- Method for continuously preparing dimethyl azodiisobutyrate by using micro-channel reactor
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The invention discloses a method for continuously preparing dimethyl azodiisobutyrate by using a micro-channel reactor, which comprises the following steps: 1, heating butyronitrile, and dissolving the butyronitrile in a benzene solvent to obtain a mixed solution with the mass concentration of butyronitrile of 5-30%; inputting the mixed solution and methanol into a first mixing zone of a micro-channel reactor for mixing to obtain a first mixed material; 2, mixing the mixed material and hydrogen chloride gas in a second mixing zone of a micro-channel reactor, and introducing the mixture into the micro-channel reactor for primary reaction; and 3, mixing the reaction solution after the heat preservation reaction with water, introducing the mixture into a micro-channel reactor, carrying out asecondary reaction, standing, performing centrifuging to obtain a crude product of dimethyl azobisisobutyrate after the reaction is finished, and performing recrystallizing to obtain dimethyl azobisisobutyrate. According to the method, the reaction rate and the raw material utilization rate are increased, the batch quality difference caused by reaction temperature fluctuation is avoided, the reaction is easy to control, the production period is short, and the total yield can reach 75% or above.
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Paragraph 0031-0037
(2020/11/23)
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- Dimethyl 2,2'-azobis(2-methylpropionate) preparation method
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The invention discloses a dimethyl 2,2'-azobis(2-methylpropionate) preparation method, which comprises: pouring 2,2'-azobisisobutyronitrile, methanol and dichloroethane in a reactor with a stirring and reflux device; starting stirring, slowly adding thionyl chloride in a dropwise manner under cooling, controlling the temperature of the material, and carrying out thermal insulation to carry out a reaction; after completing the reaction, adding into cold water in a dropwise manner, and carrying out a hydrolysis reaction; after completing the hydrolysis reaction, standing, and carrying out first layering; washing the organic phase obtained after the first layering with water, and carrying out second layering; carrying out pressure reducing distillation on the organic phase after the second layering until the dichloroethane is subjected to complete distillation recovery to obtain a liquid dimethyl 2,2'-azobis(2-methylpropionate); and carrying out low temperature cooling on the liquid dimethyl 2,2'-azobis(2-methylpropionate) to obtain a white solid dimethyl 2,2'-azobis(2-methylpropionate) product, wherein the product content (HPLC) of the obtained white solid dimethyl 2,2'-azobis(2-methylpropionate) is more than 98%, and the yield is 85-95%. According to the present invention, the hydrogen chloride gas is replaced with the cheap thionyl chloride, and the thionyl chloride is liquid-state at normal temperature, such that the speed and the dosage are conveniently controlled during the dropwise addition, and the reaction time is shortened to 6 h.
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Paragraph 0008; 0021-0038
(2019/10/04)
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- 2,2'-azo(2-methyl-N-(2-hydroxyethyl)propionamide) preparation method
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The invention discloses a 2,2'-azo(2-methyl-N-(2-hydroxyethyl)propionamide) preparation method, which comprises: adding 2,2'-azobisisobutyronitrile, methanol and toluene to a reactor having a stirring and reflux device, starting stirring, slowly introducing hydrogen chloride gas under cooling, and controlling the temperature of the material and carrying out a thermal insulation reaction; after completing the reaction, adding the reaction liquid into water in a dropwise manner, carrying out a hydrolysis reaction, layering after completing the hydrolysis, adding a small amount of methanol to the organic phase, and carrying out pressure reducing distillation for a certain time; after completing the distillation, slowly adding the organic phase into a mixed solution of sodium methoxide and monoethanolamine in a dropwise manner, and carrying out thermal insulation; after completing the thermal insulation, carrying out solid-liquid separation by a centrifuge, continuously washing the solid with water, crystallizing, carrying out centrifugation until the material is dried, placing the material in a drying device, and drying; and after the drying, cooling the material to a normal temperature to obtain the 2,2'-azo(2-methyl-N-(2-hydroxyethyl)propionamide) product, wherein the product content (HPLC) is more than 98%, and the yield is 55-75%.
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Paragraph 0014; 0032-0060
(2019/10/04)
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- METHOD FOR PRODUCING AZO COMPOUNDS
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PROBLEM TO BE SOLVED: To provide a method that can produce azo compounds at good yields by making oxygen or an oxygen-containing gas act on hydrazo groups of hydrazo compounds when oxidatively dehydrogenating them. SOLUTION: Azo compounds are produced by making oxygen or an oxygen-containing gas act on hydrazo compounds in the presence of vanadium or cerium compounds, and a solvent. SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
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Paragraph 0048; 0062
(2018/05/03)
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- METHOD FOR PRODUCING AZO COMPOUNDS
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PROBLEM TO BE SOLVED: To provide a method that can produce azo compounds at good yields by making oxygen or an oxygen-containing gas act on hydrazo compounds when oxidatively dehydrogenating them. SOLUTION: Azo compounds are produced by making oxygen or an oxygen-containing gas act on hydrazo compounds in the presence of nitrite compounds, bromine compounds and a solvent. SELECTED DRAWING: None COPYRIGHT: (C)2018,JPOandINPIT
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Paragraph 0046
(2018/04/14)
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- Preparation method of azodiisobutyrate
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The invention discloses a preparation method of azodiisobutyrate. The preparation method mainly includes the steps of adding azodiisobutyronitrile, alcohol (R-OH), solvents and ion exchange resins into a reactor with stirring, reacting at a specific temperature for a period of time, and filtering to remove the ion exchange resins; concentrating filtrate and removing the solvents so as to obtain the azodiisobutyrate shown as structural formula in the description, wherein R can be methyl, ethyl, propyl, isopropyl, butyl, isobutyl, pentyl, hexyl, isooctyl, dodecyl, cetyl and octadecyl. With the ion exchange resins as a catalyst, the preparation method is convenient to implement and for after-treatment, environment friendly and little corrosive to equipment, and the catalyst is reusable, high in conversion rate and simple in process.
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Paragraph 0017
(2017/10/07)
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- COMPOUNDERS FOR ENHANCING GENERATION OF CHEMICAL SPECIES
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A reagent that enhances acid generation of a photoacid generator and composition containing such reagent is disclosed. Also described is a method for manufacturing a device, the method including applying a liquid containing a composition to a member such that a coating film including the composition is formed on the member; and exposing the coating film to at least one of a first electromagnetic ray and a first particle ray such that a first portion of the coating film is exposed to the at least one of the first electromagnetic ray and the first particle ray while a second portion of the coating film is not exposed to the at least one of the first electromagnetic ray and the first particle ray.
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Page/Page column
(2015/05/26)
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- Ink composition, inkjet recording method, and printed article
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The present invention provides an ink composition having excellent ink ejection stability and stretching property, curable with a high sensitivity by irradiation of radiation rays, and capable of forming an image excellent in rubfastness and blocking resistance, an inkjet recording method using the ink composition, and a printed article. The ink composition includes (a) a polymer having a siloxane structure and a polymerizable group on a side chain thereof, (b) a polymerizable compound, and (c) a photopolymerization initiator, and the inkjet recording method includes a step of ejecting the ink composition onto a recording medium to be recorded with an inkjet recording apparatus and a step of curing the ink composition by irradiating active radiation rays on the ejected ink composition.
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- Bu3SnH-mediated radical cyclisation onto azoles
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Alkyl radicals have been cyclised onto pyrroles, imidazoles and pyrazoles, and acyl radicals cyclised onto pyrroles, using Bu3SnH-, (TMS)3SiH- and Bu3GeH-mediated aromatic homolytic substitution for the synthesis of bicyclic N-heterocycles. The reactions yield intermediate π-radicals that lose hydrogen in the?rearomatisation step of the aromatic homolytic substitution. Mechanistic studies of these rearomatisation steps indicate aromatic homolytic substitution in which the initiator or breakdown products from the inhibitor are responsible for the H-abstraction step.
- Allin, Steven M.,Barton, William R.S.,Russell Bowman,Bridge (née Mann), Emma,Elsegood, Mark R.J.,McInally, Tom,McKee, Vickie
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p. 7745 - 7758
(2008/12/21)
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- Process for preparing azoiminoethers and azocarboxylic acid esters and novel azocboxylic acid mixed esters
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The invention concerns a method for preparing an azoiminoether hydrochloride which consists in reacting an azonitrile with an alcohol and hydrochloric acid in an aromatic solvent, wherein the molar ratio R=HCl/azonitrile is >2 when the alcohol is methanol and >3 when the alcohol is ethanol or a higher alcohol. The invention also concerns a method for preparing an azocarboxylic acid ester which consists in the synthesis of an azoiminoether hydrochloride by the inventive method and, hydrolysis in the presence of the resulting azoiminoether hydrochloride. Said methods enable to obtain liquid composition of azocarboxylic acid esters. The invention further concerns mixed azoiminoether salts of formula (II′). The invention also concerns mixed azoiminocarboxylic acid esters corresponding to the formula (III′).
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Page column 9
(2010/11/30)
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- Hydrosilylation of unsaturated compounds
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A method for hydrosilylating an olefinically unsaturated compound comprising contacting the unsaturated compound with a source of silicon in the presence of an azo-containing free-radical catalyst, the hydrosilylated product being a useful crosslinking agent.
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- The Cross-Reaction Between 1-Methoxycarbonyl-and 1-Butoxycarbonyl-1-methylethyl: Simultaneous Generation of Unlike Radicals from an Unsymmetrical Azo Precursor
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The title radicals (1a) and (1b) were generated simultaneously by thermolysis of the unsymmetrical diazene, butyl methyl azoisobutyrate (2d).In the presence of the radical scavenger 2,2,6,6-tetramethylpiperidin-1-yloxyl (4) the products of the geminate cross-reaction show that 45percent of radical pairs react by combination and 55percent by disproportionation.The disproportionation reaction shows a slight preference for hydrogen transfer from the butyl ester (1b) to the methyl ester (1a) radical.In the absence of scavenger (4), the encounter reactions of the two radicals show aslight preference for the cross-reaction over the two self-reactions which is most likely largely due to the imbalance in radical concentrations caused by the greater reactivity toward addition to olefins of the methyl ester radical.
- Kelly, David P.,Serelis, Algirdas K.,Solomon, David H.,Thompson, Philip E.
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p. 1631 - 1639
(2007/10/02)
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- The Self-Reactions of 1-Methoxycarbonyl-1-methylethyl and Higher Ester Radicals: Combination vs Disproportionation and Oligomeric Products from Secondary Reactions
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The geminate self-reactions of the title methyl, ethyl and butyl ester radicals (2a-c), formed by decomposition of the corresponding azo precursors (1a-c) in the presence of stable nitroxide radical scavengers, were found on the basis of product analysis to comprise combination and disproportionation in the ratios 56 : 44 (methyl), 58 : 42 (ethyl) and 47 : 53 (butyl).In the absence of radical scavengers, extensive oligomerization is observed.Hydrogenation and degradation were used in conjunction with g.l.c.-m.s. to deduce the identities of the dimeric, trimeric and tetrameric products, which were in most cases subsequently confirmed by isolation and n.m.r. analysis.Of particular interest is the highly regioselective disproportionation of radical (3) to give dimethyl 4-methylpent-1-ene-2,4-dicarboxylate (8), and the further reaction of (8) with (2a) to form branched oligomers (10) and (15).
- Bizilj, Snezna,Kelly, David P.,Serelis, Algirdas K.,Solomon, David H.,White, Kathleen E.
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p. 1657 - 1673
(2007/10/02)
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