CN104857972B - It is a kind of by synthesis gas coproduction low-carbon alcohols and the catalyst and preparation method of liquid fuel - Google Patents
It is a kind of by synthesis gas coproduction low-carbon alcohols and the catalyst and preparation method of liquid fuel Download PDFInfo
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- CN104857972B CN104857972B CN201510192652.4A CN201510192652A CN104857972B CN 104857972 B CN104857972 B CN 104857972B CN 201510192652 A CN201510192652 A CN 201510192652A CN 104857972 B CN104857972 B CN 104857972B
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Abstract
It is a kind of by synthesis gas coproduction low-carbon alcohols and the catalyst and preparation method of liquid fuel, it belongs to one-carbon chemical and technical field of coal chemical industry.The catalyst is CuCoRhM/SiO2, is Co, Cu, Rh, M1, M2 catalyst of SiO2 loads.M1 be Mn, Zr, Zn one kind or two kinds, M2 is alkali metal Li, Na, K and alkaline-earth metal Mg, Ca, Sr, Ba one or more.The molar percentage composition of the catalyst is Cu：1~20%, Co：1~20%, Rh：0.01~2%, M1：0.5~8%, SiO2：50~80%, M2：0.1~5%.The catalyst is used for synthesis gas coproduction low-carbon alcohols and liquid hydrocarbon, and high catalytic efficiency, liquid hydrocarbon and low-carbon alcohols separation are easy, preferably solves the problems, such as that existing formate low-carbon alcohol catalyst efficiency is not high enough and selectivity is not good enough, can significantly improve the economy of building-up process.
Description
Technical field
The present invention relates to a kind of by synthesis gas coproduction low-carbon alcohols and the catalyst and preparation method of liquid fuel, it belongs to one
Carbon geochemistry and technical field of coal chemical industry.
Technical background
The energy resource structure feature in China is " rich coal, oil starvation, few gas ", and wherein coal accounts for 97.7%, and oil 1.6%, natural gas is only
Have 1.7%.Oil and natural gas proportion is high well below world average level, crude oil import interdependency.The coal system of research and development
Low-carbon alcohols and oily catalyst technology are in short supply to alleviation China's oil source, depend on import unduly and improve energy security, have weight
Want meaning.Low carbon mixed alcohol is high-quality vehicle fuel, has more preferable combustibility with the compound that oil product is mixed to prepare, is
Gasoline carries high-octane good additive, can be as being important industrial chemicals after separation.
At present, main three developing direction of coal liquifaction are：F- T synthesis, coal low-carbon alcohols, coproduction low-carbon alcohols and liquid
Fuel.Wherein, single artificial oil and the space-time yield of low-carbon alcohols are relatively low, and the space-time of coproduction low-carbon alcohols and liquid fuel technology
Yield is 0.4~0.6g/h.ml, and production efficiency greatly improves, and set of device can complete F- T synthesis and higher alcohols synthesis simultaneously,
As the prior development direction of coal clean fuel.It is to develop this skill to research and develop high performance catalyst and corresponding technique
The key of art.
The content of the invention
One kind is provided by coproduction low-carbon alcohols and liquid fuel catalyst to solve the problems of the prior art present invention
And preparation method thereof.
The technical scheme is that：It is a kind of by synthesis gas coproduction low-carbon alcohols and the catalyst of liquid fuel, the catalyst
By SiO2Cu, Co, Rh, M1, M2 catalyst of load；M1 is Mn, Zr, Zn one or two, and M2 is alkali metal Li, Na, K
With alkaline-earth metal Mg, Ca, Sr, Ba one or two；The molar content of each component is Cu in catalyst：1~20%, Co：
1~20%, Rh：0.01~2%, M1：0.5~8%, SiO2：50~80%, M2：0.1~5%.
Further, the catalyst has by SiO2Cu, Co, Rh, Mn, Li catalyst of load；Each component rubs in catalyst
Your percentage composition is Cu：1~20%, Co：1~20%, Rh：0.01~2%, Mn：0.5~8%, SiO2：50~80%, Li：0.1~
5%。
Further, the catalyst has by SiO2Cu, Co, Rh, Mn, Li, Mg catalyst of load；Each component in catalyst
Molar content is Cu：1~20%, Co：1~20%, Rh：0.01~2%, Mn：0.5~8%, SiO2：50~80%, Li：0.1
~5%, Mn：0.1~5%, Li+Mn：0.1~5%.
It is a kind of by synthesis gas coproduction low-carbon alcohols and the preparation method of the catalyst of liquid fuel, comprise the following steps：
（1）Co (NO will be contained3)2·6H2O and Cu (NO3)2·3H2The O aqueous solution, it is molten to add 20% silicon under being stirred at 50 DEG C
In glue, pH value is adjusted to 6.5 with ammoniacal liquor, generates sediment, filtering, and sediment is fully washed with water；
（2）Sediment after washing is divided into dry sediment and aqueous deposit two parts, dry sediment accounts for precipitation
To 2/3rds, dry sediment is calcined 4 hours the half of thing gross mass after 120 DEG C are dried at 350 DEG C, is crushed
Afterwards with aqueous deposit kneading, extrusion, dry, be calcined at 120 DEG C of dryings, 350 DEG C 4 hours predecessor；
（3）With containing Rh salt, M1 salt, the aqueous solution of M2 salt and equi-volume impregnating dipping gained predecessor, at 120 DEG C
Grinding screen takes the particle of 40~60 mesh after dry 4h, obtains catalyst；The Rh salt is Rh nitrate or chloride, and M1 salt is
M1 nitrate, M2 salt are Li, Na, K carbonate, bicarbonate, nitrate or Mg, Ca, Sr, Ba nitrate, formates.
It is a kind of by synthesis gas coproduction low-carbon alcohols and the preparation method of the catalyst of liquid fuel, comprise the following steps：
（1）With containing Co (NO3)2.6H2O、Cu(NO3)2.3H2O, the aqueous solution of M1 salt and M2 salt, equi-volume impregnating leaching
The gross porosity SiO of the mesh of stain 40~602, after 120 DEG C are dried, it is calcined 6h at 350 DEG C and obtains predecessor；
（2）With salt containing Rh, M1 salt, M2 salt the aqueous solution, equi-volume impregnating dipping gained predecessor, 120 DEG C of dryings
4h, catalyst is made；
The Rh salt is Rh nitrate or chloride, and M1 salt is M1 nitrate, the leaching of alkali metal Li, Na, K in M2
Stain thing is hydroxide, carbonate, bicarbonate, and alkaline-earth metal Mg, Ca, Sr, Ba salt are solvable for nitrate and formates etc.
Property salt.Described SiO2 sources are common silica gel or Ludox.
Beneficial effects of the present invention：The catalyst is CuCoRhM/SiO2, is that Co, Cu, Rh, M1, M2 of SiO2 loads are urged
Agent.M1 be Mn, Zr, Zn one kind or two kinds, M2 be alkali metal Li, Na, K and alkaline-earth metal Mg, Ca, Sr, Ba one kind or
It is a variety of.The molar percentage composition of the catalyst is Cu：1~20%, Co：1~20%, Rh：0.01~2%, M1：0.5~8%,
SiO2：50~80%, M2：0.1~5%.The catalyst is used for synthesis gas coproduction low-carbon alcohols and liquid hydrocarbon, high catalytic efficiency, liquid
Hydrocarbon and low-carbon alcohols separation are easy, preferably solve that existing formate low-carbon alcohol catalyst efficiency is not high enough and selectivity is not good enough asks
Topic, it can significantly improve the economy of building-up process.
Embodiment
With reference to embodiment, the present invention will be further described, and the present invention includes but is not limited to the following examples.
Embodiment 1
Containing 178 g Co (NO3)2.6H2O and 48.3 g Cu (NO3)23H2O 1 aqueous solution, at 50 DEG C and stir
Under be added in the Ludox of 600 g 20%, adjust pH value to 6.5 with 25% ammoniacal liquor.The precipitation of generation is filtered, fully washed with water
Wash, take out 2/3rds of sediment, dried 4 hours at 120 DEG C, be calcined 4 hours at 350 DEG C, be ground into tiny powder,
Mediated with together with undried precipitation, extrusion, being calcined 4h after 120 DEG C are dried, at 350 DEG C is made predecessor.With containing 0.96
g RhCl3.2H2O、0.60 g Mn(NO3)2.4H2O and 0.93 g LiNO3The aqueous solution and equi-volume impregnating dipping gained
Predecessor, after 120 DEG C are dried, grinding screen takes the particle of 40~60 mesh, and catalyst 1 is made.
Embodiment 2
(the NO of Co containing 178g3)2.6H2O and 48.3 g Cu (NO3)23H2O 1 aqueous solution, under 50 DEG C of stirrings
It is added in the Ludox of 600 g 20%, pH value is adjusted to 6.5 with 25% ammoniacal liquor.The precipitation of generation is filtered, fully washed with water,
7/10ths of precipitation are taken out, is dried at 120 DEG C after being calcined 4 hours at 350 DEG C, is ground into tiny powder, it is and unseasoned
Sediment mediate, extrusion, 120 DEG C dry after at 350 DEG C be calcined 4h be made predecessor.With containing 0.72 g
RhCl3.nH2O、0.43 g Mn(NO3)2.4H2O and 0.62 gLiNO3The aqueous solution and equi-volume impregnating dipping gained before
Thing is driven, the broken Sieve of powder takes the particle of 40~60 mesh after 120 DEG C of dry 4h, and catalyst 2 is made.
Embodiment 3
Containing 232 g Co (NO3)2.6H2O and 48.3 g Cu (NO3)2·3H2O 1 aqueous solution, under 50 DEG C of stirrings
Add in 20% Ludox 600g, pH value is adjusted to 6.5 with 25% ammoniacal liquor.The sediment of generation filters out, and is fully washed with water.Take out
3/5ths of precipitation, after 120 DEG C are dried, it is calcined 4 hours at 350 DEG C, is ground into tiny powder, it is and remaining aqueous
Sediment kneading, extrusion, dry, predecessor is calcined 4 hours to obtain at 120 DEG C of dryings, 350 DEG C.With containing 1.03 g Rh
(NO3)3.2H2O、0.64 g Mn(NO3)2.4H2O、1.00 g LiNO3The aqueous solution and equi-volume impregnating dipping gained before
Thing is driven, the broken Sieve of powder takes the particle of 40~60 mesh after 120 DEG C of dry 4h, obtains catalyst 3.
Embodiment 4
With containing 78.6g Co (NO3)2.6H2O and 22.81 g Cu (NO3)2.3H2O、2g Mg(NO3)2.6H2The O aqueous solution
With the gross porosity SiO of the equi-volume impregnating dipping mesh of 120 g 40~602, after 120 DEG C are dried, 6h predecessors are calcined at 350 DEG C.
With containing 0.55g RhCl3.2H2O、0.30 g Mn(NO3)2With 0.57 g LiNO3The aqueous solution dipping gained predecessor,
Catalyst 4 is made in 120 DEG C of dry 4h.
Embodiment 5
With containing 78.7 g Co (NO3)2.6H2O、22.8 g Cu(NO3)2.3H2O 0.6 g LiNO3With 2g Mg
(NO3)2.6H2The gross porosity SiO of the O aqueous solution and equi-volume impregnating the dipping mesh of 120g 40~602, after 120 DEG C are dried,
350 DEG C of roasting 6h obtain predecessor.With RhCl containing 0.55g3.2H2O、0.30 g Mn(NO3)2·4H2O and 0.57 g LiNO3's
Catalyst 5 is made in the predecessor of the aqueous solution and equi-volume impregnating dipping gained, 120 DEG C of dry 4h.
Evaluating catalyst method
Above catalyst sample is used to evaluate its reactivity and selectivity.Evaluation method：The purposes of 5ml 40~60 are taken to urge
Agent sample, dilute (volume ratio 1 with quartz sand：1).Use 10%H2/N2Gaseous mixture reduces 6 hours at 400 DEG C, and reaction condition is：
250 DEG C, pressure 5MPa, air speed 5000h of temperature-1.Unstripped gas forms H2：CO2=2：1.
Table 1
With the catalyst coproduction low-carbon alcohols and liquid-fuel oil of the present invention, there is higher catalytic efficiency, can obtain preferably
Economic benefit.
Claims (3)
- It is 1. a kind of by synthesis gas coproduction low-carbon alcohols and the catalyst of liquid fuel, it is characterised in that：The catalyst is by SiO2Load Cu, Co, Rh, M1, M2 catalyst, wherein M1 be Mn, Zr, Zn one kind or two kinds, M2 is Li, Na, K, Mg, Ca, Sr, Ba It is one or two kinds of；The molar percentage composition of the catalyst is Cu：1~20%, Co：1~20%, Rh：0.01~2%, M1：0.5~ 8%, SiO2：50~80%, M2：0.1~5%.
- 2. it is according to claim 1 a kind of by synthesis gas coproduction low-carbon alcohols and the preparation method of the catalyst of liquid fuel, It is characterised in that it includes following steps：（1）Co (NO will be contained3)2·6H2O and Cu (NO3)2·3H2The O aqueous solution, 20% Ludox is added under 50 DEG C of stirrings In, pH value is adjusted to 6.5 with 25% ammoniacal liquor, generates sediment, filtering, and sediment is fully washed with water；（2）Sediment after washing is divided into two parts, for portion through being dried to dry sediment, another is moist aqueous precipitate Thing, dry sediment account for the half of sediment gross mass to 2/3rds；Dry sediment is after 120 DEG C are dried, in 350 Be calcined 4 hours at DEG C, after crushing with aqueous deposit kneading, extrusion, dry, be calcined 3-8 at 120 DEG C of dryings, 200-600 DEG C Hour obtains predecessor；（3）With containing Rh salt, M1 salt, the aqueous solution of M2 salt and equi-volume impregnating dipping gained predecessor, in 120 DEG C of dryings Grinding screen takes the particle of 40~60 mesh after 4h, obtains catalyst；The Rh salt is Rh nitrate or chloride, and M1 salt is M1's Nitrate, M2 salt are Li, Na, K carbonate, bicarbonate, nitrate or Mg, Ca, Sr, Ba nitrate, formates.
- 3. it is according to claim 1 a kind of by synthesis gas coproduction low-carbon alcohols and the preparation method of the catalyst of liquid fuel, It is characterised in that it includes following steps：（1）With containing Co (NO3)2·6H2O、Cu(NO3)2·3H2The aqueous solution of O and M2 salt, equi-volume impregnating dipping 40~60 Purpose gross porosity SiO2, after 120 DEG C are dried, it is calcined 3-8h at 200-600 DEG C and obtains predecessor；（2）With salt containing Rh, M1 salt, M2 salt the aqueous solution, equi-volume impregnating dipping gained predecessor, 120 DEG C of drys 4h, make Obtain catalyst；The Rh salt is Rh nitrate or chloride, and M1 salt is M1 nitrate, and M2 salt is Li, Na, K carbonate, carbonic acid Hydrogen salt, the nitrate of nitrate or Mg, Ca, Sr, Ba, formates.
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| CN109569652B (en) * | 2018-12-18 | 2022-04-01 | 中国科学院上海高等研究院 | Catalyst for catalytic conversion of synthesis gas and preparation method and application thereof |
| CN110898848B (en) * | 2019-08-14 | 2023-04-21 | 新奥科技发展有限公司 | Catalyst for preparing low-carbon alcohol from synthesis gas and preparation method thereof |
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| US6713591B1 (en) * | 1999-08-31 | 2004-03-30 | Nippon Steel Chemicals Co., Ltd. | Aromatic oligomer and use thereof |
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