Note: Descriptions are shown in the official language in which they were submitted.
BASF Aktiengesell5chaft 940339 0~2. 0050/4507~
- 21 96336
Pr-paration of aspartic acid poly~o~ Ate~ w~th improved ~iode-
_ gra~h~ 1; ty and uce thereo~
5 The pre~ent invention relates to a proce~ ~or prepar~ng aspartic
acid polyconden~ate~ with i~rvved biodegra~h;l~ty by the ther-
mal polyCondensation of a~partic acid and to the use of the poly-
conden~ate~ as additive in detergents and cleaner~.
10 Numerous ~.Gces~es are known for preparing aspartic acid polycon-
densates. one po~ibility i~ the ther~al polycondensation of
a~partic acid in the absence of cataly~t~. Such a process i5
known for ~mrl e from US_A -5 057 597. In t~is proce~ inely
divided aspartic acid i6 polycondensed ln an agitated powder bed
15 at t~mperature~ from about 180 to 250 C with distillati~e re~oYal
of water, the particle size being not more than 150 ~m. The
polymerization takes place ~n solid phase withou~ melting of the
aspartic acid crystals. ~or thi~ reason no sticky phase~ occur in
the course of the polycondensatlon. ~he reaction product~ can be
20 carried off for further use without further ~-OL~up or purifi-
cation 6tep~.
US-A-5 221 733 likewi~ disclose~ a proce~8 for the thermal poly-
condensation of aspartic acid whercin pulverulent L-aspartic acid
2~ is initially heated to a temperature of about 18a C to start off
the conden~ation and then the reaction mixture is heated and con-
densed at a temperature o~ at least 216 C until at lea~t 80~ of
the a~partic acid has been condensed to form poly~ucclnimide. ~he
polysuccinimide is subseguently hydrolyz~d with a ba~e, the prod -
30 uct being a polya~partic a~id salt.
The abo~e-de~cribed processes ~eek to ~-xi i~e the con~ercion of
the aspa~tic acid used in the poly~on~n~ation~ ~owever, they
have the disadvantage that the polyconden8ation ~s acco~panied by
35 the format~on of by-products which are not readily biodegradable.
EP-A-0 454 126 di~close~ u~ing polyaspartic acid in amounts ~rom
5 to 50~ by weight as b~ r in detergent formulations contain-
ing from 10 to 40% by weig~t of at leant one sur~ace-ac~ive agent
40 and from 5 to 50~ by w~ight of at lea3t one ~odium aluminum
~ilicate .
EP--~--O 511 037 disclo3es detergent for~lAt~on9 cv~u~t~Lising for
example poly~ucc;nimide a~ at least par~ially biodegrada~le
45 builder.
sASF Aktiengesellschaft 940339 O.Z. 0050/45075
21 96336
It is an o~ject of the present invention to provide a pro~e~ for
preparing polycondensate~ of aspartic acid with better biodegrad-
_ ability than those obtained by existing proce~e~.
5 We have found that th~s o~ct $~ achieved by a pro~e~ for pre-
paring aspartic acid polycondensates with il,.~,G~ed biodegradabil-
ity, which c~Lises polycondensing ~inely di~ided aspartic acid
by thermal polyeonden~ation in Rolid phase at t~r~rature~ from
180 to 250 C until not more than 70~ by weight of the theoreti-
10 cally possibl~ amount of water which is formed in the course ofthe polycondensation ha~ been ~ ~ed from the reaction mixture.
The aspartic acid polyconden~ate~ thus obt~ h~ are used as
additive in detergent~ and cleaner8.
15 ~he process of the present invention in~ol~es subjecting a finely
divided a~par~ic acid to thermal polyconden~ation in ~olid phase.
The aFpartic acid can be uaed in the polyconden~ation in the form
of ~ry_tals or a~ '.er. ~he aspartic ac~d cry~tal~ range in
~ize for example fro~ 0.001 to 5 mm. Aspartic acid powders have
20 for ~mrle a~erage particle ~ er~ from 0.0~ to 3~ preferably
from 0.1 to 2, ~m. The polycondensation is carried out in custom-
ary apparatus, for exa~ple in a tumble dryer or in a stirred bed
of solids. In the laboratory, the polycondenQation i~ usually
carried out in a rotary evaporator. Apparatu~ suitable for carry-
2s ing ou~ the polycondensation on an industriaI scale includes forexample paddle dryers, di~k dryers, plough share ~ixers, paddle
mixer~, extruders, fluidized bed_ with or wi~hout stirring,
double cone mixers, rotary tubes, bed~ of ~olid~ with or wtthou~
stirring, cone mixerR, silos, tubular reactor~, ~tirred tanks
30 (especially with cro~sbeam ~tirrers), conveyor belts, drum mixers
and ball mill~.
The polycondensation of the aspartic acid according to ~he pres-
ent inventlon is effected thermally, ie. by 5imply heating ~inely
35 divided polyaspartic acid to tG~Le~a~ures f~om 180 to 250 C,
pre~erably 200-240 C. A th~ -l polycondensation is carried out
without the use of catalyQt_, ~uch as pho~phoric acid or hydro-
chloric acid. Since ~he a~partic acid c~ystals do not melt in the
cour~e of the ~herma~ polyco~ensation, no ~ticky phases occur,
40 so that finely divided poly~on~n~ates are o~tained. The a~erage
diameter and the particle size distribu~ion of ~he polyconden-
sate~ obtained sub~ta~tially correspond to the average dia~eter
and the particle ~ize di~tribution of the finely divided a~partic
acid used as ~tarttng material.
sASF Akt~eng~ellsch~ft 940339 o.z. 0050t45075
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~ccording to the present invention, the polycondensation i~ car-
ried on only until 70~ by weight of the theore~ically possible
_ amount of water formed ln the course of the polycondensation has
been .l v~d from the reaction m~xture. The course of the poly-
5 condensation i9 therefore very easy to monitor by determin~ng the
amount o~ water removed from the reaction mixture. For example,
the amount of wat~r di~tilled out of the reaction mixture can be
determined volumetrically or gra~imetrically. As ~oon as 10~ by
weight, proferably not more than 60~ by weight, of ~he theoreti-
10 cally possible a~ount of water formed in the course o~ the poly-
condensation has been remo~ed from the reaction mixture, the
polycondensation i8 di~continued by cool; ng the reaction mixture.
To calculate the o~;mll~ theoretically possible amount of water
whieh can be el;~in~ted in the course of the polycon~en~ation, ~t
15 i assumed that the polyconden~atlon of 1 mol (133 g) aspartic
acid to polyaspartic acid w~ll on complete convers~on release
2 ~ol (36 g~ of water. The weight loss due to the ~limln~ion o~
water during the r~action is thus 27~ by weight, based on the
aspartic acid u3ed. 70~ of the t~eoretically possible amount of
20 water mean~ that the polyconden~ation is di~continued when
1. 4 mol ( 25 . 2 g) of water have ~een distilled out of the reaction
mixture. Thi~ corre~ponds to a weight 108~ of 18.9S, based on the
weight of the a~partic a~id u~ed.
25 The polyconden~ation of aspartic acid can be schematically repre-
sented as follow~:
aspartic acid H 0~ polyaspart~c acid ~ 0~ polys~ccln;~;d~
~able 1 reveals the nature of ~e calculation of the amount of
water fo~med in the course of the reaction.
BASF Akti~ngesellschaft 940339 0.2. 0050~45075
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Table 1
Amount of water di6tllled out of the polyconden6ation mixture
-
[mol~ ~ of ~qYi , po~sible [g] Based on aspartic acid
amount used t a by weigh~J
2.0 100 36.027.0
1.4 70 25.218.9
1.2 60 21.6~6.2
10 1.0 50 18.013.5
The product~ obtAi~ are a6p~ tic acid polyconden~ate~ which
contain
15 a) alpha- and beta-l;n~ed aspartic acid units of the ~tructures
- ~NH C~ - CO)n- and ~N~ CH2 - CH CO)n
CH2 COOH C00
(I) (II),
b) polyasparti~;de uni~s of the structure
~ ~ f N (IIl) and
CEI2 11
--n
C ) a8par~ic acid.
~he co~po~ition of the polycondensation product8 depend~ on the
t~mr~rature during the polyc~ n~ation and on the re i~r~e time
in the polycon~ tion zone. The polycon~len~ation can be carried
o~t for eY~rl e in ~uch a way that no aspart~c ac~d n ~or ~ur-
vive~ lnto the end product. If, for e~mrle, 1 mol of aspartic
acid i~ u~ed and initially 1 mol of water i~ di~ ~ out of the
polyconden~at~on mix~ure, thi3 will initially re~ult in the
formation of 1 mol of polya~partic acid unit~, from which 0.4 mol
4S of water i8 then ~l;~i n~tQd to leave 0.4 mol of polysuccin; mi de
units. Thi8 mean~ that a polyconden~ation 0~ 1 mol of a8par~ic
acid where 1.4 mol of water are remo~ed by dist~llation will giYe
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21 96336
rise to a product cont~i n; ng 60 mol ~ o~ polya~p -tic acid units
in the alpha- and beta-form and 40 mol ~ of polysucri~ e
_ units.
5 However, the polyco~e~ation can a7 90 be carried out in 3~ch a
way that, of l mol of a~partic acid used, 0.1 ~ol r~-in~
unchanged in the reaction mix~ure. On the assumption that 1.4 mol
o~ water have been ~ ~d from the polycondensation o~ 1 mol of
aspartic acid, the reaction mixture may contain up to 0.4 ~ol of
~o polya~partic acid units and up to 0.5 mol of polysl~cc;n;mide
units. The polyco~en~ation can also be carried out in such a way
that the u~e of 1 mol of aspartic ac~d leave~ 0.2 mol of
unchanged acpart$c acid behi~d in the reaction m xture, wherea~
the el; ;n ~tion of 1.4 mol o~ water can lead to the formation o~
15 up to 0.2 mol of polyaspartic acid units and up to 0.6 mol of
poly~ucc; n i~;d~ unit~.
Table 2 indicates ~he c ,-3i~ions of polyconden3ate3 on removing
from the react~on mlxture 70~ - the maxlmum allowed by the
20 pr~nt invent~on - of the water formed in ~he course of the
Qolycondensation.
Table 2
Composition of polyconden~ates after ti~tillati~e ~ val of 70
25 by weight of the theoretically possible amount of water
A~partic acid tmol S] 0 10 20 30
Polya~partic acid ~mol ~3 60 40 20 0
30 Polysuccin~m~d~ tmol ~] 40 50 60 70
~he ~ 09ition of polyco~s~QateQ after the distillative remo~al
~rom the aspartic acid polycondenoation mix~ure of 60 and 50~ of
the theoret~cally po~ le amount of water is i~dicated tn
35 Tables 3 and 4, re~pectiYely.
Table ~
Aspartic acid [mol %] o 10 20 30
40 Polyaspartic acid lmol %3 80 60 40 20
PolyQt~c~;n;~;de [mol ~l 20 30 40 50
Table 4
45 Aspartic acid tmol ~ 0 10 20 30
~olya~partic acid ~mol %~ 100 80 60 40
Polys~ccinim~de tmol ~] 0 10 20 30
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The polycond~n~tion i~ preferably c~rried out ~ such a way that
in any event the poly~n~raat- contalns le~s than 20 mol ~ of
_ unchanged aspartic acid. ~he aspartic acid content of the poly-
condensate can range for eY~mrle from 0 to 19% by weight.
The a~part~c acid condensation products can be analyzed for
example using spectroscopic or chromatographic ~ethods. The
analytically preparative ~eparat~on of the reaction mixture into
its individual ~v~ ents can be carried out for example by means
10 of an extraction uti~ i7ing the differences in the water solu-
bility of the ind~v~dual ~ ~nent~.
~or in~tance, the reaction mixture can be extracted first for
example with water, in which case the fract~on ~eparated off
15 con3ists e~entlally o~ polya~partic acid or a cocondensatQ which
contain~ aspar~ic acid unit~ and succin; m; de units, the aspartic
acid units being presen~ in the cocon~nsate in an amount o f more
than 50~. The water-soluble portion i~olated f rom the reaction
mixture u~ually ~V~y~ae~ from 20 to 80, preferably from 30 to
20 70, % by wei~ht, based on the a~partic acid u~ed. ~he water-in-
~oluble re~i~u~ is a~partic acid and poly~ccini~ide. It i9
treated ~or ~urther sxtraction with lN hydrochloric acid, cau~ing
aspartic acid to di~sol~e by formation of a~partic acid hydro-
chloride. The proportion of a~partic acid i8 usually below 20,
25 preferably below 15, ~ by weight, based on t~e amount of aspartic
acid u~d. The resldue wh~ch ~ insoluble in water and hydrochlo-
ric ac~d cons~ts pr~ ntly of polysuccinimide and i8 pregent
in the condensation ~LG~t in an amount from 5 to 80, preferably
from 15 to 70, ~ by weight. The quantitatiYe determina~Ton of the
30 individual ~ractions is by drying and weighing. The amount of
aspartic acid used can ~e used to calculate the percentage ~hares
of polyaspar~lc acid and poly~T~-rini~ide.
The polycon~-nsation i8 carried out within the temperature range
35 from 180 to 250 C, preferably within the t~p~rature range from
l90 to 250 c. ~he hi~her the c~ a~ion t~re~ature which i~
chosen, the shorter i9 the reaction time. At a polycondensation
t~p~ra~ure ~f 225-C, for ~ ls, 50% of the theoretical amount
o~ water for~ed in the course of the polycondensatio~ can be dis-
40 tilled out of the reaction m xture in the ~our~e of a conden~a-
tion time of about 2.5 h. The reaction mixture then contains 50~
of water-~oluble polycondensAte and 50~ of water-insoluble poly-
condensate. The K ~alue~ of the polycondenYate3 of aspartic acid
range from ~ to 30, preferably from lO to 25, determined by the
4S method of H. Fikent~cher on lS Qtrength agueous codiu~ salt 501u-
~ion~ of the polyco~n~ate at pH ? a~d 2S C. The molec~lar
BASF Aktiengesellschaft 940339 O.Z. 0050~5075
21 96336
weights M~ of the polycondensate range from 500 to 7 000, prefer-
ably from 800 ~o S 000.
In ~he ~Y~rles which follow, parts are by weight. The R values
5 of the polycondensates were dete~ by the method of
H. Pikent~cher, Cellulo~e-Chemie 13 ~1932)~ 58-64, 71-74, in
aqueous solution on the sodium salts of the polycondensates at a
concentration of lt ~y weight, a p~ of 7 and a temperature o~
25-C.
~Y~mrle 1
A 2~0 1 c~r~ity tumble dryer is charged with 50 kg of L-a~partic
acid ~average particle diameter 0.1-2 mm) and heated by mean~ of
15 an external oil cycle to a tQmperature of 240 C. During the poly-
condensation the reactor is flushed with 100 1 of nitrogen/h. As
~oon as the t~mro~ature of the finely divided a~partic acid has
reached 200 C, the polyco~den~ation starts, as i9 discernible from
the accumulation of water ~n the conden~er. once the polycon-
~0 den~ation has ~tarted at 200 C ~t ls continued untll, after3 hours, 7.5 1 of water have been 8eparated off. This amount of
water of conden~ation correqponds to a 55~ conversion. The poly-
condensate is analyzed extractlvely and spectro~opically. It is
found to eontain 5~ of a~partic acid, 50% of water-3cluble aspar-
2~ tlc ac~d polyco~e~ate and 45% of water-insoluble polysuccini-
mide. The course of the polycondensation i9 9~own in Table 5.
The react~on product iB not completely 901uble in dime~hylforma-
~;de. It can be converted with sodium hydroxide solu~ion into the
30 sodium salt of polyaspartic acid. The ~odium 3alt of the con-
den~ation product, as a 1~ strength ~olution, has a R value of
18.8 at pH 7 and 25 C.
~able 5
Time ~h~ at~l~ ~ternalA~ount of ~ of theoretic-
of oll cycle t~, ~tu~ wa~~ dio--ally po~ibl~3
t~C] t~C] tilled offamount~ of
tl] wa~er of
condensation
0 20 20 0 ~
1 150 110 0 0
2 232 203 dripping 0
3 240 21g 3.5 25.9
4 240 229 5.0 37.0
~ BASF Aktienge~ellscha~t 940339 O.Z. 0050/4S075
~8 21 96336
5 1 240 1 2~8 1 7.5 1 55.5
Co~l; n g
-
5 Comparative ~rle 1
The tumble dryer de~cribed in ~Y~p~ charged with 50 kg o~
L - aspartic acid having an average particle diameter of 0.1- 2 mm
and heated by means of an external oil cycle to a temperature of
10 240 C. The reactor i3 flushed with 100 1 of nitrogen~h. A~ soon as
the t~mr~ature o~ the reaction material has reached 200 C, the
polycondensation ~tarts, as i~ di~cernible from the fact that
water collects in the conden~er. The amount ~f wa~er i~ deter-
mined Yolumetrically. The polyc~nden~ation i~ continued under the
1~ conditions indicated in Table 6 for 6 h, in the cour~e of which
12.2 1 oS water separate off. The amount of water distilled out
of thQ reaction mlxture and the theoretically po~ible amount of
water (100~ = 13.3 ~g of water) are u6ed to calculate the ~onver-
sion. It i~ found to be g2.5~. Af~er the polycondensation ha~
20 ended, ~h~ reactor i~ found to contain 37.5 kg of water-insoluble
aspartic acid polyco~n~ate ~determ~ned ~y mean~ of the extrac-
tion method). The reaction produ~t i~ soluble in dlmethylforma-
mide. It can be con~e~ted with sodium h~ide ~olution into the
~od~um salt of polya~partic acid. ~h~ sodium ~alt of the con-
25 den.~ation product, a~ a lS qtrength aqueous solution, has aR value of 26.6 at pH 7 and 25 C.
Table 6
~i~e [h] Te~p~ Internal A~ount of * of theoretic-
of oil cycle t~ ~ ~ture water di~- ally possible
t~Cl ~~C] tilled offamount~ o~
tl3 water of
conden~ation
0 20 20 0 0
1 180 105 0 0
2 235 203 dripping 0
3 238 217 2.0 14.8
4 240 227 5.5 40.7
240 227 7.0 51.9
6 240 227 9.0 66.7
240 228 10.3 76.3
~ 240 230 12.5 92.6
45 Coo~
;F Aktieng~s~ h~ft 940339 o. z . 0050/45075
9 2 1 96336
Example~ 2 to 14
A rotary e~aporator i~ charged in each case with 133 g ~1 mol) of
aspar~ic acid (particle diameter 0.1-2 mm) and heated in an oil
5 bath which ha~ the t~srature indicated in Table 7 for the time
indicated ~n ~able 7.
Table 7
Ex. T~mp. TLme [h] ~ of th~oretic- ~ value of poly-
tocl ~lly p~ibl~ ~r~ te hydro -
a~oun~ of wat~ lyzed with NaO~
of cY~ tion
2 240 1 74 1~.0
3 240 0.5 49 12.0
4 240 0.25 40 10.0
190 5 9 8.0
6 190 7 14 ~.7
7 190 16 31 12.4
8 200 3 11 8.5
9 200 6 27 10.8
200 16 39 14.1
11 210 2 17 9.7
12 210 7 34 12.8
13 220 2 22 10.4
14 220 6 35 13.7
30 Correlation betweon ~ value and M~
R value Mw
9 1000
1400
35 13 2300
2B00
26 6500
Ecological te~t~
Ecological te~t~ were carried out in accordance with the modified
Zahn-Wellen~ test as laid down in the OECD G~ 1; nes for Testing
of Chemicals ( 1981 ), 302 B. The DOC ~tarting concentration (DOC =
di~solved organic carbon) was 200 mg/l.
' ~ASF Aktlengesellschaft 940339 O.Z. 0050~qSO75
~ 21 96336
The cour~e of the DOC dqcreasa is listed in TablQ 8 ~or ~he
polycon~n~ate~ prepared in ~le 1 and ~r~rative Example 1.
It is clsarly apparent from the DO~ decrease that early di~con-
5 tinuation of the polycondenaation at 55.~ cor,~ sion can b~ u~ed
to improve the ecolog~cal p~o~ ies of the polyaspartic acid.
For instance, 48% of the polycondensate are rapidly biodegraded
within one day without adaptio~, whereas it take~ 20 day~ ~o
achieve 40% degrada~on in the ca~e Of the comparative e~mrle.
10 A~ter an adaption pha~e of 20 days, Example 1 give3 further
degradation up to 90~. In the ca~e of the comparat~ve example,
the degradation values only rise to 80%.
~able 8
Time [d] Decrease ~n dis~olved organic carbon
~Y~rl~ 1 Compara~ive ~Y~mrle l
O O
1 48 ~1
2 50 12
4 52 16
8 52 20
12 51 42
5~ 40
28 74 54
48 90 80
30 Result:
Measures according to the pre~ent invention make it possible to
achieve a distinct ~mp~v~ ?nt in the degree of degradation of
the aspartic acid polycon~ncates over the first 8 days. ~n
addition, higher final degradation valueq are achieved at the
35 e~d.
The polycondensates of Example~ 2, 3 and 4 were subjectRd to a
Zahn-Wellen~ test. ~y day 20 the di~solved organic carbon had
decreased to the value~ indicated in Tab1Q 9.
BASF Aktienge~ell~chaft 940339 O.Z. 0050~4S075
11 21 96336
Table 9
~ ~Y~ e Decrease in di~olved organic
carbon by day 20
[%]
2 44
3 69
4 87
10Comr~rati~e ~Y~mrle 1 40
Application test6
The polyco~den~ates of a~partlc acid prepared by ~he process of
the pre~ent invention are ~uitable for u~e as water treatment
15 agents. The polyconden~ates of FY~P~ e 1 and C~r~rative
Example 1 were tested for calcium ion compatibil~ ty by preparing
in each ca~e aqueous solutions cont~ n~g 4S ppm of poly~o~en-
~a~e a~d 1000 ppm of calcium ions and detc~i n; r~g the transmi~-
sivity of the solution~. Eoth aqueous solution~ we~e found to
20 have a transmissivity of 99.8~, i.c. ~either sample combines with
calcium ion~ to form ~paringly water-soluble calc~um salts.
The polycondensates of PY~rl~ 1 and ~ , rative FYA~rle 1 were
al~o tested for dyn ~; c calcium ~arbonate ;n~; h; tion at a con-
2s centration of 2 ppm of polyco~d~n~ates
Calcium carbonate inhibition (2 ppm of polycocol.den~ateco~centrat~on~
30 Two test solutionQ are prepared. ~e~t solution 1 is water having
a hardne~ of 20- (Ger~an) and a m~gne~ium hardnes~ of 10
~German3. Test Qolution 2 is an aqueou~ solution ha~ing a ~odium
carbonate hardne~ of 4.7- (~ ) and a sodi~ bicarbonate hard-
ne~s of 12.3- (German).
A 500 ml capacity round-bottom flask equipped with ntirrer,
reflux condenser and gag ~nlet tube i8 charged with 150 ml of
test solution 1 and 150 ml of teYt ~olution 2 and al80 2 ppm oS
the in-test polymer and heated at 70-C for 1 hour or 2 hours while
~0 air is being pas~ed in at a rate of 3 1th. The flagk content~ are
cooled down and ~iltered through a fluted ~ilter. The filtrate is
titra~ed compl~Y~ ~~,ically to determine the calcium conten~ in a
conventional manner.
g5 The ~ollowing calc~um carbonate inhibition values were
determined:
BA5F Aktienge~ellscbaft 940339 O.Z. 0050~45075
' 2196336
1~
CaC03 ; nh; h; tion after
1 hour 2 hours
~Y~rle 1 45 ~ 37 %
5 Ct ,-~ative ~-~rle 15~ ~ 47 %
As the result~ show, both polyconden~ates inhibit the formation
of calcium carbonate. When u~ed as water treatment agents, for
10 example for scale ; nhi h; tion, the poly~ond~n~at~ are u~ually
used in amount~ from 1 to 500, preferably from 2 to 100, ppm.
The polyconA~n~ates o~t~in~le by the proce~s of the present
invention are al~o suitable for u~e ag detergent additive.
The polyco~Aen~ation product~ obt~;nah~e by the proce~s of the
pre~ent invention can be ~ncluded in detergents and cleaners
either directly or in the form of th~ alkali m~tal, alkaline
earth metal or am~onium ~alt~. Preference is gi~en to using the
20 sodium salt~ of the polyco~en~ates. They are ob~in~ble by
treating the polycon~en~te~ with aqueou~ baYe~. Instead of the
~odium calts it i~ also po~sible to uRe ammonium sal~s, for
ex~mrle the salts for~ed by treating polycon~ensate~ prepared
accordlng to the present lnvention with ethano~ ~m1 n~,
25 diethanolamine or triethan~l~;"e. The polycondensate~ are
included in phosphate-free or reduced-pho3p~atQ detRrgents (ie.
detergents having a pho~phate co~tent of les~ than 25~ by weigh~,
calculated a~ trisodium polyphoQphate) to enhance the detergency
and as ~ncrus~ation inhibitor. The amount~ of polycondensate
30 ra~ge ~rom 0.1 t~ 50, preferably from 1 to 30, % by weight, ba~ed
on the detergent or cleaner.
Some of thQ polycondensates prepared by the proces~ of the
pres~nt invention were ~ubjected to the CD test and al~o to a
35 determination of the ~lay-de~ch; ng power in the pre~ence of
nonionic surfactants (the test methods are ind~cated for example
in W0-A-g4/11486).
The re~ult~ ob~;ne~ in the CD test and the effectiveness test
40 werQ a~ follow~:
e F~fectivene~s
~]
t~n~
~5 1 340.2 89.2
2 291.8 81.3
~ BASF Aktiengesellschaft 940339 O.Z. OOSO/45075
21 ~6336
13
3 367.2 75.4
4 383.8 76.4
C ~rative Example 1 328.~ 87.7
As the results sho~, the effectivenes~ values and the di8persing
conctant~ of the polyconden6ate~ prepared according to the
present invention correspond to tho~e of comple~ely polycon~n~ed
aspart~c ac~ds.
The te~t of the clay-det~chi ng pow~r in the pre~ence of nonionic
surfac~ants indicate~ an effectivenes~ of 93% for polyconden6ates
a~ per Example 1 and of ~9% for the polyoon~nsates of
Comparative ~ _- e 1.
