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81results about How to "Does not generate corrosive substances" patented technology

Method for preparing 2,2-di[3-amino-4-(2,4-dinitrophenoxy)phenyl]hexafluoropropane

The invention relates to a preparation method of 2, 2-bis-[3-amino-4-(2, 4-dinitrophenoxy) phenyl] hexafluoropropane, comprising: (1) heating to reflux and segregate water for 6-18h to treat 2, 2-bis-(3-amino-4-hydroxy phenyl and 2, 4-dinitro halogenated benzene at a mol ratio of 1.0:2.0 to 2.2, in a system of salt forming agent and organic solvent, (2) concentrating reaction liquid, cooling the reactant system, adding water, precipitating solid product, filtering, washing and drying to obtain 2, 2-bis-[3-amino-4-(2, 4-dinitrophenoxy) phenyl] hexafluoropropane crystal. The preparation method of 2, 2-bis-[3-amino-4-(2, 4-dinitrophenoxy) phenyl] hexafluoropropane has simple operation, high yield and purity, wherein the solvent can be recovered easily and repeatedly used. The invention has low generation of three wastes and environment-friendly property, which is suitable for industrial production.
Owner:DONGHUA UNIV

Method for preparing 2,2-dual [3-amido-4-(4-nitrophenoxy)phenyl group]-1,1,1,3,3,3-hexa-fluoropropane

The invention discloses a making method of 2,2-di [3-amino-4-(4-nitrobenzeneoxy) phenyl]-1,1,1,3,3,3-hexafluoropropane, which comprises the following steps: (1) heating 2, 2-di (3-amino-4-hydroxybenzene)-1,1,1,3,3,3-hexafluoropropane and 4-halogenated nitrobenzene with molar rate at 1. 00: 2. 00-3. 00 under inert gas to reflux and do diversion reaction for 4-18h; (2) condensing the reacting liquid; cooling the reactant system; adding water; evolving solid product; filtering; washing; drying; obtaining the product. The invention simplifies the operation with high receiving rate and purity, which is easy to recycle solvent to use reciprocally to reduce three wastes for industrialized manufacturing.
Owner:DONGHUA UNIV

Method for preparing 4,4'-di(4-aminophenoxy)-3,3',5,5'-tetramethylbiphenyl

The invention relates to a preparation method of 4, 4'-dia(4-aminophenoxy)-3, 3', 5, 5'-tetramethylbenzene, which comprises that 3, 3', 5, 5'- tetramethyl-4', 4'-biphenyl diphenol, and 4- halogenated nitrobenzene, in salt forming agents, strongly polar protonic or water insoluble organic solvent system, are heated, refluxed and divided, concentrated , cooled, and added with water, while the product is precipitated, filtered, washed, and dried to obtain 4, 4'-dia(4-aminophenoxy)-3, 3', 5, 5'-tetramethylbenzene, and the 4, 4'-dia(4-aminophenoxy)-3, 3', 5, 5'-tetramethylbenzene in the reduction system of ferric chloride / 20-85% hydrazine hydrate, the cooperation of alcohol solvent and active carbon, is reacted to obtain final product. The invention has simple and environment-friend operation, which can be used for industrialization production, while the product can reach more than 99% of purity, and the solvent can be reclaimed.
Owner:DONGHUA UNIV

BAHPP type polyimide humidity-sensitive capacitor and preparing method thereof

The invention relates to a BAHPP type polyimide humidity-sensitive capacitor and a preparing method thereof. The humidity-sensitive capacitor is composed of a substrate, a lower electrode, a BAHPP type humidity-sensing polyimide coating and an upper electrode, wherein 2, 2-bis(3-amino-4-hydroxyphenyl)propane (BAHPP), aromatic diamine and aromatic dianhydride react to obtain BAHPP type humidity-sensing polyimide. The preparing method comprises the steps of: placing the substrate into a drying box for drying after cleaning the substrate; carrying out drying; then preparing the lower electrode by means of vacuum vapor plating; guiding a lower electrode lead by JP-6 conductive adhesive; then coating a BAHPP type humidity-sensing polyimide precursor solution in a spin manner; carrying out imidization; preparing the upper electrode by means of vacuum vapor plating; carrying out slicing; flushing with deionized water; carrying out drying; carrying out screening; carrying out surface modifying; guiding an upper electrode lead with JP-6 conductive adhesive; and preparing the BAHPP type polyimide humidity-sensitive capacitor. The BAHPP type polyimide humidity-sensitive capacitor and the preparing method thereof has the advantages of high sensitivity, small humidity hysteresis, simple preparing process, low cost, good market prospect and the like.
Owner:DONGHUA UNIV +1

Process for preparing biphthalimide

The invention relates to a method for preparing biphthalimide, comprising following steps: (1) putting binary primary amine and ortho-phthalic anhydride with the molar ratio being 1.0: 2.0-2.5 in strong polar non-polar organic solvent, reacting for 1-5 hours at 0- 10 Deg. C and getting clean, transparent and homogeneous solution; (2) adding azeotropic anhydrating agent, heating to 110- 150 Deg. C, refluxing imination catalyst and reacting for 1- 10 hours, cooling, crystallizing, filtering, washing and drying, getting biphthalimide, and volume ratio between strong non-polar organic solvent and azeotropic anhydrating agent is 1.0: 0.1- 10. The invention is characterized by high productivity, high purity of above 99%, reusable solvent, simple operation, environment-friendly and suitability for industrial production.
Owner:DONGHUA UNIV

Method for preparing N-methyl phthalimide compound

The invention relates to a preparation method for N-methyl phthalimide compound, which is a synthetic method for preparing N-methyl phthalimide compound under the action of tertiary amine as catalyst by using phthalimide compound as raw material and dimethyl carbonate as a methylating agent. The preparation method has the advantages of simple operation, low toxicity and little environment pollution, which is applied to industrial production. Meanwhile, the obtained product is high in yield with purity being more than 98 percent.
Owner:DONGHUA UNIV

Method for preparing 4,4'-di(2,4-dinitro-phenoxy) sulfone

The invention relates to a method for preparing 4, 4'-double (2, 4- dinitrophenoxy) sulfone, which comprises the steps that: (1) 4, 4'-dihydroxy diphenyl sulfone and 2, 4- dinitrohalobenzenes with a molar ratio ranging from 1.0 : 2.0 to 1.0 : 2.2 are subject to a heat refluxing and water diversion reaction for 6 to 18 hours in a system comprising salt forming agents and organic solvents; (2) the reaction solution is concentrated, the reactant system is cooled, and the water is added in the reactant system so as to precipitate the solid product; the obtained product is filtered, washed and dried so as to obtain 4, 4'-double (2, 4- dinitrophenoxy) sulfone. The invention has simple operations and high product yield and purity, the solvents can be conveniently recycled and can be repeatedly used with few wastes, and the invention is environmentally friendly and suitable for industrialized production.
Owner:DONGHUA UNIV

Method for preparing 2,2-di(3-amido-4-(2,4-dinitrophenoxy) phenyl] propane

The invention relates to a method for preparing 2, 2-double [3- amino-4-(2, 4- dinitrophenoxy) phenyl] propane, which comprises the steps that: (1) 2, 2-double(3- amino-4- hydroxyphenyl) propane and 2, 4-dinitrohalobenzenes with a molar ratio ranging from 1.0 : 2.0 to 1.0 : 2.2 are subject to a heat refluxing and water diversion reaction for 6 to 18 hours in a system comprising the nitrogen atmosphere, salt forming agents and organic solvents; (2) the reaction solution is concentrated, the reactant system is cooled and the water is added in the reactant system so as to precipitate the solid product; the obtained solutions are filtered and the obtained products are washed and dried so as obtain 2, 2-double [3- amino-4-(2, 4- dinitrophenoxy) phenyl] propane Crystal. The invention has simple operations and high product yield and purity, the solvents can be conveniently recycled and can be repeatedly used with few wastes, and the invention is environmentally friendly and suitable for industrialized production.
Owner:DONGHUA UNIV

Preparation method of 2,2 bi-[3-nitryl-4-(2,6-dinitryl-4-trifluoromethyl phenoxy)phenyl] propane

The present invention relates to a preparation method of 2, 2-bis [3-nitro-4-(2, 6-dinitro-4-trifluoromethyl phenoxy) benzyl] propane. The preparation method comprises the following steps: firstly, 2, 2-bis (3-nitro-4-hydroxyphenyl) propane and 2, 6-dinitro-4-trifluoromethylphenyl halide with a molar ratio of from 1.0 to 2.0 to 2.2 are added into a system of salifying agent and organic solvent, and the system is heated and perform refluxing and water segregation reaction of 6 to 18 hours; secondly, the reaction solution is condensed, the reactant system is cooled, water is added, and solid products are separated, filtered, washed and dried to prepare the 2, 2-bis [3-nitro-4-(2, 6-dinitro-4-trifluoromethyl phenoxy) benzyl] propane. The present invention has the advantages that the operation is simple, the yield rate and purity of the product are high, the solvent recovery is convenient and the solvent can be repeatedly used, the three wastes are less, the preparation method is environment friendly, and the present invention is suitable for industrial production.
Owner:DONGHUA UNIV

Method for preparing 3,7-di(2,4-dinitrophenoxy)-2-naphthoic acid

The invention relates to a preparation method of 3, 7-bi-(2, 4-dinitrophenoxy)-2-naphthoic acid, which comprises (1), heating, refluxing and water segregating for 3-18h to treat 3, 7-dihydroxynaphthalene-2-aminic acid and 2, 4-dinitro halogenated benzene at the mol ratio of 1.0:2.0-2.2, in the system of salt forming agent and organic solvent, (2), condensing reaction liquid, cooling reactant system, adding water, precipitating solid product, filtering, immerging in dilute acid solution, filtering, washing and drying to obtain 3, 7-bi-(2, 4-dinitrophenoxy)-2-naphthoic acid. The preparation method of 3, 7-bi-(2, 4-dinitrophenoxy)-2-naphthoic acid has simple operation, high yield and purity, easily recovered and circulated solvent, less generation of three wastes, environment-friend property and application in industrial production.
Owner:DONGHUA UNIV

Preparation method of 4,4'-bi(2-trifluoromethyl-4-aminophenoxyl)biphenyl

The invention relates to a preparation method of 4,4'-bi(2-trifluoromethyl-4-aminophenoxyl)biphenyl, comprising the steps of adding 4,4'-bi(2-trifluoromethyl-4-nitrophenoxyl)biphenyl, an organic mixed solvent containing alcohols, and a catalyst in a high pressure reaction kettle, infusing hydrogen, stirring, substituting residual air, continuously infusing hydrogen, heating and raising temperature, reacting for 2-4 hours, cooling the reaction system to room temperature, slowly discharging pressure, and infusing nitrogen to substitute all residual air so as to ensure that the high pressure reaction kettle is in inert atmosphere, filtering, recovering filter residue, maintaining the mother liquid, condensing the mother liquid such that the solid content of the mother liquid is in the range of 40-80%, cooling, putting the mother liquid aside, separating out white crystal product, filtering, washing and drying to obtain 4,4'-bi(2-trifluoromethyl-4-aminophenoxyl)biphenyl solid. The method has a simple technology, low cost, high purity and yield, and is environment-friendly and suitable for commercial production.
Owner:DONGHUA UNIV

Preparation method of 2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene

The invention relates to a preparation method of 2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene, comprising the steps of adding 2,5-bi(2-trifluoromethyl-4-nitrophenoxyl)toluene, an organic solvent, and a palladium / carbon catalyst in a reaction kettle, heating the reaction kettle, stirring, raising temperature to 70-80 DEG C, dripping a hydrazine hydrate aqueous solution, strictly controlling thedripping time within 1-1.5 hours, reacting for 2-4 hours at 70-80 DEG C after finishing dripping the aqueous solution, filtering when the solution is hot, removing filter residues, maintaining the mother liquid, dripping deionised water into the mother liquid while stirring, putting the mother liquid aside for 5-8 hours, separating out white solid product, filtering, washing and drying to obtain2,5-bi(2-trifluoromethyl-4-aminophenoxyl)toluene solid. The method has a simple technology, low cost, high purity and yield, and is environment-friendly and suitable for commercial production.
Owner:DONGHUA UNIV

Process for producing 3,3',5,5'-tetramethyl-4,4'-di(2-trifluoromethyl-4-nitrophenoxy)biphenyl

The invention relates to a preparation method of 3, 3', 5, 5'- tetramethyl -4, 4'-double (2-trifluoromethane-4-nitrobenzene oxy) diphenyl. The invention comprises the following steps: (1) mixing 3, 3', 5, 5'-tetramethyl-4, 4'-dihydroxy diphenyl and 2-chlorine-5-nitryl trifluoromethyl benzene by the mol ratio of 1.0:2.0-2.6, and then adding the mixture into a mixed solvent of salifying agent, soluble organic solvent and non-soluble organic solvent for reaction for 4 to 15 hours at 100 to 180 DEG C; (2) filtering when the solvent is hot, eliminating filter residue, condensing mother liquid, cooling and stewing to precipitate a butter yellow solid product, and then filtering, washing and drying the product to obtain the butter yellow solid powder of 3, 3', 5, 5'-tetramethyl-4, 4'-double(2- trifluoromethyl-4-nitrobenzene oxy) diphenyl. The method with simple process, low cost, environment-friendliness and high purity and yield is applicable to the industrial production.
Owner:DONGHUA UNIV

Method for preparing 4,4'-bis(4-nitro-2-trifluoromethylphenoxy)diphenylsulfone

The invention relates to a method for preparing 4,4'-bis(4-nitro-2-trifluoromethylphenoxy)diphenylsulfone, which comprises the following steps: adding 4,4'-dihydroxydiphenylsulfone and 2-chloro-5-nitrotrifluoromethylbenzene into a reaction kettle; adding a salt forming agent, strong polar aprotic organic solvent and an organic entrainer, stirring the mixture in the reaction kettle at room temperature for 30 minutes, and heating the mixture for azeotropic water separation reaction for 12 to 15 hours; and filtering the hot solution, removing filter residue, concentrating mother solution, cooling and standing the mother solution to precipitate a milky crystal product, filtering the solution, and washing and drying the milky crystal product to obtain the 4,4'-bis(4-nitro-2-trifluoromethylphenoxy)diphenylsulfone. The preparation method has the advantages that: the operation is simple, the raw material resource is readily available, the cost is low, and no corrosive substance is related to or generated; few kinds of organic solvents are used, and the organic solvents can be used repeatedly and circularly and are environmentally-friendly; and the product has a high yield up to more than 98 percent, a purity up to 99.8 percent and a melting point of from 198.4 to 199.2 DEG C and is suitable for industrial production.
Owner:DONGHUA UNIV

Preparation of 1,4-bis(2,4- dinitrophenoxy)-2,3,5- trimethylbenzene

The invention relates to a method to prepare 1,4-bi(2,4-binitro-4-dinitro-phenoxyl) -2,3,5-trimethylbenzene, including the following steps: (1), 2,3,5-trimethyl-hydroquinone and 2,4-binitro-halogenated benzene based on molar ratio of 1.0:2.0-2.2 are heated to reflux and react for 6-18 hours in a system with salt forming agent and organic solvent;(2) after reaction, the solution is concentrated and cooled, and then water is added to separate out the solid product, after that the solution is filtrated, washed and dried, getting 1,4-bi(2,4-binitro-4-dinitro-phenoxyl)-2,3,5-trimethylbenzene crystalloid. The method is simple in operation with high yield and the product is high in purity; the solvent is convenient to recycle and can be used repeatedly; with little wastes(gas, liquid and solid) and being environment-friendly, the method is applicable to industrial production.
Owner:DONGHUA UNIV +1

Preparation of 1,4-bis(2,4- dinitrophenoxy)-2,3,5- trimethylbenzene

The invention relates to a method to prepare 1,4-bi(2,4-binitro-4-dinitro-phenoxyl) -2,3,5-trimethylbenzene, including the following steps: (1), 2,3,5-trimethyl-hydroquinone and 2,4-binitro-halogenated benzene based on molar ratio of 1.0:2.0-2.2 are heated to reflux and react for 6-18 hours in a system with salt forming agent and organic solvent;(2) after reaction, the solution is concentrated and cooled, and then water is added to separate out the solid product, after that the solution is filtrated, washed and dried, getting 1,4-bi(2,4-binitro-4-dinitro-phenoxyl)-2,3,5-trimethylbenzene crystalloid. The method is simple in operation with high yield and the product is high in purity; the solvent is convenient to recycle and can be used repeatedly; with little wastes(gas, liquid and solid)and being environment-friendly, the method is applicable to industrial production.
Owner:DONGHUA UNIV +1

4,4'-bis(4-nitrophenoxy)phenyl sulfide preparation method

The invention relates to a method for preparing 4, 4'-bis (4-nitrophenoxy) diphenyl sulfide ether which comprises the steps: (1) 4,4'-thiobis-phenol and 4-halogenated nitrobenzene with the mol ratio of 1.00 to between 2.00 and 2.22 are subjected to heating reflux water separation reaction for 4 to 18 hours in a system formed by a salt forming agent and an organic solvent; and (2) reaction liquid is concentrated, a reactant system is cooled, water is added to precipitate a solid product, and the 4, 4'-bis (4-nitrophenoxy) diphenyl sulfide ether is obtained through filtration, washing and drying. The method has simple operation, and high yield and purity of products, ensures that the solvent is convenient to reclaim and can be repeatedly used, has less three wastes, is environment-friendly,and is suitable for industrialized production.
Owner:DONGHUA UNIV +1

Process for producing 4,4'bis(2,4-dinitrophenoxy) biphenyl

The invention relates to a preparation method of 4,4'-double (2,4-dinitro phenoxy) biphenyl, which comprises the following steps: first the 4,4'-biphenyl diphenol and 2,4-dinitro halogenated benzene with the molar ratio of 1.0:2.0 to 2.2 are in heating refluxing water division reaction for 6 to 18 hours in a system of a salt forming agent and an organic solvent; second reaction solution is concentrated, reactant system is cooled, water is added, solid products is precipitated, filtered, washed and dried to obtain the 4,4'-double (2,4-dinitro phenoxy) biphenyl. The preparation method is characterized by simple operation, high product yield and purity, solvent being conveniently recovered and reused, little three waste, being environment friendly and being suitable for industrial production.
Owner:DONGHUA UNIV

Method for preparing 2,7-di(2,4-dinitrophenoxy) naphthalene

The invention relates to a method for preparing 2, 7-double (-2, 4 dinitrophenoxy) naphthalene, which comprises the steps that: (1) 2, 7-naphthalenediol and 2, 4- dinitrohalobenzenes with a molar ratio ranging from 1.0 : 2.0 to 1.0 : 2.2 are subject to a heat refluxing and water diversion reaction for 6 to 18 hours in a system comprising the salt forming agents and organic solvents; (2) the reaction solution is concentrated, the reactant system is cooled and the water is added in the reactant system to precipitate the solid product; the obtained solutions are filtered, the obtained products are washed and dried so as to obtain 2, 4-double (-2, 4 dinitrophenoxy) naphthalene. The invention has simple operations and high product yield and purity, the solvents can be conveniently recycled and can be repeatedly used with few wastes, and the invention is environmentally friendly and suitable for industrialized production.
Owner:DONGHUA UNIV

Preparation of 4,4'-bis(2,6- binitro-4-trifluoromethyl phenoxy)-3,3',5,5'-tetramethyl biphenyl

The invention relates to a method for making 4, 4'-bis (2,6-dinitro-4-trifluoromethylphenoxy)-3,3'5,5'-tetramethyldiphenyl, comprising the steps of: (1) carrying out heating, refluxing and water diversion of 4, 4'-dihydroxyl-3,3',5,5'-tetramethyldiphenyl and 2,6-dinitro-4-trifluoromethyl halogenated benzene mixed in a molar ratio of 1.0 : 2.0-2.2 in systems of salt forming agent and organic solvent for a reaction of 6 to 18 hours; (2) condensing reaction liquid, cooling a reactant system, adding water, separating out a solid product, and filtering, washing and drying the solid product to obtain 4, 4'-bis (2,6-dinitro-4-trifluoromethylphenoxy)-3,3'5,5'-tetramethyldiphenyl crystal. The invention has the advantages of simple operation, high product yield and high purity, convenient solvent recycling, repeated use, less three wastes, environment protection, and is suitable for industrialized production.
Owner:DONGHUA UNIV

Method for preparing 1,4-di(2,4-dinitrophenoxy)naphthalene

The invention relates to a preparation method of 1, 4-bis-(2, 4-dinitrophenoxy) naphthalene, comprising: (1) heating to reflux and segregate water for 3-18h to treat 1, 4-naphthalenediol and 2, 4-dinitro halogenated benzene at a mol ratio of 1.0:2.0 to 2.2, in a system of salt forming agent and organic solvent; (2) concentrating reaction liquid, cooling the reactant system, adding water, precipitating solid product, filtering, washing and drying to obtain 1, 4-bis-(2, 4-dinitrophenoxy) naphthalene. The preparation method of 1, 4-bis-(2, 4-dinitrophenoxy) naphthalene has simple operation, highyield and purity, wherein the solvent can be recovered easily and repeatedly used. The invention has low generation of three wastes and environment-friendly property, which is suitable for industrialproduction.
Owner:DONGHUA UNIV

Method for preparing 1,3,5-tri(2,4-dinitrophenoxy) benzene

The invention relates to a method for preparing 1, 3, 5-three(-2, 4 dinitrophenoxy) benzene, which comprises the steps that: (1) 1, 3, 5-phloroglucin and 2, 4-dinitrohalobenzenes with a molar ratio ranging from 1.0 : 3.0 to 1.0 : 3.2 are subject to a heat refluxing and water diversion reaction for 6 to 18 hours in a system comprising the salt forming agents and organic solvents; (2) the reaction solution is concentrated, the reactant system is cooled and the water is added in the reactant system so as to precipitate the solid product; the obtained solutions are filtered, the obtained productsare washed and dried so as to, obtain 1, 3, 5-three (-2, 4 dinitrophenoxy) benzene. The invention has simple operations and high product yield and purity, the solvents can be conveniently recycled and can be repeatedly used with few wastes, and the invention is environmentally friendly and suitable for industrialized production.
Owner:DONGHUA UNIV

A kind of biphenyl type polyimide humidity sensitive capacitor and preparation method thereof

The invention relates to a humidity-sensitive biphenyl polyimide capacitor and a making method thereof. The humidity-sensitive capacitor is composed of a substrate, a lower electrode, a humidity-sensitive biphenyl polyimide coating layer and an upper electrode, wherein humidity-sensitive biphenyl polyimide is prepared through a reaction of 3,3'-diamino-4,4'-dihydroxybiphenyl, aromatic diamine and aromatic dianhydride. The making method comprises the following steps: cleaning the substrate by using a cleaning solution, putting the cleaned substrate in a drying box, drying, carrying out vacuum vapor plating to make the lower electrode, guiding a lower electrode leading wire through a JP-6 conductive adhesive, spin-coating a humidity-sensitive biphenyl polyimide precursor solution, imidizing, carrying out vacuum vapor plating to make the upper electrode, slicing, flushing by using deionized water, drying, screening, carrying out surface modification, and guiding an upper electrode leading wire through the JP-6 conductive adhesive to make the humidity-sensitive biphenyl polyimide capacitor. The humidity-sensitive biphenyl polyimide capacitor has the advantages of high sensitivity, small humidity hysteresis, simple manufacturing process, low cost and good market prospect.
Owner:DONGHUA UNIV +1

Method for preparing 4,4', di(2,6-dinitro-4-trifluoromethyl phenoxy)diphenyl ether

The invention relates to a preparation method of 4, 4'-bis (2, 6-dinitro-4-trifluoromethyl phenoxy) diphenyl ether, including the following steps: (1) in salifying agents and the organic solvent system, 4, 4'-dihydroxy diphenyl ether and 2, 6-dinitro-4-trifluoromethyl halogeno benzene with a molar ratio of 1.0:2.0 to 2.2 carry on heating reflux water reaction for six to eighteen hours; (2) the reaction liquid is condensed; the reactant system is cooled; water is added to precipitate solid product; after filtered, washed and dried, the crystal of 4, 4'- bis(2, 6-dinitro-4 trifluoromethyl phenoxy) diphenyl ether is obtained. The method of the invention has the advantages of simple operation, high yield and purity of products, convenient recovery of solvent, repeated use, fewer three wastes, friendly environment and applicable to the industrial production.
Owner:DONGHUA UNIV

Preparation of 1,4-bis(2-trifluoromethyl-4-nitrophenoxy)-2,5-di-t-butylbenzene

The invention relates to a method for preparing 1, 4-dual (2-trifluoromethyl-4-nitrophenoxy)-2, 5-dual tert-butylbenzene, comprising the steps: (1) 2, 5-dual tert-butylbenzene-1, 4-hydroquinone and 2-chlorine-5-nitryl trifluoromethyl benzene are dissolved into the mixed solvent of salt forming agent, strongly polar aprotic organic solvent and organic entrainer according to the mol ratio of 1.0:2.0-2.4, and heated for azeotropic water diversion reaction for 12-20h; (2) the mixture is filtered in heat, filter residue is removed, master liquor is concentrated and cooled in a static way, and milky yellow crystal product is separated out, filtered, washed and dried to obtain the 1, 4-dual (2-trifluoromethyl-4-nitrophenoxy)-2, 5-dual tert-butylbenzene. The preparation method has simple operation, wide raw material source and low cost, and does not relate to corrosive substance; the using sorts of the organic solvent are less, and the organic solvent can be repeatedly recycled and environment-friendly; furthermore, the yield of the product reaches over 92%, and the purity reaches 99.7%, so that the method is suitable for commercial process.
Owner:DONGHUA UNIV

Method for preparing 3,5-di(2,4-dinitrophenoxy)trifluorotoluene

The invention relates to a preparation method of 3, 5-bi-(2, 4-dinitrophenoxy) benzotrifluoride, which comprises (1), heating, refluxing and water segregating for 3-18h to treat 3, 5-dihydroxy benzotrifluoride and 2, 4-dinitro halogenated benzene at the mol ratio of 1.0:2.0-2.2, in the system of salt forming agent and organic solvent, (2), condensing reaction liquid, cooling reactant system, adding water, precipitating solid product, filtering, washing and drying to obtain 3, 5-bi-(2, 4-dinitrophenoxy) benzotrifluoride. The preparation method of 3, 5-bi-(2, 4-dinitrophenoxy) benzotrifluoride has simple operation, high yield and purity, easily recovered and circulated solvent, less generation of three wastes, environment-friend property and application in industrial production.
Owner:DONGHUA UNIV

Process for producing 2,2-di[4-(2-trifluoromethyl-4-nitrophenoxy)phenyl] hexafluoroacetore

The invention relates to a preparation method of 2, 2-double [4-(2-trifluoromethane-4-nitrobenzene oxy) phenyl] hexafluoropropane. The invention comprises the following steps: (1) mixing 2, 2-double(4-hydroxyl phenyl) hexafluoropropane and 2-chlorine -5-nitryl trifluoromethyl benzene by the mol ratio of 1.0:2.0-2.5, then adding the mixtrue into a mixed solvent of a salifying agent and anhydrous organic solvent for reaction for 5 to 10 hours at 110 to 200 DEG C; (2) filtering when the solvent is hot, eliminating filter residue, condensing mother liquid, cooling and stewing to precipitate a milky solid product, and then filtering, washing and drying the product to obtain the milky solid powder of 2, 2-double [4-(2-trifluoromethyl-4-nitrobenzene oxy) phenyl] hexafluoropropane. The method with simple process, low cost, environment-friendliness and high purity and yield rate is applicable to the industrial production.
Owner:DONGHUA UNIV

Method for preparing 1,4-bis(2,6-di-nitryl-4-trifluoromethyl phenoxy)-2,5 bi-utylbenzene

The present invention relates to a preparation method of 1, 4-bi (2, 6-dinitro-4-trifluoromethyl phenoxy)-2, 5-di-tert-butyl benzene. The preparation method comprises the following steps: (1) 2, 5-di-tert-butyl hydroquinone and 2, 6-dinitro-4-trifluoromethyl halogenated benzene with the molar ratio of from 1.0 : 2.0 to 2.2 are put in the system of salt-forming agent and organic solvent for 6 to 18 hours with heated reflux reaction and water diversion; (2) the reaction solution is concentrated; the reaction system is cooled; water is added; solid products are separated, filtered, washed and dried to prepare the crystals of the 1, 4-bi (2, 6-dinitro-4-trifluoromethyl phenoxy)-2, 5-di-tert-butyl benzene. The preparation method has the advantages of simple operation, high yield of the product, high purity of the product, convenient recovery of the solvent that can be used repeatedly, less three-waste, less environmental pollution, and suitability for the industrial production.
Owner:DONGHUA UNIV

Method for preparing 1,4-di(2,6-dinitryl-4-trifluoromethyl phenoxy)-2,6-dimethyl benzene

The invention relates to a method for preparing 1,4-bis(2,6-binitro-4-trifluoromethylphenoxy)-2,6-dimethylbenzene, which comprises (1) allowing 2,6-dimethoxybenzene and 2,6-binitro-4-trifluoromethyl halogenated benzene at molar ratio of 1.0:(2.0-2.2) to react in a system of salifying agent and organic solvent while refluxing by heating for water separation for 6-18 hours; and (2) concentrating the reactant liquor, cooling the reactant system, adding water, adding water to separate out solid product, filtering, washing and drying to obtain product crystal. The method has simple process, convenient solvent recovery, repeated used of the solvent, less three wastes, environment friendliness, and suitability for industrialized production. The obtained product has high yield hand purity.
Owner:DONGHUA UNIV
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