WO2008148647A1 - Procede de fabrication d'une solution de sels de diacides/diamines - Google Patents
Procede de fabrication d'une solution de sels de diacides/diamines Download PDFInfo
- Publication number
- WO2008148647A1 WO2008148647A1 PCT/EP2008/056328 EP2008056328W WO2008148647A1 WO 2008148647 A1 WO2008148647 A1 WO 2008148647A1 EP 2008056328 W EP2008056328 W EP 2008056328W WO 2008148647 A1 WO2008148647 A1 WO 2008148647A1
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- WO
- WIPO (PCT)
- Prior art keywords
- diamine
- reactor
- diacid
- solution
- weight
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C229/00—Compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C229/02—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton
- C07C229/04—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated
- C07C229/26—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having more than one amino group bound to the carbon skeleton, e.g. lysine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C211/00—Compounds containing amino groups bound to a carbon skeleton
- C07C211/01—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms
- C07C211/02—Compounds containing amino groups bound to a carbon skeleton having amino groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
- C07C211/09—Diamines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C55/00—Saturated compounds having more than one carboxyl group bound to acyclic carbon atoms
- C07C55/02—Dicarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00002—Chemical plants
- B01J2219/00004—Scale aspects
- B01J2219/00006—Large-scale industrial plants
Definitions
- the present invention relates to a method of manufacturing a solution of a diamine salt and diacid for the manufacture of polyamide.
- the invention relates to a process for the manufacture of a concentrated solution of hexamethylene diammonium adipate salt, also called nylon salt, used as a raw material for the manufacture of polyamide, more specifically PA66.
- an aqueous solution of a salt formed by reaction between a molecule of diamine and a molecule of diacid is generally used. This solution is heated to evaporate the water at first and then to initiate the polymerization by polycondensation, to obtain macromolecular chains comprising amide functions.
- the salt solution generally contains stoichiometric amounts of diacids and diamines.
- the weight concentration of nylon salt is generally between 50% and 65%. This solution is usually stored before being transported if necessary, and then fed into the polymerization plants.
- the maximum permissible Nylon salt concentration to avoid precipitation problems is of the order of 70% by weight at atmospheric pressure. Beyond this concentration, it is necessary to heat the solution at temperatures between 110 and 160 0 C under a pressure above atmospheric pressure to prevent precipitation. These temperature and pressure domains are hardly compatible with storage and transport.
- US Patent 4,442,260 discloses a process of producing an aqueous solution containing 31 to 40% water, 73.5 to 77.5% adipic acid and 22.5 to 26.5% d. hexamethylene diamine, then evaporating a large part of the water to obtain a non-stoichiometric salt weight concentration of 89 to 96%, and adding hexamethylenediamine to obtain a stoichiometric ratio of diacid / diamine equal to 1.
- One of the aims of the present invention is to provide a method for preparing a concentrated solution of Nylon salt or diacid and diamine salt, using the minimum energy exchange with the outside is to say minimizing the intake and evacuation of calories.
- the invention provides a method of manufacturing an aqueous solution of diamine and diacid salts obtained by mixing a diacid and a diamine, at a weight concentration of salt of between 50 and 80%, characterized in that it consists of:
- ie water representing at least 10% of the total quantity of water to be fed into said reactor, a stream comprising diacid, a stream comprising diamine and optionally a flow of water at the temperature Ti, the flows of the feed stream comprising diacid and the feed stream comprising diamine being controlled to constantly have a temperature of the solution in the reactor below the temperature of d boiling under the operating pressure thereof and a diacid / diamine molar ratio greater than 1.1, the amount of acid fed corresponding to at least 90% by weight of the total mass of the acid required to produce the amount desired amount of aqueous salt solution, the amount of water fed representing at least 75% by weight of the total mass of water required to produce the desired amount of the aqueous salt solution,
- Suitable diamines for the invention include hexamethylenediamine (HMD) as the preferred monomer and the most used, and also heptamethylene diamine, tetramethylene diamine, octamethylene diamine, nonamethylene diamine, decamethylene diamine, 2-methylpentamethylenediamine, undecamethylenediamine, dodecamethylenediamine, xylylene diamine, isophorone diamine. It is possible to use a mixture of several diamine monomers.
- HMD hexamethylenediamine
- the diamine is fed in pure form or, preferably, in the form of concentrated aqueous solution.
- a solution comprising at least 50% by weight of diamine, preferably at least 85% and even more preferably about 90% by weight is preferentially used.
- the stream comprising the diamine may contain other compounds without departing from the scope of the invention.
- diacids for the invention there may be mentioned suberic acid, sebacic, dodecanedioic, isophthalic, terephthalic, azelaic, pimelic, naphthalene dicarboxylic, for example. It is possible to use a mixture of several diacid monomers. Adipic acid is the preferred and most used monomer. It is implemented in powder form. However, it can also be fed into the reactor as an aqueous solution or suspension.
- the flow comprising the diamine may contain other compounds, solvents, without departing from the scope of the invention.
- the product streams fed into the first reactor may be preferably separate.
- the diamine can be added with water and some of the diacid.
- the diacid is fed, preferably, in powder form. However, it may be supplied in the form of an aqueous solution or dispersion or in dissolved form, for example, in an aqueous solution of diamine / diacid salt, without departing from the scope of the invention.
- the process of the invention is advantageously carried out by maintaining the various reactors, more particularly the second and third reactors described below, in an oxygen-free atmosphere, for example under an atmosphere constituted by nitrogen. , rare gases, water vapor or a mixture thereof.
- the oxygen-free atmosphere is obtained either by continuously feeding a stream of nitrogen, or by maintaining a nitrogen pressure in the various reactors and by generating water vapor by boiling the solution.
- the exhaust or removal of nitrogen is carried out through a condenser mounted on the reactor.
- the water entrained with the nitrogen is condensed and recycled to the reactor.
- This embodiment also allows the evacuation of the oxygen present, for example in dissolved form, in the solution and thus avoids oxidation of the monomers, especially the diamine.
- the oxygen may be provided in particular by the diacid monomer.
- the dissolved oxygen is removed by entrainment by the water vapor generated by the boiling of the solution in the second reactor, when the temperature of the solution is equal to this temperature of 30.degree. boiling.
- the method of the invention may be carried out in a discontinuous mode or a continuous mode. These two embodiments are described in detail below.
- the method of the invention can be implemented in any type of reactor. More particularly, the reactors comprise mechanical agitation and may be equipped with means for maintaining them in temperature, especially during periods of stopping or change of production campaign.
- the method of the invention is implemented, preferably, in an installation comprising several reactors connected in series, each reactor corresponding to the completion of a process step.
- the various process steps can be carried out successively in the same reactor.
- the installation may comprise several reactors connected in parallel for carrying out a process step.
- the concentrated solution of salt obtained according to the process of the invention can be fed directly and continuously into a polymerization plant, or can be stored before transfer and use.
- Figure 1 shows a block diagram of an installation for implementing the method according to a discontinuous embodiment
- Figure 2 shows a block diagram of an installation for implementing the method according to a continuous embodiment.
- the invention is also illustrated by the examples of manufacturing solutions concentrated in nylon salt obtained according to the batch embodiment of the process.
- AA adipic acid
- HMD hexamethylenediamine
- the plant comprises a first agitated reactor 1 in which adipic acid 2, generally in the form of a powder, and a hexamethylenediamine liquid stream 3 are added. Water 4 is also introduced into this reactor.
- Hexamethylenediamine is advantageously a concentrated aqueous solution comprising 90% by weight of HMD.
- the various products are added to the reactor 1 which contains a small amount of adipic acid solution and hexamethylenediamine in water, rich in adipic acid, and called foot of solution.
- This aqueous solution is advantageously a small part of the solution prepared in an earlier operation and, advantageously, as a composition, substantially the final composition of the solution to be prepared in this reactor 1, namely a diacid / diamine molar ratio equal to at about 2.4 and a dissolved species weight concentration of about 57%.
- the amount of solution present in the reactor at the beginning of the step is at least about 5%, preferably between 5% and 40%, preferably between 10% and 35% of the total amount of solution produced in the reactor.
- no heat exchange is implemented between the reactor and the environment, or outside, that is to say that the reactor operates in almost adiabatic mode .
- the temperature in reactor 1 rises slightly because of the neutralization reaction between HMD and adipic acid.
- the temperature of the solution in the reactor during the entire operation and at the end of the stage, will always be at a low temperature advantageously less than
- This low temperature level is advantageous for limiting the oxidation of HMD by the oxygen present in the medium.
- This oxygen may in particular be provided by the adipic acid powder.
- adipic acid and HMD necessary to obtain an aqueous solution containing adipic acid, diacid and diamine salt, with a total molar ratio of diacid / diamine equal to 2.4 and a weight concentration of 57% dissolved species are fed into the reactor.
- the volume of reaction medium in the reactor advantageously represents at least 80% of the useful volume of the reactor 1
- the solution is fed into a second reactor 5 called the neutralization reactor, by a pump 7.
- This reactor 5 is equipped with a condenser 8 and advantageously an external loop for circulating the solution and / or an agitator (not shown).
- hexamethylenediamine 9 is fed to obtain a molar ratio AA / HMD close to 1, 01.
- the first reactor 1 no significant heat exchange is advantageously achieved with the outside. So the heat of the reaction of neutralization of the amine by the acid causes an increase in the temperature in the reactor 5 to reach the maximum boiling point of the mixture at the operating pressure.
- the evaporated water is condensed in the condenser 8 to obtain a total reflux of the water.
- This temperature characteristic for boiling is advantageous because it makes it possible to eliminate, by entrainment with water vapor, the oxygen present in the medium in particular in dissolved form.
- the heat exchange achieved in this condenser is very small and represents only a very small part of the heat released by the neutralization reaction.
- Water may also be added to adjust the concentration of hexamethylene ammonium adipate salt at a concentration by weight greater than 50%, preferably between 60 and 75% by weight.
- the water may be advantageously mixed with the hexamethylenediamine stream.
- the solution obtained in the second reactor 5 is fed into a third reactor 10 provided with agitation (not shown) and advantageously a condenser 11.
- This third reactor 10 also called adjustment reactor, is similar in principle to the second reactor and comprises an addition 6 of HMD and water to adjust the AA / HMD ratio to a value between 0.995 and 1 , 005, and adjust if necessary, the salt concentration to the desired value.
- the solution thus obtained can be used directly in a polymerization plant or be stored in a storage tank 12 or in suitable containers for transport.
- the reactors of the plant are maintained in an oxygen-free atmosphere by feeding, for example, nitrogen into the empty reactor, and maintaining this nitrogen atmosphere during filling and reactor emptying.
- the nitrogen supplies of each reactor are not shown in the appended figure.
- the reactors are provided with a thermal insulation to limit the exchange of heat with the external environment and thus limit heat loss.
- the dissolved oxygen will be driven away by the nitrogen that escapes from the reactor during filling thereof.
- This evacuation of the nitrogen is preferably carried out through a condenser to thereby condense the water vapor entrained by the nitrogen.
- the process comprises a first step of dissolution of the adipic acid implemented in the reactor 13.
- the adipic acid is fed by a worm system 14, simultaneously with water 15 and a stream 16 of concentrated nylon salt solution to obtain in the reactor 13 a solution containing a diacid / diamine molar ratio of between 1.5 and 5, preferably about 2.4, and a weight concentration of species dissolved between 40 and 75%, for example equal to 57%.
- the diamine is fed into the reactor 13 by a flow independent of the flow of concentrated salt solution, the total diamine supply in the reactor 13 can be obtained either by the sole supply of diamine or by the flow of concentrated salt solution or by the addition of these two streams.
- an external circulation loop 17 comprising a pump 18 is illustrated.
- Part of the solution circulating in the loop feeds a reactor 19 also equipped with an external neutralization loop 20 comprising a pump 28 and two static mixers 21 and 22. Upstream of each mixer is located a supply 23 of HMD and a feed 24 in monomers to adjust the diacid / diamine molar ratio to a value between 0.99 and 1.01.
- This molar ratio is advantageously controlled and adjusted by measuring the pH of the solution and the addition of diamine and / or additional diacid downstream of the pH measurement.
- the heat released by the neutralization allows a increasing the temperature of the solution until, at most, the boiling temperature of the solution at the operating pressure is reached.
- a condenser 26 is provided on the reactor 19.
- a portion of the solution produced in the reactor 19 is sent to the first reactor 13 through line 16, the other portion 27 is directed to unrepresented storage.
- the diamine is introduced into the first reactor by a separate feed 29 in pure form or aqueous solution.
- the two feeds 16 and 29 of diamine in the first reactor can be present simultaneously.
- Example 1 Production of an aqueous solution of nylon salt at 62% by weight, according to the batch process.
- This foot of solution is a small part of the solution obtained in the reactor 1 in the previous manufacturing operation.
- Adipic acid and HMD are added simultaneously ensuring that the mixture is always in acid excess (molar ratio AA / HMD greater than 1.1).
- the homogeneity of the solution is provided by mechanical stirring.
- the dissolved species (56.6% by weight) consist of 75.1% by weight of adipic acid and 24.9% by weight of hexamethylenediamine.
- the final temperature of the solution is 63 ° C.
- step 1 82.3 kg (ie about 85.5%) of the solution obtained in step 1 are transferred to the reactor 5 of Figure 1, thermally insulated and equipped with a condenser 8. Part of the solution obtained is stored as a solution foot in reactor 1 for subsequent operation.
- the energy or heat released by the neutralization reaction causes the increase of the temperature of the medium to the boiling point, namely 108 0 C in the example described.
- the vapors produced are condensed in the condenser 8 and form a total reflux in the reactor 5.
- the energy evacuated by the condensation of the vapors corresponds to the surplus neutralization energy.
- the method makes it possible to maintain the system at a temperature of 108 ° C. (beginning of boiling at atmospheric pressure), without requiring the use of means for evacuating the calories generated by the neutralization reaction.
- the concentration and the pH of the solution are then adjusted by the addition of 0.9 kg of water at a temperature of 40 ° C. and 0.43 kg of an aqueous HMD solution at 90% by weight. and at a temperature of 45 ° C, after transfer of the solution into a third reactor.
- the solution is an aqueous solution containing 62.0% by weight of nylon salt with a molar ratio of adipic acid / HMD equal to 1.003 and a pH equal to 7.21.
- the pH is measured at 20 ° C. on a sample of the diluted solution with water to obtain a dissolved species concentration equal to 100 g / l.
- the solution obtained is then stored in a reservoir 12 shown in FIG. 1.
- Example 2 Production of 68% nylon salt according to the batch process.
- This foot of solution is a small part of the solution obtained in the reactor 1 in the previous manufacturing operation.
- Adipic acid and HMD are added simultaneously ensuring that the mixture is always in acid excess (molar ratio AA / HMD greater than 1, 1).
- the homogeneity of the solution is ensured by mechanical stirring.
- the dissolved species 63.5% by weight
- the final temperature of the solution is 68 ° C.
- the energy or heat released by the neutralization reaction causes the rise of the temperature of the medium to the boiling point, namely 110 0 C, in the example described.
- the vapors produced are condensed in the condenser 8 and form a total reflux in the reactor 5.
- the energy evacuated by the condensation of the vapors corresponds to the excess neutralization energy.
- the process makes it possible to maintain the system at a temperature of 110 ° C. (boiling point at atmospheric pressure).
- the concentration and the pH of the solution are then adjusted by adding 1.0 kg of water at a temperature of 40 ° C. and 0.47 kg of an aqueous HMD solution at 90% by weight of water. HMD and at a temperature of 45 ° C, after transfer of the solution into a third reactor 10 provided with a condenser 11. At the end of this step, the solution is an aqueous solution containing 68.0% by weight of salt Nylon with a molar ratio AA / HMD equal to 1.003.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Polyamides (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims
Priority Applications (10)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
ES08759929T ES2394735T3 (es) | 2007-06-04 | 2008-05-22 | Procedimiento de fabricación de una solución de sales de diácidos/diaminas |
PL08759929T PL2155648T3 (pl) | 2007-06-04 | 2008-05-22 | Sposób wytwarzania roztworu soli dikwasów/diamin |
CN2008800186963A CN101679184B (zh) | 2007-06-04 | 2008-05-22 | 二酸/二胺盐溶液的制造方法 |
EP08759929A EP2155648B1 (fr) | 2007-06-04 | 2008-05-22 | Procede de fabrication d'une solution de sels de diacides/diamines |
JP2010510728A JP5209047B2 (ja) | 2007-06-04 | 2008-05-22 | 二酸/ジアミンの塩の溶液の製造方法 |
BRPI0811341A BRPI0811341B1 (pt) | 2007-06-04 | 2008-05-22 | "processo de fabricação de solução aquosa de sal de diaminas e diácidos" |
MX2009013150A MX2009013150A (es) | 2007-06-04 | 2008-05-22 | Procedimiento para producir una solucion de sales de diacido/diamina. |
KR1020097025170A KR101141093B1 (ko) | 2007-06-04 | 2008-05-22 | 이산/디아민 염 용액의 제조 공정 |
US12/451,851 US8772439B2 (en) | 2007-06-04 | 2008-05-22 | Production of solutions of diacid/diamine salts |
IL202077A IL202077A (en) | 2007-06-04 | 2009-11-12 | A process for producing a solution of diacid / diamine salts |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR0703933A FR2916756B1 (fr) | 2007-06-04 | 2007-06-04 | Procede de fabrication d'une solution de sels de diacides/diamines |
FR07/03933 | 2007-06-04 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2008148647A1 true WO2008148647A1 (fr) | 2008-12-11 |
Family
ID=39004755
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2008/056328 WO2008148647A1 (fr) | 2007-06-04 | 2008-05-22 | Procede de fabrication d'une solution de sels de diacides/diamines |
Country Status (15)
Country | Link |
---|---|
US (1) | US8772439B2 (fr) |
EP (1) | EP2155648B1 (fr) |
JP (1) | JP5209047B2 (fr) |
KR (1) | KR101141093B1 (fr) |
CN (1) | CN101679184B (fr) |
AR (1) | AR068973A1 (fr) |
BR (1) | BRPI0811341B1 (fr) |
ES (1) | ES2394735T3 (fr) |
FR (1) | FR2916756B1 (fr) |
IL (1) | IL202077A (fr) |
MX (1) | MX2009013150A (fr) |
PL (1) | PL2155648T3 (fr) |
RU (1) | RU2434842C2 (fr) |
TW (1) | TW200911748A (fr) |
WO (1) | WO2008148647A1 (fr) |
Cited By (2)
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RU2488603C2 (ru) * | 2009-04-09 | 2013-07-27 | Родиа Операсьон | Способ получения раствора солей двухосновных кислот и диаминов |
EP3842472A1 (fr) | 2019-12-23 | 2021-06-30 | Polytechnyl S.A.S. | Procédé de production d'une solution aqueuse concentrée d'un sel de diamine et d'acide dicarboxylique |
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FR2943348B1 (fr) * | 2009-03-20 | 2012-12-21 | Rhodia Operations | Procede de fabrication de polyamide |
FR2959511B1 (fr) * | 2010-04-30 | 2012-06-01 | Rhodia Operations | Procede de fabrication de polyamide |
EP2546227B1 (fr) * | 2011-07-11 | 2016-05-04 | Uhde Inventa-Fischer GmbH | Procédé de fabrication d'une solution aqueuse de sels |
US9475753B2 (en) * | 2011-07-26 | 2016-10-25 | Dsm Ip Assets B.V. | Process for preparing a diamine/dicarboxylic acid salt |
FR2981600B1 (fr) | 2011-10-25 | 2013-11-15 | Rhodia Operations | Procede de preparation de granules de polyamide |
US20140296472A1 (en) | 2011-12-05 | 2014-10-02 | Invista North America S.A R.L. | Process for the preparation of polyamides |
FR2984332B1 (fr) | 2011-12-15 | 2015-12-11 | Rhodia Operations | Procede de preparation de granules de polyamide et utilisations |
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- 2008-05-22 PL PL08759929T patent/PL2155648T3/pl unknown
- 2008-05-22 MX MX2009013150A patent/MX2009013150A/es active IP Right Grant
- 2008-05-22 JP JP2010510728A patent/JP5209047B2/ja active Active
- 2008-05-22 RU RU2009148794/04A patent/RU2434842C2/ru not_active IP Right Cessation
- 2008-05-22 KR KR1020097025170A patent/KR101141093B1/ko active IP Right Grant
- 2008-05-22 ES ES08759929T patent/ES2394735T3/es active Active
- 2008-05-22 EP EP08759929A patent/EP2155648B1/fr active Active
- 2008-05-22 BR BRPI0811341A patent/BRPI0811341B1/pt active IP Right Grant
- 2008-05-22 CN CN2008800186963A patent/CN101679184B/zh active Active
- 2008-05-22 US US12/451,851 patent/US8772439B2/en active Active
- 2008-06-03 TW TW097120608A patent/TW200911748A/zh unknown
- 2008-06-03 AR ARP080102333A patent/AR068973A1/es unknown
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- 2009-11-12 IL IL202077A patent/IL202077A/en active IP Right Grant
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US4442260A (en) * | 1983-03-14 | 1984-04-10 | E. I. Du Pont De Nemours & Company | Preparation of salt solution useful for making nylon |
US5801278A (en) * | 1997-03-07 | 1998-09-01 | E. I. Du Pont De Nemours And Companh | Low water diamine-dicarboxylic acid salt preparation |
Cited By (3)
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RU2488603C2 (ru) * | 2009-04-09 | 2013-07-27 | Родиа Операсьон | Способ получения раствора солей двухосновных кислот и диаминов |
EP3842472A1 (fr) | 2019-12-23 | 2021-06-30 | Polytechnyl S.A.S. | Procédé de production d'une solution aqueuse concentrée d'un sel de diamine et d'acide dicarboxylique |
WO2021130300A1 (fr) | 2019-12-23 | 2021-07-01 | Polytechnyl S.a.s. | Procédé de production d'une solution aqueuse concentrée d'un sel d'une diamine et d'un acide dicarboxylique |
Also Published As
Publication number | Publication date |
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CN101679184A (zh) | 2010-03-24 |
IL202077A (en) | 2014-01-30 |
TW200911748A (en) | 2009-03-16 |
KR20090131683A (ko) | 2009-12-29 |
CN101679184B (zh) | 2013-11-20 |
RU2434842C2 (ru) | 2011-11-27 |
PL2155648T3 (pl) | 2013-01-31 |
JP2010529066A (ja) | 2010-08-26 |
EP2155648B1 (fr) | 2012-09-12 |
BRPI0811341A2 (pt) | 2014-10-29 |
FR2916756A1 (fr) | 2008-12-05 |
FR2916756B1 (fr) | 2009-07-17 |
JP5209047B2 (ja) | 2013-06-12 |
BRPI0811341B1 (pt) | 2017-01-31 |
US8772439B2 (en) | 2014-07-08 |
KR101141093B1 (ko) | 2012-05-03 |
IL202077A0 (en) | 2010-06-16 |
MX2009013150A (es) | 2010-01-20 |
RU2009148794A (ru) | 2011-07-20 |
US20100168375A1 (en) | 2010-07-01 |
ES2394735T3 (es) | 2013-02-05 |
AR068973A1 (es) | 2009-12-23 |
EP2155648A1 (fr) | 2010-02-24 |
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