kg, charge ratio is as follows:
Preparation method is:
By proportioning, in stirring-type reactor, by 4 parts
stibium doping stannic oxide (ATO) nano-powderbe distributed in 1000 parts of ethanol, add 0.02 part of SBW-III organic boron coupling agent again, 2h is reacted under normal temperature (25 DEG C), then 70 parts of polyalkylene glycol (PAG) lubricants, 2 are added, 6-nonadienol 4 parts, react 10h under normal temperature (25 DEG C), namely obtain nanometer expanding material, for subsequent use.
Step (2) mixture, by every part of 1Kg, charge ratio is as follows:
Preparation method is: by proportioning, the nanometer expanding material that 7.5 parts of steps (1) are prepared and 400 part 2,3,3,3-tetrafluoeopropene (HFO1234yf), 200 parts of CF3Is, 0.007 part of 1-allyl group-3-butyl imidazole nitrate ion liquid in stirring-type reactor under liquid phase pre-mixing 25h, then (Corning Incorporated produces to join high-throughput microchannel glass reactor, GEN-2 type glass reactor) in, with flow velocity 80Kg/h flow velocity through being mixed to get product fully.Be numbered WN-5.
Performance test:
Embodiment 1-5 products obtained therefrom is according to ANSI/ASHRAE 86-1994 standard " the flock point testing method of refrigeration-grade oil " (Methods of Testing the Floe.Point of Refrigeration Grade Oils), determine the compatibility of PAG lubricant base fluid and embodiment 1-5 products obtained therefrom, wherein the weight percent concentration of lubricant is 20 % by weight.Lubricant and refrigeration agent are joined in heavy-walled glass tubes by weight.Then by the seal of tube.When solution temperature is from room temperature (20 DEG C) to-60 DEG C (refrigeration cycle) and when slowly changing to+95 DEG C (heating cycle) from room temperature, detected by visual observations and be separated.In cooling and heating cycle, all observe temperature when being separated (being namely separated into two-phase), the Schwellenwert under given % by weight lubricant concentration is recorded as separation temperature (critical solution temperature, CST), data are in table 1.
Table 1: embodiment 1-5 products obtained therefrom performance data
| Numbering | Separation temperature DEG C | GWP |
| WN－1 | -7 | 10 |
| WN－2 | -1 | 14 |
| WN－3 | -8 | 9 |
| WN－4 | -6 | 10 |
| WN－5 | -5 | 14 |
Claims (6)
1. a fluorine-containing idohydrocarbon composition, is characterized in that by weight, it consists of:
2. fluorine-containing idohydrocarbon composition according to claim 1, is characterized in that by weight, and described nanometer expanding material consists of:
3. fluorine-containing idohydrocarbon composition according to claim 2, is characterized in that described lubricant is polyalkylene glycol or polyol ester class.
4. fluorine-containing idohydrocarbon composition according to claim 2, is characterized in that described
stibium doping stannic oxide nano-powderparticle diameter be 1 ~ 10nm.
5. the preparation method of fluorine-containing idohydrocarbon composition according to claim 2, is characterized in that comprising the following steps:
(a) by weight, by 1-5 part
antimony doped stannic oxide nano powderbe distributed in 1000 parts of ethanol, then add chelate coordinate organic boron coupling agent 0.01-0.05 part, react 1-5h under normal temperature, then add 10-100 part lubricant, 1-5 part 2,6-nonadienol, react 2-10h under normal temperature, obtain nanometer expanding material, for subsequent use;
B () by weight, the nanometer expanding material that step (a) is prepared 0.5 ~ 10 part, 2,3,3,3-tetrafluoeopropene 80 ~ 900 parts, CF3I, 10 ~ 300 parts, 1-allyl group-3-butyl imidazole nitrate ion liquid 0.0008 ~ 0.01 part of mixture obtains fluorine-containing idohydrocarbon composition product.
6. the preparation method of fluorine-containing idohydrocarbon composition according to claim 5, it is characterized in that the mixture described in step (b) refers to first pre-mixing 10-30h under liquid phase, then join in the glass reactor of high-throughput microchannel, be mixed to get fluorine-containing idohydrocarbon composition product with flow velocity 10-100Kg/h.
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| CN111057523A (en) * | 2019-11-14 | 2020-04-24 | 浙江巨化新材料研究院有限公司 | Medium-high temperature heat pump mixed working medium |
| CN111057523B (en) * | 2019-11-14 | 2021-03-16 | 浙江巨化新材料研究院有限公司 | Medium-high temperature heat pump mixed working medium |
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