CN104592944B - A kind of nano fluorine-contained compositions of olefines and preparation method thereof - Google Patents
A kind of nano fluorine-contained compositions of olefines and preparation method thereof Download PDFInfo
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- CN104592944B CN104592944B CN201410820770.0A CN201410820770A CN104592944B CN 104592944 B CN104592944 B CN 104592944B CN 201410820770 A CN201410820770 A CN 201410820770A CN 104592944 B CN104592944 B CN 104592944B
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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
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/04—Materials undergoing a change of physical state when used the change of state being from liquid to vapour or vice versa
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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
- C09K2205/00—Aspects relating to compounds used in compression type refrigeration systems
- C09K2205/10—Components
- C09K2205/12—Hydrocarbons
- C09K2205/122—Halogenated hydrocarbons
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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
- C09K2205/00—Aspects relating to compounds used in compression type refrigeration systems
- C09K2205/34—The mixture being non-azeotropic
Abstract
The invention discloses a kind of nano fluorine-contained compositions of olefines, in parts by weight, form and be：2,3,3,3 55~80 parts of tetrafluoropropenes, 0.01~0.05 part of nano flame retardant suspension, 0~40 part of 2 butylene of cis 1,1,1,4,4,4 hexafluoro, 0~30 part of ammonia.The invention also discloses the preparation method of the nano fluorine-contained compositions of olefines.The present invention has the advantages of technique is simple, cost is low, green, product good flame resistance.
Description
Technical field
The present invention relates to refrigerant art, and in particular to a kind of nano fluorine-contained compositions of olefines and preparation method thereof.
Background technology
HFO-1234yf has fabulous environmental performance, and its global warming potential (GWP) is 4, ozone depletion potential (ODP)
For 0, Life cycle carbon emission is low.HFO-1234yf is suitable with HFC-134a toxicity, and has preferable cycle performance, is
The main substitute of HFC-134a refrigerants.But one of the characteristics of material is obvious is that it has combustibility.Therefore researcher
A variety of compositions containing HFO-1234yf are developed, it is flammable to reduce it by adding fire retardant.
A kind of the heat transfer system of heat-transfer fluid, method and group are utilized as China Patent Publication No. CN102971394A is disclosed
Compound, the heat-transfer fluid include：(a) about 30 weight % to about 65 weight % HFC-134a；(b) about 0 weight %
To about 70 weight % HFO1234ze；About 0 weight % to about 70 weight %s HFO-1234yf, condition be this (c)
HFO-1234ze and HFO-1234yf total amount is at least about 35 weight % in composition, and the percentage by weight is based on the combination
Component (a)-(c) total amount in thing.The addition that the invention refer to fire retardant can reduce combustibility.
And for example China Patent Publication No. CN101636466A provides azeotrope-like comprising tetrafluoropropene and CF3I
Composition and application thereof, including for refrigerant composition earl august eugene lund ian robert, refrigeration system, foaming agent and sprayable composition, bag
Include aerosol propellants.CF in said composition3I components can be used as fire retardant, for suppressing HFO1234yf combustibility.
Existing method, which is employed to add fire retardant or nonflammable component, improves anti-flammability because fire retardant with
The poor compatibility of HFO1234yf tetrafluoropropenes, disperses uneven, reduce refrigerant flame retardant effect, while it is prepared
Refrigerant product has higher GWP compared with HFO1234yf either simplex matter, still has considerable influence to environment.
The content of the invention
The technical problem to be solved in the present invention is the defects of overcoming prior art, there is provided a kind of technique is simple, cost is low, green
Nano fluorine-contained compositions of olefines that colour circle is protected and preparation method thereof.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions：A kind of nano fluorine-contained alkene
Composition, in parts by weight, form and be：
In parts by weight, described nano flame retardant suspension composition is preferably：
Described nanometric magnesium hydroxide fire retardant granularity is preferably 1~100nm.
Described silane coupler is preferably one kind in KH-550, KH-570, KH-560, A-151, A-171.
Described fluorinated epoxide is preferably trifluoromethyl oxirane or double (trifluoromethyl) oxirane of l, l-.
The present invention also provides the preparation method of the nano fluorine-contained compositions of olefines, comprises the following steps：
(a) by proportioning, by 50~70 parts of nanometric magnesium hydroxide fire retardants, 0.1~1 part of silane coupler, 5~10 parts of fluorine
Change epoxides, 24~40 parts of methanol 10~20h of mixing, obtain nano flame retardant suspension；
(b) by proportioning, 0.01~0.05 part of nano flame retardant suspension, 2,3,3, the 3- tetrafluoropropenes that step (a) is obtained
55~80 parts, the obtained nano fluorine-contained alkene of 0~30 part of cis 0~40 part of -1,1,1,4,4,4- hexafluoros -2- butylene, ammonia mixture
Composition.
Mixture described in step (b) preferably refers to 5~10h of turbulent flow circulation mixing under liquid phase state.
The preparation method of the nano fluorine-contained compositions of olefines of the present invention, the nano flame retardant containing fire retardant is prepared first and is suspended
Liquid, i.e., nanometric magnesium hydroxide fire retardant and silane coupler, fluorinated epoxide, methanol are sufficiently mixed, generation nanometer resistance
Fire suspension；Again by nano flame retardant suspension and 2,3,3,3- tetrafluoropropenes (HFO1234yf) and cis -1,1, Isosorbide-5-Nitrae, 4,4- six
The mixture of one or both of fluoro- 2- butylene (Z-HFO-1336mzzm), ammonia is added to turbulent recirculating still with certain proportioning
In, obtain product by sufficient turbulent mixture.HFO1234yf, Z-HFO-1336mzzm, ammonia and nano ion liquid in product
There are good solubility and diffusivity, can effectively reduce HFO1234yf flammable performance.
The commercially available acquirement of raw material and equipment in the present invention, as nanometric magnesium hydroxide fire retardant can use Wuxi City pool
The product of brightness Chemical Co., Ltd..Fluorinated epoxide can useSuzhou Yacoo Chemical Reagent CorporationThe trifluoro of production
Methyl oxirane, l, double (trifluoromethyl) product of ethylene oxide of l-, preferably trifluoromethyl oxirane (C3H3F3O).2,3,3,
3- tetrafluoropropenes (HFO1234yf, molecular formula:C3H2F4) can be using the product of Juhua Group Co..Cis -1,1, Isosorbide-5-Nitrae, 4,4-
Hexafluoro -2- butylene (Z-HFO-1336mzzm) can use the product of Juhua Group Co..Silane coupler can use Nanjing forward
Product K H-550, KH-570, KH-560, A-151, A-171 of Chemical Co., Ltd.'s production etc., preferably KH-550.Turbulent flow circulation
Kettle can use the turbulent recirculating still product that Wuhan Engineering Univ develops.
Compared with prior art, the invention has the advantages that：
1st, technique is simple, cost is low, by nanometric magnesium hydroxide fire retardant and silane coupler, fluorinated epoxide, first
Alcohol is sufficiently mixed, and generates nano flame retardant suspension；Again by nano flame retardant suspension and 2,3,3,3- tetrafluoropropenes (HFO1234yf)
Mixture with one or both of cis-1,1,1,4,4,4-hexafluoro-2-butene (Z-HFO-1336mzzm), ammonia is with certain
Proportioning is added in turbulent recirculating still, material be in turbulent condition, the mixing of storeroom or scattered more quick, uniform, greatly
Preparation technology is simplified greatly, reduces cost, is advantageous to industrialization large-scale production；
2nd, the product good flame resistance being prepared, suspended due to introducing the nano flame retardant with flame retardant effect in component
Liquid, the anti-flammability of refrigerant, while the introducing of fluorinated epoxide are improved, slow down 2,3,3,3- tetrafluoropropenes
(HFO1234yf) degraded trend, HFO1234yf flammable performance, and HFO1234yf, Z- in product can effectively be reduced
HFO-1336mzzm, ammonia and nano ion liquid have good solubility and diffusivity, can further reduce HFO1234yf's
Flammable performance, the anti-flammability of refrigerant is improved, product LFL values (volume %) of the invention are more than 12.4；
3rd, green, the refrigerant composition earl august eugene lund ian robert global warming potential (GWP) of preparation of the invention is below 13, ozone damage
It is 0 to consume potentiality (ODP).
Embodiment
The present invention is further detailed below in conjunction with specific embodiment, but the invention is not limited in described reality
Apply example.
Raw material of the present invention and the commercially available acquirement of equipment, which part raw material and description of equipment are as follows：
Trifluoromethyl oxirane (C3H3F3O double (trifluoromethyl) oxirane of), l, l-：Suzhou subfamily chemical reagent stock Part Co., LtdProduct.
2,3,3,3- tetrafluoropropenes (HFO1234yf, molecular formula:C3H2F4)：The product of Juhua Group Co..
Cis-1,1,1,4,4,4-hexafluoro-2-butene (Z-HFO-1336mzzm)：The product of Juhua Group Co..
Silane coupler (KH-550, KH-570, KH-560, A-151, A-171)：The production of Nanjing Chemical Co., Ltd. forward
Product.
Nanometric magnesium hydroxide fire retardant：Wuxi City Ze Hui Chemical Co., Ltd.s, 1~100nm of granularity.
Turbulent recirculating still：The product of Wuhan Engineering Univ.
Embodiment 1
The preparation of step (1) nano flame retardant suspension, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 60 parts of nanometric magnesium hydroxide fire retardants, 0.5 part of silicon are added in 200L reactors
Alkane coupling agent KH-550,8 parts of trifluoromethyl oxirane, 31.5 parts of methanol, 15h is mixed, obtains nano flame retardant suspension；
Step (2) mixture, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 70 parts of HFO1234yf, 15 parts of Z-HFO- are added in 200L turbulent flow recirculating stills
Nano flame retardant suspension, the 14.97 parts of ammonia that 1336mzzm, 0.03 part of step (1) are prepared, the turbulent flow circulation under liquid phase state
8h is mixed, obtains product.Numbering is WN-1.
Embodiment 2
The preparation of step (1) nano flame retardant suspension, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 50 parts of nanometric magnesium hydroxide fire retardants, 0.1 part of silicon are added in 200L reactors
Alkane coupling agent kh-570,10 parts of l, l- double (trifluoromethyl) oxirane, 39.9 parts of methanol, mix 10h, obtain nano flame retardant and hang
Supernatant liquid；
Step (2) mixture, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 60 parts of HFO1234yf, 10 parts of Z-HFO- are added in 200L turbulent flow recirculating stills
Nano flame retardant suspension, the 29.99 parts of ammonia that 1336mzzm, 0.01 part of step (1) are prepared, the turbulent flow circulation under liquid phase state
5h is mixed, obtains product.Numbering is WN-2.
Embodiment 3
The preparation of step (1) nano flame retardant suspension, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 70 parts of nanometric magnesium hydroxide fire retardants, 1 part of silane are added in 200L reactors
Coupling agent KH-560,5 parts of trifluoromethyl oxirane, 24 parts of methanol, 20h is mixed, obtains nano flame retardant suspension；
Step (2) mixture, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 80 parts of HFO1234yf, 5 parts of Z-HFO- are added in 200L turbulent flow recirculating stills
Nano flame retardant suspension, the 14.95 parts of ammonia that 1336mzzm, 0.05 part of step (1) are prepared, the turbulent flow circulation under liquid phase state
10h is mixed, obtains product.Numbering is WN-3.
Embodiment 4
The preparation of step (1) nano flame retardant suspension, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 54 parts of nanometric magnesium hydroxide fire retardants, 1 part of silane are added in 200L reactors
Coupling agent A-151,5 parts of trifluoromethyl oxirane, 40 parts of methanol, 15h is mixed, that is, obtains nano flame retardant suspension；
Step (2) mixture, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 59.95 parts of HFO1234yf, 30 parts of Z-HFO- are added in 200L turbulent flow recirculating stills
Nano flame retardant suspension, the 10 parts of ammonia that 1336mzzm, 0.04 part of step (1) are prepared, turbulent flow circulation is mixed under liquid phase state
7h is closed, obtains product.Numbering is WN-4.
Embodiment 5
The preparation of step (1) nano flame retardant suspension, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 64 parts of nanometric magnesium hydroxide fire retardants, 1 part of silane are added in 200L reactors
Coupling agent A-171,5 parts of l, l- double (trifluoromethyl) oxirane, 30 parts of methanol, mix 15h, obtain nano flame retardant suspension；
Step (2) mixture, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 64.95 parts of HFO1234yf, 5 parts of Z-HFO- are added in 200L turbulent flow recirculating stills
Nano flame retardant suspension, the 30 parts of ammonia that 1336mzzm, 0.02 part of step (1) are prepared, turbulent flow circulation is mixed under liquid phase state
6h is closed, obtains product.Numbering is WN-5.
Embodiment 6
The preparation of step (1) nano flame retardant suspension, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 60 parts of nanometric magnesium hydroxide fire retardants, 0.5 part of silicon are added in 200L reactors
Alkane coupling agent KH-550,8 parts of trifluoromethyl oxirane, 31.5 parts of methanol, 15h is mixed, obtains nano flame retardant suspension；
Step (2) mixture, based on every part of 1Kg, charge ratio is as follows：
79.97 parts of HFO1234yf
0.03 part of nano flame retardant suspension
20 parts of ammonia
Preparation method is：By proportioning, 79.97 parts of HFO1234yf, 0.03 part of step are added in 200L turbulent flow recirculating stills
(1) nano flame retardant suspension, the 20 parts of ammonia being prepared, turbulent flow circulation mixing 8h, obtains product under liquid phase state.Numbering is
WN-6。
Embodiment 7
The preparation of step (1) nano flame retardant suspension, based on every part of 1Kg, charge ratio is as follows：
Preparation method is：By proportioning, 60 parts of nanometric magnesium hydroxide fire retardants, 0.5 part of silicon are added in 200L reactors
Alkane coupling agent KH-550,8 parts of trifluoromethyl oxirane, 31.5 parts of methanol, 15h is mixed, obtains nano flame retardant suspension；
Step (2) mixture, based on every part of 1Kg, charge ratio is as follows：
60 parts of HFO1234yf
39.97 parts of Z-HFO-1336mzzm
0.03 part of nano flame retardant suspension
Preparation method is：By proportioning, 60 parts of HFO1234yf, 39.97 parts of Z-HFO- are added in 200L turbulent flow recirculating stills
The nano flame retardant suspension that 1336mzzm, 0.03 part of step (1) are prepared, turbulent flow circulation mixing 8h, is obtained under liquid phase state
To product.Numbering is WN-7.
Performance test：
Embodiment 1-7 products obtained therefroms do burning test according to U.S.'s ASTM-E681-01 standards, and wherein LFL is burning pole
The lower limit value of limit, LFL values are bigger, and flammability is lower.LFL value experimental results are shown in Table 1.
Table 1：Embodiment 1-7 products obtained therefroms and HFO1234yf performance comparisions
| Numbering | LFL values (volume %) | GWP |
| WN-1 | 13.8 | 8 |
| WN-2 | 14.2 | 12 |
| WN-3 | 14.5 | 9 |
| WN-4 | 15.2 | 10 |
| WN-5 | 16.8 | 10 |
| WN-6 | 12.9 | 13 |
| WN-7 | 12.4 | 12 |
| HFO1234yf | 6.9 | 4 |
Claims (5)
1. a kind of nano fluorine-contained compositions of olefines, it is characterised in that be prepared from following components in parts by weight：
Described nano flame retardant suspension forms：
Preparation process is as follows：
(a) by proportioning, nanometric magnesium hydroxide fire retardant, silane coupler, fluorinated epoxide, methanol are mixed into 10~20h,
Obtain nano flame retardant suspension；
(b) by proportioning, nano flame retardant suspension that step (a) is obtained, 2,3,3,3- tetrafluoropropenes, cis -1,1, Isosorbide-5-Nitrae, 4,
4- hexafluoro -2- butylene, ammonia 5~10h of turbulent flow circulation mixing under liquid phase state obtain nano fluorine-contained compositions of olefines.
2. nano fluorine-contained compositions of olefines according to claim 1, it is characterised in that described nanometric magnesium hydroxide resistance
It is 1~100nm to fire agent granularity.
3. nano fluorine-contained compositions of olefines according to claim 1, it is characterised in that described silane coupler is KH-
550th, one kind in KH-570, KH-560, A-151, A-171.
4. nano fluorine-contained compositions of olefines according to claim 1, it is characterised in that described fluorinated epoxide is three
Methyl fluoride oxirane or double (trifluoromethyl) oxirane of l, l-.
5. the preparation method of the nano fluorine-contained compositions of olefines described in claim 1, it is characterised in that comprise the following steps：
(a) by proportioning, by 50~70 parts of nanometric magnesium hydroxide fire retardants, 0.1~1 part of silane coupler, 5~10 parts of fluorination rings
Oxide, 24~40 parts of methanol mix 10~20h, obtain nano flame retardant suspension；
(b) by proportioning, 0.01~0.05 part of nano flame retardant suspension that step (a) is obtained, 2,3,3,3- tetrafluoropropenes 55~
80 parts, cis 0~40 part of -1,1,1,4,4,4- hexafluoros -2- butylene, 0~30 part of ammonia under liquid phase state turbulent flow circulation mixing 5~
10h obtains nano fluorine-contained compositions of olefines.
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