Organic compounds -- part of the class 532-570 series – Organic compounds – Amino nitrogen containing
Patent
1998-12-10
2000-05-16
Kumar, Shailendra
Organic compounds -- part of the class 532-570 series
Organic compounds
Amino nitrogen containing
525418, 525419, 525420, 5263031, 526304, 526307, 526312, 528190, 528327, 528328, 528363, 562571, C07C23102, C08F 2054, C08G 6910
Patent
active
06063961&
DESCRIPTION:
BRIEF SUMMARY
The present invention relates to a process for preparing cocondensates of aspartic acid and amines by heating aspartic acid and amines in the presence of acidic catalysts while mixing at up to 300.degree. C. in an extruder.
WO-A-94/01486 discloses the preparation of modified polyaspartic acids. According to one version of the disclosed process, mixtures of aspartic acid and a comonomer which has at least one functional group are polycondensed at from 100 to 270.degree. C. Examples of suitable comonomers are fatty acids, polybasic carboxylic acids, anhydrides of polybasic carboxylic acids, alcohols, amines, alkoxylated alcohols and alkoxylated amines. The polycondensation is effected in the presence of acidic catalysts, for example phosphoric acid, hydrochloric acid or sulfuric acid. The polycocondensates are used as additives in washing and cleaning compositions, for example.
WO-A-96/05241 discloses a process for preparing polyaspartic acid by polycondensation of finely divided aspartic acid at above 150.degree. C. in the presence of acidic catalysts. It is not until the reaction zone that the acidic catalysts first come into contact with the aspartic acid which has been heated to at least 150.degree. C. The acidic catalysts are preferably sprayed onto the surfaces of the fine aspartic acid particles in such a way that no tacky solutions are produced thereon. This avoids the formation of an aggregated or clumped polymer mass.
Prior DE application 19 517 715.0, unpublished at the priority date of the present invention, discloses a process for preparing polycocondensates of aspartic acid by adding a catalytic acid and at least one comonomer to a hot aspartic acid at 150-210.degree. C. in such a way that the formation of tacky solutions is avoided. The cocondensation is preferably effected in a fluidized bed.
EP-A-0 644 257 discloses a process for the thermal polycondensation of aspartic acid in the presence of acidic catalysts. The polycondensation can optionally take place in the presence of polyfunctional monomers such as diamines or polyamines. It is effected within the temperature range from 110 to 300.degree. C. under intensive mixing of the reactants, for example in a single- or multiple-screw extruder. The product obtained is a finely divided, optionally modified, polyaspartic acid containing more than 80% of the starting aspartic acid in condensed form.
The above-described processes have the disadvantage that amine comonomers give rise to particularly tacky reaction masses which are very difficult to handle.
It is an object of the present invention to provide an improved process for preparing cocondensates of aspartic acid and amines.
We have found that this object is achieved by this invention by a process for preparing cocondensates of aspartic acid and amines by heating aspartic acid and amines in the presence of acidic catalysts while mixing at up to 300.degree. C. in an extruder, which comprises supplying the feed region of the extruder with particulate aspartic acid and a downstream metering zone with at least one amine and at least one acidic catalyst, condensing the resulting mixture to such an extent by heating that the downstream end of the extruder discharges a precondensate which contains at least 20-95% by weight of the starting aspartic acid in condensed form, and then completing the condensation of the precondensate at from 150 to 300.degree. C.
The aspartic acid used can be L-, DL- or D-aspartic acid or a mixture thereof. The aspartic acid can have any desired crystal size and crystal form. The average particle diameter of the aspartic acid crystals can be for example from 0.01 to 5, preferably from 0.1 to 2, mm.
The finely divided aspartic acid is condensed with primary, secondary or tertiary amines. Preference is given to using alkylmonoamines having up to 100 carbon atoms in the alkyl chain. Particular preference is given to primary and secondary alkylmonoamines having from 1 to 30 carbon atoms for use as cocondensable compounds. Examples of such amines are tallow fatty amine, hydr
REFERENCES:
patent: 5510426 (1996-04-01), Wood
patent: 5747635 (1998-05-01), Kroner et al.
BASF - Aktiengesellschaft
Kumar Shailendra
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