CN105771983A - Catalyst for hydrogenation of unsaturated hydrocarbon in carbon monoxide industrial gas into saturated hydrocarbon, preparation method and application thereof - Google Patents
Catalyst for hydrogenation of unsaturated hydrocarbon in carbon monoxide industrial gas into saturated hydrocarbon, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to hydrogenation reaction catalysts, in particular to a catalyst for hydrogenation of unsaturated hydrocarbon in carbon monoxide industrial gas into saturated hydrocarbon, a preparation method and application thereof. The catalyst comprises, by weight percentage, 0.05-0.5% of a main active component, 0.5-5% of a first assistant, 0.5-10% of a second assistant, and the balance a carrier. Specifically, the main active component is palladium, the first assistant can be one or two of K, Mg, Ca, Na, Ba, Ag, Cu, Mn, Zr and W, the second assistant can be one or two of rare earth metals Ce, La and Sm, and the carrier can be Al2O3 or Al2O3-TiO2. The unsaturated hydrocarbon hydrogenation catalyst prepared by the method provided by the invention has the characteristics of high hydrogenation precision, high selectivity, low operation temperature, large unit volume air processing capacity and the like, is suitable for hydrogenation of unsaturated hydrocarbon into corresponding saturated hydrocarbon, and is especially suitable for hydrogenation removal of unsaturated hydrocarbon impurities from carbon monoxide containing industrial gas.
Description
Technical field
The present invention relates to catalyst for hydrogenation, in a kind of carbon monoxide industrial gases, hydrogenation of unsaturated hydrocarbons is Catalysts and its preparation method and the application of saturated hydrocarbons specifically.
Background technology
In the energy resource structure of China, main based on coal, along with developing rapidly of coal chemical technology in recent years, coal, coke increase year by year in make consumption and the demand of the industry such as chemical industry, metallurgy, many chemical industry, carbide and metallurgical production enterprise are using coal or coke as reducing agent, and its production process produces a large amount of industrial tail gas rich in CO.These tail gas contain CO and account for 20～90%, possibly together with H2、CO2And unsaturated hydrocarbons, direct point " sky lamp " emptying will cause the serious wasting of resources and environmental pollution.The previous important utilization orientation of order is exactly the converter gas by calcium carbide stove exhaust, gas acetylene furnace exhaust gas and iron and steel enterprise etc. purify rich in the industrial tail gas of carbon monoxide after be used for the high value added products such as synthesizing glycol, methane or methanol, the quality in life-span and product for ensureing subsequent synthetic processes catalyst, it is necessary to carry out impurity such as the ethylene in unstrpped gas, propylene and butylene purifying elimination.
The method being currently used for hydrogenation of unsaturated hydrocarbons elimination comprises two big classes, and a class is the sulfide type catalyst of active component based on Co-Mo, and the sulfur content purified in gas is had certain requirement by such catalyst, is not therefore suitable for low-sulfur or the source of the gas without sulfur；Equations of The Second Kind is that such catalyst is primarily adapted for use in noble gas or H with Pd or the Pt noble metal catalyst series being active component2In source, in the CO source of the gas containing 20-90% concentration because of CO strong adsorption on active center thus causing that hydrogenation activity is not enough.Therefore, rarely have about the open report of hydrogenation of unsaturated hydrocarbons elimination in the industrial gases containing CO.
Chinese invention patent CN1466486A discloses a kind of unsaturated hydrocarbon selective hydrogenation catalyst, including carrier, active component Pd and rare earth metal, and the auxiliary agent such as Ag, Bi.This catalyst is mainly used in the C in cracking petroleum hydrocarbon technique2-C4Alkynes or alkadienes be selectively hydrogenated into corresponding alkene.
Chinese invention patent CN102218323B relates to a kind of hydrogenation of unsaturated hydrocarbons catalyst, and this catalyst includes carrier, active component and auxiliary agent, and wherein active component is the mixture of nickel oxide and other metal-oxides.This catalyst is mainly for the treatment of the tail gas in the indirect oils preparation industry of coal or the unsaturated hydrocarbons in synthesis gas.The catalyst of this invention is with Ni for main active component, need before use to carry out high temperature reduction activation, Ni is again good CO hydrogenation catalyst simultaneously, it is adaptable to may bringing the risk of temperature control because CO is hydrogenated with side reaction during containing CO gas, the safety of execute-in-place is poor.
Chinese invention patent CN1470488A relates to a kind of catalyst saturated for fatty monoolefin hydrogenation, and active component is NiO-Mo2O3And B, P, Si thrin or several, carrier is activated alumina, and this catalyst is mainly used in C4～C20Fat olefins hydrogenation, be especially suitable for light olefin such as ethylene, propylene, butene oligomerization gasoline hydrogenation saturated.
Above catalyst is all unsuitable for simultaneously rich in CO and H2Industrial tail gas in the unsaturated hydrocarbons such as impurity such as ethylene, propylene and butylene add hydrogen purification.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the present invention provides hydrogenation of unsaturated hydrocarbons in a kind of carbon monoxide industrial gases to be Catalysts and its preparation method and the application of saturated hydrocarbons.
For achieving the above object, the technical solution used in the present invention is:
In a kind of carbon monoxide industrial gases, hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons, it is characterised in that: catalyst is main active component, the first auxiliary agent, the second auxiliary agent and carrier；By weight percentage, main active component content is 0.05～0.5%, and the content of the first auxiliary agent is 0.5～5%, and the content of the second auxiliary agent is 0.5～10%, and surplus is carrier；
Wherein, main active component is palladium, and the first auxiliary agent is one or both in K, Mg, Ca, Na, Ba, Ag, Cu, Mn, Zr, W, and the second auxiliary agent is one or both in rare earth metal Ce, La, Sm, and carrier is Al2O3Or Al2O3-TiO2。
In described carbon monoxide industrial gases, hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons, it is characterised in that: described Al2O3The preparation of carrier is: alumina powder jointed a, water-aluminum hydroxide and boehmite powder are sufficiently mixed, and sprays rolling or extruded rear dried with the dust technology of volumetric concentration 5-10%, after drying in 400-800 DEG C of roasting 3-8 hour；Wherein alumina powder jointed weight accounts for the 10-35% of vehicle weight, and the consumption of a water-aluminum hydroxide is with Al2O3Meter accounts for the 25-45% of vehicle weight, and the consumption of boehmite powder is with Al2O3Meter accounts for the 20-65% of vehicle weight.
In described carbon monoxide industrial gases, hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons, it is characterised in that: described carrier TiO2-Al2O3Preparation, by alumina powder jointed a, water-aluminum hydroxide and boehmite powder be sufficiently mixed containing titanium salt, spray dried after rolling or extruded moulding with the dust technology of volumetric concentration 5-10%, after drying in 400-800 DEG C of roasting 3-8 hour.
In described carbon monoxide industrial gases, hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons, it is characterised in that: described alumina powder jointed for boehmite powder through obtaining after roasting at 600-800 DEG C.
In described carbon monoxide industrial gases, hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons, it is characterised in that: described is metatitanic acid, butyl titanate or tetraethyl titanate containing titanium salt, and its consumption contains titanium oxide 0.5-10% by weight.
In described carbon monoxide industrial gases, hydrogenation of unsaturated hydrocarbons is the preparation method of the catalyst of saturated hydrocarbons, it is characterized in that: according to the above ratio main active component and auxiliary agent are impregnated respectively absorption or on carrier when co-impregnation is adsorbed on rolling, dried roasting 2-8 hour at 300-600 DEG C, then carry out liquid-phase reduction with 1-3% (volumetric concentration) hydrazine hydrate, namely obtain catalyst with deionized water wash to neutral post-drying.
In described carbon monoxide industrial gases, hydrogenation of unsaturated hydrocarbons is the application of the catalyst of saturated hydrocarbons, it is characterized in that: described catalyst is as the hydrogenation catalyst of unsaturated hydrocarbons impurity in the industrial gases containing carbon monoxide, in the application by the saturated hydrocarbons that hydrogenation of unsaturated hydrocarbons catalysis is correspondence.
The present invention compared with prior art has the advantage that
1. the hydrogenation of unsaturated hydrocarbons catalyst hydrogenation activity height of the present invention, good stability, good operation safety, it has deep hydrogenation detergent power in rich in the industrial gases of carbon monoxide and good opens stopping performance, without prereduction activation processing after on-the-spot filling, drive simple to operate, go through activity of repeatedly stopping undamped.
2. catalyst of the present invention makes the selectivity of hydrogenation of unsaturated hydrocarbons higher than 99%, thus avoid rich in CO and H2The temperature control that reaction causes；Operation temperature window is wider, between 110～220 DEG C, away from the disproportionation temperature 250 DEG C of CO；Operation air speed is high, at 2000～5000h-1Between, it is possible to save catalyst amount, additionally it is possible to the O simultaneously contained in elimination unstripped gas2, export O2Content is less than 10ppm.
Detailed description of the invention
By the examples below, technical scheme is described in further detail.
Embodiment 1
The preparation of carrier: take 143g boehmite powder and obtain alumina powder 100g in 4 hours through 800 DEG C of roastings.
Take above-mentioned alumina powder 100g, aluminium hydroxide 300g, boehmite powder 500g and tetraethyl titanate 100g, add the dilute nitric acid solution mix homogeneously of 150ml volumetric concentration 10%, use banded extruder molding, make the strip carrier of φ 3*4mm, 120 DEG C dry 4 hours, 600 DEG C of roastings 4 hours, obtains carrier standby；
Take 6g barium nitrate, 13g manganese nitrate solution (50wt%), 5g cerous nitrate, 0.17g Palladous chloride. mixed dissolution in 40g deionized water after be immersed in the above-mentioned carrier of 100g, 120 DEG C dry 4 hours, 500 DEG C of roastings 4 hours, then carry out liquid-phase reduction with 1% (volumetric concentration) hydrazine hydrate, namely obtain catalyst of the present invention with deionized water wash to neutral post-drying；
Appreciation condition: air speed 4000h-1, 2.0Mpa, gas composition is calculated as with percent by volume: ethylene 0.2%, CO27%, acetylene 0.02%, CO25%, O20.4%, propylene 0.2%, butylene 0.1%, remaining for H2；
Evaluation result: when 160 DEG C total hydrogenation of unsaturated hydrocarbons be the conversion ratio of saturated hydrocarbons higher than 98%, hydrogenation selectivity is more than 99%.
Embodiment 2
The preparation of carrier: take 286g boehmite powder and obtain alumina powder 200g in 4 hours through 600 DEG C of roastings.
Take above-mentioned alumina powder 200g, adding aluminum hydroxide 200g, butyl titanate 100g, boehmite powder 500g are sufficiently mixed；Be rolled onto the bead of φ 3-4 with the salpeter solution spray-stain that 50ml volumetric concentration is 5%, 120 DEG C dry 4 hours, 500 DEG C of roastings 4 hours, obtains carrier standby；
Take 5g potassium nitrate, 10g manganese nitrate (50wt%) solution, 4g lanthanum carbonate cerium, 0.25g Palladous chloride. mixed dissolution in 43g deionized water after be immersed in the above-mentioned carrier of 100g, 120 DEG C dry 4 hours, 400 DEG C of roastings 4 hours, then carry out liquid-phase reduction with 2% (volumetric concentration) hydrazine hydrate, namely obtain catalyst of the present invention with deionized water wash to neutral post-drying.
Appreciation condition: air speed 4000h-1, 2.0Mpa, gas composition is calculated as with percent by volume: ethylene 0.2%, CO27%, acetylene 0.02%, CO25%, O20.4%, propylene 0.2%, butylene 0.1%, remaining for H2；
Evaluation result: when 150 DEG C total hydrogenation of unsaturated hydrocarbons be the conversion ratio of saturated hydrocarbons higher than 98%, hydrogenation selectivity is more than 99%.
Embodiment 3
The preparation of carrier: take 143g boehmite powder and obtain alumina powder 100g in 4 hours through 700 DEG C of roastings.
Take above-mentioned alumina powder 100g, aluminium hydroxide 300g, boehmite powder 500g and tetraethyl titanate 100g, add the dilute nitric acid solution mix homogeneously of 150ml volumetric concentration 10%, with bowling machine rolling molding, make φ 4mm ball type carrier, 120 DEG C dry 4 hours, 600 DEG C of roastings 4 hours, obtains carrier standby；
Take 3g magnesium nitrate, 13g copper nitrate, 5g nitric acid shirt, 0.25g Palladous chloride. mixed dissolution in 48g deionized water after impregnated in the above-mentioned carrier of 100g, 120 DEG C dry 4 hours, 600 DEG C of roastings 4 hours, then carry out liquid-phase reduction with 3% (volumetric concentration) hydrazine hydrate, namely obtain catalyst of the present invention with deionized water wash to neutral post-drying；
Appreciation condition: air speed 4000h-1, 2.0Mpa, gas composition is calculated as with percent by volume: ethylene 0.2%, CO27%, acetylene 0.02%, CO25%, O20.4%, propylene 0.2%, butylene 0.1%, remaining for H2；
Evaluation result: when 160 DEG C total hydrogenation of unsaturated hydrocarbons be the conversion ratio of saturated hydrocarbons higher than 98%, hydrogenation selectivity is more than 99%.
Embodiment 4
Taking and impregnated in the carrier that 100g above-described embodiment 3 obtains after 13g copper nitrate is dissolved in 51g deionized water, 120 DEG C dry 2 hours, 300 DEG C of roastings 2 hours；Then the carrier after roasting is put in the 48g solution containing 2.5g nitric acid shirt dipping absorption, 120 DEG C dry 2 hours, 300 DEG C of roastings 2 hours；The carrier after after baking is put in the 45g solution containing 0.25g Palladous chloride. dipping absorption again, 120 DEG C dry 2 hours, 300 DEG C of roastings 2 hours.Finally carry out liquid-phase reduction with 3% (volumetric concentration) hydrazine hydrate, namely obtain catalyst of the present invention with deionized water wash to neutral post-drying；
Appreciation condition: air speed 4000h-1, 2.0Mpa, gas composition is calculated as with percent by volume: ethylene 0.2%, CO27%, CO25%, O20.4%, propylene 0.2%, butylene 0.1%, remaining for H2；
Evaluation result: when 140 DEG C total hydrogenation of unsaturated hydrocarbons be the conversion ratio of saturated hydrocarbons higher than 98%, hydrogenation selectivity is more than 99%.
Embodiment 5
Adopt the catalyst that embodiment 4 prepares, according to the appreciation condition of above-described embodiment 4, catalyst is evaluated, in 150 DEG C of stability tests having carried out 1000 hours, after 1000 hours, total hydrogenation of unsaturated hydrocarbons is that the conversion ratio of saturated hydrocarbons remains above 98%, hydrogenation selectivity is more than 99%, and after 1000 hours, then through going through, to repeat the parking back end hydrogenation performance that goes into operation for five times undamped.
Being used in commercial side-stream test by this catalyst again, properly functioning 5 months of this catalyst, Hydrogenation is without obvious performance degradation simultaneously.
Embodiment 6
Take 13g copper nitrate, 2.5g ammonium metatungstate, 3g ammonium ceric nitrate, 0.5g Palladous chloride. mixed dissolution in 48g deionized water after impregnated in 100g above-described embodiment 2 obtain carrier in, 120 DEG C dry 4 hours, 500 DEG C of roastings 4 hours, then carry out liquid-phase reduction with 1% (volumetric concentration) hydrazine hydrate, namely obtain catalyst of the present invention with deionized water wash to neutral post-drying；
Appreciation condition: air speed 4000h-1, 1.7Mpa, gas composition is calculated as with percent by volume:
Ethylene 20ppm, ethane 300ppm, CO26%, propylene 50ppm, butylene 30ppm, remaining for H2；
Evaluation result: when 110 DEG C total hydrogenation of unsaturated hydrocarbons be the conversion ratio of saturated hydrocarbons higher than 99%, hydrogenation selectivity is 100%.
Embodiment 7
Adopt the catalyst of embodiment 6 preparation, according to the appreciation condition of above-described embodiment 6, catalyst is evaluated, in 140 DEG C of stability tests having carried out 1000 hours.After thousand hours, total hydrogenation of unsaturated hydrocarbons is that the conversion ratio of saturated hydrocarbons remains above 99%, and hydrogenation selectivity is 100%.
Comparative example 1
The preparation of carrier: take 143g boehmite powder and obtain alumina powder 100g in 4 hours through 800 DEG C of roastings.
Take above-mentioned alumina powder 100g, aluminium hydroxide 300g, boehmite powder 500g and tetraethyl titanate 100g, add the dilute nitric acid solution mix homogeneously of 150ml volumetric concentration 10%, use banded extruder molding, make the strip carrier of φ 3*4mm, 120 DEG C dry 4 hours, 600 DEG C of roastings 4 hours, obtains carrier standby；
Taking is immersed in the above-mentioned carrier of 100g after 0.17g Palladous chloride. is dissolved in 53g deionized water, 120 DEG C dry 4 hours, 500 DEG C of roastings 4 hours, then carry out liquid-phase reduction with 1-3% (volumetric concentration) hydrazine hydrate, standby to neutral post-drying with deionized water wash；
By the catalyst of above-mentioned acquisition under the appreciation condition identical with embodiment 1, when 160 DEG C, total hydrogenation of unsaturated hydrocarbons is the conversion ratio of saturated hydrocarbons is 30%, and when 220 DEG C, total hydrogenation of unsaturated hydrocarbons is the conversion ratio of saturated hydrocarbons is 75%.
Comparative example 2
It is CN102218323 according to China Patent Publication No., name is called that recording in a kind of hydrogenation of unsaturated hydrocarbons catalyst is prepared with the Ni catalyst (referring to description embodiment 1) being main active component, the catalyst obtained needs reduction activation at 400 DEG C in hydrogeneous atmosphere before use, operates air speed 1000～2000h-1, temperature is 200～300 DEG C.It is known that Ni is good CO hydrogenation catalyst, it is adaptable to may bringing the risk of temperature control because CO is hydrogenated with side reaction during containing CO gas, the safety of execute-in-place is poor.
Claims (7)
1. in carbon monoxide industrial gases, hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons, it is characterised in that: catalyst is main active component, the first auxiliary agent, the second auxiliary agent and carrier；By weight percentage, main active component content is 0.05～0.5%, and the content of the first auxiliary agent is 0.5～5%, and the content of the second auxiliary agent is 0.5～10%, and surplus is carrier；
Wherein, main active component is palladium, and the first auxiliary agent is one or both in K, Mg, Ca, Na, Ba, Ag, Cu, Mn, Zr, W, and the second auxiliary agent is one or both in rare earth metal Ce, La, Sm, and carrier is Al2O3Or Al2O3-TiO2。
2. hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons in carbon monoxide industrial gases according to claim 1, it is characterised in that: described Al2O3The preparation of carrier is: alumina powder jointed a, water-aluminum hydroxide and boehmite powder are sufficiently mixed, and sprays rolling or extruded rear dried with the dust technology of volumetric concentration 5-10%, after drying in 400-800 DEG C of roasting 3-8 hour；Wherein alumina powder jointed weight accounts for the 10-35% of vehicle weight, and the consumption of a water-aluminum hydroxide is with Al2O3Meter accounts for the 25-45% of vehicle weight, and the consumption of boehmite powder is with Al2O3Meter accounts for the 20-65% of vehicle weight.
3. hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons in carbon monoxide industrial gases according to claim 1, it is characterised in that: described carrier TiO2-Al2O3Preparation, by alumina powder jointed a, water-aluminum hydroxide and boehmite powder be sufficiently mixed containing titanium salt, spray dried after rolling or extruded moulding with the dust technology of volumetric concentration 5-10%, after drying in 400-800 DEG C of roasting 3-8 hour.
4. in the carbon monoxide industrial gases according to claim 2 and 3, hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons, it is characterised in that: described alumina powder jointed for boehmite powder through obtaining after roasting at 600-800 DEG C.
5. in carbon monoxide industrial gases according to claim 3, hydrogenation of unsaturated hydrocarbons is the catalyst of saturated hydrocarbons, it is characterised in that: described is metatitanic acid, butyl titanate or tetraethyl titanate containing titanium salt, and its consumption contains titanium oxide 0.5-10% by weight.
6. in the carbon monoxide industrial gases described in a claim 1, hydrogenation of unsaturated hydrocarbons is the preparation method of the catalyst of saturated hydrocarbons, it is characterized in that: according to the above ratio main active component and auxiliary agent are impregnated respectively absorption or on carrier when co-impregnation is adsorbed on rolling, dried roasting 2-8 hour at 300-600 DEG C, then carry out liquid-phase reduction with 1-3% (volumetric concentration) hydrazine hydrate, namely obtain catalyst with deionized water wash to neutral post-drying.
7. in the carbon monoxide industrial gases described in a claim 1, hydrogenation of unsaturated hydrocarbons is the application of the catalyst of saturated hydrocarbons, it is characterized in that: described catalyst is as the hydrogenation catalyst of unsaturated hydrocarbons impurity in the industrial gases containing carbon monoxide, in the application by the saturated hydrocarbons that hydrogenation of unsaturated hydrocarbons catalysis is correspondence.
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| CN108837831A (en) * | 2018-06-29 | 2018-11-20 | 万华化学集团股份有限公司 | A kind of selective hydrogenation of butadiene 1- butylene catalyst and its preparation method and application |
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| CN108837831A (en) * | 2018-06-29 | 2018-11-20 | 万华化学集团股份有限公司 | A kind of selective hydrogenation of butadiene 1- butylene catalyst and its preparation method and application |
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