CN104857981A - Metal nitride catalyst for acetic acid hydrogenation synthesis of isopropanol and manufacturing method and application thereof - Google Patents

Metal nitride catalyst for acetic acid hydrogenation synthesis of isopropanol and manufacturing method and application thereof Download PDF

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CN104857981A
CN104857981A CN201510201600.9A CN201510201600A CN104857981A CN 104857981 A CN104857981 A CN 104857981A CN 201510201600 A CN201510201600 A CN 201510201600A CN 104857981 A CN104857981 A CN 104857981A
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acetic acid
catalyst
metal nitride
isopropyl alcohol
atmosphere
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CN104857981B (en
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李德宝
郭荷芹
肖勇
侯博
贾丽涛
陈从标
鲁怀乾
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Shanxi Institute of Coal Chemistry of CAS
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Abstract

A metal nitride catalyst for acetic acid hydrogenation synthesis of isopropanol comprises an iron nitride, an additive metal nitride and a carrier, the molar composition of the catalyst is as follows: iron in the iron nitride: metal in the additive metal nitride: carrier = 8-25: 3-10:100. The metal nitride catalyst has the advantages of simple isopropanol synthesis process, and no equipment corrosion.

Description

A kind of metal nitride catalyst of acetic acid hydrogenation synthesis isopropyl alcohol and method for making thereof and application
Technical field
The present invention relates to a kind of catalyst of petrohol and method for making thereof and application, specifically a kind of nitride metal Catalysts and its preparation method for acetic acid hydrogenation synthesis isopropyl alcohol and application.
Background technology
Isopropyl alcohol (Isopropyl Alcohol, be called for short IPA) have another name called IPA, dimethylcarbinol, it is a kind of organic solvent of function admirable, still the important intermediate of multiple organic compound is produced, can be used as the raw material of synthetic glycerine, isopropyl acetate and acetone etc., also be widely used as oil-fired antifreeze additive, for the aspect such as automobile and aviation fuel.In addition, isopropyl alcohol also can be used for manufacturing bactericide, pesticide, cleaning agent and disinfection preservative etc.Have been widely used at field tools such as agricultural chemicals, electronics industry, medicine, coating, daily-use chemical industry and organic syntheses, exploitation prospect is wide.
Production method mainly propylene hydration method and the acetone hydrogenation method of industrial isopropyl alcohol.Propylene hydration method can be divided into propylene indirect hydration method and direct hydration method two kinds.Propylene indirect hydration method is dissolved in sulfuric acid solution by propylene esterification generation isopropyl acid sulphate and sulfuric acid diisopropyl ester occur, then through hydrolysis, refine and obtain isopropyl alcohol.This method flow process is complicated, selective lower, and equipment corrosion is serious, and waste water and exhaust-gas treatment are comparatively difficult, are eliminated gradually after the eighties in 20th century.Propylene direct hydration method makes propylene that hydration reaction directly occur in the presence of a catalyst to generate isopropyl alcohol, and by-product normal propyl alcohol, is the main method of current industrial production isopropyl alcohol simultaneously.Due to state's inner propene resource scarcity, the production cost of propylene hydration method petrohol remains high.Acetone hydrogenation method petrohol adopts copper or zinc oxide to be carried catalyst or nickel-base catalyst, 70 ~ 200 DEG C, under condition of normal pressure, acetone hydrogenation generates isopropyl alcohol, can be divided into the method for acetone gas phase hydrogenation a kind of copper nickel-base catalyst catalysis acetone gas phase hydrogenation petrohol as CN201110293568.3 discloses; The method of liquid-phase hydrogenatin a kind of nickel-base catalyst catalysis acetone liquid-phase hydrogenatin petrohol as CN201110300319.4 discloses, US7799958 discloses the method for acetone liquid-phase hydrogenatin petrohol, by least 2 hydrogenation reaction stages, acetone liquid-phase hydrogenatin is converted into isopropyl alcohol.Acetone liquid-phase hydrogenatin petrohol reaction pressure is high, and equipment investment is large, and cost is high, and gas phase hydrogenation petrohol reacts heat exchange efficiency is low, and when industrial production, heat of reaction cannot shift out, poor operability.
Summary of the invention
The object of the present invention is to provide a kind of Catalysts and its preparation method for acetic acid one step hydrogenation synthesis isopropyl alcohol and application, to solve existing isopropyl alcohol synthesis technique long flow path, the problem that equipment corrosion is serious.
Catalyst of the present invention is made up of the nitride of iron, promoter metal nitride and carrier, mole consisting of of catalyst: the iron in nitrided iron: the metal in promoter metal nitride: carrier=8-25:3-10:100.
Promoter metal nitride as above is cobalt nitride, nickel oxide, molybdenum nitride, one or more in tungsten nitride.
Carrier as above is zirconium dioxide, silica, alundum (Al2O3) or titanium dioxide etc., preferred nano zirconium dioxide, nano silicon, γ-Al 2o 3or anatase titania
Method for preparing catalyst provided by the invention is:
(1) ferric nitrate and solubility promoter metal compound are joined in deionized water, stir and make it dissolve completely, obtain solution A;
(2) in solution A, add carrier, in 30-60 DEG C of dipping 2-10h, 80-120 DEG C of dry 10-24h, 400-600 DEG C of roasting 4-6h, obtain load metal oxide;
(3) by load metal oxide at pure NH 3in atmosphere with the ramp of 0.5-3 DEG C/min to 550-750 DEG C, and nitrogenize 3-8h at this temperature, nitrogenize air speed is 6000-15000h -1, after nitrogenize completes, 3000-7000h in ammonia atmosphere -1after being down to room temperature, pass into O 2content is the O of 0.5v%-2.5v% 2with the gaseous mixture of inert gas, by its surface passivation, namely obtain metal nitride catalyst.
In step described above (1), described solubility promoter metal compound is cobalt nitrate, cobalt acetate, nickel nitrate, ammonium tetramolybdate, ammonium heptamolybdate, ammonium tungstate, ammonium phosphotungstate.
In nitride preparation method as above, it is characterized in that described inert atmosphere is N 2, one in He, Ar.
Catalyst application method of the present invention is:
By above-mentioned catalyst application in fixed bed reactors: at H before reaction 2be warming up to 400-600 DEG C with 0.5-3 DEG C/min under atmosphere, and reduce 3-6h, H at this temperature 2gas space velocity is 2000-7000h -1, H 2atmosphere drops to reaction temperature 250-330 DEG C, passes into the acetic acid steam and H that are preheated to 130 ~ 180 DEG C 2hybrid reaction gas, acetic acid steam shared volume in hybrid reaction gas consists of 5 ~ 50v%, and reaction gas air speed is 2000-5000ml/g cat.h, operating pressure is 3.0 ~ 5.0MPa.
The present invention's advantage is compared to the prior art:
1) catalyst is cheap, and preparation method is simple, easy to operate.
2) reaction process flow process is short, produces isopropyl alcohol cost low.
3) reaction condition is gentle, and acetic acid conversion ratio is high, the selective height of isopropyl alcohol.
Detailed description of the invention:
By by following embodiment, the present invention is invented below, but the present invention is not limited in these examples.
Embodiment 1
By 3.23g Fe (NO 3) 2.9H 2o and 1.45g Co (NO 3) 2.6H 2o is dissolved in 12.0ml deionized water, stirs and makes it dissolve completely.12.32g nanometer ZrO is added in above-mentioned solution 2, 30 DEG C of dippings 10h, 100 DEG C of dry 16h, 500 DEG C of roasting 5h, obtain FeCoO x/ ZrO 2.
By the FeCoO obtained x/ ZrO 2at NH 3550 DEG C are warmed up to 0.5 DEG C/min in atmosphere, and nitrogenize 8h at this temperature, nitrogenize air speed is 15000h -1.After nitrogenize completes, in 7000h -1nH 3after being cooled to room temperature in atmosphere, pass into O 2content is the O of 1.0v% 2with N 2the mist of composition, by its surface passivation, obtains ZrO 2the iron cobalt nitride catalyst of load.
By above-mentioned catalyst application in tubular fixed-bed reactor: at H before reaction 2be warming up to 500 DEG C with 1 DEG C/min under atmosphere, and reduce 4h, H at this temperature 2gas space velocity is 3000h -1, H 2atmosphere drops to reaction temperature 280 DEG C, passes into the acetic acid steam and H that are preheated to 150 DEG C 2gaseous mixture, acetic acid steam shared volume in reaction gas consists of 30v%, and reaction gas air speed is 2000ml/g cat.h, operating pressure is 3.0MPa.
Catalyst fixed bed reactivity worth is in table 1.
Embodiment 2
By 4.04g Fe (NO 3) 2.9H 2o, 1.45g Co (NO 3) 2.6H 2o and 0.87g Ni (NO 3) 2.6H 2o is dissolved in 6.5ml deionized water, stirs and makes it dissolve completely.6.0g Nano-meter SiO_2 is added in above-mentioned solution 2, 40 DEG C of dippings 8h, 120 DEG C of dry 12h, 600 DEG C of roasting 4h, obtain FeCoNiO x/ SiO 2.
By the FeCoNiO obtained x/ SiO 2at NH 3600 DEG C are warmed up to 1 DEG C/min in atmosphere, and nitrogenize 6h at this temperature, nitrogenize air speed is 10000h -1.After nitrogenize completes, in 5000h -1nH 3after being cooled to room temperature in atmosphere, pass into O 2content is the O of 2.5v% 2the mist formed with Ar, by its surface passivation, obtains SiO 2the iron-cobalt-nickel nitride catalyst of load.
By above-mentioned catalyst application in tubular fixed-bed reactor: at H before reaction 2be warming up to 500 DEG C with 2 DEG C/min under atmosphere, and reduce 4h, H at this temperature 2gas space velocity is 2500h -1, H 2atmosphere drops to reaction temperature 290 DEG C, passes into the acetic acid steam and H that are preheated to 140 DEG C 2gaseous mixture, acetic acid steam shared volume in reaction gas consists of 20v%, and reaction gas air speed is 3000ml/g cat.h, operating pressure is 3.5MPa.
Catalyst fixed bed reactivity worth is in table 1.
Embodiment 3
By 6.01g Fe (NO 3) 2.9H 2o and 0.87g Ni (NO 3) 2.6H 2o is dissolved in 11.5ml deionized water, stirs and makes it dissolve completely.12.32g nanometer ZrO is added in above-mentioned solution 2, 50 DEG C of dippings 4h, 80 DEG C of dry 24h, 400 DEG C of roasting 6h, obtain FeNiO x/ ZrO 2.
By the FeNiO obtained x/ ZrO 2at NH 3750 DEG C are warmed up to 2 DEG C/min in atmosphere, and nitrogenize 3h at this temperature, nitrogenize air speed is 6000h -1.After nitrogenize completes, in 3000h -1nH 3after being cooled to room temperature in atmosphere, pass into O 2content is the O of 0.5v% 2the mist formed with He, by its surface passivation, obtains ZrO 2the iron nickel nitride catalyst of load.
By above-mentioned catalyst application in tubular fixed-bed reactor: at H before reaction 2be warming up to 400 DEG C with 0.5 DEG C/min under atmosphere, and reduce 6h, H at this temperature 2gas space velocity is 4000h -1, H 2atmosphere drops to reaction temperature 260 DEG C, passes into the acetic acid steam and H that are preheated to 130 DEG C 2gaseous mixture, acetic acid steam shared volume in reaction gas consists of 50v%, and reaction gas air speed is 6000ml/g cat.h, operating pressure is 4.0MPa.
Catalyst fixed bed reactivity worth is in table 1.
Embodiment 4
By 8.07g Fe (NO 3) 2.9H 2o and 1.45g Ni (NO 3) 2.6H 2o is dissolved in 6.0ml deionized water, stirs and makes it dissolve completely.5.1g γ-Al is added in above-mentioned solution 2o 3, 60 DEG C of dippings 2h, 100 DEG C of dry 18h, 600 DEG C of roasting 4h, obtain FeNiO x/ γ-Al 2o 3.
By the FeNiO obtained x/ γ-Al 2o 3at NH 3600 DEG C are warmed up to 3 DEG C/min in atmosphere, and nitrogenize 4h at this temperature, nitrogenize air speed is 8000h -1.After nitrogenize completes, in 5000h -1nH 3after being cooled to room temperature in atmosphere, pass into O 2content is the O of 0.5v% 2with N 2the mist of composition, by its surface passivation, obtains γ-Al 2o 3the iron nickel nitride catalyst of load.
By above-mentioned catalyst application in tubular fixed-bed reactor: at H before reaction 2be warming up to 600 DEG C with 3 DEG C/min under atmosphere, and reduce 3h, H at this temperature 2gas space velocity is 5000h -1, H 2atmosphere drops to reaction temperature 310 DEG C, passes into the acetic acid steam and H that are preheated to 160 DEG C 2gaseous mixture, acetic acid steam shared volume in reaction gas consists of 10v%, and reaction gas air speed is 7000ml/g cat.h, operating pressure is 5.0MPa.
Catalyst fixed bed reactivity worth is in table 1.
Embodiment 5
By 10.09g Fe (NO 3) 2.9H 2o and 1.03g (NH 4) 2mo 2o 7.4H 2o is dissolved in 11.0ml deionized water, stirs and makes it dissolve completely.12.32g nanometer ZrO is added in above-mentioned solution 2, 40 DEG C of dippings 6h, 120 DEG C of dry 12h, 500 DEG C of roasting 5h, obtain FeMoO x/ ZrO 2.
By the FeMoO obtained x/ ZrO 2at NH 3600 DEG C are warmed up to 1.5 DEG C/min in atmosphere, and nitrogenize 5h at this temperature, nitrogenize air speed is 8000h -1.After nitrogenize completes, in 5000h -1nH 3after being cooled to room temperature in atmosphere, pass into O 2content is the O of 1.0v% 2with N 2the mist of composition, by its surface passivation, obtains ZrO 2the iron Molybdenum nitride catalysts of load.
By above-mentioned catalyst application in tubular fixed-bed reactor: at H before reaction 2be warming up to 500 DEG C with 1.5 DEG C/min under atmosphere, and reduce 4h, H at this temperature 2gas space velocity is 7000h -1, H 2atmosphere drops to reaction temperature 290 DEG C, passes into the acetic acid steam and H that are preheated to 150 DEG C 2gaseous mixture, acetic acid steam shared volume in reaction gas consists of 5v%, and reaction gas air speed is 4000ml/g cat.h, operating pressure is 3.5MPa.
Catalyst fixed bed reactivity worth is in table 1.
Embodiment 6
By 6.06g Fe (NO 3) 2.9H 2o and 0.82g (NH 4) 2mo 2o 7.4H 2o is dissolved in 6.5ml deionized water, stirs and makes it dissolve completely.6.0g Nano-meter SiO_2 is added in above-mentioned solution 2, 40 DEG C of dippings 6h, 120 DEG C of dry 12h, 500 DEG C of roasting 5h, obtain FeMoO x/ SiO 2.
By the FeMoO obtained x/ SiO 2at NH 3600 DEG C are warmed up to 1.5 DEG C/min in atmosphere, and nitrogenize 5h at this temperature, nitrogenize air speed is 8000h -1.After nitrogenize completes, in 5000h -1nH 3after being cooled to room temperature in atmosphere, pass into O 2content is the O of 1.5v% 2with N 2the mist of composition, by its surface passivation, obtains SiO 2the iron Molybdenum nitride catalysts of load.
By above-mentioned catalyst application in tubular fixed-bed reactor: at H before reaction 2be warming up to 400 DEG C with 2 DEG C/min under atmosphere, and reduce 5h, H at this temperature 2gas space velocity is 3000h -1, H 2atmosphere drops to reaction temperature 330 DEG C, passes into the acetic acid steam and H that are preheated to 140 DEG C 2gaseous mixture, acetic acid steam shared volume in reaction gas consists of 20v%, and reaction gas air speed is 3000ml/g cat.h, operating pressure is 4.0MPa.
Catalyst fixed bed reactivity worth is in table 1.
Embodiment 7
By 6.06g Fe (NO 3) 2.9H 2o and 1.25g (NH 4) 3pW 12o 40.3H 2o is dissolved in 13.0ml deionized water, stirs and makes it dissolve completely.12.32g nanometer ZrO is added in above-mentioned solution 2, 40 DEG C of dippings 6h, 120 DEG C of dry 12h, 500 DEG C of roasting 5h, obtain FeWO x/ ZrO 2.
By the FeWO obtained x/ ZrO 2at NH 3600 DEG C are warmed up to 1.5 DEG C/min in atmosphere, and nitrogenize 5h at this temperature, nitrogenize air speed is 8000h -1.After nitrogenize completes, in 5000h -1nH 3after being cooled to room temperature in atmosphere, pass into O 2content is the O of 1.5v% 2the mist formed with Ar, by its surface passivation, obtains ZrO 2the ferrotungsten nitride catalyst of load.
By above-mentioned catalyst application in tubular fixed-bed reactor: at H before reaction 2be warming up to 450 DEG C with 2 DEG C/min under atmosphere, and reduce 4h, H at this temperature 2gas space velocity is 3500h -1, H 2atmosphere drops to reaction temperature 290 DEG C, passes into the acetic acid steam and H that are preheated to 150 DEG C 2gaseous mixture, acetic acid steam shared volume in reaction gas consists of 20v%, and reaction gas air speed is 2500ml/g cat.h, operating pressure is 4.0MPa.
Catalyst fixed bed reactivity worth is in table 1.
Embodiment 8
By 6.06g Fe (NO 3) 2.9H 2o and 1.5g H 18n 2o 9w is dissolved in 12.5ml deionized water, stirs and makes it dissolve completely.8.0gTiO is added in above-mentioned solution 2, 40 DEG C of dippings 6h, 120 DEG C of dry 12h, 500 DEG C of roasting 5h, obtain FeWO x/ TiO 2.
By the FeWO obtained x/ TiO 2at NH 3600 DEG C are warmed up to 1.5 DEG C/min in atmosphere, and nitrogenize 5h at this temperature, nitrogenize air speed is 8000h -1.After nitrogenize completes, in 5000h -1nH 3after being cooled to room temperature in atmosphere, pass into O 2content is the O of 1.5v% 2with N 2the mist of composition, by its surface passivation, obtains TiO 2the ferrotungsten nitride catalyst of load.
By above-mentioned catalyst application in tubular fixed-bed reactor: at H before reaction 2be warming up to 400 DEG C with 2 DEG C/min under atmosphere, and reduce 5h, H at this temperature 2gas space velocity is 3000h -1, H 2atmosphere drops to reaction temperature 290 DEG C, passes into the acetic acid steam and H that are preheated to 150 DEG C 2gaseous mixture, acetic acid steam shared volume in reaction gas consists of 20v%, and reaction gas air speed is 2500ml/g cat.h, operating pressure is 3.5MPa.
Catalyst fixed bed reactivity worth is in table 1.
Acetic synthesis isopropanol reaction performance on table 1 nitride catalyst
As can be seen from Table 1, metal nitride catalyst provided by the invention can transform one-step synthesis isopropyl alcohol by catalysis acetic acid, and reaction condition is gentle, and acetic acid conversion ratio is high, the selective height of isopropyl alcohol.
The foregoing is only the preferred embodiments of the present invention and oneself, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (8)

1. the metal nitride catalyst of an acetic acid hydrogenation synthesis isopropyl alcohol, it is characterized in that catalyst is made up of the nitride of iron, promoter metal nitride and carrier, mole consisting of of catalyst: the iron in nitrided iron: the metal in promoter metal nitride: carrier=8-25:3-10:100.
2. the metal nitride catalyst of a kind of acetic acid hydrogenation synthesis isopropyl alcohol as claimed in claim 1, is characterized in that described promoter metal nitride is cobalt nitride, nickel oxide, molybdenum nitride, one or more in tungsten nitride.
3. the metal nitride catalyst of a kind of acetic acid hydrogenation synthesis isopropyl alcohol as claimed in claim 1, is characterized in that described carrier is zirconium dioxide, silica, alundum (Al2O3) or titanium dioxide.
4. the metal nitride catalyst of a kind of acetic acid hydrogenation synthesis isopropyl alcohol as claimed in claim 3, is characterized in that described carrier is nano zirconium dioxide, nano silicon, γ-Al 2o 3or anatase titania.
5. the preparation method of the metal nitride catalyst of a kind of acetic acid hydrogenation synthesis isopropyl alcohol as described in any one of claim 1-4, is characterized in that comprising the steps:
(1) ferric nitrate and solubility promoter metal compound are joined in deionized water, stir and make it dissolve completely, obtain solution A;
(2) in solution A, add carrier, in 30-60 DEG C of dipping 2-10h, 80-120 DEG C of dry 10-24h, 400-600 DEG C of roasting 4-6h, obtain load metal oxide;
(3) by load metal oxide at pure NH 3in atmosphere with the ramp of 0.5-3 DEG C/min to 550-750 DEG C, and nitrogenize 3-8h at this temperature, nitrogenize air speed is 6000-15000h -1, after nitrogenize completes, 3000-7000h in ammonia atmosphere -1after being down to room temperature, pass into O 2content is the O of 0.5v%-2.5v% 2with the gaseous mixture of inert gas, by its surface passivation, namely obtain metal nitride catalyst.
6. the preparation method of the metal nitride catalyst of a kind of acetic acid hydrogenation synthesis isopropyl alcohol as claimed in claim 5, it is characterized in that the solubility promoter metal compound in described step (1) is cobalt nitrate, cobalt acetate, nickel nitrate, ammonium tetramolybdate, ammonium heptamolybdate, ammonium tungstate or ammonium phosphotungstate.
7. the preparation method of the metal nitride catalyst of a kind of acetic acid hydrogenation synthesis isopropyl alcohol as claimed in claim 5, is characterized in that described inert atmosphere is N 2, one in He, Ar.
8. the application of the metal nitride catalyst of a kind of acetic acid hydrogenation synthesis isopropyl alcohol as described in any one of claim 1-4, is characterized in that comprising the steps:
By catalyst application in fixed bed reactors: at H before reaction 2be warming up to 400-600 DEG C with 0.5-3 DEG C/min under atmosphere, and reduce 3-6h, H at this temperature 2gas space velocity is 2000-7000h -1, H 2atmosphere drops to reaction temperature 250-330 DEG C, passes into the acetic acid steam and H that are preheated to 130 ~ 180 DEG C 2hybrid reaction gas, acetic acid steam shared volume in hybrid reaction gas consists of 5 ~ 50v%, and reaction gas air speed is 2000-5000ml/g cat.h, operating pressure is 3.0 ~ 5.0MPa.
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CN109790024A (en) * 2016-10-05 2019-05-21 埃克森美孚化学专利公司 The method for preparing metal nitride and metal carbides

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