CN208213197U - A kind of device efficiently synthesizing trifluoroiodomethane - Google Patents

Abstract

The utility model discloses a kind of device for efficiently synthesizing trifluoroiodomethane, described device includes reactor, and the reactor inlet connects CF₃COOH vaporizer and iodine evaporator；The reactor outlet is sequentially connected the first collector, the second collector, caustic treater, drier, absorber, cold-trap.The high-purity C F prepared using utility model device₃I product, has that reaction rate is fast, selectivity is good, yield is high, reactant utilization rate is high, energy saving, is expected to realization industrialized production, meets the current market demand.

Description

A kind of device efficiently synthesizing trifluoroiodomethane

Technical field

The utility model relates to a kind of devices for efficiently synthesizing trifluoroiodomethane.

Background technique

Trifluoroiodomethane (CF₃I latent value (GWP) < 5 of greenhouse effects), the latent value (ODP) of ozone depletion is 0, is combined State is classified as the major components of the 3rd generation environmental protection refrigerant.Other than it can be used as new gas extinguishing chemical and refrigerant, in fluorine-containing centre Other fields such as body, conductor etching, foaming agent also have wide practical use.

CF₃I document report CF₃I synthesis technology is numerous, and main method has:

(1) perfluorocarboxylic acid salt pyrolysismethod: with CF₃COM (M=Ag, Na, K, Hg, Pb, Ba) and iodine (I₂) it is raw material, in strong pole Property solvent in heat resolve prepare CF₃I, this is also to be suggested the synthetic method with industrialization and practical value earliest, (J.Am.Chem.Soc.1950 (72): 584-587.3806-7, J. Chem.Soc., 1951 (2): 584-587.).Wherein with The pyrolysis yield of silver salt is higher but expensive.The discovery such as Paskovich, sodium salt or sylvite are at dimethylformamide (DMF) Under reflux, CF can be improved₃I yield is to 70% or so, (J.Org.Chem., 1967,32 (3): 833-835.).Xu Huatang etc. with It is solvent that sulfolane, which substitutes DMF, obtains CF₃The yield of I is 80% or so, (chemical reagent, 1989,11 (2): 123.).

(2) fluoroform iodide process: Japan Patent JP52068110 is reported with fluoroform (CF₃) and I H₂It is living for raw material Property charcoal carrying alkali metal or alkaline-earth metal be catalyst preparation CF₃I.Catalyst shows preferable catalytic activity, due to reaction Temperature is high, and catalyst carbon deposition is serious, and the service life is shorter, and the high polymer generated increases and recycles unreacted I₂Difficulty.

(3) it proposes in French Patent (FRP) FR2794456 with pentafluoroethane (C₂F₅) and I H₂For the synthetic route of raw material, the technique With the catalyst system similar with fluoroform iodide process, unstripped gas is catalyzed by activated carbon supported alkali or alkaline earth metal The available CF of agent bed₃I。

In conclusion existing preparation CF₃There are expensive raw material prices, at high cost for the method for I, and reaction dissolvent consumption is big, produce The a series of problems such as object yield is low, poor selectivity, raw material availability are low.Therefore, find one it is easy to operate, selectivity it is high CF₃I synthetic route is most important.

Summary of the invention

To solve the above-mentioned problems, the purpose of this utility model is to provide it is a kind of it is easy to operate, selectivity of product is high Synthesize CF₃The device of I.In order to achieve the above object, the utility model is achieved through the following technical solutions:

The utility model provides a kind of device for efficiently synthesizing trifluoroiodomethane, and described device includes reactor, described anti- Device entrance is answered to connect CF₃COOH vaporizer and iodine evaporator；The reactor outlet is sequentially connected the first collector, the second collection Device, caustic treater, drier, absorber, cold-trap.

CF is synthesized using above-mentioned apparatus₃The method of I, CF₃COOH steam and iodine vapor, under the action of catalyst, reaction generate Trifluoroiodomethane；

The catalyst is with active carbon or graphene for carrier loaded 1~10wt%KNO₃With 2~7wt% RbNO₃'s Catalyst；CF₃The molar ratio of COOH steam and iodine vapor is 1:1~2:1；Reaction temperature is 450-550 DEG C；Reaction time is 10-15min；CF₃The flow of COOH steam is 10-20mL/min.

Further, in the above-mentioned technical solutions, obtained trifluoroiodomethane is successively passed through the first collector, the second receipts Storage, caustic treater, drier and absorber remove impurity and moisture content；It is heated outside first collector using recirculated water；Alkali cleaning The lye of tank is NaOH solution；Desiccant in drier is silica gel；Adsorbent in absorber is molecular sieve.

Further, in the above-mentioned technical solutions, the temperature of level-one collector outer circulation water is 70-80 DEG C；In caustic treater The concentration of NaOH solution is 0.1-5%；Adsorbent is 5A molecular sieve in absorber.

Further, in the above-mentioned technical solutions, trifluoroiodomethane is received using cold-trap.

Further, in the above-mentioned technical solutions, the temperature for collecting trifluoroiodomethane cold-trap is -70 DEG C.

Further, in the above-mentioned technical solutions, CF₃COOH steam is that the vaporizer vaporization for being 100 DEG C by temperature generates； Iodine vapor is that the iodine evaporator for being 200 DEG C by temperature generates.

CF is efficiently synthesized using utility model device₃I is with active carbon or graphene for carrier loaded 1~10wt% KNO₃With 2~7wt%RbNO₃Catalyst, make CF₃COOH steam and iodine vapor occur in high-temperature reactor chemical reaction and Generate CF₃Then I passes sequentially through NaOH solution, silica gel and molecular sieve to effectively remove CF₃Impurity and moisture in I, are thus closed At CF₃The yield of I is up to 90%, and since catalyst selects matters, and processing step design is rationally, can not only accelerate anti- Rate is answered, yield is improved, it is energy saving so as to improve the utilization rate of reactant, it is expected to realize industrialized production, thus full The current market demand of foot.

Detailed description of the invention

Fig. 1 is the apparatus structure schematic diagram for efficiently synthesizing trifluoroiodomethane of the utility model；

In figure, 1, CF₃COOH vaporizer；2, iodine evaporator 2；3, reactor；4, the first collector；5, the second collector； 6, caustic treater；7, drier；8, absorber；9, cold-trap.

Specific embodiment

Embodiment 1

As shown in Figure 1, a kind of device for efficiently synthesizing trifluoroiodomethane, described device includes reactor 3, the reactor 3 entrances connect CF₃COOH vaporizer 1 and iodine evaporator 2；The outlet of reactor 3 is sequentially connected the first collector 4, second receipts Storage 5, caustic treater 6, drier 7, absorber 8, cold-trap 9.

Synthetic catalyst: by 3.0g KNO₃With 5g RbNO₃It is dissolved in 500mL water, 100 g active carbons is added thereto, It is ultrasonically treated 30min, is stood overnight；Filtering, dries 5h for Solid separate, then under high pure nitrogen atmosphere at 100 DEG C Catalyst is made in 500 DEG C of calcining 2h.

CF is synthesized using above-mentioned apparatus₃I

(1)CF₃1:1 enters 500 DEG C of reactors 3 in molar ratio for COOH steam and iodine vapor, and 100g is housed in reactor 3 Catalyst controls CF₃The flow of COOH steam is 20mL/min, CF₃The reaction time of COOH and iodine is that 10min generates CF₃I。

(2) make above-mentioned CF₃I gas is successively passed through the first collector 4, the second collector 5, caustic treater 6, drier 7, absorption Device 8 removes H₂O、CO₂, the impurity such as HF.It is recycled outside first collector 4 using 80 DEG C of water；Lye in caustic treater 6 is 0.5%NaOH solution；Desiccant in drier 7 is silica gel；Adsorbent in absorber 8 is 5A molecular sieve.Finally by -70 DEG C cold-trap 9 to CF₃I solution is received, CF₃The yield of I is 84.6%.

Embodiment 2

1, synthetic catalyst: by 7.0g KNO₃With 0.7g RbNO₃It is dissolved in 500mL water, 100g graphite is added thereto Alkene is ultrasonically treated 30min, stands overnight；Filtering, dries 5h for Solid separate, then in high pure nitrogen atmosphere at 100 DEG C Catalyst is made in lower 500 DEG C of calcinings 2h.

2, CF is synthesized₃I

(1)CF₃2:1 enters 550 DEG C of reactors in molar ratio for COOH steam and iodine vapor, is catalyzed in reactor equipped with 100g Agent controls CF₃The flow of COOH steam is 20mL/min, CF₃The reaction time of COOH and iodine is that 10min generates CF₃I。

(2) make above-mentioned CF₃I gas is successively passed through the first collector 4, the second collector 5, caustic treater 6, drier 7, absorption Device 8 removes H₂O、CO₂, the impurity such as HF.It is recycled outside first collector 4 using 80 DEG C of water；Lye in caustic treater 6 is 0.5%NaOH solution；Desiccant in drier 7 is silica gel；Adsorbent in absorber 8 is 5A molecular sieve.Finally by -70 DEG C cold-trap 9 to CF₃I solution is received, CF₃The yield of I is 90.7%.

Claims (2)

1. a kind of device for efficiently synthesizing trifluoroiodomethane, it is characterised in that: described device includes reactor, and the reactor enters Mouth connection CF₃COOH vaporizer and iodine evaporator；The reactor outlet is sequentially connected the first collector, the second collector, alkali Cleaning of evaporator, drier, absorber, cold-trap；First collector periphery is equipped with circulating water heating collet；It is dry in the drier Drying prescription is silica gel；Adsorbent in the absorber is molecular sieve.

2. the device according to claim 1 for efficiently synthesizing trifluoroiodomethane, it is characterised in that: adsorbed in the absorber Agent is 5A molecular sieve.