CN106111184A - A kind of isodecanol catalyst for preparing and preparation method thereof - Google Patents
A kind of isodecanol catalyst for preparing and preparation method thereof Download PDFInfo
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- CN106111184A CN106111184A CN201610471393.3A CN201610471393A CN106111184A CN 106111184 A CN106111184 A CN 106111184A CN 201610471393 A CN201610471393 A CN 201610471393A CN 106111184 A CN106111184 A CN 106111184A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 33
- PLLBRTOLHQQAQQ-UHFFFAOYSA-N 8-methylnonan-1-ol Chemical compound CC(C)CCCCCCCO PLLBRTOLHQQAQQ-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002808 molecular sieve Substances 0.000 claims abstract description 39
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 39
- MWKFXSUHUHTGQN-UHFFFAOYSA-N decan-1-ol Chemical compound CCCCCCCCCCO MWKFXSUHUHTGQN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002253 acid Substances 0.000 claims abstract description 20
- 239000011148 porous material Substances 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011959 amorphous silica alumina Substances 0.000 claims abstract description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 7
- 239000006229 carbon black Substances 0.000 claims abstract description 7
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 7
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 7
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 7
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001950 potassium oxide Inorganic materials 0.000 claims abstract description 7
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 7
- 229910000428 cobalt oxide Inorganic materials 0.000 claims abstract description 6
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims abstract description 6
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 6
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 4
- 239000012018 catalyst precursor Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910021536 Zeolite Inorganic materials 0.000 claims description 7
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 7
- 238000005984 hydrogenation reaction Methods 0.000 claims description 7
- 239000010457 zeolite Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 3
- 238000000678 plasma activation Methods 0.000 claims description 3
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- MMFCJPPRCYDLLZ-CMDGGOBGSA-N (2E)-dec-2-enal Chemical compound CCCCCCC\C=C\C=O MMFCJPPRCYDLLZ-CMDGGOBGSA-N 0.000 abstract description 6
- MMFCJPPRCYDLLZ-UHFFFAOYSA-N dec-2-enal Natural products CCCCCCCC=CC=O MMFCJPPRCYDLLZ-UHFFFAOYSA-N 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 239000007789 gas Substances 0.000 description 10
- 239000004115 Sodium Silicate Substances 0.000 description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 9
- 229910052911 sodium silicate Inorganic materials 0.000 description 9
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 6
- 229910001388 sodium aluminate Inorganic materials 0.000 description 6
- 239000012065 filter cake Substances 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000010009 beating Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- QMVPMAAFGQKVCJ-UHFFFAOYSA-N citronellol Chemical compound OCCC(C)CCC=C(C)C QMVPMAAFGQKVCJ-UHFFFAOYSA-N 0.000 description 2
- KSMVZQYAVGTKIV-UHFFFAOYSA-N decanal Chemical compound CCCCCCCCCC=O KSMVZQYAVGTKIV-UHFFFAOYSA-N 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QMVPMAAFGQKVCJ-SNVBAGLBSA-N (R)-(+)-citronellol Natural products OCC[C@H](C)CCC=C(C)C QMVPMAAFGQKVCJ-SNVBAGLBSA-N 0.000 description 1
- 239000005968 1-Decanol Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 235000015164 Iris germanica var. florentina Nutrition 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- JGQFVRIQXUFPAH-UHFFFAOYSA-N beta-citronellol Natural products OCCC(C)CCCC(C)=C JGQFVRIQXUFPAH-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000000484 citronellol Nutrition 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 244000023249 iris florentino Species 0.000 description 1
- -1 isodecyl Chemical group 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
- B01J23/8885—Tungsten containing also molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
- B01J27/13—Platinum group metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/80—Mixtures of different zeolites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/82—Phosphates
- B01J29/84—Aluminophosphates containing other elements, e.g. metals, boron
- B01J29/85—Silicoaluminophosphates [SAPO compounds]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/63—Pore volume
- B01J35/635—0.5-1.0 ml/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
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Abstract
The invention discloses a kind of decanol catalyst for preparing and preparation method thereof, be made up of the material of following weight portion: molybdenum oxide 5 parts, cobalt oxide 6 parts, tungsten oxide 3 parts, nickel oxide 3 parts, potassium oxide 4 parts, six ammonium chloropalladates 8 parts, white carbon black 3 parts, Pulvis Talci 6 parts, 8 parts of molecular sieve, amorphous silica-alumina 10 parts.The present invention uses the catalyst of technique scheme, selectivity is high, run 5000 hours continuously, still keep higher activity and stability, decenal conversion ratio can be made to reach 99.9%, and isodecanol selectivity, up to 99.9%, prepares the purity of isodecanol up to 99.9%, the catalyst pore volume of the present invention is 1mL/g, and specific surface area is 500m2/ g, the pore volume shared by hole of bore dia ＜ 3nm accounts for less than the 25% of total pore volume, and pore volume shared by the hole of bore dia ＞ 15nm accounts for more than the 25% of total pore volume, meleic acid amount 0.220 0.520mmol/g.
Description
Technical field
The present invention relates to technical field of chemical synthesis, particularly relate to a kind of isodecanol catalyst for preparing and
Preparation method.
Background technology
Decanol has another name called Decanol/decanol/1-decanol/ten carbon alcohol/nonyl carbinol, has and has that wax is fragrant, fragrant and sweet, the fragrance of a flower, fruital
Colourless transparent liquid as fragrance, with the blended liquid phase of citronellol orrisroot oil.Close for making artificial Oleum Rosae Rugosae, orange blossom type and gold
Joyous type essence etc..It is also used for lube oil additive processed, plasticizer, adhesive etc..
Patent publication No. is that the patent of invention of CN101185893A proposes a kind of for decenal gas phase hydrogenation isodecyl
Catalyst of alcohol and preparation method thereof, catalyst uses coprecipitation to prepare, and containing copper oxide, zinc oxide, aluminium oxide, activity helps
Agent, for decenal gas phase hydrogenation isodecanol, has higher decenal conversion ratio and isodecanol selectivity.
At present, there is contradiction in the activity and selectivity of liquid phase hydrogenating catalyst, and particularly selectivity is difficult to maintain normally
Level, by-product is many, brings problem to production, and in order to make product qualified, needs to expend a large amount of steam and carry out magazins' layout.
For capraldehyde Hydrogenation for the reaction of decanol, need that there is high activity and the selective hydrogenation catalyst of height simultaneously.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of selectivity high for the deficiencies in the prior art, runs continuously
5000 hours, still keeping higher activity and stability, granule is little, surface area is big, and decenal conversion ratio can be made to reach 99.9%, different
Decanol selectivity, up to 99.9%, prepares the purity of the isodecanol isodecanol catalyst for preparing up to 99.9%.
Present invention also offers the preparation method of a kind of above-mentioned catalyst, the method technique is simple, and by-product is few, without dirty
Dye, production cost is low, and the safety of technique is high.
The present invention is by the following technical solutions: a kind of decanol catalyst for preparing, is made up of the material of following weight portion: oxygen
Change molybdenum 5 parts, cobalt oxide 6 parts, tungsten oxide 3 parts, nickel oxide 3 parts, potassium oxide 4 parts, six ammonium chloropalladates 8 parts, white carbon black 3 parts, Talcum
6 parts of powder, 8 parts of molecular sieve, amorphous silica-alumina 10 parts.
The following is further improvement of the present invention:
Described molecular sieve is Y type molecular sieve, β zeolite, ZSM-2 molecular sieve and the mixture of SAPO-11 molecular sieve；
The mass ratio of Y type molecular sieve, β zeolite, ZSM-5 molecular sieve and SAPO-11 molecular sieve is 5:3:2:1.
Improve further:
The relative crystallinity of described SAPO-11 molecular sieve is 98%, and crystal particle diameter is 2.5 μm.
Improve further:
The relative crystallinity 95%～110% of described Y type molecular sieve, crystal particle diameter is 1.8 μm.
Improve further:
Described amorphous silica-alumina comprises silicon oxide 8wt%-50wt%, and specific surface area is 700-800m2/ g, pore volume is 1.6-
1.8ml/g, bore dia 8-15nm, shared pore volume accounts for the 95%-98% of total pore volume, and infrared total acid content is 0.30-
0.45mmol/g, middle strong acid amount/infrared total acid content is 0.56-0.81, and L acid amount/B acid amount is 1.40-2.30.
The preparation method of a kind of isodecanol catalyst for preparing, comprises the steps:
1), by above-mentioned molybdenum oxide 5 parts, cobalt oxide 6 parts, tungsten oxide 3 parts, nickel oxide 3 parts, potassium oxide 4 parts, six ammonium chloropalladates 8
Part, white carbon black 3 parts, Pulvis Talci 6 parts, 8 parts of molecular sieve, 10 parts of mix homogeneously of amorphous silica-alumina, compressing, obtain complex catalyst precursor
Body；
2), adding in plasma daughter generator by catalyst precursor in step 1, the power adjusting plasma generator is
Carry out plasma-activated during 50-1000W, and plasma activation time is 3-40min, prepare catalyst.
Improve further:
Step 2) in, the cavity of plasma generator is metallic cavity or glass chamber；Exciting electrode is low frequency electrode, penetrates
Frequently electrode or microwave electrodes.
Improve further:
Step 2) in, when described catalyst precursor is inserted described plasma generator, first by hydrogenation catalyst equably
It is placed in the container that electric conductivity is good, container is placed in plasma generator, opens vacuum pump, send out at plasma
The vacuum of 10-50Pa is formed in the vacuum cavity of raw device.
Improve further:
Step 2) in, the exciting electrode of described plasma generator is radio-frequency electrode, and radio-frequency electrode power is 60-100W.
The present invention uses the catalyst of technique scheme, and selectivity is high, runs 5000 hours continuously, still keeps higher
Activity and stability, decenal conversion ratio can be made to reach 99.9%, isodecanol selectivity, up to 99.9%, prepares the purity of isodecanol
Up to 99.9%, the catalyst pore volume of the present invention is 1mL/g, and specific surface area is 500m2/ g, shared by the hole of bore dia ＜ 3nm
Pore volume account for less than the 25% of total pore volume, pore volume shared by the hole of bore dia ＞ 15nm accounts for more than the 25% of total pore volume, meleic acid
Amount 0.220-0.520mmol/g.
The present invention uses above-mentioned preparation method, and technique is simple, and by-product is few, pollution-free, and production cost is low, the safety of technique
Property high.
Detailed description of the invention
Embodiment, a kind of decanol catalyst for preparing, it is made up of the material of following weight portion: molybdenum oxide 5 parts, cobalt oxide 6
Part, tungsten oxide 3 parts, nickel oxide 3 parts, potassium oxide 4 parts, six ammonium chloropalladates 8 parts, white carbon black 3 parts, Pulvis Talci 6 parts, 8 parts of molecular sieve,
Amorphous silica-alumina 10 parts.
Described molecular sieve is Y type molecular sieve, β zeolite, ZSM-2 molecular sieve and the mixture of SAPO-11 molecular sieve, Y
The mass ratio of type molecular sieve, β zeolite, ZSM-5 molecular sieve and SAPO-11 molecular sieve is 5:3:2:1.
The relative crystallinity of described SAPO-11 molecular sieve is 98%, and crystal particle diameter is 2.5 μm.
The relative crystallinity 95%～110% of described Y type molecular sieve, crystal particle diameter is 1.8 μm.
Described amorphous silica-alumina comprises silicon oxide 8wt%-50wt%, and specific surface area is 700-800m2/ g, pore volume is
1.6-1.8ml/g, bore dia 8-15nm, shared pore volume accounts for the 95%-98% of total pore volume, and infrared total acid content is 0.30-
0.45mmol/g, middle strong acid amount/infrared total acid content is 0.56-0.81, and L acid amount/B acid amount is 1.40-2.30.
The preparation method of amorphous silica-alumina described above is as follows:
A, respectively preparation sodium aluminate solution and sodium silicate solution；
B, by sodium aluminate solution adds part or all of sodium silicate solution, then pass to CO2Gas, controlling reaction temperature is
10-40 DEG C, the pH value controlling cemented into bundles is 8-11；Wherein as the CO being passed through2 Gas flow accounts for the 40% of total intake
～100%, add excess silicon acid sodium solution；
C, at the control temperature and pH value of step b, the mixture of step b gained ventilates and stablizes 40-60 minute；
D, the solidliquid mixture of step c gained is filtered, Cake Wash；
E, the filter cake of step d gained is pulled an oar, then carry out hydrothermal treatment consists, through filtering, being dried, obtain amorphous silica-alumina；Institute
The hydrothermal conditions stated is as follows: at 120-150 DEG C, processes 2-5 hour under 0.5-4.0MPa water vapor pressure.
In step b, as the CO being passed through2When gas flow accounts for the 50%-80% of total intake, add surplus
Remaining sodium silicate solution.
In described step a, the concentration of sodium aluminate solution is 15-55g Al2O3/ l, sodium silicate solution dense
Degree is 50-200g SiO2/l。
Step b adds all or part of sodium silicate solution, is whole sodium silicate solutions of being added
5wt%-100wt%.
Described CO2The concentration of gas is 30v%-60v%.
The detailed process employing following methods of step b:
(1), in sodium aluminate, add whole sodium silicate after, be passed through CO2Gas；
(2), in sodium aluminate, after addition part sodium silicate, it is passed through whole CO2Gas, then adds excess silicon in mixture
Acid sodium solution；
(3), in sodium aluminate, after addition part sodium silicate, it is passed through part CO2Gas, more logical CO2Gas is while adding
Enter excess silicon acid sodium solution.
Washing described in step d is that 50-90 DEG C of deionized water of filter cake is washed till neutrality.
Making beating described in step e is to be 8:1-10:1 by solid-liquid volume ratio, and add water in filter cake making beating.
Drying condition described in step e is as follows: dry 6-8 hour at 110-130 DEG C.
The preparation method of above-mentioned Y type molecular sieve includes following process: fresh NaY Crystallization of Zeolite serosity is filtering
Rinsing molecular sieve filter cake with the alkali liquor of molecular sieve butt quality 4-6 times during separation, concentration of lye is 0.001-0.5mol/L, alkali
Liquid temp is 30-90 DEG C；Then above-mentioned NaY molecular sieve filter cake is pulled an oar, adds the compound solution containing H+ ion,
The pH value making NaY molecular sieve pulp is maintained at 2.5-7.0, and reaction temperature is 5-100 DEG C, exchange reaction 0.2-6
Hour, swap with the sodium in zeolite with H+, after H+ exchange, have filtration, washing, roasting process.
The preparation method of a kind of isodecanol catalyst for preparing, comprises the steps:
1), by above-mentioned molybdenum oxide 5 parts, cobalt oxide 6 parts, tungsten oxide 3 parts, nickel oxide 3 parts, potassium oxide 4 parts, six ammonium chloropalladates 8
Part, white carbon black 3 parts, Pulvis Talci 6 parts, 8 parts of molecular sieve, 10 parts of mix homogeneously of amorphous silica-alumina, compressing, obtain complex catalyst precursor
Body；
2), adding in plasma daughter generator by catalyst precursor in step 1, the power adjusting plasma generator is
Carry out plasma-activated during 50-1000W, and plasma activation time is 3～40min, prepare catalyst.
Step 2) cavity of plasma generator is metallic cavity or glass chamber；Exciting electrode is low-frequency electrical
Pole, radio-frequency electrode or microwave electrodes；
Step 2) in, when described catalyst precursor is inserted described plasma generator, first that hydrogenation catalyst is uniform
Be placed in the container that electric conductivity is good, container is placed in plasma generator, opens vacuum pump, at plasma
The vacuum of 10-50Pa is formed in the vacuum cavity of generator；
Step 2) described in the exciting electrode of plasma generator be radio-frequency electrode, radio-frequency electrode power is 60-100W.
Claims (9)
1. a decanol catalyst for preparing, it is characterised in that: it is made up of the material of following weight portion: molybdenum oxide 5 parts, oxidation
Cobalt 6 parts, tungsten oxide 3 parts, nickel oxide 3 parts, potassium oxide 4 parts, six ammonium chloropalladates 8 parts, white carbon black 3 parts, Pulvis Talci 6 parts, molecular sieve 8
Part, amorphous silica-alumina 10 parts.
Decanol catalyst for preparing the most according to claim 1, it is characterised in that: described molecular sieve is Y type molecular sieve, β
Zeolite, ZSM-2 molecular sieve and the mixture of SAPO-11 molecular sieve；
The mass ratio of Y type molecular sieve, β zeolite, ZSM-5 molecular sieve and SAPO-11 molecular sieve is 5:3:2:1.
Decanol catalyst for preparing the most according to claim 2, it is characterised in that: described SAPO-11 molecular sieve relative
Degree of crystallinity is 98%, and crystal particle diameter is 2.5 μm.
Decanol catalyst for preparing the most according to claim 2, it is characterised in that: the relative crystallization of described Y type molecular sieve
Degree 95%～110%, crystal particle diameter is 1.8 μm.
Decanol catalyst for preparing the most according to claim 2, it is characterised in that: described amorphous silica-alumina comprises silicon oxide
8wt%-50wt%, specific surface area is 700-800m2/ g, pore volume is 1.6-1.8ml/g, bore dia 8-15nm, shared hole
Holding the 95%-98% accounting for total pore volume, infrared total acid content is 0.30-0.45mmol/g, and middle strong acid amount/infrared total acid content is
0.56-0.81, L acid amount/B acid amount is 1.40-2.30.
6. the preparation method of an isodecanol catalyst for preparing, it is characterised in that: comprise the steps:
1), by above-mentioned molybdenum oxide 5 parts, cobalt oxide 6 parts, tungsten oxide 3 parts, nickel oxide 3 parts, potassium oxide 4 parts, six ammonium chloropalladates 8
Part, white carbon black 3 parts, Pulvis Talci 6 parts, 8 parts of molecular sieve, 10 parts of mix homogeneously of amorphous silica-alumina, compressing, obtain complex catalyst precursor
Body；
2), adding in plasma generator by catalyst precursor in step 1, the power adjusting plasma generator is
Carry out plasma-activated during 50-1000W, and plasma activation time is 3-40min, prepare catalyst.
7. according to claim 6 the preparation method of isodecanol catalyst for preparing, it is characterised in that: step 2) in, wait from
The cavity of daughter generator is metallic cavity or glass chamber；Exciting electrode is low frequency electrode, radio-frequency electrode or microwave electrodes.
8. according to claim 6 the preparation method of isodecanol catalyst for preparing, it is characterised in that: step 2) in, will
When described catalyst precursor inserts described plasma generator, first hydrogenation catalyst is evenly placed upon electric conductivity good
Container in, container is placed in plasma generator, opens vacuum pump, in the vacuum cavity of plasma generator
Form the vacuum of 10-50Pa.
9. according to claim 6 the preparation method of isodecanol catalyst for preparing, it is characterised in that: step 2) in, described
The exciting electrode of plasma generator is radio-frequency electrode, and radio-frequency electrode power is 60-100W.
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