- Method for preparing 2, 2-bis (3-nitro-4-hydroxyphenyl) hexafluoropropane by microchannel reactor
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The invention discloses a method for preparing 2, 2-bis (3-nitro-4-hydroxyphenyl) hexafluoropropane by a microchannel reactor. The method comprises the following steps: (1) fully mixing and preheating bisphenol AF and an organic solvent to obtain a bisphenol AF solution, and respectively introducing the bisphenol AF solution and a preheated nitrating agent as two strands of materials into a continuous flow microchannel reactor through a metering pump; (2) controlling the flow rate of the material through a metering pump, enabling the bisphenol AF solution and the nitrating agent to respectively enter a micro-channel reactor module for mixed reaction, and enabling a product to flow out from an outlet of the reactor; and (3) carrying out post-treatment on the material obtained from the outlet of the microchannel reactor to obtain a pure product of 2, 2-bis (3-nitro-4-hydroxyphenyl) hexafluoropropane. The method provided by the invention can realize continuous production, has mild reaction conditions, high reaction efficiency and high yield, and is suitable for industrial production.
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Paragraph 0029-0046
(2021/07/14)
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- Preparation method of 5, 5'-(perfluoropropane-2, 2-diyl) bis (2-(allyloxy) aniline)
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The invention provides a preparation method of 5, 5'-(perfluoropropane-2, 2-diyl) bis (2-(allyloxy) aniline), and relates to the technical field of synthesis of chemical intermediates. The preparation method comprises the steps of dissolving 4, 4 '-(hexafluoroisopropylidene) diphenol in glacial acetic acid and nitric acid, reacting to obtain 2, 2-bis (3-nitro-4-hydroxyphenyl) hexafluoropropane, dissolving the product in acetonitrile, adding potassium carbonate and 3-bromopropylene, and reacting to obtain 5, 5'-(perfluoropropane-2, 2-diyl) bis (2-(allyloxy) nitrobenzene); and reacting 5, 5 '-(perfluoropropane-2, 2-diyl) bis (2-(allyloxy) nitrobenzene), iron powder and ammonium chloride to obtain 5, 5'-(perfluoropropane-2, 2-diyl) bis (2-(allyloxy) aniline). The synthetic route is mild in reaction condition, simple in reaction and post-treatment process operation, low in reaction danger coefficient, low in production cost and suitable for industrial large-scale production.
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Paragraph 0034; 0041-0044; 0053-0054; 0064
(2021/11/14)
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- Preparation method for bis(3-amino-4-hydroxyphenyl)hexafluoropropane
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The invention belongs to the technical field of electronic chemical materials, and more specifically relates to a preparation method for bis(3-amino-4-hydroxyphenyl)hexafluoropropane. The preparationmethod for the bis(3-amino-4-hydroxyphenyl)hexafluoropropane disclosed by the invention comprises the following steps: step 1, introducing hexafluoroacetone into a reactant (I) in the presence of a catalyst for a reaction so as to obtain a compound (II); step 2, allowing the compound (II) obtained in the step 1 with nitric acid and sulfuric acid so as to obtain a compound (III); step 3, adding thecompound (III) obtained in the step 2 into inorganic base for a reaction so as to obtain a compound (IV); and step 4, carrying out catalytic hydrogenation on the compound (IV) obtained in the step 3so as to obtain the bis(3-amino-4-hydroxyphenyl)hexafluoropropane.
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Paragraph 0110-0115
(2020/07/13)
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- Environmentally friendly preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane
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The invention relates to an environmentally friendly preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane. The technology comprises the following steps: preparing a 1,2-dichloroethane solution of bisphenol AF; preparing a 1,2-dichloroethane solution of N2O5; carrying out a nitration reaction to generate 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane; filtering the 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, washing the 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, and layering the 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane to obtain a lower layer organic phase; carrying out dehydration drying, filtering the obtained material, and carrying out vacuum distillation to obtain crude 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane; and re-crystallizing the crude 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, cooling the re-crystallized 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, filtering the cooled 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane, and carrying out vacuum drying to obtain purified 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane. The preparation technology adopts dinitrogen pentoxide (N2O5) as a nitration agent and allows the reaction to be carried out a low temperature, so pollution of waste acids is thoroughly eliminated, and toxic, harmful and highly risky byproducts are reduced, and the nitration reaction is clean and environmentally friendly.
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Paragraph 0032; 0033; 0034
(2016/12/12)
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- Method of producing 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane
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Disclosed herein is a method of producing 2,2-bis(3-nitro-4-hydroxphenyl)hexafluoropropane, which comprises (a) preparing 2,2-bis(4-hydroxyphenyl)hexafluoropropane and a lower fatty acid; and (b) allowing the 2,2-bis(4-hydroxyphenyl)hexafluoropropane to react with nitric acid in the lower fatty acid.
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