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Патент USA US2122113

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PES5 'FÜR PRÜDÜCENG S'H‘ÀEILE SUEL
,E0 A
TESTER @MTS @F LEU@
vr-psass m par s'ra'ra
Roger Ratti, Basel, gvvitaerd, assignor to tf if
~ ilarit-
it@
à H
e
@i i Switaerl
È. À.,
a. aspiramos .time 2e, i935, sensi
(el.
It is known that the acid sulphuric acid esters
of the ieuco-vat-dyestuüs, like the acid sulphuric
acid esters of phenols, are stable towards alkalles,
but are decomposed by acids. They are brought
s)
paste. the water is eliminated at about 60° C.
in a vacuum dryer. There is obtained a dark
red powder which can easily be ground and dis
solves easily in water to a red solution.
5 onto the market in form of their alkali salts. - In
order- to obtain them as stable preparations in
powder iorm, it sumces in most cases to take
care that there is present a certain amount oi _
Example 2
100 kilos of the sodium salt of the acid sul-` '
phuric acid ester ofthe leuco-compound of the
alkali in excess, ,for example sodium carbonate._ green vat-dyestuff described in Example l of the my
10
llt has now been found, that some sulphuric
specification N_o. 212,471, in the form of
acid esters oi leuca-vat-dyestuüs, especially German
esters of leuco-vat-dyestuiïs of the anthraquinone a paste, containing 15 per cent of the vat-dye
series, undergo, even in the presence of a great
excess of alkali.' a slow decomposition, whereas
15.> in the form oi a paste they are stable for years.
It is indeed possible to dry these paste prepara-`
tions and to grind them. However, after a rel
atively short time, ya slow progressive decom
` position of the powdered preparations sets in and
20 cannot be restrained by the alkali in excess, which
is present and is intended to neutralize liberated
acid in order to thus avoid aciditication of the
mass.
It appears that the oxygen of the air
plays a part in this slow decomposition.
According to the present invention, a way has
25
been found, according to‘which the above men
tioned sulphuric acid esters, for instance the po~
tassium salt oi the tetrasulphuric acid ester of
the
30
tetrahydro-dichloro- 1 : 2-42’ z 1’-dianthraqui-
none azine, which, in spite of the excessvof the
alkali present, are liable to decomposition, can
be transformed into stable preparations in pow
der iorm. For this purpose the moist alkalilmlt
oi’ the ester is `intimately mixed with an excess of
35 alkali, with an aqueous solution of an agglutinant
and with urea. The thus obtained paste isevap
orated to dryness, preferably under reduced pres
sure.
As agglutinants there may be cited glu-a -
cose, cane-sugar molasses, sulphite cellulose waste
40
liquor, dextrln, -gum, glue and similar substances:
also mixtures of any of these substances may of
course be used.
'
*
.
'
invention is illustrated bi’ the following
examples.
d5 `
,
Example 1
300 kilos oi the potassium salt of the acid
sulphur-ic acid ester of leuco» Bz 2: Bz 2'-`dimethoxydibenzanthrone in form oi a paste con
50 taining 20 per cent orthe vat-dyestuñ in the
form oi the ester are mixed in a ball-mill with
ß kilos ci caustic soda solution (33%), 15 mios
of commercial molasses-syrup and. 10 kilos ci
'nrw dissolved in 20 litres of water. As ‘soon
55 as the mass has become mixed to a homogeneous
stuiî in the form of lthe ester, are mixed in a
ball-mill with 1 kilo of caustic soda solutiony
(30%)', 7.5 kilos of commercial molasses syrup ya,
and 7.5 kilos of urea dissolved in 8 litres of was
ter. When the whole is converted into a homoß;
geneous pastathe mass is ydried as described in
Example 1.
'
20
.
1. A process for producing stable ester 'salts
of leuco-vat-dyestuiîs in dry state, applicable to
ester salts, which are liable to decomposition,
even in the presence of an excess of alkali, said
process comprising intimately mixing the moist 25
alkali salts oi such esters containing an excess
of alkali with an agglutinant and urea to form
a paste and iinally evaporating the paste to dry
neSS.
'
'
Ü
'
-
2. A process yfor producing stable ester salts of so
leuco-vat-dyestuffs in dry state, applicable to
ester salts, which are liable to decomposition,
even in the presence of an excess of alkali, said
process comprising intimately mixing the rmoist
alkali salts ,of such esters containing an excess 35
of alkali with an agglutinant and urea to form
a paste, iìnally evaporating the paste to dryness
and grinding the same. '
'
\
'
3. A process for producing stable ester salts
or leuco-vat-dyestuüs in dry stata-applicable to 40
ester salts, which are liable to decomposition,
even in the presence of an excess of alkali, said
process comprising intimately mixing the moist
alkali salts of such esters containing an excess
.of alkali with molasses and urea to form a paste, 45
ñnally evaporating the paste to dryness and
grinding the same.
.
4. A process for producing stable lester salts
of leuco-vat-Sdyestuñ’s in dry'state, applicable to
ester salts, which are liable to decomposition. 50.
even in the presence of an excess of alkali, said
process comprising intimately mixing the moist
alkali salt of the acid sulphuric acid ester oi’
leuco-dimethoxy-dibenzanthrone containing an
excess of alkali with an agglutinant andA urea. to, M
2
3,122,118
form a paste, finally evaporating the paste to
dryness and grinding the same.
- ,
5. A process for producing stable ester salts
or leuco-vat-dvestufis in dry state, applicable to
ester salts, which are liable to decomposition,
even in the presence of an excess of alkali, said
process comprising intimately mixing the moist
alkali salt of the acid sulphuric acid ester of leuco
dimethoxydibenzanthrone containing an excess
of alkali with molasses and urea to form a. paste,
ñnally. evaporating the paste to dryness and
grinding the same.
.
ROGER RATI'I.
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