Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
The invention provides a process for surface-sizing paper,
which comprises impregnating the paper with an aqueous sizing
liquor and drying it,
the sizing liquor containing 0.02 to 0.2 percent by welght
of a water-dispersible or water-soluble salt of ~ reactlon
product which is prepared from
la) l epoxide group equivalent of a polyglycidyl ether of
2,2-bis~(4' hydroxyphenyl)-propane,
~bl 0.1 to 0.85 amino group equivalent of a mono-
fatty amine o 12 to 24 carbon atoms,
5e~ 0.3 to 2 amino group equi~alents of a polyalkylene-
aminopolyamide of
tc'~ a polymerised aliphatic unsaturated ~atty acid
which is derived from fatty aclds of 16 to 22
carbon atoms, and
(c") an aliphatic polyalkylenepolyamine of 4 to 1
carbon atoms,
~d) optionally 0.1 to l mole of an epihalohydrin or of a
nitrile of ~n ethylenically unsaturated monocarboxylic
~ acid of 3 or 4 carbon atoms, and
: (e~ an acid,
~n ~he presence of an inert organic ~olvent at t~mperature~
of up to 95C, the pH of a sample of the reaction mixture
of (a), (b), /c) and optionally (d) upon dilu~ion to ~0 to
40 percen$ by weight of reaction product b~i~g ad~usted to
2 ~o 8 wlth co~lpon¢n~ ~e)~
- 2 -
~3 '
.. . . . . , , , . ., . ., .~ : . ...... . ..
.
'. ''
7~
The epoxides (a) from which the salts of the reactions
products are obtained preferably have an epoxide content of
1.8 to 5.8~ in particular of 5 to 5.5, epoxy group
equîvalents/kg.
Particularly preferred epoxides have the formula
Cl) ~ 3 ~H3
~2 -O ~ C ~ O-CH~-CHOH-CH2- -O ~ C ~ O-CH~
~l2~o~ CH3 ~ CH3 HC~C~2~
wherein z has an average value of O to 0.65. Preferably, z is
0. Such epoxides are obtained for example by reaction of
epichlorohydrin wîth 2,2-bis-~4'-hydroxyphenyl~-propane.
Saturated or unsaturated mono-fatty amînes contaîning 12 to
24, pree~ably 16 tc 22, and in particular 16 to 18, carbon
atams are particularly suitable as components (b).
The amines are accordingly for example laurylamîne, arachîdyl-
~mine or behenylamine and, in particular, palmitylamîne,
stearylamine or oleylamine. Mixtures of such æmines, such as
those obtainable as technical products9 can also be used.
The polymerised unsaturated fatty acids used as componen~ ~c')
for the formation of the polyalkyleneaminopolyamide (c~ are
. ~ 3 -
:
;
- . . ~ - . . .
7~, .
preerably dimerised to trimerised fatty acids which are
derived from monocarboxylic acids containing 16 to 22~ in
particular 16 to 18, carbon atoms. These monocarboxylic acids
are fatty acids which have at least one, preferably 2 to 5,
ethylenically unsaturated bonds, for example oleic acid,
hiragonic acid, elaeostearic acid, licanic acid, arichidonic
acid, clu~adonic acid and, in particular, linoleic and
linolenic acid. These fatty acids can be obtained from
natural oils, wherein they occur mainly as glycerides.
The dL~eric to trimeric fatty acids ~c~) are ohtained by
d~merisation of the monocarboxylic acids using methods known
per se. The so-called d~meric fatty acids always contain some
trimeric acids and a small amount of monomeric acids.
The dimerised to trimerised linoleic or linolenic acids are
particularly suitable fox use as componen~ (c'). The technical
products of these acids as a rule contain 75 to 95 per cent by
weight of dimeric acid, 4 to 25 percent by weight of trimeric
acid and a trace to 3% of monomeric acid The molar ratio of
d~meric acid to trimeric acid is accordingly about 5:1 to ~ .
36~
Particularly suitable as component (c") are polyalkylenepoly-
amlnes of the formula
-(CH2-CH2~NH)n-CH2-CH2-NH
4 -
~ 7 6
wherein n is 1, 2 or 3, i.e~ diethylenetriamine triethylene_
tetramine, or tetraethylenepentamine. Triethylenete~ramine is
especially preferred,
In the case of amine mixtures, it is also possible for n to
have a non-integral value 7 for example between 1 and 2.
Technical amine mixtures of the indicated kind are also
preferred.
Especially preferred as component (c) is a polyalkylene-
~minopolyamide derived fr~ dimerised to tr~merised linoleic
or linolenic acid and triethylenetetramine.
Mono-atty amines as component (b) and polyalkylene~minopoly-
~mid~s as componen~ (c), which each contain 3 to b~ amino group
equivalents/kg, are preferred.
The react;on products of epoxides as component (a), atty
amines as component (b) and polyalkyleneaminopolyæmides as
corQponent (c)~ can also be obtained m conjunction w~h a fourth
component (d). Ad~antageously, a nitrile of acryllc or
methacrylic acid is used as component (d). However, epichloro-
hydridrin is the preferred component (d).
.
If the component (d) is used in conjunction with c~mponerlts
(a), (b) and (c), preferably 0,1 to 0.5,and especially 0~1 to
0~2, mole of component ~d) is used per epo~ide group equiva-
lent of component (a). However~ in the process of the present
: ~;
~ 5
,, , "
, ,~.
. ~ . ,
576
invention9 chie~ly salts of reaction products are used which
are ~btained only from the components (a), (b)~ ~c) and (e3,
i.e. in the absence of component ~d~. In this case,
preferably 0.4 to 0.8, especially 0.4 to 0.6, amino group
equivalent of component (b) and preferably 0.3 to 1.5,
especially 0.3 to O.S, amino group equivalent of component
(c) are used per epoxide group equivalent o~ c~nponent (a).
As a rule, the components (a) and (b) ara reacted together
firs~ to give an epoxide/fatty amine reaction product and
subsequently with the polyalkyleneaminopolyæmide as component
(c) and optionally further reacted with the nitrile of the
unsaturated monocarboxylic acid or with the epihalohydrin as
c~mponent (d). If c~mponent (d3 is used in conjunction with
componeD~s (a), ~b) and (c), although its use ;5 less
preferred~ then the reaction of the polyalkyleneaminopoly-
amide as component ~c) with the nitrile of the indicated kind
or with the epihalohydr in as component (d) and with the
epoxide/fatty amine reaction product derived from the
componen~s (a~ and (b), may ~ake place in any order.
AccordingIy~ the c~mponent (d) can first be reacted with
componen~ (c) and then with the epoxide/fatty amine reaction
produc~ derived from components (a) and (b) or vice versa. In
many cases, if ~here are no great differences m the
reactivity j the reaction can al~ be carried out s~ul~aneous-
ly.' : '
:
_ 6 --
. ~ , . . . .
The reaction to give the reaction product of the component~(a), (b), (c) and optionally (d) is carried out in sucll a way
tha~ polyaddition products which are dispersible or, in
particular, soluble in water are produced, by adjusting the
pH o~ a sa~ple of the reac~ion mixture which has been diluted
to 10 to 40, preferably 25 to 35, percent by weight with an
inert organic solvent or pre~erably with wat~rJ to 2 to 8,
preerably to 3 to 5.S, at some stage before completion of
~he reactîons. Inorganic or organic acids are used as
component (e) for adjusting this pH value.
.
Suitable inorganic acids for this purpose are ln particular
hydrochloric acid~ nitric acid, preferably phosphoricacid and ~n
part;cular orthophosphoric or sulphamic acid. Suitable
organic acids are both aromatic and, in particular~ aliphatic
mono- or dicarboxylic acids containing not more than 20 carbon
atoms, or a functional derivative thereof, in par~ic~lar the
anllydride. Preferred aliphatic acids are mono- or dicarboxylic
acids containi~g not more than 18 carbon atoms, preferably
lower saturated monocarboxylic acids of ~ to 4 carbon atoms,
or example formic, acetic or propionic acid,higher sahtra-~ed or
unsaturated,optionally hydroxylated fatty acids of 12 to
18 carbon atoms, for example lauric, myristic, oleic3 stearic
.
or ricinic acid9 saturated or unsaturated dicarboxylic acids
of 4 to 18, in par~icular 4 to 109 carbon a~omsy for example
malonl C5 fumaric, glutaric, adipic, pimelic, suberic, azelaic
:
- 7 -
'' :
. . ~ . . .
: . . ~ . ~ . : .
7 6
and sebacic acid, or cycloaliphatic acids, such as the
resinic acids of 20 carbon atoms, for ex~mple levopimaric,
dex~ropImaric and abietic acid. Suitable anhydrides are in
particular those of an aliphatic or aromatic9 preferably
unsaturated, dicarboxylic acid of 4 to 8 carbon at~ms, for
example maleic or phthalic anhydride. Mixtures of these acids
can also be used, in particular teshnical mixtures of fa~ty
ac;ds, for example cocontlt fatty acid~ or of resinic acids,
for example colophonium. The volatile saturated monocarboxylic
acids of 1 to 4 carbon atoms, for examp~e fonmic acid and,
in particular7 acetic a~id, are especially preferred, For
example, formic acid and, in particular, acetic acid, are
used especially if~ ater the use of the other acids of the
indicated kind, only water-dispersible salts are obtained. In
this case, after the additional use o~ for example formic
acid or~ in particular, acetic acid, salts are obtained which
are water-soluble. The water-soluble salts are preferred to
the~water-dispersible salts. Especially preferred as
component (e) are orthophosphoric acid, sulphamic acid3
azelaic acid or colophonium, optionally in the presence of
acetic acid, i. e. sulphamic acid by itself on the one hand,
and ortho-phosphoric acid, azelaic acid or colophonium with
the subsequent addi~ion of ace~ic acid on the other.
'
~ 8~- :
.
.. ... . ,. ~ . - -
,- . , , . ~ . - : :
. . , .,. - . . . , : ... .
. - ~
3~976
.It is advisable to add a certain amount of acid to the
reaction mixture ~mmedia~ely upon or shortly before the
reaction ~ the epoxide/~atty amine reaction product of the
components (a) and (b) with the polyalkyleneaminopolyamide
as component (c), and also to add fur~her acid con~inuously
or in portîons during the course of the further reaction.
Furthexmore, the process is preferabl~ carried out at
temperatures of up to 95C, for example betwPen 25 and 95C,
in particular between 60~ and 96C.
The resultant salts o~ ~he reaction products are at least
dispersible or preferably soluble in water.
The reaction of the components (a), ~b), (c), (e) and
optionally (d) is preferably carried out in an inert organic
solvent which is unable to reaot with these c~mponents.
Suitable organic solvents are in particular water-soluble
organic solv:ents, preferably those which are miscible with
water to an unlimited extent, ~or example cycloaliphatic or
aliphatic ethers conkaining 2 or 3 oxygen atoms and 2 to
$ ¢arbon at~ms, for example dioxane, ethylene glyeol mono-n-
butyl ether ~=n-butyl glycol), diethylene glycol mono-n-butyl
ether and, in particulax, alkanols of 1 to 4 carbon~atoms, for
example isopropanol~ ethanol and methanol.
: _ 9
- . . , . ~ :
- , -
~ 7 ~
The reaction can also be carried out in the presence of
water-insoluble organic solvents~ for example in petrol
hydro~arbons, such as petrol or petroleum ether, benzene, or
ben~enes which are halogenated or substituted by lower alkyl
groups, such as toluene3 xylene or chl.orobenzenes; alicyclic
compounds, such as tetralin or cyclohexane; and carbon
tetrachloride, ethylene ~hloride3 ethylene bromide, s-
te~rachloroethane and especially trichloroethylene or
perchloroethylene.
As ~ rule, all the reactions are carried ou~ in the same
solvent~ the preferred solvent being isopropanol.
The reaction mixture which has been adjusted with acid to the
above pH value is advantageously diIuted, after completion of
the r~actions7 with an inert organic water-soluble solvent of
the indicated kind or preferably with wa~er to gi~e a
preparation for use in the present invention containing lO to
40~ preferably 25 to 35, percent by weight of salts of the
reaction products. Such preparations, which are in the form
o~ solutions or dispersions, and in most cases are slightly
opalescent to cloudy solutions, are dis~.inguished by high
stability.
` 10 _ ~
Preparations with desirable properties in respect o their
use in the present invention are also obtained if~ after the
addition of the acid and of the water, the preparation is
further stored at room temperature or elevated temperature,
for example for 4 hours a~ 70C or for a longer period at a
l~wer temperature.
Be~ore their use in the present ln~ention, the preparat;ons
o the salts of ~he reaction products are diluted with water
to give an aqueous sizing liquor having a salt content of
0.02 to 0.2, preferably 0.06 to 0.14~ pPrcen~ by weight. In
the pro~ess of the invention3 the siæing liquor is applied to
~le paper for example by spraying, preferably by padding, as
a rule at room temperature. Subsequen~ly the ~mpregnated paper
is dried at 60 to 140C, preferably at 90 to llO~C, for 0.1
to 10, preferably for 2 to 6, minutes. After drying, a paper
is o~tained which has a surface coating of reaction product
~,
salts of 50 to 150, pre~erably ~0 to 120~ mg/m~.
The paper to be sized in the process of the inven~ion is any
kind of paper of any surface weigh~, for example paper and
cardboard of bleached and un~leached sulphite or sulphate
cellulose. The surface-sized paper trea~ed according to the
proc ss of ~he invention also cons~itutes a further object of
the invention.
:
.
-- ; : :
The subs~antial advantage attaching to the process of the
present invention is that, even when very small amounts of
reaction product salts are applied to the surface of the
paper, good sizing effects are attained which are conirmed
by positive test resul~sg such as the alkali droplet test,
ink flotation time, and determination o the water absorp~ion
according to the method of Cobb. In particular, the small
surface coatings make a rapid operation possible~ so that a~
a drying temperature of for example 90 to 110C, good
surface siæings are attained even within about 20 to 40
seconds. Furthermore, the reaction product salts used
according to the invention have good c~mpatibility with the
customary assistants us~d în the paper industry, such as dyes,
pigments~ binders, in particular fluorescent brightening agents
and other additives. In addition, the reaction product salts
do not ~end to produce an unde~irable foam fonmation.
In the following Manu~acturing Directions and subsequent
app~ica~ion Example~ the parts and percentages are by weight.
- 12 -
':
.. , . - , , , , , . :- ,
. ~ ~ , . . .
- , . -, ~ . . . .
- . .
. ~ -. - .- . , :
Manufacturing Directions
A. To a solution of 56.2 parts (0.2 amino group equivalent~ of
a fatty amine mixture of palmitylamine, stearylamine and
oleylamine in 15 parts of isopropanol is added at 80 to 90C
in the course of 1 hour a solution of 75 parts ~0.4 epoxide
group equivalent) of an epoxide, formed from 2,2-bis-(4'-
hydroxyphenyl)-propane and epichlorohydrin, in 15 parts of
isopropanol ~len the addition of epoxide is complete~ the
reaction mixture is kept for a quarter of an hour at 85 ~o
9QC. Then a solution of 42.75 parts (0.17 amino group
equivalent~ of a polyethyleneaminopolyam;de derived from
polymerised linoleic acid and triethylenete~ramine in 15 parts
of isopropanol is added to the reaction mixture. After the
addition of the poly~ide, the reaction mixture is kept for
2 hours at 85 to 90C. A mixture of 12.5 parts of 85%
orthophosphoric acid and 13 parts of acetic acid (as glacial
acetic acid~ is then added to the reaction mixture in the
course of 1/2 hour and sub~equently 412 parts of deionised
water are added. A low-viscosity solution with a solids
content of 30~0 and a pH value of 4 is obtained.
- 13 _
' ' ' ~,- . '-, . ' ' :, .. .
-
: , ~. . . - .
' ' ~: '. '
~L$~ 76
B. to Z, AA and BB. The procedure of Manufacturing Direction A
is repeated, except that, instead of the phosphoric acid/
acetic acid mixture, the amount indicated in Table 1 of the
acids or acid mixtures is added. The solids content of the
solutions obtained is uniformly 30% as in A. The amount of
water required to obtain this solids content and the pH valu~
o~ the solutions obtained are als~ given in Table 1.
'
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CC. To a solution of 18.9 (0.07 amino group equi~alent) of a
fatty amine mixture of palmitylamine, stearylamine and
oleylamine in 20 parts of isopropanol is added at 80 to 85C
in ~he course of 1 hour a solution of 19 parts ~0.1 epoxîde
group equivalent) of an epoxide, formed from 2,2-bis-(4'-
hydroxyphenyl)-propane and epichlorohydrin, in 15 parts of
isopropanol. When the addition of epoxide i5 c~mplete~ the
reaction mixture is kept at 85 to 90C for a quarter o~ an
hour. Then a solution of 37.8 parts (0.~5 amino group
equivalent) of a polyethyleneaminopolyamide,~erived from
pol~merised linoleic acid and triet~ylenetetramine,in 15 parts
of isopropanol is added to the reaction mixture. After the
addition of the polyamide, the reaction mixture is kept for
2 hours at 85 to 90C
A solution of 9 . 6 parts of colophonium in 7 . 2 parts of glacial
acetic acid is then added to the reaction mixturc~ which is
subsequently kept or 20 minutes at 85C. The reaction mixture
is then diluted with deionised water, to give a solu~ion wi~h
a solids content of 30% and a pH value of 7
~ .
:
17 - :
:
:
.:
,~
~Lh~ 7~
DD. To a solution of 32.4 parts (0.12 am;no group equivalent3
of a fatty amine mixture of palmitylamine, stearylamine and
oleylamine in 25 parts of ethylene glycol mono- n-bu~yl ether
is added at 80 to 85C in the course of 1 hour a solution of
38 parts (0.2 epoxide group equivalent) of an epoxide, formed
from 2~2-bis-(4'-hydroxyphenyl~-propane and epichlorohydrin,
in 25 parts of ethylene glycol mono-n-hutyl ether. When the
addition of epo~ide is complete~ ~he reaction mix~ure is kept
for a quarter of an hour a~ 85 to 90~C. A solution of 1-~.6
parts (0.07 ~mino group equivalent) of a pvlyethyleneamino-
polyamide,derived from polymerised linoleic acid and tri-
ethylenet~tramine,in 15 parts of ethylene glycol n-butyl ether
is then added to the reaction mixture. After the addition of
the polyamide~ the reaction mixture is kept for 2 hours at
85 to 9~C.
A solution of 7.76 parts of sulphamic acid in 159 parts of
water is then added to the reaction mixture, giving a solution
with a solids content of 30% and a pH value of 5.9.
. :
'~
, - .
.
- ~8 _
~, . .
~3~7
Example 1
A filter paper of pure cellulose having a weigh~ per uni~
area of 140 g/m is padded at a rate of 4m/min and a pressure
of 10 kg/m with an aqueous liquor which contains 0.1% of
salts of the corresponding reaction products by dil.uting with
water the solutions obtained i~ accordance with Manuacturing
Directions A to Z, ~A and BB. The padded paper is dried for
30 minutes at 120 to 125C.
The surface-sizing of the treated paper is assessed by means
of the ~ollowing tests:
Water absorption according to the method of Cobb at 30 seconds
duration of effect ~WA Cobb30) according to DIN 53 132.
The lower the water absorption, the bet~er the surface-sizillg
o~ the treated paper.
Ink flotation time (IFT) with test ink according to DIN 53 126
In accordance with DIN 53 126, test ink "Blue" for paper is
poured i~to a porcelain dish measuring 10 x 12 cm until a level
of 0.5 cm is a~tained~ The paper for testing is folded into
lit~le boa~s with upright edge (4 x 4 cm). Using tweezers~ the
boats are set on the surface of the ink. Simultaneously a
stop-watch is released and the t~me is measured up to the point
when a visible striking through of the in~ occurs. The result
i9 measured in seconds, rounded off to an interval of 1~ seconds.
~ 19 _
:
,, . ~ ........ . . ...... , . . ............... . -
.. . ... ...
~$~6
Using untreated paper~ the test ink strike~ through
lmmedia~ely. The longer the test ink ~akes to strike ~hrough
the sized paper, the better the siæingO
Alk~l;ro ~Iro~ylet test (ADT)
_
Using a 1 ml pipette, one droplet of an aqueous lN sodium
hydroxide solution is allowed ~o fall rom aheight of 5 cm
onto the paper to be tested, which is kept in the horizorltal
position, and simultaneously a stop-watch is released.
The interval of time required until the paper has absorbed
the droplet is then measured. The result is reported in
seconds, rounded off to an interval of 10 seconcls
Unsized paper absorbs the alkali droplet ~mmediately, whereas
the slower the absorption on sized paper the better the ~iz;ng
effect. The test results of the paper treated according to the
invention and of the untreated paper are reported in Table II.
.
The figures represent the average o~ 4 measurements at
WA Cobb30~
. .
'
0 _ :
.. . . . .... . ~ . - ,, .. , . ~ . . .
Table II
, _ _ _ . _
Reactlon product _
salts contained Appl cation WA Co~30 est Result s _
liquors according ry g/m2 IFT ATD
to Manufacturing mg/m sec, sec.
Instruction
~ _ ~ . .. __ ~ . . .
A~60 22 ~lS00 ~1500
B ~0 24 >1500 ~1500
C~60 -34 ~1500 ~1500
D~60 30 ~1500 >1500
. _ ~O . . ~ ~~~500~~~--~r500
F118 23 ~1500 2~0
G87 25 >1500 150
H~60 22 ~1500 >1500
~60- ~ . ~ï~soo > lSob
~~60 29 >1500 >lS00
.- . K~60 28 ~1500 >1500
~~60 _ ~7 >1~00 _ ~1500
_ ~ --- - 60 --~ 27 >lS00 ~lS00
N ~60 28 ~1500 $1500
0 - ~60 27 ~1500 >lS00
P _ ~0 _ 25 ~15~0 ~1500
_ __ _ _ ~J60 29 ~1500 ~1500
R N60 29 ~lS00 >1500
S ~60 3~ >lS0~ >1500
T ~60 25 >1500 ~1500
~-~ 0 - 30 1250 ~1140
V ~60 31 >lS00 ~lS00
~ ~60 ~9 ~150~ ~lS00
_ ~ , _ "J60 28 ~1500 ~1500
untr~e~t~ed PaPe~r~ 0 ioo ~ 10 - 10
~ . __ . ___ _. _. .... ,
S~milar results are obtained when using solu~ions which
contain the salts of the reaction products according to
Manufacturing Directions Y, Z, BB, CC and DD.
21
,:
.
- : ~ ,, . : . .
- , :: .
' ' - ' ~ . ~ ' : ' ~ ' - , , .: - . :
~ 7
Exam~le 2
The procedure of Example 1 is repeated, except that the
filter paper is padded with aqueous liquors which contain
0.1% of salts of the corresponding reaction products by
diluting with water the solutions obtained in Manufacturing
Directions CC and DD. The padded paper is dried a~ a rate
o~ 4 m/min on a drum having a surface temperatllre of 100C.
The surface-sizing of the treated paper is assessed by the
tests described in EX~plP 1. The results of these tests are
reported in Table III.
Table III
. . ................... . . _ ... . __ .
Reaction product salts ~ T st R lt
con-tained in the - Applica~on e esu s
treatmen~ liquors dry WA Cobb _
according to 2 2 30 IFT ATD
Manufacturlng Direction mg/mg/m sec. _sec.
_ . . . ~ 60 22 >1500 ~1200
DD 60 23 1500 >1200
- untreat~d paper 0 100 10 10
S~milar results are obtained w~len using solutions which
contain salts of the reaction products of Manufacturing
Directions A to Z, AA and BB~
. .
~ .
: - 22 - ~
:: -
