cas 2855-13-2, Isophorondiamine | Articles data

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Method for preparing IPDI (isophorone diisocyanate)
The invention discloses a method for preparing IPDI (isophorone diisocyanate). The method comprises the following steps: (1) isophorone and hydrogen cyanide are subjected to a reaction in the presenceof a catalyst to obtain isophorone nitrile; (2) isophorone nitrile obtained in step (1), ammonia and hydrogen are subjected to a reaction in the presence of a catalyst to obtain isophorone diamine; (3) isophorone diamine is subjected to a phosgenation reaction to obtain IPDI, wherein the content of impurities containing secondary amine groups in isophorone diamine subjected to the phosgenation reaction in step (3) is smaller than or equal to 0.5wt%, preferably smaller than or equal to 0.3wt%, and more preferably smaller than or equal to 0.1wt%. By means of the method, content of hydrolyzed chlorine in the IPDI product can be effectively reduced, the yellowing resistance of the product is effectively improved, and the harm that downstream products are unqualified due to existence of hydrolyzed chlorine in the product is reduced.
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(2019/06/13)

Synthesis method of isophorone diamine
The invention relates to a synthesis method of isophorone diamine. The method includes the following steps that 1, in the presence of a catalyst, isophorone (IP) and nitromethane (NM) are subjected to addition reaction, and a nitromethyl-isophorone (NMIP) crude product is prepared; 2, the nitromethyl-isophorone (NMIP) crude product prepared in the step 1 is purified, and a nitromethyl-isophorone(NMIP) pure product is prepared; 3, the nitromethyl-isophorone (NMIP) pure product prepared in the step 2 is dissolved in a solvent, organic acid ammonia salt is added, reaction is conducted in the presence of a catalyst to generate isophorone diamine synthetic liquid, and finally, an isophorone diamine product is obtained through purification. According to the method, highly toxic hydrocyanic acid does not serve as necessary raw materials, high-pressure hydrogen and liquid ammonia are not used as raw materials for reaction, the technological process is safe and environmentally friendly, investments are saved, and the economic benefits are remarkable.
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Paragraph 0040; 0041; 0043; 0044

(2018/03/24)

Process For Preparing Amino Compounds From Nitrile Compounds
The present invention relates to a process for hydrogenating nitrile compounds to amino compounds, in which the cross-sectional loading of the reactor during the hydrogenation is less than or equal to 4.0 kg/m2*s, based on the liquid phase.
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Paragraph 0074; 0075; 076

(2018/12/11)

A process for preparing isophorone diamine
The invention discloses a method for preparing isophorone diamine, and is characterized in that the method comprises the following steps: 1) under the condition of an organic amine catalyst, with isophorone and nitromethane as raw materials, synthesizing 3-nitromethyl-3,5,5-trimethylcyclohexanone, wherein the reaction temperature is 0 DEG C-150 DEG C, and the amount of the organic amine catalyst is 1-300% of the mass of the substance amount of isophorone; and 2) under conditions of liquid ammonia, hydrogen and a metal cobalt catalyst, allowing 3-nitromethyl-3,5,5-trimethylcyclohexanone to undergo a reaction to generate isophorone diamine, wherein the reaction temperature is 30-300 DEG C, the liquid ammonia amount is 1-50 times of the substance amount of 3-nitromethyl-3,5,5-trimethylcyclohexanone, and the hydrogen pressure is 0.1-10 MPa. The nitromethane with lower toxicity is used for replacing highly-toxic hydrogen cyanide or thiocyanate, and thus the method is a technical route which is safer in process and friendlier to the environment.
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Paragraph 0049-0052; 0054

(2017/08/26)

PROCESS FOR PREPARING 3 AMINOMETHYL-3,5,5-TRIMETHYLCYCLOHEXYLAMINE
Process for preparing isophoronediamine, characterized in that A) isophoronenitrile is subjected directly in one stage to aminating hydrogenation to give isophoronediamine in the presence of ammonia, hydrogen, a hydrogenation catalyst and possibly further additions, and in the presence or absence of organic solvents; or B) isophoronenitrile is first converted fully or partly in at least two or more than two stages to isophoronenitrile imine, and this isophoronenitrile imine is subjected to aminating hydrogenation to give isophoronediamine as a pure substance or in a mixture with other components and/or isophoronenitrile, in the presence of at least ammonia, hydrogen and a catalyst.
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Paragraph 0138-0139

(2018/01/18)

A 3-aminomethyl -3, 5, 5-trimethyl method for preparing cyclohexylamine
The invention discloses a method for preparing 3-aminomethyl-3,5,5-trimethyl cyclohexylamine (IPDA). The method comprises the following steps: (a), reacting isophorone and halogenated isobutenyl magnesium to obtain 3-(2-methylpropenyl)-3,5,5-trimethyl cyclohexanone (IPA); (b), carrying out zonization reaction on the IPA and ozone to obtain 3-formyl-3,5,5-trimethyl-ring cyclohexanone (IPFM); (c) carrying out imidization reaction on the IPFM and ammonia to obtain 3-aminomethyl-3,5,5-trimethylcyclohexylimide (IPMI); and (d) carrying out catalytic hydrogenation reaction on the IPMI to obtain the IPDA. The method has the advantages that no HCN and hydrazine hydrate are used, no 3-amino-3,5,5-trimethyl-cyclohexanol (IPAA) which is difficult to separate is generated, the device cost is low, the reaction conditions are mild, the process chain is relatively complete and the yield of products are relatively high.
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Paragraph 0017; 0092-0093; 0096-0097

(2017/03/17)

3-aminomethyl -3, 5, 5-trimethyl method for preparing cyclohexylamine (by machine translation)
The present invention provides a 3-aminomethyl -3, 5, 5-trimethyl method for preparing cyclohexylamine. 3-cyano -3, 5, 5-trimethyl cyclohexyl imine the inferior amination reaction material, in the subsequent steps, with the assistance of the circulating material in the 1st 1st-stage hydrogenation reaction by the hydrogenation reaction material, and can effectively inhibit the generation of HCN product, then in the heating can decompose under the action of the alkaline additive to 2nd stage hydrogenation reaction, then heating the alkaline additive decomposition, decomposition reaction material as circulation material part of a 1st-stage hydrogenation reaction to return as adjuvant, 3rd levels of the remaining part of the hydrogenation reaction, to obtain 3-aminomethyl -3, 5, 5-trimethyl cyclohexane, in the product can be effectively reduced 3-cyano -3, 5, 5-trimethyl cyclohexane and secondary amines the content of the product. (by machine translation)
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Paragraph 0061-0065

(2017/03/14)

PROCESS FOR PREPARING 3-AMINOMETHYL-3,5,5-TRIMETHYLCYCLOHEXYLAMINE
Isophoronediamine, is prepared by A) subjecting isophoronenitrile directly in one stage to aminating hydrogenation to give isophoronediamine in the presence of ammonia, hydrogen, a hydrogenation catalyst and an optional additive, and in the presence or absence of an organic solvent; or B) first converting isophoronenitrile fully or partly in at least two or more than two stages to isophoronenitrile imine, and subjecting the isophoronenitrile imine to aminating hydrogenation to give isophoronediamine as a pure substance or in a mixture with another component and/or isophoronenitrile, in the presence of at least ammonia, hydrogen and a catalyst.
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Paragraph 0173

(2016/10/27)

A simple preparation process of isophorone diamine
The invention relates to a simple preparation method of isophorone diamine, and belongs to the technical field of chemical material processing. The preparation method comprises three steps including raw material pretreatment, hydrogenation and purification. The preparation method has the advantages that the process is simple, the implementation is easy, the cost is low, the conversion efficiency is high, and the like. The preparation method is suitable for being popularized and used in industry in a large scale.
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Paragraph 0019-0023

(2017/02/23)

METHOD FOR PREPARING 3-AMINOMETHYL-3,5,5-TRIMETHYL CYCLOHEXYLAMINE
The present invention provides a method for preparing 3-aminomethyl-3,5,5-trimethyl cyclohexylamine. The method comprises: a) reacting 3-cyano-3,5,5-trimethyl cyclohexanone with excess primary amine as well as removing the water generated from the reaction, so that IPN is substantially converted into imine compounds; b) in the presence of an ammonolysis catalyst, mixing the product of step a) with liquid ammonia, making the imine compound perform ammonolysis reaction to generate 3-cyano-3,5,5-trimethyl cyclohexylimine and the primary amine; and c) in the presence of hydrogen and a hydrogenation catalyst, hydrogenating 3-cyano-3,5,5-trimethyl cyclohexylimine obtained in step b) to obtain 3-aminomethyl-3,5,5-trimethyl cyclohexylamine. The method of the present invention avoids the generation of 3,5,5-trimethyl cyclohexanol and 3-aminomethyl-3,5,5-trimethyl cyclohexanol as the major by-products in the prior art, thereby improving the yield of 3-aminomethyl-3,5,5-trimethyl cyclohexylamine.
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Paragraph 0041-0044; 0048-0051

(2015/11/03)

METHOD FOR PREPARING 3-AMINOMETHYL-3,5,5-TRIMETHYL CYCLOHEXYLAMINE
The present invention provides a method for preparing 3-aminomethyl-3,5,5-trimethyl cyclohexylamine. The method comprises: a) reacting 3-cyano-3,5,5-trimethyl cyclohexanone with excess primary amine as well as removing the water generated from the reaction, so that IPN is substantially converted into imine compounds; b) in the presence of an ammonolysis catalyst, mixing the product of step a) with liquid ammonia, making the imine compound perform ammonolysis reaction to generate 3-cyano-3,5,5-trimethyl cyclohexylimine and the primary amine; and c) in the presence of hydrogen and a hydrogenation catalyst, hydrogenating 3-cyano-3,5,5-trimethyl cyclohexylimine obtained in step b) to obtain 3-aminomethyl-3,5,5-trimethyl cyclohexylamine. The method of the present invention avoids the generation of 3,5,5-trimethyl cyclohexanol and 3-aminomethyl-3,5,5-trimethyl cyclohexanol as the major by-products in the prior art, thereby improving the yield of 3-aminomethyl-3,5,5-trimethyl cyclohexylamine.
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Paragraph 0058-0063; 0071-0074

(2016/12/22)

3-AMINOMETHYL-3, 5, 5-TRIMETHYL CYCLOHEXYLAMINE PREPARATION METHOD
Provided is a 3-aminomethyl-3,5,5-trimethylcyclohexylamine preparation method. A feeding flow of 3-cyano-3,5,5-trimethylcyclohexylimine is reacted with NH3 and hydrogen in the presence of a hydrogenation catalyst; the method is characterized by: firstly adding a basic compound to the feeding flow of 3-cyano-3,5,5-trimethylcyclohexylimine, and then after a portion of 3-cyano-3,5,5-trimethylcyclohexylimine has reacted, adding an acidic compound to reaction materials for further hydrogenation reaction to prepare the product. The method ensures that the aminonitrile content in the product is low, thus effectively reducing the duration of the reaction and greatly reducing the consumption of the catalyst during the hydrogenation reaction process.
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Paragraph 0036-0037

(2014/07/07)

3-AMINOMETHYL-3, 5, 5-TRIMETHYL CYCLOHEXYLAMINE PREPARATION METHOD
Provided is a 3-aminomethyl-3,5,5-trimethylcyclohexylamine preparation method. A feeding flow of 3-cyano-3,5,5-trimethylcyclohexylimine is reacted with NH3 and hydrogen in the presence of a hydrogenation catalyst; the method is characterized by: firstly adding a basic compound to the feeding flow of 3-cyano-3,5,5-trimethylcyclohexylimine, and then after a portion of 3-cyano-3,5,5-trimethylcyclohexylimine has reacted, adding an acidic compound to reaction materials for further hydrogenation reaction to prepare the product. The method ensures that the aminonitrile content in the product is low, thus effectively reducing the duration of the reaction and greatly reducing the consumption of the catalyst during the hydrogenation reaction process.
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Paragraph 0062; 0063; 0064

(2014/05/25)

PROCESS FOR PREPARING 3-AMINOMETHYL-3,5,5-TRIMETHYLCYCLOHEXYLAMINE
The invention relates to an improved process for preparing 3-aminomethyl-3,5,5-trimethylcyclohexylamine, referred to hereinafter as isophoronediamine or, in abbreviated form, IPDA, by: I. preparation of isophorone by catalyzed aldol condensations with acetone as reactant; II. reaction of isophorone with HCN to form isophoronenitrile (IPN, 3-cyano-3,5,5-trimethylcyclohexanone); III. catalytic hydrogenation and/or catalytic reductive amination (also referred to as aminative hydrogenation) of 3-cyano-3,5,5-trimethylcyclohexanone, hereinafter called isophoronenitrile or, in abbreviated form, IPN, to give the isophoronediamine.
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Paragraph 0233; 0234; 0235

(2013/10/07)

PROCESS FOR PREPARING 3-AMINOMETHYL-3,5,5-TRIMETHYLCYCLOHEXYLAMINE
The invention relates to an improved process for preparing 3-aminomethyl-3,5,5-trimethylcyclohexylamine, referred to hereinafter as isophoronediamine or IPDA for short, by means of catalytic hydrogenation and/or catalytic reductive amination (also referred to as aminating hydrogenation) of 3-cyano-3,5,5-trimethylcyclohexanone, also called isophoronenitrile or IPN for short hereinafter.
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Paragraph 0046

(2013/10/08)

PROCESS FOR HYDROGENATING NITRILES
The present invention relates to a process for hydrogenating nitriles by means of hydrogen in the presence of a catalyst in a reactor, where the catalyst is arranged in a fixed bed, wherein the cross-sectional loading in the reactor is in the range from 5 kg/(m2s) to 50 kg/(m2s). The present invention further relates to a process for preparing downstream products of isophoronediamine (IPDA) or N,N-dimethylaminopropylamine (DMAPA) from amines prepared according to the invention.
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Page/Page column 8

(2012/10/08)

PROCESS FOR HYDROGENATING NITRILES
The present invention relates to a process for hydrogenating organic nitriles by means of hydrogen in the presence of a catalyst in a reactor, where the shaped body catalyst is arranged in a fixed bed, wherein the shaped body in the shape of spheres or rods has in each case a diameter 3 mm or less, in the shape of tablets a height of 4 mm or less, and in the case of all other geometries in each case has an equivalent diameter L=1/a′ of 0.70 mm or less, where a′ is the external surface area per unit volume (mms2/mmp3), where: a ′ = A p V p , where Ap is the external surface area of the catalyst particle (mms2) and Vp is the volume of the catalyst particle (mmp3). The present invention further relates to a process for preparing downstream products of isophoronediamine (IPDA) or N,N-dimethylaminopropylamine (DMAPA) from amines prepared according to the invention.
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Page/Page column 8

(2012/10/08)

PROCESS FOR PREPARING 3-AMINOMETHYL-3,5,5-TRIMETHYLCYCLOHEXYLAMINE
The invention relates to an improved process for preparing 3-aminomethyl-3,5,5-trimethylcyclohexylamine, referred to hereinafter as isophoronediamine or IPD for short, by aminating hydrogenation of 3-cyano-3,5,5-trimethylcyclohexanone, referred to hereinafter as isophoronenitrile or IPN for short, in the presence of a shaped Raney hydrogenation catalyst.
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Page/Page column 5

(2010/03/04)

PROCESS FOR PREPARING AMINES BY CONDITIONING THE CATALYST WITH AMMONIA
The invention relates to a process for preparing amines by conditioning the catalyst with ammonia.
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Page/Page column 6

(2009/03/07)

Process for producing amines
A process is disclosed for producing an amine by carrying out a reductive amination of a cyclic ketone or by carrying out a reduction of an imino derivative of a cyclic ketone to the corresponding amine which process is characterized in using a cobalt catalyst containing a carbonate of an alkaline earth metal and/or lanthanum oxide.
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(2008/06/13)

Process for producing amines
Amines are produced in high yield by the process which comprises allowing a cyclic ketone to react with ammonia in the presence of active carbon to produce imino derivatives and then, allowing the imino derivatives to react with hydrogen in the presence of a hydrogenating catalyst.
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(2008/06/13)

Multistep, continuous preparation of organic polyisocyanates
A multistep process for the continuous preparation of organic polyisocyanates, preferably aliphatic or cycloaliphatic diisocyanates, by reacting the corresponding organic polyamines with carbonic acid derivatives and alcohols to give monomeric polyurethanes and pyrolyzing the latter involves separating the resultant polyisocyanates and worthless residues in certain reaction steps and recycling the reusable by-products into earlier steps.
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(2008/06/13)

Process for the production of 3-aminomethyl-3,5,5-trialkylcyclohexylamine
A method is disclosed for the selective preparation of 3-aminomethyl-3,5,5-trialkylcyclohexylamine by preparing dried 3-cyano-3,5,5-trialkylcyclohexylimine from the reaction of 3-cyano-3,5,5-trialkylcyclohexanone with ammonia in the presence of a drying agent in an amount at least sufficient to retain the water present or generated during the imine-forming reaction, and hydrogenating the dried 3-cyano-3,5,5-trialkylcyclohexylimine in the presence of a cobalt-containing catalyst at elevated temperature and pressure.
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(2008/06/13)

Cosmetic composition containing an amide-amine type condensate, and a cosmetic treating process using said condensate
A cosmetic composition for improving the suppleness of the skin or hair and for protecting the keratin of the skin or hair from degradation by atmospheric agents or light comprises in a cosmetic or dermatologic acceptable vehicle a saturated condensate resulting from the polyaddition of a bis-acrylamide and a sterically hindered primary diamine, the condensate being saturated by hydrogenation or by addition of a thiol or an amine on the double bonds of the acrylamide residue.
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(2008/06/13)