CN107570181A - A kind of preparation method of fluorination catalyst - Google Patents
A kind of preparation method of fluorination catalyst Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of fluorination catalyst, including：1) chromic salts, magnesium salts are dissolved in water to obtain salting liquid, after ammonification water sedimentation, filtering, dry, roasting, crushing obtain powder；2) other metal salts are dissolved in water to obtain salting liquid, after ammonification water sedimentation, filtering, dry, roasting, crushing obtain powder；3) by the powder of step 1) and step 2) powder mechanical mixture, tabletting obtains being catalyzed precursor；4) catalysis precursor is fluorinated to obtain fluorination catalyst.The fluorination catalyst prepared using the method for the present invention is suitable for fluorine chlorine substitution gas phase fluorination, it is especially suitable for R125 and R134a preparation, and the service life of the fluorination catalyst of the invention prepared is longer, during using preparation with R125, after continuous catalytic reaction 500h, catalyst remains in that greater activity.
Description
Technical field
The present invention relates to a kind of preparation method and application of fluorination catalyst, and in particular to one kind is used for halogenated hydrocarbons and fluorination
The preparation method of the catalyst of the gas phase fluorination of hydrogen, the system of R125 and R134a catalyst is prepared in particular for catalysis
Preparation Method.
Background technology
In fluorine chemical field, because hydrogen fluorohydrocarbon (HFCs) ODP (ODP) is 0, global warming potential
Value (GWP) is smaller, and refrigeration performance is similar to fluorochlorohydrocarbon (CFCs), is CFCs ideal substitute, is widely used in large-scale business
Industry refrigerant, foaming agent, extinguishing chemical etc., such as refrigerant R125 and R134a.
Gas phase exchange chloride for fluoride is the key reaction of selective synthesis fluorochemical, because its is simple and easy to do, warp
Ji is practical, has the advantages that pollution is few easy to operate, oneself is through being widely used in the industrial processes of HFC.Wherein, gas phase
Fluorination catalyst is that (core in the process route of (HFCs), efficient fluorination catalyst can solve mesh very well to production fluorohydrocarbon
The problem of selectivity of product is low is marked, so as to largely improve the yield of target product.It is catalyzed in existing gas phase fluorination
In agent preparation method, catalyst preparation generally use infusion process and coprecipitation, but catalyst activity component prepared by infusion process
Being be combined with each other with carrier, power is weak, and active component is easily lost in process of production, causes catalyst performance to reduce, industrial main
Produced using coprecipitation.
Chinese CN 101507922A disclose improves catalysis by adding the auxiliary agents such as magnesium, aluminium, indium, gallium, zinc in the catalyst
The method of agent activity, the preparation method are combined using infusion process and coprecipitation and prepare catalyst, and catalyst described in this article closes
It is relatively low into R134a activity, the influence to accessory substance selectivity is not referred in patent.Chinese patent CN103143344B is disclosed
It is a kind of high than table chromium-based fluorination catalyst and preparation method thereof, the patent by preparation process to containing the first active component
Chromium base and the second active component other metal ions solution in add polyethylene glycol having of being formed compounded with ionic liquid
Machine complexing agent prepares chromium-based fluorination catalyst.It is synthesized in the patent although the specific surface area of catalyst significantly increases
Selective highest of the catalyst when catalysis prepares pentafluoroethane (HFC-125 or R125) also there was only 70.70, still do not meet
Requirement of the existing market to fluorination catalyst high selectivity.Chinese patent CN 1935360A are disclosed for preparing pentafluoroethane
Catalyst and preparation method thereof, heat treatment is selected from magnesium hydroxide, iron hydroxide, hydroxide at a temperature of not higher than 300 DEG C
The metal hydroxides of aluminium, vanadium hydroxide and aluminium hydroxide obtains oxide powder, and catalyst is prepared using mechanical mixing, should
When fluorination catalyst is applied to prepare R125 as initiation material using PCE, R125 selectivity is greatly improved, still, by-product
Thing R115 selectivity is still undesirable, and the specific surface area of the fluorination catalyst is smaller, and catalyst is not also introduced in patent
Service life.Due at present during R125 is synthesized, caused accessory substance five fluorine monochlorethane (R115 or CFC-
115) boiling point is close with R125, and azeotropism be present, it is difficult to is isolated with common distillation technology, generally with extraction essence
The method of evaporating is isolated purification, so as to largely improve its energy consumption and cost in industrial separation purification process, therefore, at present
It is badly in need of a kind of catalyst having in terms of catalysis prepares R125 compared with high selectivity of synthesis.In addition, used for fluorination catalyst
During easy carbon distribution, catalyst life is short, for synthesize R134a refrigerants two anticatalyst conversion ratios it is still relatively low, one
It can not directly obtain compared with quantum jump, and notional result is shown in many patents, performance is lower in actual moving process.
The catalyst for being presently used for gas phase fluorination catalytic reaction is mainly Cr base catalyst, is generally added in preparation process
Add Al, In, B, Ga, Mg, Ca, Sr, Ba, Sc, Ti, Zr etc. to improve the activity of fluorination catalyst, and carry out using coprecipitation
Prepare.Inventor has found that in catalyst preparation process other metallic elements carry out precipitating instead with metal Cr in alkaline solution
Seasonable reaction rate is different, and some metallic elements are close with metal Cr precipitation reaction speed, and then difference is larger for some.
Because precipitation reaction speed is different, nucleus generation speed is also different in precipitation reaction, causes catalyst microstructure and crystalline phase to be sent out
Raw larger difference.Therefore, in catalyst preparation process, to consider precipitation reaction speed will to be differed into larger metallic element
Separately precipitation, the same or like metallic element of precipitation reaction speed is co-precipitated together, so that it is formed in precipitation process
Double salt, the formation of double salt can further improve the uniformity of sediment composition.The present invention is as starting point, there is provided Yi Zhonggai
The preparation method of the fluorination catalyst entered.
The content of the invention
For fluorination catalyst activity present in prior art is relatively low, R125 yields are low, catalyst life is short, Yi Jicong
When R133 gas phase fluorinations synthesize R134a the problems such as catalyst activity low (because reactions steps thermodynamics is obstructed), by gold in the present invention
Belong to Cr and magnesium coprecipitation, roasting, and larger other metallic elements and metal Cr will be differed with metal Cr precipitation reaction speed
Separately precipitation, roasting, there is provided a kind of preparation method of improved fluorination catalyst.
Specifically, the preparation method of fluorination catalyst provided by the invention, comprises the following steps：
1) chromic salts, magnesium salts are dissolved in water to obtain salting liquid, after ammonification water sedimentation, filtering, dry, roasting, crushing obtain
Powder；
2) other metal salts are dissolved in water to obtain salting liquid, after ammonification water sedimentation, filtering, dry, roasting, crushing obtain
Powder；
3) the powder mechanical mixture for obtaining step 1) and step 2), tabletting obtain being catalyzed precursor；
4) catalysis precursor is fluorinated to obtain fluorination catalyst.
In preparation method provided by the invention, the magnesium salts is selected from magnesium carbonate, magnesium bicarbonate, magnesium nitrate, magnesium chloride, sulfuric acid
Magnesium, preferably magnesium chloride.Other metals in other described metal salts can need to be selected according to catalyst formulation, Suo Youneng
The metal of enhancing catalyst activity can serve as selecting object.Technical scheme for convenience of explanation, one is provided herein
A little citings, but not limited to this.In embodiments of the present invention, other metal salts in the step 2) are selected from In salt, Ga
One or both of salt, Sn salt, Fe salt, Co salt, Cu salt, La salt, the type of corresponding metal salt are selected from nitrate, chlorination
Salt, sulfate.In some embodiments, other metal salts are InCl3；In some embodiments, other metal salts are
InCl3And CoCl2；In other embodiments, other metal salts are InCl3And FeCl3；Also in some embodiments, its
His metal salt is SnCl3And CoCl2。
In preparation method provided by the invention, chromic salts, magnesium salts, other metal salts mass ratio can be according to selected gold
Category type is adjusted.In embodiments of the present invention, chromic salts, magnesium salts, the mass ratio of other metal salts are 92~96:0.5
~3:1.5~6.In some embodiments, chromic salts, magnesium salts, the mass ratio of other metal salts are 94~96:1~2:1.05~
5；In other embodiments, chromic salts, magnesium salts, the mass ratio of other metal salts are 95~96:1~2:3~4.
In preparation method provided by the invention, the pH value in step 1) during ammonification water sedimentation is 9~12, in some embodiment party
In formula, the pH value in step 1) is 9,10 or 11.PH value in the step 2) during ammonification water sedimentation is 6~13, in some realities
Apply in mode, pH value is 8~11 in the step 2).
In preparation method provided by the invention, drying temperature in step 1) is 80~150 DEG C, drying time is 5~
12h.In some embodiments, drying temperature is 90~120 DEG C.In some embodiments, drying time is 6~10h.
In preparation method provided by the invention, drying temperature in step 2) is 90~130 DEG C, drying time is 5~
15h.In some embodiments, drying temperature is 100~120 DEG C.In some embodiments, drying time is 6~10h.
In preparation method provided by the invention, the roasting is carried out all in inert gas.
Wherein, the temperature of roasting is 300~400 DEG C in the step 1), and roasting time is 2~8h；In some embodiment party
In formula, the temperature of roasting is 350 DEG C；In other embodiments, roasting time 5h, 4h or 3h.
The temperature of roasting is 300~700 DEG C in the step 2), and roasting time is 2~8h；In some embodiments,
The temperature of roasting is 350 DEG C, 500 DEG C, 600 DEG C, 650 DEG C or 700 DEG C；In other embodiments, roasting time 6h, 5h
Or 4h.
In preparation method provided by the invention, graphite auxiliary agent can also be added in powder during tabletting.When adding graphite, graphite
Quality be gross mass 1%~5%.
In preparation method provided by the invention, the fluorination in the step 4) is under inert gas and HF mixed gas
Carry out, fluorination temperature is 200~400 DEG C.In some embodiments, it is 300~350 DEG C to be fluorinated temperature.
Fluorination catalyst prepared by a kind of above method of the present invention, the specific surface area of the fluorating catalyst former body are
320~350m2/g.In some embodiments, the specific surface area of fluorating catalyst former body is 333.60m2/g、340.41m2/
g、331.01m2/g、335.71m2/ g or 325.29m2/g。
Fluorination catalyst prepared by method provided by the present invention is suitable for fluorine chlorine substitution gas phase fluorination, especially suitable
Share the preparation in R125 and R134a.
" water " used in embodiments of the present invention is deionized water.
" other metal salts " in the present invention refers to other metal salts in addition to chromic salts and magnesium salts.
Heretofore described " inert gas " refers to the gas for not participating in reaction during roasting and fluorination, such as
Nitrogen, argon gas etc..
" drying " of the present invention, refer to borrow energy to make material reclaimed water or solvent gasify, and take away generated steam
Process.Drying mode is drying drying used by some embodiments of the present invention.It should be pointed out that identical effect can be reached
The drying means of fruit also includes but is not limited to drying, vacuum drying, freeze-drying, pneumatic conveying drying, microwave drying, infrared drying
With dielectric dry etc..
Term " washing " of the present invention, refers to by certain effect to weaken or eliminate between impurity and material
Interaction, makes the combination of impurity and material be changed into the combination of impurity and solvent, impurity is departed from material.The present invention
Some embodiments in refer to the process of be rinsed material to pH ≈ 7 with water, ethanol.
Terminology used in the present invention " filtering " represent gravity or other external force effect under by medium by fluid with it is non-
The operation of fluid separation, the medium includes but is not limited to filter paper, gauze, filter core, pellicle, filter screen etc., in theory, containing more
The material of pore structure can turn into the medium of filtering；The equipment of filtering includes but is not limited to vacuum or decompressor, pressurization dress
Put, centrifugal device etc..
Unless explicitly stated otherwise in contrast, otherwise, all scopes that the present invention quotes include end value.For example, " roasting
Temperature is 300~400 DEG C ", the span for representing temperature during roasting is 300 DEG C≤T≤400 DEG C.
Terminology used in the present invention "one" or " one kind " describes key element and component described herein.So do only
It is for convenience, and to provide general meaning to the scope of the present invention.This description should be read to include one or extremely
It is few one, and the odd number also includes plural number, unless it is obvious that it is meant otherwise.
Numeral in the present invention is approximation, no matter whether uses the wording such as " about " or " about ".The numerical value of numeral has
It is possible that the difference such as 1%, 2%, 5%, 7%, 8%, 10%.It is any to have whenever a numeral with N values is disclosed
The numeral that N+/- 1%, N+/- 2%, N+/- 3%, N+/- 5%, N+/- 7%, N+/- 8% or N+/- 10% are worth can be by clearly public
Open, wherein " +/- " refers to add deduct, and the scope between N-10% to N+10% is also disclosed.
Unless otherwise defined, the otherwise implication of all scientific and technical terminologies used herein and common skill of the art
As art personnel are generally understood that.Although similar or equivalent method and material also can use with approach described herein and material
In the implementation or test of embodiment of the present invention, but suitable method and material is described below.What is be mentioned above is all
Publication, patent application, patent and other bibliography are incorporated herein in a manner of being cited in full text, except non-quoted physical segment
Fall.If conflict occurs, it is defined by this specification and its included definition.In addition, material, method and embodiment are only exemplary
, it is no intended to limited.
The beneficial effects of the present invention are：
1) in method for preparing catalyst of the invention, by will differ with metal Cr precipitation reaction speed larger metal and
Cr separates precipitation reaction, makes that during precipitated metal double salt can be formed, and regulation catalyst nucleus in precipitation reaction produces speed,
The catalyst for making to obtain has excellent dispersiveness and homogeneity, can improve the service life of catalyst, reduces production cost.
2) when catalyst prepared by the present invention is applied to R125 preparation, R125 selectivity significantly improves, target product
Overall selectivity reach as high as 98.08%, and the catalyst prepared has longer service life, continuous catalytic reaction 500h
Afterwards, raw material R123 conversion ratio stills remain in 80% or so.
3) when catalyst prepared by the present invention is applied to R134a preparation, substantially increase gas phase fluorination synthesis R134a's
Catalyst activity, R133a conversion ratio reach as high as 33.27%.
Brief description of the drawings
Fig. 1：Comparative example 1 and the life diagram of the fluorination catalyst of embodiment 2
Embodiment
As described below is the preferred embodiment of the present invention, and what the present invention was protected is not limited to the following side of being preferable to carry out
Formula.It should be pointed out that for those skilled in the art on the basis of this innovation and creation design, some deformations for making and
Improve, protection scope of the present invention is belonged to, in order to further describe the present invention, below in conjunction with the accompanying drawings with for specific embodiment
It is bright.
Comparative example 1
Weigh 500g CrCl3·6H2O、4.56g MgCl2、4.42g InCl3、10.13g CoCl211.45L is dissolved in go
In ionized water, mixed salt solution is mixed with ammoniacal liquor to pH value of solution=9, the dry 6h of 110 DEG C of baking oven is plunged the sample into after filtration washing
After be transferred to roaster, in N2350 DEG C of high-temperature roasting 4h in atmosphere, the sample comminution after roasting sieve and add 2% graphite (quality
Fraction) additive is well mixed, and compression molding obtains catalyst precursor.
Then above-mentioned catalyst precursor is fitted into reactor, is passed through the nitrogen and HF mixed gas fluorine at 350 DEG C
Change, chromium-based fluorination catalyst is made.
Specific surface area and pore structure tester is used to analyze the specific surface area of its presoma as 320.52m2/g。
Embodiment 1
Weigh 500g CrCl3.6H2O、4.56g MgCl2It is dissolved in 10.5L deionized waters, mixed salt solution and ammoniacal liquor is mixed
PH value of solution=10 are bonded to, roaster are transferred to after the dry 8h of 120 DEG C of baking oven is plunged the sample into after filtration washing, in N2350 in atmosphere
DEG C high-temperature roasting 3h, black powder is made after crushing.
Weigh 8.85g InCl3It is dissolved in deionized water, mixed salt solution is mixed to pH value of solution=10 with ammoniacal liquor, crosses diafiltration
Wash after plunge the sample into the dry 9h of 100 DEG C of baking oven after be transferred to roaster, in N2600 DEG C of high-temperature roasting 6h in atmosphere, after crushing
Mixed with above-mentioned black powder, compression molding obtains catalyst precursor.
Then above-mentioned catalyst precursor is fitted into reactor, is passed through the nitrogen and HF mixed gas fluorine at 320 DEG C
Change, chromium-based fluorination catalyst is made.
Specific surface area and pore structure tester is used to analyze the specific surface area of its presoma as 333.60m2/g。
Embodiment 2
Weigh 500g CrCl3.6H20、9.11g MgCl2It is dissolved in 9.5L deionized waters, mixed salt solution is mixed with ammoniacal liquor
To pH value of solution=9, roaster is transferred to after the dry 7h of 90 DEG C of baking oven is plunged the sample into after filtration washing, in N2350 DEG C of height in atmosphere
Temperature roasting 5h, is made black powder after crushing.
Weigh 6.64g InCl3With 20.25g CoCl2It is dissolved in deionized water, mixed salt solution is mixed to solution with ammoniacal liquor
PH=9, filtration washing is transferred to roaster after the dry 6h of 110 DEG C of baking oven is plunged the sample into after obtaining, in N2650 DEG C of high temperature roastings in atmosphere
6h is burnt, is mixed after crushing with above-mentioned black powder, compression molding obtains catalyst precursor.
Then above-mentioned catalyst precursor is fitted into reactor, is passed through the nitrogen and HF mixed gas fluorine at 350 DEG C
Change, chromium-based fluorination catalyst is made.
Specific surface area and pore structure tester is used to analyze the specific surface area of its presoma as 340.41m2/g。
Embodiment 3
Weigh 500g CrCl3.6H20、4.56g MgCl2Be dissolved in 8L deionized waters, mixed salt solution is mixed with ammoniacal liquor to
PH value of solution=11, roaster is transferred to after plunging the sample into the dry 8h of 120 DEG C of baking oven after filtration washing, in N2350 DEG C of height in atmosphere
Temperature roasting 3h, is made black powder after crushing.
Weigh 11.06g InCl3With 6.65g FeCl3It is dissolved in deionized water, mixed salt solution is mixed to solution with ammoniacal liquor
PH=11, filtration washing is transferred to roaster after the dry 7h of 120 DEG C of baking oven is plunged the sample into after obtaining, in N2700 DEG C of high temperature in atmosphere
4h is calcined, is mixed after crushing with above-mentioned black powder, compression molding obtains catalyst precursor.
Then above-mentioned catalyst precursor is fitted into reactor, is passed through the nitrogen and HF mixed gas fluorine at 320 DEG C
Change, chromium-based fluorination catalyst is made.
Specific surface area and pore structure tester is used to analyze the specific surface area of its presoma as 331.01m2/g。
Embodiment 4
Weigh 500g CrCl3.6H20、13.67g MgCl2It is dissolved in 11.45L deionized waters, by mixed salt solution and ammoniacal liquor
Mix to pH value of solution=11, roaster is transferred to after plunging the sample into the dry 9h of 120 DEG C of baking oven after filtration washing, in N2In atmosphere
350 DEG C of high-temperature roasting 4h, black powder is made after crushing.
Weigh 5.13g SnCl4With 15.19g CoCl2It is dissolved in deionized water, mixed salt solution is mixed to solution with ammoniacal liquor
PH=10, filtration washing is transferred to roaster after the dry 8h of 120 DEG C of baking oven is plunged the sample into after obtaining, in N2350 DEG C of high temperature in atmosphere
5h is calcined, is mixed after crushing with above-mentioned black powder, compression molding obtains catalyst precursor.
Then above-mentioned catalyst precursor is fitted into reactor, is passed through the nitrogen and HF mixed gas fluorine at 340 DEG C
Change, chromium-based fluorination catalyst is made.
Specific surface area and pore structure tester is used to analyze the specific surface area of its presoma as 335.71m2/g。
Embodiment 5
Weigh 500g CrCl3.6H20、13.67g MgCl2It is dissolved in 10.5L deionized waters, mixed salt solution and ammoniacal liquor is mixed
PH value of solution=10 are bonded to, roaster are transferred to after the dry 8h of 110 DEG C of baking oven is plunged the sample into after filtration washing, in N2350 in atmosphere
DEG C high-temperature roasting 5h, black powder is made after crushing.
Weigh 2.21g SnCl4With 20.25g FeCl3It is dissolved in deionized water, mixed salt solution is mixed to solution with ammoniacal liquor
PH=8, filtration washing is transferred to roaster after the dry 7h of 110 DEG C of baking oven is plunged the sample into after obtaining, in N2500 DEG C of high temperature roastings in atmosphere
5h is burnt, is mixed after crushing with above-mentioned black powder, compression molding obtains catalyst precursor.
Then above-mentioned catalyst precursor is fitted into reactor, is passed through the nitrogen and HF mixed gas fluorine at 330 DEG C
Change, chromium-based fluorination catalyst is made.
Specific surface area and pore structure tester is used to analyze the specific surface area of its presoma as 325.29m2/g。
Embodiment 6
Fluorination catalyst prepared by comparative example 1, embodiment 1~5 is used for the evaluation experimental for synthesizing R125, evaluation respectively
Condition is as follows：Load 100mL fluorination catalysts in self-control fixed bed, reaction temperature control is 310~350 DEG C.Lead in reactor
Enter R123 and HF, R123 flow is 36g/h, and HF flows are 78g/h.R123 and HF enters reactor reaction after mixing, production
Thing gas scrubbing, alkali cleaning use gas chromatographic analysis after removing HCl and HF.R123 conversion ratio and R124, R125 is selectively shown in Table
1。
From data in table 1, by the use of R123 as initiation material, compared with comparative example 1, the fluorine that is prepared by embodiment 1-5
When changing catalyst reaction, R125 selectivity significantly improves, and the overall selectivity of target product is up to more than 94.5%, especially
Be separately precipitated by other metal salts, roasting technique prepare catalyst reaction when, R125 selectivity more than 32%,
The overall selectivity of product is up to more than 96%.
Catalyst prepared by comparative example 1 and embodiment 2 carries out life test, and test result shows (see accompanying drawing 1), continuously
After reacting 500h, raw material R123 conversion ratio stills remain in 80% or so, and the catalyst for showing to prepare remains in that higher
Catalytic activity.
Evaluation experimental result of the fluorination catalyst of table 1 to synthesis R125
Embodiment 6
Fluorination catalyst prepared by comparative example 1, embodiment 1~5 is used for the evaluation experimental for synthesizing R134a respectively, commented
Valency condition is as follows：Load 100mL fluorination catalysts in self-control fixed bed, reaction temperature control is 310~350 DEG C.In reactor
R133a and HF are passed through, R133a flow is 24g/h, and HF flows are 60g/h.It is anti-that R133a and HF enters reactor after mixing
Should, product gas washing, alkali cleaning use gas chromatographic analysis after removing HCl and HF.R133a conversion ratio and R134a is selectively shown in
Table 2.
Evaluation experimental result of the fluorination catalyst of table 2 to synthesis R134a
From data in table 2, compared with comparative example 1, during the fluorination catalyst catalytic reaction prepared by embodiment 2,
R133a conversion ratio significantly improves, catalyst prepared by the technique separately precipitated by other metal salts and chromic salts and magnesium salts, being calcined
During catalytic reaction, R133a conversion ratio reaches as high as 33.27%.
Claims (10)
1. a kind of preparation method of fluorination catalyst, it is characterised in that comprise the following steps：
1) chromic salts, magnesium salts are dissolved in water to obtain salting liquid, after ammonification water sedimentation, filtering, dry, roasting, crushing obtain powder；
2) other metal salts are dissolved in water to obtain salting liquid, after ammonification water sedimentation, filtering, dry, roasting, crushing obtain powder
End；
3) the powder mechanical mixture for obtaining step 1) and step 2), tabletting obtain being catalyzed precursor；
4) catalysis precursor is fluorinated to obtain fluorination catalyst.
2. the preparation method of fluorination catalyst according to claim 1, it is characterised in that chromic salts, magnesium salts, other metal salts
Mass ratio be 92~96:0.5~3:1.5~6.
3. the preparation method of fluorination catalyst according to claim 1, it is characterised in that other gold in the step 2)
Belong to salt and be selected from one or both of In salt, Ga salt, Sn salt, Fe salt, Co salt, Cu salt, La salt.
4. the preparation method of fluorination catalyst according to claim 1, it is characterised in that the salting liquid in the step 1)
It is 9~12 to be added to pH value when being precipitated in ammoniacal liquor；Salting liquid in the step 2) is added to pH value when being precipitated in ammoniacal liquor
For 6~13.
5. the preparation method of fluorination catalyst according to claim 1, it is characterised in that dry temperature in the step 1)
Spend for 80~150 DEG C, drying time is 5~12h；Drying temperature in the step 2) is 90~130 DEG C, drying time 5
~15h.
6. the preparation method of fluorination catalyst according to claim 1, it is characterised in that the temperature of roasting in the step 1)
Spend for 300~400 DEG C, roasting time is 2~8h.
7. the preparation method of fluorination catalyst according to claim 1, it is characterised in that the temperature of roasting in the step 2)
Spend for 300~700 DEG C, roasting time is 2~8h.
8. the preparation method of fluorination catalyst according to claim 1, it is characterised in that the fluorination in the step 4) is
Carried out under inert gas and HF mixed gas, fluorination temperature is 200~400 DEG C.
9. fluorination catalyst prepared by a kind of preparation method of fluorination catalyst according to any one of claim 1~8.
10. the application of fluorination catalyst as claimed in claim 9, it is characterised in that the fluorination catalyst, which is used to be catalyzed, to be prepared
In R125 and R134a fluorination reaction.
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| CN108579726A (en) * | 2018-04-10 | 2018-09-28 | 湖北省宏源药业科技股份有限公司 | A method of preparing chromium-based fluorination catalyst using chromic acid lotion is discarded |
| CN109179517A (en) * | 2018-09-27 | 2019-01-11 | 无锡玖和隆工程科技有限公司 | A kind of preparation method of cobalt trifluoride granulating |
| CN109806858A (en) * | 2019-02-18 | 2019-05-28 | 南通宝凯化工有限公司 | A kind of preparation method of catalysts for gas phase fluorination |
| CN112794788A (en) * | 2021-04-08 | 2021-05-14 | 北京宇极科技发展有限公司 | Method for synthesizing fluoroisobutylene by using hexafluoropropylene as starting material |
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| CN108579726A (en) * | 2018-04-10 | 2018-09-28 | 湖北省宏源药业科技股份有限公司 | A method of preparing chromium-based fluorination catalyst using chromic acid lotion is discarded |
| CN109179517A (en) * | 2018-09-27 | 2019-01-11 | 无锡玖和隆工程科技有限公司 | A kind of preparation method of cobalt trifluoride granulating |
| CN109806858A (en) * | 2019-02-18 | 2019-05-28 | 南通宝凯化工有限公司 | A kind of preparation method of catalysts for gas phase fluorination |
| CN112794788A (en) * | 2021-04-08 | 2021-05-14 | 北京宇极科技发展有限公司 | Method for synthesizing fluoroisobutylene by using hexafluoropropylene as starting material |
| CN112794788B (en) * | 2021-04-08 | 2021-07-09 | 泉州宇极新材料科技有限公司 | Method for synthesizing fluoroisobutylene by using hexafluoropropylene as starting material |
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