- Synthesis method of 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane
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The invention discloses a synthesis method of 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane, which comprises the following steps: acetylating o-aminophenol serving as a starting material to obtain o-acetamidophenol, condensing the o-acetamidophenol with hexafluoroacetone trihydrate to obtain 2, 2-bis (3-acetamido-4-hydroxyphenyl) hexafluoropropane, and finally deacetylating to obtain the 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane. The synthetic route does not need catalytic hydrogenation or nitration, and compared with the existing route for synthesizing 2, 2-bis (3-amino-4-hydroxyphenyl) hexafluoropropane, the synthetic route provided by the invention has the advantages of higher safety, more environmental friendliness, lower production cost and basically equivalent yield, thereby being more suitable for industrial mass production.
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Paragraph 0030; 0033; 0034; 0037-0039
(2021/04/29)
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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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- Synthesis method of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride
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The invention belongs to the technical field of synthesis of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride, in particular to a synthesis method of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride. The synthesis method has the advantages of easy separation of intermediate products, high yield, less waste and good economic benefit, and a mixed solvent of isobutanol and butyl acetate is adoptedto reduce the solubility of the product, facilitate the separation of the product and increase the yield. Besides, the Pd/C catalyst is pretreated, a proper amount of sulfide is added for pretreatment, the sulfur poisoning resistance of the catalyst is improved, the service life of the catalyst is prolonged, and the application frequency of the catalyst is increased; because nitro compounds contain trace amount of sulfides such as sulfuric acid and like, catalyst is easily poisoned. In the step 2, an alumina-silica gel catalyst is added so that 2, 2-bis (3-amino-4-hydroxyphenyl) molecules canbe adsorbed on the surface of the catalyst in a flat shape, hydroxyl is closer to the surface of the catalyst, and the amination reaction of hydroxyl is facilitated; in the step 4, a small amount of urea is added in the cyanolysis reaction to prevent diazonium salt from being oxidized, becoming tar and other side reactions.
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Paragraph 0009; 0011; 0014
(2020/09/09)
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- Synthesis process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride
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The invention belongs to the technical field of synthesis of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride, in particular to a synthesis process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride. The synthesis process has the advantages of easy separation of intermediate products, high yield, less waste and good economic benefit, adopts a mixed solvent of long-chain alcohol and ester, reduces the solubility of the product, is beneficial to product separation, and has higher yield. Besides, the Pd/C catalyst is pretreated, a proper amount of sulfide is added for pretreatment, the sulfurpoisoning resistance of the catalyst is improved, the service life of the catalyst is prolonged, and the application frequency of the catalyst is increased; because nitro compounds contain trace amount of sulfides such as sulfuric acid and like, catalyst is easily poisoned. In the step 2, an alumina-silica gel catalyst is added so that 2, 2-bis (3-amino-4-hydroxyphenyl) molecules can be adsorbed on the surface of the catalyst in a flat shape, hydroxyl is closer to the surface of the catalyst, and the amination reaction of hydroxyl is facilitated; in the step 4, a small amount of urea is addedin the cyanolysis reaction to prevent diazonium salt from being oxidized, becoming tar and other side reactions.
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Paragraph 0010; 0012; 0015
(2020/09/09)
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- Preparation process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride
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The invention belongs to the technical field of synthesis of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride, in particular to a preparation process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride. The preparation process has the advantages of easy separation of intermediate products, high yield, fewer wastes and favorable economic benefit, and adopts a mixed solvent of amyl alcohol and butyl acetate to lower the solubility of the product, thereby being beneficial to product separation and higher yield. Besides, the Pd/C catalyst is pretreated, a proper amount of sulfide is added for pretreatment, the sulfur poisoning resistance of the catalyst is improved, the service life of the catalyst is prolonged, and the application frequency of the catalyst is increased; because nitro compounds contain trace amount of sulfides such as sulfuric acid and like, catalyst is easily poisoned. In the step 2, an alumina-silica gel catalyst is added so that 2, 2-bis (3-amino-4-hydroxyphenyl) molecules can be adsorbed on the surface of the catalyst in a flat shape, hydroxyl is closer to the surface of the catalyst, and the amination reaction of hydroxyl is facilitated; in the step 4, a small amount of urea is added in the cyanolysis reaction to prevent diazonium salt from being oxidized, becoming tar and other side reactions.
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Paragraph 0011; 0014
(2020/09/09)
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- Method for producing bis(3-amino-4-hydroxyphenyl) compounds
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Disclosed is a method for producing bis(3-amino-4-hydroxyphenyl) compounds, which comprises reducing bis(3-nitro-4-hydroxyphenyl) compounds with hydrazines in the presence of a catalyst. The method produces bis(3-amino-4-hydroxyphenyl) compounds of high quality under mild conditions at high yields. The products can be isolated and purified in a simple manner to have a higher purity. The method is suitable to industrial-scale production of the products.
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