CN101543779A - Method for preparing catalyst for producing HFC-125 by hydrogenating and dechlorinating CFC-115 - Google Patents
Method for preparing catalyst for producing HFC-125 by hydrogenating and dechlorinating CFC-115 Download PDFInfo
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- CN101543779A CN101543779A CN200910098452A CN200910098452A CN101543779A CN 101543779 A CN101543779 A CN 101543779A CN 200910098452 A CN200910098452 A CN 200910098452A CN 200910098452 A CN200910098452 A CN 200910098452A CN 101543779 A CN101543779 A CN 101543779A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 36
- RFCAUADVODFSLZ-UHFFFAOYSA-N 1-Chloro-1,1,2,2,2-pentafluoroethane Chemical compound FC(F)(F)C(F)(F)Cl RFCAUADVODFSLZ-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 235000019406 chloropentafluoroethane Nutrition 0.000 title claims abstract description 30
- GTLACDSXYULKMZ-UHFFFAOYSA-N pentafluoroethane Chemical compound FC(F)C(F)(F)F GTLACDSXYULKMZ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 230000000382 dechlorinating effect Effects 0.000 title abstract 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000002360 preparation method Methods 0.000 claims abstract description 39
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 37
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- 238000005554 pickling Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 61
- 238000006298 dechlorination reaction Methods 0.000 claims description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 15
- 238000002803 maceration Methods 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229910052763 palladium Inorganic materials 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 4
- 235000021110 pickles Nutrition 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 238000006424 Flood reaction Methods 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 150000004820 halides Chemical class 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000012018 catalyst precursor Substances 0.000 abstract 3
- 238000006243 chemical reaction Methods 0.000 description 18
- RWRIWBAIICGTTQ-UHFFFAOYSA-N difluoromethane Chemical compound FCF RWRIWBAIICGTTQ-UHFFFAOYSA-N 0.000 description 12
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 6
- 235000019404 dichlorodifluoromethane Nutrition 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 101150003085 Pdcl gene Proteins 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000969 carrier Substances 0.000 description 3
- 238000007605 air drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VEZJSKSPVQQGIS-UHFFFAOYSA-N 1-chloro-2-fluoroethane Chemical class FCCCl VEZJSKSPVQQGIS-UHFFFAOYSA-N 0.000 description 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000000779 depleting effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000002815 homogeneous catalyst Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 235000015243 ice cream Nutrition 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Landscapes
- Catalysts (AREA)
Abstract
The invention provides a method for preparing a catalyst for producing HFC-125 as an ODS substitute by hydrogenating and dechlorinating CFC-115. The catalyst takes Pd as an active component and takes granular active carbon as a carrier. The method comprises the following steps for preparing the catalyst that: the carrier active carbon is put into an acid-pickling solution for pretreatment; the carrier active carbon subjected to acid-pickling pretreatment is repeatedly washed to be neutral by use of deionized water; the dried neutral carrier active carbon is pre-infiltrated with an infiltrating solution; a Pd-containing compound is prepared into a Pd-source impregnating solution which is then added to the infiltrating solution; the carrier active carbon is impregnated with the infiltrating solution added with the Pd-source impregnating solution for a while and added with precipitant, and continues to be impregnated for a while so as to form a catalyst precursor; the catalyst precursor is taken out from the impregnating solution; and a catalyst product is obtained by drying, roasting and reducing the catalyst precursor. The method has the characteristics of simple preparation process and low cost for production and use.
Description
Technical field
The present invention relates to a kind of carried noble metal Pd/C Preparation of catalysts method that is used for hydrogenation reaction, particularly be used for CFC-115 (1,1,1,2,2-five fluoro-2-monochlorethanes) hydrogenation-dechlorination production HFC-125 (1,1,1,2, the 2-pentafluoroethane) the Preparation of catalysts method.
Background technology
CFC-115 mainly as cold-producing medium, is widely used in the refrigeration plants such as food showcase, ice cream maker and low temperature refrigerator.Yet because CFC-115 belongs to ozone-depleting material (ODS), its ODP (ODP) is 0.6, must stop to produce CFC-115 by Montreal protocol China before 2010.China is in the consumption of ozone layer depleting substances such as regulation complete prohibition on July 1st, 2007 freon.The ideal substitute of CFC-115 is HFC-125, and its ODP (ODP) is 0.0.By realizing the conversion of CFC-115 to HFC-125 once simple hydrogenation-dechlorination step of step, setting up process that a step hydrogenation-dechlorination prepares HFC-125 in the existing at home CFC-115 of production technological process is just satisfying and is continuing and the research and development demand of permanent production technology, can greatly reduce the investment of producing ODS substitute HFC-125, thereby realize the smooth transition of domestic existing CFC-115 technical process.
The preparation of Hydrodechlorinating catalyst is the most key in this process, and present existing Hydrodechlorinating catalyst has that Ni is catalyst based, metal carbides, homogeneous catalyst RhCl (PPh
3)
3, loaded noble metal catalyst etc.Studies show that carried noble metal Pd catalyst generates HFCs to the CFCs hydrogenation-dechlorination high activity, selectivity are arranged.Active carbon is because its high-specific surface area, chemical inertness and heat endurance, wide material sources and characteristic such as cheap are often used as the noble metal carrier under non-oxidation agent condition.It mainly is that CFC-12 generates the HFC-32 reaction that the maximum CFCs hydrogenation-dechlorination of research at present generates the HFCs reaction.Japan Patent No.339182JP 0601 731PCT adopts the Pd/C catalyst that CFC-12 is changed into HFC-32, and the conversion ratio of its CFC-12 is 80%, and the productive rate of HFC-32 is 20%.Canadian Patent CA.No.119:94820t utilizes Pd/Al
2O
3Be applied to CFC-12 and generate the HFC-32 reaction, but the performance that the HCl that generates in course of reaction owing to metal oxide carrier and a spot of HF can change catalyst with this class inorganic oxide carrier generation chemical reaction, and the stability of catalyst is not fine.U.S. Pat 6963016 is added a spot of Al in active carbon
2O
3Generate the HFC-32 reaction for preparing carriers Pd/C catalyst is applied to CFC-12, the conversion ratio of CFC-12 is 85%, and the selectivity of HFC-32 is 80%, yet there are no open report but the Pd/C catalyst is applied to the reaction that CFC-115 changes into HFC-125.
Summary of the invention
The object of the present invention is to provide a kind of Pd/C Preparation of catalysts method of the CFC-115 of being used for hydrogenation-dechlorination system HFC-125 reaction, the Pd/C catalyst for preparing by this method has good hydrogenation-dechlorination activity and selectivity.
A kind of CFC-115 of being used for hydrogenation-dechlorination of the present invention is produced HFC-125 Preparation of catalysts method: this catalyst is carrier with the active carbon, load active component Pd, and this Preparation of catalysts step is as follows:
(1) carrier active carbon is put into pickle, water-bath backflow pickling preliminary treatment 4～10h, pickle adopts one or more in hydrochloric acid, nitric acid or the phosphoric acid;
(2) extremely neutral through the pretreated carrier active carbon of pickling with the deionized water cyclic washing, drying for standby;
(3) the neutral carrier active carbon after the pickling preliminary treatment with drying soaks into 1～2h in advance with infiltrate;
(4) preparation Pd source maceration extract will contain the Pd compound and be mixed with Pd source maceration extract, and Pd source maceration extract is added in the infiltrate, add carrier active carbon floods 4～6h in the infiltrate that is added with Pd source maceration extract after precipitating reagent continue dipping 1～2h catalyst precarsor;
(5) catalyst precarsor is taken out from maceration extract, the taking-up mode adopt water bath method, rotary evaporation, filtration or centrifugal in a kind of;
(6) be catalyst prod after catalyst precarsor drying, roasting, the reduction.
Produce HFC-125 Preparation of catalysts method at above-mentioned a kind of CFC-115 hydrogenation-dechlorination that is used for, carrier active carbon adopts granular active carbon, and the particle diameter of granular active carbon is 3～5mm.
Produce HFC-125 Preparation of catalysts method at above-mentioned a kind of CFC-115 hydrogenation-dechlorination that is used for, pre-infiltrate adopts a kind of in hydrochloric acid, the ethylene glycol.
Produce HFC-125 Preparation of catalysts method at above-mentioned a kind of CFC-115 hydrogenation-dechlorination that is used for, a kind of in the complex compound, organic palladium of halide, acetate, nitrate, the acid of chlorine palladium, the palladium ammonia of Pd adopted in the Pd source, and palladium bichloride (PdCl is adopted in preferred Pd source
2), palladium nitrate (Pd (NO
3)
2) in a kind of.
Produce HFC-125 Preparation of catalysts method at above-mentioned a kind of CFC-115 hydrogenation-dechlorination that is used for, precipitating reagent adopts a kind of in NaOH, ammoniacal liquor, sodium carbonate, the urea.
Producing HFC-125 Preparation of catalysts method at above-mentioned a kind of CFC-115 hydrogenation-dechlorination that is used for, is hydrogen reducing in the reduction mode described in this Preparation of catalysts step (6).
Produce HFC-125 Preparation of catalysts method at above-mentioned a kind of CFC-115 hydrogenation-dechlorination that is used for, the load capacity of Pd is 0.5～5.0wt% in this catalyst.
The present invention compares with the method for existing preparation Pd/C catalyst, it is simple that the present invention has preparation process, raw material can directly adopt the characteristics of finished industrial product granular active carbon, has avoided adopting Powdered Activated Carbon to prepare and has needed the shortcoming of shaping once more when catalyst uses, and has reduced production and use cost; In the present invention, Pd/C Preparation of catalysts method provided by the invention adopts infusion process, and this method method has that preparation process is simple, do not adopt organic complexing agent in the preparation process, be suitable for characteristics such as industrial mass production.
The specific embodiment
The invention will be further described below by embodiment.
Embodiment 1
(average grain diameter is about 3～5mm), specific area 1000～1700m with 10g finished particle shape
2The active carbon concentration of/g is 60 ℃ of following water-bath backflow 4h of nitric acid of 30%, uses the deionized water cyclic washing to neutral then, and is standby in 100 ℃ of following forced air drying 2h.
The preparation of Pd source maceration extract takes by weighing the PdCl about about 1g
2Solid is got the 2.43ml concentrated hydrochloric acid and is joined PdCl
2In the solid, treat that its solid dissolves the back fully and adds deionized water and be diluted in the volumetric flask of 50ml standby.
Get pretreated active carbon 2g, the hydrochloric acid that adds 10ml 0.01M soaks into active carbon 1h in advance.Load capacity according to Pd is 1wt%, pipettes PdCl
2The about 3ml of solution adds 10ml ethylene glycol, and sonic oscillation joins after 10 minutes in the active carbon that soaks in advance and floods 5h, adds the Na of 1M then
2CO
3Solution is regulated between pH value to 7～8, continues to use the distilled water filtering and washing of heat until no Cl behind the stirring dipping 2h
-Exist, then after 35 ℃ of following air dried overnight, in N
2The following 350 ℃ of roasting 2h of atmosphere get catalyst precarsor, and reaction uses catalyst at V
H2: V
N2=1:19 (overall flow rate: 20ml/min) in the atmosphere, 350 ℃ of following online reduction 3h.
Embodiment 2～5
Changing nitric acid pretreatment concentration preliminary treatment active carbon, adopt salpeter solution (5%～67%) active carbon after 60 ℃ of following water-bath backflow 4h obtain preliminary treatment of variable concentrations, is the preparing carriers catalyst with it.Catalyst preparation step is with embodiment 1.
Embodiment 6～9
Changing nitric acid pretreatment temperature preliminary treatment active carbon, adopt salpeter solution active carbon after water-bath backflow 4h obtains preliminary treatment under the different temperature (60 ℃～100 ℃) of 47% concentration, is the preparing carriers catalyst with it.Catalyst preparation step is with embodiment 1.
Embodiment 10
(average grain diameter is about 3～5mm), specific area 1000～1700m with 10g finished particle shape
2The active carbon concentration of/g is 60 ℃ of following water-bath backflow 4h of nitric acid of 20%, uses the deionized water cyclic washing to neutral then, and is standby in 100 ℃ of following forced air drying 2h.
The preparation of Pd source maceration extract takes by weighing the Pd (NO about about 0.3g
3)
2Solid adds 10ml 67% red fuming nitric acid (RFNA), treats that its solid dissolves the back fully and adds deionized water and be diluted in the volumetric flask of 50ml standby.
Get pretreated active carbon 2g, the hydrochloric acid that adds 10ml 0.01M soaks into active carbon 1h in advance.Load capacity according to Pd is 1wt%, pipettes Pd (NO
3)
2The about 10ml of solution behind the dipping 7h, at 95 ℃ of following water bath methods, follows after 35 ℃ of following air dried overnight, in N in the active carbon that adding is soaked in advance
2The following 350 ℃ of roasting 2h of atmosphere get catalyst precarsor, and reaction uses catalyst at V
H2: V
N2=1:19 (overall flow rate: 20ml/min) in the atmosphere, 350 ℃ of following online reduction 3h.
Embodiment 11～13
Adopt different infiltrates, be respectively 0.1M NaOH, 1M NH
4OH, 0.01M EDTA soak into active carbon in advance, investigate the catalyst reaction Effect on Performance of different infiltrates to preparation.Other steps of Preparation of Catalyst are with embodiment 10.
Comparative example
Directly adopt the finished particle shaped activated carbon of buying, directly prepare catalyst as catalyst carrier without nitric acid pretreatment.Other steps of Preparation of Catalyst are with embodiment 10.
The prepared catalyst of each embodiment of table 1 and comparative example adopts contains Pd compound, carrier active carbon processing mode and the infiltrate of selecting for use.
The prepared catalyst reaction evaluation result of each embodiment of table 2 and comparative example.
The catalyst activity appreciation condition: catalyst and quartz sand (40-60 order) mix charge ratio with mass ratio 1:3: H
2: CFC-115=2:1 (volume ratio); Total air speed: 1200ml g
-1h
-1Reaction pressure: normal pressure; Reaction temperature: 380 ℃.
| CFC-115 conversion ratio/% | HFC-125 selectivity/% | Productive rate/% | |
| Embodiment 1 | 20.9 | 85.3 | 17.8 |
| Embodiment 2 | 54.8 | 87.9 | 48.2 |
| Embodiment 3 | 62.9 | 86.7 | 54.5 |
| Embodiment 4 | 52.4 | 88.0 | 46.1 |
| Embodiment 5 | 68.1 | 88.5 | 60.3 |
| Embodiment 6 | 32.5 | 90.5 | 29.4 |
| Embodiment 7 | 28.4 | 92.0 | 26.1 |
| Embodiment 8 | 16.5 | 90.1 | 14.9 |
| Embodiment 9 | 26.0 | 89.0 | 23.1 |
| Embodiment 10 | 81.2 | 76.6 | 62.2 |
| Embodiment 11 | 70.7 | 68.4 | 48.4 |
| Embodiment 12 | 72.4 | 70.4 | 51.0 |
| Embodiment 13 | 45.8 | 70.1 | 32.1 |
| Comparative example | 15.3 | 88.2 | 13.5 |
Claims (8)
1, a kind of CFC-115 hydrogenation-dechlorination that is used for is produced HFC-125 Preparation of catalysts method, it is characterized in that this catalyst is carrier with the active carbon, load active component Pd, and this Preparation of catalysts step is as follows:
(1) carrier active carbon is put into pickle, water-bath backflow pickling preliminary treatment 4～10h, pickle adopts one or more in hydrochloric acid, nitric acid or the phosphoric acid;
(2) extremely neutral through the pretreated carrier active carbon of pickling with the deionized water cyclic washing, drying for standby;
(3) the neutral carrier active carbon after the pickling preliminary treatment with drying soaks into 1～2h in advance with infiltrate;
(4) preparation Pd source maceration extract will contain the Pd compound and be mixed with Pd source maceration extract, and Pd source maceration extract is added in the infiltrate, add carrier active carbon floods 4～6h in the infiltrate that is added with Pd source maceration extract after precipitating reagent continue dipping 1-2h catalyst precarsor;
(5) catalyst precarsor is taken out from maceration extract, the taking-up mode adopt water bath method, rotary evaporation, filtration or centrifugal in a kind of;
(6) be catalyst prod after catalyst precarsor drying, roasting, the reduction.
2, a kind of CFC-115 hydrogenation-dechlorination that is used for according to claim 1 is produced HFC-125 Preparation of catalysts method, it is characterized in that carrier active carbon adopts granular active carbon.
3, a kind of CFC-115 hydrogenation-dechlorination that is used for according to claim 1 is produced HFC-125 Preparation of catalysts method, it is characterized in that pre-infiltrate adopts a kind of in hydrochloric acid, the ethylene glycol.
4, a kind of CFC-115 hydrogenation-dechlorination that is used for according to claim 1 is produced HFC-125 Preparation of catalysts method, it is characterized in that the Pd source adopts a kind of in the complex compound of the halide of Pd, acetate, nitrate, the acid of chlorine palladium, palladium ammonia, the organic palladium.
5, a kind of CFC-115 hydrogenation-dechlorination that is used for according to claim 4 is produced HFC-125 Preparation of catalysts method, it is characterized in that the Pd source adopts a kind of in palladium bichloride, the palladium nitrate.
6, a kind of CFC-115 hydrogenation-dechlorination that is used for according to claim 1 is produced HFC-125 Preparation of catalysts method, it is characterized in that precipitating reagent adopts a kind of in NaOH, ammoniacal liquor, sodium carbonate, the urea.
7, a kind of CFC-115 hydrogenation-dechlorination that is used for according to claim 1 is produced HFC-125 Preparation of catalysts method, it is characterized in that in the reduction mode described in this Preparation of catalysts step (6) be hydrogen reducing.
8, a kind of CFC-115 hydrogenation-dechlorination that is used for according to claim 1 is produced HFC-125 Preparation of catalysts method, and the load capacity that it is characterized in that Pd in the catalyst is 0.5～5.0wt%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745409B (en) * | 2010-01-21 | 2012-06-27 | 浙江师范大学 | Preparation and application of catalytic agent used for directionally converting CFC-115 into HFC-125 by hydrogenation and dechlorination |
| CN103691430A (en) * | 2012-09-28 | 2014-04-02 | 中化蓝天集团有限公司 | Catalyst for tetrafluorodichloroethane hydrodechlorination and preparation method thereof |
| CN104014335A (en) * | 2013-03-01 | 2014-09-03 | 中化蓝天集团有限公司 | Catalyst for preparing methyl fluoride by hydrogenating and dechlorinating dichloromonofluoromethane, and preparation method and application of catalyst |
| CN104588003A (en) * | 2014-12-24 | 2015-05-06 | 中国科学院青岛生物能源与过程研究所 | Heterogeneous metal catalyst and application thereof in preparation of isobutyl alcohol from methanol and alcohol aqueous solution |
| CN105688952A (en) * | 2016-03-17 | 2016-06-22 | 中国天辰工程有限公司 | Hydrodechlorination palladium-carbon catalyst and preparation method |
| CN106693961A (en) * | 2017-01-10 | 2017-05-24 | 江西省汉氏贵金属有限公司 | Palladium-carbon catalyst and preparation method and application thereof |
| CN106693960A (en) * | 2016-11-16 | 2017-05-24 | 北京工业大学 | Supported palladium catalyst for synthesizing 1,4-cyclohexanedicarboxylic acid |
| CN109046342A (en) * | 2018-07-13 | 2018-12-21 | 南京卡邦科技有限公司 | A kind of preparation method of nanocatalyst |
| CN109513452A (en) * | 2018-11-29 | 2019-03-26 | 东莞东阳光科研发有限公司 | Film catalyst, its presoma and carrier and preparation method thereof |
-
2009
- 2009-05-06 CN CN200910098452A patent/CN101543779A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101745409B (en) * | 2010-01-21 | 2012-06-27 | 浙江师范大学 | Preparation and application of catalytic agent used for directionally converting CFC-115 into HFC-125 by hydrogenation and dechlorination |
| CN103691430A (en) * | 2012-09-28 | 2014-04-02 | 中化蓝天集团有限公司 | Catalyst for tetrafluorodichloroethane hydrodechlorination and preparation method thereof |
| CN104014335A (en) * | 2013-03-01 | 2014-09-03 | 中化蓝天集团有限公司 | Catalyst for preparing methyl fluoride by hydrogenating and dechlorinating dichloromonofluoromethane, and preparation method and application of catalyst |
| CN104014335B (en) * | 2013-03-01 | 2017-07-07 | 中化蓝天集团有限公司 | Catalyst, its preparation method and the application of a fluoromethane are prepared for monofluorodichloromethane hydrogenation-dechlorination |
| CN104588003A (en) * | 2014-12-24 | 2015-05-06 | 中国科学院青岛生物能源与过程研究所 | Heterogeneous metal catalyst and application thereof in preparation of isobutyl alcohol from methanol and alcohol aqueous solution |
| CN105688952A (en) * | 2016-03-17 | 2016-06-22 | 中国天辰工程有限公司 | Hydrodechlorination palladium-carbon catalyst and preparation method |
| CN106693960A (en) * | 2016-11-16 | 2017-05-24 | 北京工业大学 | Supported palladium catalyst for synthesizing 1,4-cyclohexanedicarboxylic acid |
| CN106693961A (en) * | 2017-01-10 | 2017-05-24 | 江西省汉氏贵金属有限公司 | Palladium-carbon catalyst and preparation method and application thereof |
| CN109046342A (en) * | 2018-07-13 | 2018-12-21 | 南京卡邦科技有限公司 | A kind of preparation method of nanocatalyst |
| CN109513452A (en) * | 2018-11-29 | 2019-03-26 | 东莞东阳光科研发有限公司 | Film catalyst, its presoma and carrier and preparation method thereof |
| CN109513452B (en) * | 2018-11-29 | 2019-10-18 | 东莞东阳光科研发有限公司 | Film catalyst, its presoma and carrier and preparation method thereof |
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