CN104971733B - A kind of catalyst for synthesizing the enanthol of 2 propyl group 1 - Google Patents
A kind of catalyst for synthesizing the enanthol of 2 propyl group 1 Download PDFInfo
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- CN104971733B CN104971733B CN201510368524.0A CN201510368524A CN104971733B CN 104971733 B CN104971733 B CN 104971733B CN 201510368524 A CN201510368524 A CN 201510368524A CN 104971733 B CN104971733 B CN 104971733B
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Abstract
The invention discloses a kind of catalyst for synthesizing the enanthol of 2 propyl group 1, and the preparation method of the application catalyst hydrogenation preparation enanthol of 2 propyl group 1, the catalyst is using Ni, Mo, Zn, Cu as active component, combined using Hydrothermal Synthesiss and kneading method and be prepared from, use this catalyst with the heptenal Hydrogenation of 2 propyl group 2 for the enanthol of 2 propyl group 1, the heptenal conversion ratio of 2 propyl group of reactant 2 is more than 99%, and the enanthol yield of 2 propyl group of product 1 is more than 98%, purity 99%.
Description
Technical field
The present invention relates to organic synthesis field, it is related to a kind of catalyst of synthesis 2- propyl group -1-heptanol.
Background technology
2- propyl enanthols (2-PH) are the preferred raw materials of synthetic environment-friendly phthalic ester plasticizer.Plasticizer is modeling
The kind being had the call in feed additives.The maximum consumer field of plasticizer is soft PVC (PVC) product, wherein adjacent
Phthalic easter plastizer accounts for 88%.DOP (o-phthalic acid dibutyl ester) and DEHP (diisooctyl phthalate) is comprehensive
The common plasticizer of function admirable is closed, having the advantages that plasticising, performance is good, relative low price.But because safety problem, from 20
The later stage nineties in century, developed country DOP yield and consumption figure drastically decline.2004-2008 BASF AG is in Europe
Put out a new product-phthalic acid two (2- propyl group) heptyl ester (DPHP) with the U.S., be promoted and use in European ＆ American Market.DPHP's
Volatility is significantly lower than DOP, shows that DPHP can greatly improve the temperature tolerance grade of plasticising product, reduces and is led because contacting naturally
The human-body safety problem of cause.In terms of plasticizer efficiency, its tensile strength is minimum, and elongation at break is high, is in like product
In best level.DPHP has excellent cryogenic property, and its low-temperature flexibility is better than DOP, and its light, heat and colour stability might as well
In DOP.DPHP is considered as the optimal kind for substituting DOP.
2- propyl group -2- heptenals the Hydrogenation that is used for of current wide coverage is thunder Buddhist nun for the catalyst of 2- propyl group -1-heptanol
Raney nickel effect is more excellent, but the catalyst is expensive, and storage and transport have very big danger.Believe ten thousand Feng Cuihua in the village
The catalyst of the HTC NiO series of agent company can also be applied to catalysis 2- propyl group -2- heptenal hydrogenation, it was reported that 2- in product
Propyl group -1-heptanol content is 96% or so, but its raw material is 2- propyl group -1-heptanol and 2- propyl group -2- heptenal mixed feedings,
There is the problem of later separation cost is higher.
The content of the invention
The present invention synthesizes 2- for problems present in existing 2- propyl group -1-heptanol preparation process there is provided one kind
The catalyst of propyl group -1-heptanol, the catalyst is combined using Ni, Mo, Zn, Cu as active component using Hydrothermal Synthesiss and kneading method
It is prepared from, uses this catalyst with 2- propyl group -2- heptenals Hydrogenation for 2- propyl group -1-heptanol, reactant 2- propyl group -2-
Heptenal conversion ratio is more than 99%, and product 2- propyl group -1-heptanol yield is more than 98%, purity 99%.
The topmost improvement of the present invention is the provision of a kind of brand-new catalyst, and the catalyst includes active component and load
Body, wherein described carrier is γ-Al2O3, described active component is Ni, Mo, Zn, Cu oxide, such as NiO, MoO3、
ZnO, CuO form, wherein carrier account for the 20-70wt% of whole catalyst, and surplus is the metal oxide of active component, and this is urged
Agent is combined using Hydrothermal Synthesiss and kneading method to be prepared from, and is concretely comprised the following steps：
According to said components part by weight by the metal oxide precursor of active component and carrier γ-Al2O3Presoma
It is added in the heatable autoclave with stirring, wherein metal in the metal oxide precursor of active component
The weight proportion of oxide is NiO 0-60wt%, MoO30-40wt%, ZnO0-30wt%, CuO 0-30wt%,；
Backward reactor in add reactor volume 60-70% deionized water, adjusted with ammoniacal liquor or sodium hydroxide solution
The pH of section system is 6-8, then tightens autoclave spiral cover, control mixing speed and heating-up temperature (temperature is 100-180 DEG C,
Mixing speed is 100-150 revs/min), system is stirred 12 hours, it is rear to stop stirring, aging 8- is stood at 100-180 DEG C
10h, afterwards with deionized water filtration washing insoluble matter while hot, removes heteroion, the insoluble matter after washing dries 4- at 100 DEG C
6 hours；
Added after to above-mentioned drying in product after auxiliary agent, extruded moulding obtains catalyst；
Auxiliary dosage employed in it is：Nitric acid 3-4%, citric acid 2.5-3.5%, sesbania powder 3-5%, above-mentioned consumption
To account for the percentage of products weight after drying；
Specifically extrusion is：
After the product after drying is mixed with auxiliary agent according to the above ratio, on the trifolium-shaped orifice plate for being 3mm in aperture, extrusion
Shaping, then dries at room temperature, is dried 4 hours at 100-120 DEG C, is calcined 4h at 400-550 DEG C again afterwards, you can
To finished catalyst；
The auxiliary agent matched using aforementioned proportion, can play a part of bonding and reaming, so as to improve catalyst and reaction
The contact area of thing, can preferably play wherein effect of the active component in catalytic reaction；
Cost, the carrier γ-Al typically used are added and saved for convenience in preparation process2O3Presoma it is preferred
, only need to be according to γ-Al using aluminum hydroxide solid elastomer2O3Consumption convert aluminum hydroxide solid elastomer consumption.
Same reason, in above-mentioned catalyst, the active component metal oxide used is with oxide correspondence
The form of presoma add, and these presomas are selected generally from nickel nitrate, nickel sulfate, nickelous carbonate, molybdenum oxide, seven molybdic acids
One or more mixtures in ammonium, zinc nitrate, zinc sulfate, zinc carbonate, copper sulphate, copper nitrate, copper carbonate, only need to be by when using
Converted the consumption of its presoma according to the consumption of metal oxide.
After above-mentioned catalyst is obtained, inventor is further optimized with 2- propyl group -2- heptenal Hydrogenations
The processing step of standby 2- propyl group -1-heptanol, acquisition is comprised the following steps that：
1. the catalyst after roasting, is cut into 2-3mm length, 10ml is taken, the fixed bed for being loaded on 10ml is miniature anti-
Answer in device constant temperature zone, φ 3 porcelain ball, and the progress device hermeticity experiment under reaction pressure 1-6MPa loaded up and down, it is ensured that
Air-tightness is good；
2. after, determining that air-tightness is good, under 50ml/min nitrogen flow, catalyst is dried processing, 150 DEG C
Under dehydrate 2 hours；
3. hydrogen gas stream, is switched, in hydrogen-oil ratio 100:1-800:Catalyst is activated under 1 hydrogen flow rate,
Activated 24 hours at 300-500 DEG C, cool after activation, make temperature constant at 80-240 DEG C；
4., according to 0.25-2.0h-1Reaction velocity, adjusts feed pump inlet amount, and raw material is 2- propyl group -2- heptenals；Charging
Afterwards after 4h, you can obtain product 2- propyl group -1-heptanol.
Reaction result shows that reactant 2- propyl group -2- heptenals conversion ratio is more than 99%, and product 2- propyl group -1-heptanol is pure
Degree is more than 99%.
And compared with prior art, conversion ratio and purity of the invention is above prior art, and catalyst is prepared into
This is greatly reduced than the catalyst used in the prior art, is entered while realizing with 2- propyl group -2- heptenals merely
Material can be obtained by product 2- propyl group -1-heptanol, and the method cost produced than existing mixed feeding is substantially reduced, and purity is also
Increase therefore with higher realizability and promotional value.
In summary, after the catalyst provided using the present invention and corresponding technique, compared with prior art with high
Conversion ratio and selectivity, under the same terms, the yield of 2- propyl group -1-heptanol is not only increased, while the product obtained can
Technical grade even analytically pure standard is reached, subsequently refined step is eliminated, improves value-added content of product, reduce production
Cost.
Embodiment
The present invention is further illustrated with reference to embodiment, can make those skilled in the art that this hair is more completely understood
It is bright, but do not limit the invention in any way.
Embodiment 1
A kind of catalyst of synthesis 2- propyl group -1-heptanol, the carrier is γ-Al2O3, active component is Ni, Mo, Cu
Oxide, the preparation method of described catalyst is as follows：
45.9g aluminum hydroxide solid elastomer, 194g nickel nitrate, 23.7g ammonium heptamolybdate and 7.9g copper carbonate are placed in
In the autoclave of 1L band stirring, 500ml deionized water is added, stirring makes addition material uniformly mix, rear to add
The pH value of 10wt% sodium hydroxide solution regulation system is 6.0；Reactor top cover is screwed, starts heating system, temperature reaches
To after 120 DEG C, timing stirring 12h, after stirring is stopped, aging 10h is stood in reactor.After pressure release, material is taken out, taken advantage of
Heat removes foreign ion with deionized water filtration washing.Product after washing is dried at room temperature, dried in 100 DEG C of baking oven
It is dry 6 hours, addition 3g sesbania powders, 6.2g salpeter solutions (65% mass fraction) after taking-up, 2.5g citric acids, after being well mixed,
The catalyst of clover shape is extruded on banded extruder, is dried at room temperature, is dried at 100 DEG C and is calcined 4h at 4h, 400 DEG C, obtained
To 2- propyl group -2- heptene aldehyde hydrogenating catalysts.
Realize 2- propyl group -2- heptenals Hydrogenations for 2- third on 10ml micro fixed-bed reactors using above-mentioned catalyst
The technique of base -1-heptanol：
1. the catalyst after roasting, is cut into 2-3mm length, 10ml is measured, the fixed bed for being loaded on 10ml is miniature
In reactor constant temperature zone, φ 3 porcelain ball is loaded up and down, and carries out device hermeticity experiment under reaction pressure 3.0MPa, is protected
Demonstrate,prove air-tightness good.
2., dehydrated 2 hours with 50ml/min nitrogen flow, catalyst being dried at processing, 150 DEG C.
3. hydrogen gas stream, is switched, in hydrogen-oil ratio 400:Catalyst is activated under 1 hydrogen flow rate, it is living at 350 DEG C
Change 24 hours, rear cooling makes temperature constant at 160 DEG C.
4., according to 1.0h-1Reaction velocity, adjusts feed pump inlet amount, and raw material is 2- propyl group -2- heptenals.4h after charging
Afterwards, product 2- propyl group -1-heptanol is obtained.
By analysis, reactant 2- propyl group -2- heptenals conversion ratio is more than 99%, and product 2- propyl group -1-heptanol purity is big
In 99%.
Embodiment 2
A kind of catalyst of synthesis 2- propyl group -1-heptanol, the carrier used is γ-Al2O3, active component be Ni, Mo, Zn
Oxide.The preparation method of described catalyst is as follows：
23g aluminum hydroxide solid elastomer, 83.5g nickelous carbonate, 25g molybdenum oxide and 36.7g zinc nitrate are placed in 1L's
In autoclave with stirring, 500ml deionized water is added, stirring makes addition material uniformly mix, 10wt% is added afterwards
Sodium hydroxide solution regulation system pH value be 6.5.Reactor top cover is screwed, starts heating system, temperature reaches 120 DEG C
Afterwards, timing stirring 10h, after stirring is stopped, aging 8h is stood in reactor.After pressure release, material is taken out, spend while hot from
Sub- water filtration washing removes foreign ion.Product after washing is dried at room temperature, dried 4 hours in 100 DEG C of baking oven,
3.5g sesbania powders, 6.2g salpeter solutions (65% mass fraction), 3g citric acids, after being well mixed, in banded extruder are added after taking-up
On be extruded into the catalyst of clover shape, dry at room temperature, dried at 100 DEG C and be calcined 4h at 4h, 450 DEG C, obtain 2- propyl group-
2- heptene aldehyde hydrogenating catalysts.
Realize 2- propyl group -2- heptenals Hydrogenation for the work of 2- propyl group -1-heptanol on 10ml micro fixed-bed reactors
Skill：
1. the catalyst after roasting, is cut into 2-3mm length, 10ml is measured, the fixed bed for being loaded on 10ml is miniature
In reactor constant temperature zone, φ 3 porcelain ball is loaded up and down, and carries out device hermeticity experiment under reaction pressure 3.5MPa, is protected
Demonstrate,prove air-tightness good.
2., dehydrated 2 hours with 50ml/min nitrogen flow, catalyst being dried at processing, 150 DEG C.
3. hydrogen gas stream, is switched, in hydrogen-oil ratio 500:Catalyst is activated under 1 hydrogen flow rate, it is living at 400 DEG C
Change 24 hours, rear cooling makes temperature constant at 240 DEG C.
4., according to 1.0h-1Reaction velocity, adjusts feed pump inlet amount, and raw material is 2- propyl group -2- heptenals.4h after charging
Afterwards, product 2- propyl group -1-heptanol is obtained.
By analysis, reactant 2- propyl group -2- heptenals conversion ratio is more than 98%, and product 2- propyl group -1-heptanol purity is big
In 95%.
Embodiment 3
A kind of catalyst of synthesis 2- propyl group -1-heptanol, the carrier used is γ-Al2O3, active component be Ni, Zn, Cu
Oxide, the preparation method of described catalyst is as follows：
30.6g aluminum hydroxide solid elastomer, 210.6g nickel sulfate, 23.4g copper nitrate and 19.9g zinc sulfate are placed in
In the autoclave of 1L band stirring, 600ml deionized water is added, stirring makes addition material uniformly mix, ammonia is added afterwards
The pH value of aqueous solution regulation system is 6.5.Reactor top cover is screwed, starts heating system, temperature is reached after 140 DEG C, timing
Stir 12h, after stirring is stopped, aging 10h is stood in reactor.After pressure release, material is taken out, deionized water mistake is used while hot
Filter washing removes foreign ion.Product after washing is dried at room temperature, dried 6 hours in 100 DEG C of baking oven, after taking-up
3.5g sesbania powders, 6.0g salpeter solutions (65% mass fraction) are added, 3g citric acids after being well mixed, are extruded on banded extruder
The catalyst of clover shape, dries at room temperature, is dried at 100 DEG C and is calcined 4h at 4h, 400 DEG C, obtains 2- propyl group -2- heptene
Aldehyde hydrogenating catalyst.
Realize 2- propyl group -2- heptenals Hydrogenation for the work of 2- propyl group -1-heptanol on 10ml micro fixed-bed reactors
Skill：
1. the catalyst after roasting, is cut into 2-3mm length, 10ml is measured, the fixed bed for being loaded on 10ml is miniature
In reactor constant temperature zone, φ 3 porcelain ball is loaded up and down, and carries out device hermeticity experiment under reaction pressure 5.0MPa, is protected
Demonstrate,prove air-tightness good.
2., dehydrated 2 hours with 50ml/min nitrogen flow, catalyst being dried at processing, 150 DEG C.
3. hydrogen gas stream, is switched, in hydrogen-oil ratio 600:Catalyst is activated under 1 hydrogen flow rate, it is living at 500 DEG C
Change 24 hours, rear cooling makes temperature constant at 180 DEG C.
4., according to 1.5h-1Reaction velocity, adjusts feed pump inlet amount, and raw material is 2- propyl group -2- heptenals.4h after charging
Afterwards, product 2- propyl group -1-heptanol is obtained.
By analysis, reactant 2- propyl group -2- heptenals conversion ratio is more than 92%, and product 2- propyl group -1-heptanol purity is big
In 96%.
Embodiment 4
A kind of catalyst of synthesis 2- propyl group -1-heptanol, uses carrier for γ-Al2O3, active component is Zn, Mo, Cu
Oxide, the preparation method of described catalyst is as follows：
30.6g aluminum hydroxide solid elastomer, 30g molybdenum oxide, 77.8g copper sulphate and 38.5g zinc carbonate are placed in 1L
Band stirring autoclave in, add 500ml deionized water, stirring the material of addition is uniformly mixed, ammonia is added afterwards
The pH value of aqueous solution regulation system is 7.0.Reactor top cover is screwed, starts heating system, temperature is reached after 140 DEG C, timing
Stir 12h, after stirring is stopped, aging 10h is stood in reactor.After pressure release, material is taken out, deionized water mistake is used while hot
Filter washing removes foreign ion.Product after washing is dried at room temperature, dried 5 hours in 100 DEG C of baking oven, after taking-up
3.5g sesbania powders, 6.0g salpeter solutions (65% mass fraction) are added, 3g citric acids after being well mixed, are extruded on banded extruder
The catalyst of clover shape, dries at room temperature, is dried at 100 DEG C and is calcined 4h at 4h, 550 DEG C, obtains 2- propyl group -2- heptene
Aldehyde hydrogenating catalyst.
Realize 2- propyl group -2- heptenals Hydrogenation for the work of 2- propyl group -1-heptanol on 10ml micro fixed-bed reactors
Skill：
1. the catalyst after roasting, is cut into 2-3mm length, 10ml is measured, the fixed bed for being loaded on 10ml is miniature
In reactor constant temperature zone, φ 3 porcelain ball is loaded up and down, and carries out device hermeticity experiment under reaction pressure 6.0MPa, is protected
Demonstrate,prove air-tightness good.
2., dehydrated 2 hours with 50ml/min nitrogen flow, catalyst being dried at processing, 150 DEG C.
3. hydrogen gas stream, is switched, in hydrogen-oil ratio 300:Catalyst is activated under 1 hydrogen flow rate, it is living at 400 DEG C
Change 24 hours, rear cooling makes temperature constant at 100 DEG C.
4., according to 0.5h-1Reaction velocity, adjusts feed pump inlet amount, and raw material is 2- propyl group -2- heptenals.4h after charging
Afterwards, product 2- propyl group -1-heptanol is obtained.
By analysis, reactant 2- propyl group -2- heptenals conversion ratio is more than 95%, and product 2- propyl group -1-heptanol purity is big
In 92%.
Embodiment 5
A kind of catalyst of synthesis 2- propyl group -1-heptanol, the carrier used is γ-Al2O3, active component be Ni oxidation
Thing, the preparation method of described catalyst is as follows：
In the autoclave that the nickelous carbonate of 107g aluminum hydroxide solid elastomer, 50.1g is placed in the stirring of 1L band, add
500ml deionized water, stirring makes the material of addition uniformly mix, and the rear pH value for adding ammonia spirit regulation system is 6.5.Will
Reactor top cover is screwed, and starts heating system, temperature reached after 130 DEG C, timing stirring 10h, after stirring is stopped, in reactor
Interior standing aging 10h.After pressure release, material is taken out, foreign ion is removed with deionized water filtration washing while hot.After washing
Product is dried at room temperature, is dried 6 hours in 100 DEG C of baking oven, and 4g sesbania powders, 6.0g salpeter solutions are added after taking-up
(65% mass fraction), 3.5g citric acids after being well mixed, are extruded into the catalyst of clover shape, at room temperature on banded extruder
Dry, dried at 100 DEG C and be calcined 4h at 4h, 350 DEG C, obtain 2- propyl group -2- heptene aldehyde hydrogenating catalysts.
Realize 2- propyl group -2- heptenals Hydrogenation for the work of 2- propyl group -1-heptanol on 10ml micro fixed-bed reactors
Skill：
1. the catalyst after roasting, is cut into 2-3mm length, 10ml is measured, the fixed bed for being loaded on 10ml is miniature
In reactor constant temperature zone, φ 3 porcelain ball is loaded up and down, and carries out device hermeticity experiment under reaction pressure 4.0MPa, is protected
Demonstrate,prove air-tightness good.
2., dehydrated 2 hours with 50ml/min nitrogen flow, catalyst being dried at processing, 150 DEG C.
3. hydrogen gas stream, is switched, in hydrogen-oil ratio 800:Catalyst is activated under 1 hydrogen flow rate, it is living at 450 DEG C
Change 24 hours, rear cooling makes temperature constant at 80 DEG C.
4., according to 1.0h-1Reaction velocity, adjusts feed pump inlet amount, and raw material is 2- propyl group -2- heptenals.4h after charging
Afterwards, product 2- propyl group -1-heptanol is obtained.
By analysis, reactant 2- propyl group -2- heptenals conversion ratio is more than 98%, and product 2- propyl group -1-heptanol purity is big
In 98%.
Embodiment 6
A kind of catalyst of synthesis 2- propyl group -1-heptanol, the carrier used is γ-Al2O3, active component be Ni, Mo oxygen
Compound, the preparation method of described catalyst is as follows：
31g aluminum hydroxide solid elastomer, 30g molybdenum oxide, 83.5g nickelous carbonate are placed in the reaction under high pressure that 1L band is stirred
In kettle, 500ml deionized water is added, stirring makes the material of addition uniformly mix, the rear PH for adding ammonia spirit regulation system
It is worth for 6.0.Reactor top cover is screwed, starts heating system, temperature reached after 180 DEG C, timing stirring 12h, after stirring is stopped
Only, aging 10h is stood in reactor.After pressure release, material is taken out, while hot with deionized water filtration washing remove impurity from
Son.Product after washing is dried at room temperature, dried 6 hours in 100 DEG C of baking oven, added after taking-up 4g sesbania powders,
6.0g salpeter solutions (65% mass fraction), 3.0g citric acids after being well mixed, are extruded into urging for clover shape on banded extruder
Agent, dries at room temperature, is dried at 100 DEG C and is calcined 4h at 4h, 500 DEG C, obtains 2- propyl group -2- heptene aldehyde hydrogenating catalysts.
Realize 2- propyl group -2- heptenals Hydrogenation for the work of 2- propyl group -1-heptanol on 10ml micro fixed-bed reactors
Skill：
1. the catalyst after roasting, is cut into 2-3mm length, 10ml is measured, the fixed bed for being loaded on 10ml is miniature
In reactor constant temperature zone, φ 3 porcelain ball is loaded up and down, and carries out device hermeticity experiment under reaction pressure 4.0MPa, is protected
Demonstrate,prove air-tightness good.
2., dehydrated 2 hours with 50ml/min nitrogen flow, catalyst being dried at processing, 150 DEG C.
3. hydrogen gas stream, is switched, in hydrogen-oil ratio 600:Catalyst is activated under 1 hydrogen flow rate, it is living at 350 DEG C
Change 24 hours, rear cooling makes temperature constant at 120 DEG C.
4., according to 1.0h-1Reaction velocity, adjusts feed pump inlet amount, and raw material is 2- propyl group -2- heptenals.4h after charging
Afterwards, product 2- propyl group -1-heptanol is obtained.
By analysis, reactant 2- propyl group -2- heptenals conversion ratio is more than 97%, and product 2- propyl group -1-heptanol purity is big
In 97%.
It can be seen that after the catalyst provided using the present invention and corresponding technique, compared with prior art with high conversion
Under rate and selectivity, the same terms, the production cost of catalyst is reduced, the yield of 2- propyl group -1-heptanol is not only increased, together
When the product that is obtained can reach technical grade even analytically pure standard, eliminate subsequently refined step, improve product
Added value, reduces the cost of production.
Claims (4)
1. a kind of catalyst of synthesis 2- propyl group -1-heptanol, including active component and carrier, it is characterised in that：Described carrier
For γ-Al2O3, described active component is Ni, Mo, Zn, Cu oxide, and wherein carrier accounts for the 20- of whole catalyst
70wt%, the catalyst is combined using Hydrothermal Synthesiss and kneading method to be prepared from, and is concretely comprised the following steps：
According to said components part by weight by the metal oxide precursor of active component and carrier γ-Al2O3Presoma together
Be added in the heatable autoclave with stirring, backward reactor in addition reactor volume 60-70% go
Ionized water, the pH with ammoniacal liquor or sodium hydroxide solution regulation system is 6-8, then tightens autoclave spiral cover, control stirring speed
Degree and heating-up temperature, temperature are 100-180 DEG C, and mixing speed is 100-150 revs/min, and system is stirred 12 hours, rear to stop
Stirring, stands aging 8-10h at 100-180 DEG C, afterwards with deionized water filtration washing insoluble matter while hot, removes heteroion,
Insoluble matter after washing is dried 4-6 hours at 100 DEG C；
Added after to above-mentioned drying in product after auxiliary agent, extruded moulding obtains catalyst；
The weight proportion of metal oxide is NiO0-60wt%, MoO wherein in the metal oxide precursor of active component3 0-
40wt%, ZnO 0-30wt%, CuO 0-30wt%,
Auxiliary dosage employed in it is：Nitric acid 3-4%, citric acid 2.5-3.5%, sesbania powder 3-5%, above-mentioned consumption is to account for
The percentage of products weight after drying；
Carrier γ-the Al2O3Presoma use aluminum hydroxide solid elastomer.
2. catalyst according to claim 1, it is characterised in that：
The metal oxide precursor of described active component be selected from nickel nitrate, nickel sulfate, nickelous carbonate, molybdenum oxide, ammonium heptamolybdate,
One or more mixtures in zinc nitrate, zinc sulfate, zinc carbonate, copper sulphate, copper nitrate, copper carbonate.
3. catalyst according to claim 1, it is characterised in that：Described extruded moulding process is：
After the product after drying is mixed with auxiliary agent according to the above ratio, aperture for 3mm trifolium-shaped orifice plate on, extrusion into
Type, then dries at room temperature, is dried 4 hours at 100-120 DEG C, is calcined 4h at 400-550 DEG C again afterwards, you can obtain
Finished catalyst.
4. catalyst described in application claim 1 is in method of the 2- propyl group -2- heptenals Hydrogenation for 2- propyl group -1-heptanol, its
It is characterised by comprising the following steps that：
1. the catalyst after roasting, is cut into 2-3mm length, 10ml is taken, 10ml fixed-bed micro-reactor is loaded on
In constant temperature zone, φ 3 porcelain ball, and the progress device hermeticity experiment under reaction pressure 1-6MPa are loaded up and down, it is ensured that airtight
Property is good；
2. after, determining that air-tightness is good, under 50ml/min nitrogen flow, catalyst is dried at processing, 150 DEG C and taken off
Water is dried 2 hours；
3. hydrogen gas stream, is switched, in hydrogen-oil ratio 100:1-800:Catalyst is activated under 1 hydrogen flow rate, in 300-500
Activated 24 hours at DEG C, cool after activation, make temperature constant at 80-240 DEG C；
4., according to 0.25-2.0h-1Reaction velocity, adjusts feed pump inlet amount, and raw material is 2- propyl group -2- heptenals；4h after charging
Afterwards, you can obtain product 2- propyl group -1-heptanol.
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| CN107262143A (en) * | 2017-07-13 | 2017-10-20 | 武汉凯迪工程技术研究总院有限公司 | Hydrogenation catalyst suitable for producing aviation kerosine and its preparation method and application |
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| DE3913835A1 (en) * | 1989-04-27 | 1990-10-31 | Basf Ag | CATALYST FOR THE HYDROGENATION OF ALIPHATIC UN-SOLUBLE COMPOUNDS |
| CN100344370C (en) * | 2006-02-28 | 2007-10-24 | 上海华谊丙烯酸有限公司 | Catalyst for hydrogenating 3-hydroxy propaldehyde to prepare 1, 3-propylene glycol |
| CN101185893A (en) * | 2006-11-17 | 2008-05-28 | 南化集团研究院 | Catalyst for preparation of decyl alcohols by gas-phase hydrogenation of decylenaldehydes and preparation method thereof |
| CN103785399B (en) * | 2012-11-01 | 2016-03-02 | 中国石油化工股份有限公司 | A kind of preparation method of Hydrodemetalation catalyst |
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