A preparation method for 4,4'-bipyridine, comprising: using pyridine as a raw material, preheating and gasifying the pyridine, then, catalyzed by a loaded Ni/HY catalyst, generating 4,4'-bipyridine via a dehydrogenation coupling reaction; the nickel loading of the loaded Ni/HY catalyst is 5%-30%, and the carrier of the loaded Ni/HY catalyst is an HY molecular sieve. Cheap pyridine is used as the raw material, and production costs are low; the loaded Ni/HY catalyst is used to obtain 4,4'-bipyridine via a one-step catalytic coupling dehydrogenation reaction, the target product selectivity is high, and the reaction process is simple and easy to operate; moreover, the amount of "three wastes" generated is low, which is environmentally friendly, and suitable for continuous, industrial production of 4,4'-bipyridine.
C07D 213/22 - Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing two or more pyridine rings directly linked together, e.g. bipyridyl
Disclosed is a 3-methylpiperidine dehydrogenation catalyst, which uses a metal oxide as a carrier, a noble metal as an active component, and an alkali metal and alkaline earth metal as auxiliary agents. The active component and the auxiliary agents are loaded by means of impregnation; the loading amount of the active component is 0.05-0.5%; and the loading amount of the auxiliary agents is 0.1-1.0%. Also disclosed is a method for preparing 3-methylpyridine: using 3-methylpiperidine as a raw material, carrying out vaporization by heating, and using a fixed bed reactor filled with the 3-methylpiperidine dehydrogenation catalyst to obtain 3-methylpyridine. The catalyst has a service life of more than 3000 hours and can maintain a conversion rate of 3-methylpiperidine of higher than 99% and a yield of 3-methylpyridine of high than 98%. The 3-methylpiperidine dehydrogenation catalyst of the present invention is used for 3-methylpiperidine dehydrogenation to prepare 3-methylpyridine, can achieve less noble metal loading and a high 3-methylpyridine yield, and has a long service life as well as significant cost advantages and good industrial application prospects.
B01J 23/58 - Platinum group metals with alkali- or alkaline earth metals or beryllium
C07D 213/133 - Preparation by dehydrogenation of hydrogenated pyridine compounds
C07D 213/16 - Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
The present invention discloses a catalyst for preparing pyridine base from syngas. The catalyst includes a carrier, an active component, a first auxiliary and a second auxiliary. The carrier is molecular sieves. The active component is Rh. The first auxiliary is one or more of Mn, Fe, Na and La. The second auxiliary is one or more of Zn, Co, Cr, Bi and Cu. The active component Rh is 0.5-3% of a mass of the carrier. The first auxiliary is 0.05-5% of the mass of the carrier. The second auxiliary is 0.5-15% of the mass of the carrier. The present invention further discloses application of the catalyst to preparation of pyridine base by catalyzing syngas, where the syngas and an ammonia donor are used as reaction raw materials for reaction to generate pyridine base products. The catalyst of the present invention can couple a cyclization reaction of generating acetaldehyde through hydrogenation of carbon monoxide with a condensation reaction of aldehyde and ammonia to convert the syngas into the pyridine base through one-step catalysis, with a carbon monoxide conversion rate of 8-20% and a pyridine base selectivity of 10-18%.
B01J 29/70 - Crystalline aluminosilicate zeolitesIsomorphous compounds thereof of types characterised by their specific structure not provided for in groups
B01J 29/40 - Crystalline aluminosilicate zeolitesIsomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
B01J 29/65 - Crystalline aluminosilicate zeolitesIsomorphous compounds thereof of the ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38
C07D 213/16 - Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
B01J 29/48 - Crystalline aluminosilicate zeolitesIsomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
B01J 29/69 - Crystalline aluminosilicate zeolitesIsomorphous compounds thereof of the ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
B01J 29/78 - Crystalline aluminosilicate zeolitesIsomorphous compounds thereof of types characterised by their specific structure not provided for in groups containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
C07D 213/10 - Preparation by ring-closure involving the use of ammonia, amines, amine salts, or nitriles from acetaldehyde or cyclic polymers thereof
2 alkyl, Cl, or Br. The method of the present invention features wide adaptability to raw materials, high atomic utilization rate, high catalyst activity, long service life, and fewer by-products.
C07D 213/22 - Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing two or more pyridine rings directly linked together, e.g. bipyridyl
A method for preparing 1,1′-ethylene-2,2′-bipyridinium dichloride includes mixing an aqueous diquat dibromide solution with hydrochloric acid, adding dropwise to a mixture of an organic solvent, a bromine absorbent, and an oxidant, and reacting to produce 1,1′-ethylene-2,2′-bipyridinium dichloride.
C07D 401/04 - Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings directly linked by a ring-member-to-ring- member bond
The present invention relates to the field of chemistry, and disclosed thereby is a green preparation method for a diquat anion salt, the method comprising: reacting a diquat dibromide mother liquor with an oxidant in the presence of hydrochloric acid or sulfuric acid to obtain a reaction solution containing a diquat dichloride salt or diquat disulfate salt; filtering the reaction solution; adjusting the pH of the filtrate; concentrating to obtain a diquat dichloride mother liquor or diquat disulfate mother liquor; mixing a filter cake with an organic solvent; introducing ethylene to react until the system pressure no longer changes; filtering the reaction solution to obtain a filtrate containing 1,2-dibromoethane and a diquat dibromide salt solid; washing and drying the diquat dibromide salt to prepare a diquat dibromide mother liquor; recovering the filtrate to obtain 1,2-dibromoethane, and reacting same with bipyridine to produce a diquat dibromide salt. The method of the present invention is simple and is suitable for industrial production, the cation loss rate is less than 0.5%, and the bromine recovery rate is more than 96%, thereby realizing the recycling of bromine and avoiding the waste of bromine.
Disclosed is a catalyst for preparing a pyridine base from synthetic gas, the catalyst comprising a carrier, an active component, a first auxiliary agent and a second auxiliary agent, wherein the carrier is a molecular sieve, the active component is Rh, the first auxiliary agent is one or more of Mn, Fe, Na and La, and the second auxiliary agent is one or more of Zn, Co, Cr, Bi and Cu; and Rh is 0.5-3% of the mass of the carrier, the first auxiliary agent is 0.05-5% of the mass of the carrier, and the second auxiliary agent is 0.5-15% of the mass of the carrier. The catalyst is applied to the preparation of a pyridine base by catalyzing synthetic gas, wherein the synthetic gas and an ammonia donor are used as reaction raw materials and reacted to obtain a pyridine base product. The catalyst can couple the cyclization and condensation reactions in which acetaldehyde and aldehyde ammonia are generated by the hydrogenation of carbon monoxide, and realize the conversion from synthetic gas to a pyridine base by means of one-step catalysis. The conversion rate of carbon monoxide is 8-20%, and the selectivity of the pyridine base is 10-18%.
B01J 29/48 - Crystalline aluminosilicate zeolitesIsomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
B01J 29/69 - Crystalline aluminosilicate zeolitesIsomorphous compounds thereof of the ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38 containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
B01J 29/78 - Crystalline aluminosilicate zeolitesIsomorphous compounds thereof of types characterised by their specific structure not provided for in groups containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
C07D 213/10 - Preparation by ring-closure involving the use of ammonia, amines, amine salts, or nitriles from acetaldehyde or cyclic polymers thereof
C07D 213/16 - Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
8.
METHOD FOR PREPARING 2,2'-DIPYRIDINE AND DERIVATIVES THEREOF
122 alkyl, Cl, or Br. The method of the present invention features wide adaptability to raw materials, high atomic utilization rate, high catalyst activity, long service life, and fewer by-products.
C07D 213/22 - Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing two or more pyridine rings directly linked together, e.g. bipyridyl
C07D 213/127 - Preparation from compounds containing pyridine rings
B01J 23/83 - Catalysts comprising metals or metal oxides or hydroxides, not provided for in group of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups with rare earths or actinides
9.
METHOD FOR PREPARING 1,1'-ETHYLENE-2,2'-BIPYRIDYL DICHLORIDE SALT
Disclosed is a method for preparing 1,1'-ethylene-2,2'-bipyridyl dichloride salt, the method involving mixing an aqueous solution of diquat dibromide with hydrochloric acid, and then dropwise adding same to a mixed solution of an organic solvent, a bromine absorbent and an oxidant for reaction to obtain the 1,1'-ethylene-2,2'-bipyridine dichloride salt.
patents
