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Патент USA US2136017

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2435,0117
Patented Nov. 8, 1938
‘
UNITED," STATES PATENT oF'Fi-cE
1
_
‘
2,136,017
'Y METHOD iron MANUFACTURING SULPHUR '
.
COLORS
‘
,.
Simon Norman, Providence, R. 1., assignor to' In
dustrial Dyestuff ‘Company, East Providence,“
R. I., a corporation of Rhode Island
, - .
I No Drawing. " Application ‘June 22, 1936.‘
Serial No. 86,699
.
8 Claims.
(Cl. 260-—129)
This case in a continuation in part of my
earlier application, Serial No.. 46,629, ?led
October24, 1935.
,
:This invention relates to an improved manu:
facture of sulphur colorsnby a new method,
whichfwcan be used‘ on a large variety of inter
mediates that’ vcan be thionated.
’ These v intermediates
consist
of
phenazines,
and ‘more particularly the substituted phena
10
zines.
‘
‘
>
In manufacturing sulphur colors from inter
mediates, like m'ethyl-hydroxy-amino-phenazine
or diaminophenazine and substituted diphenyli
amines and paramidophenol and their homo
15 logs, it has been customary to employ, as thionat
ing agents, alkali metal polysulphides or mix
tures of soda ash, sodium sulphide and sulphur.
I have discovered that by the use of a hot solu
tion of certain alkylene amines and sulphur con
20 taining substances, sulphur colors are produced
giving di?erent shades and properties as com
pared with those obtained when using the thio
nating agents, which are at present being used
in the manufacture of- sulphur colors from these
25 same intermediates. As a speci?c instance, a
hot solution of ethylene diamine and sulphur, or
homologs of same and sulphur will produce the
above stated shades.
In the following examples, it should be under
30 stood that I am not restricted as to tempera
ture, duration of time, or quantities used, as
various shades of colors result at temperatures
ranging from 110° C., or even less, up to 200° C.
The reactions given further can be performed
35 successfully under pressure, such as in an auto
clave.
'
'
It should further be understood that while
these examples disclose the use of water or
glycerine as the liquid medium for the thionat
40 ing, other higher boiling point media can be
used, such as ethylene glycol, ethyl ether of
ethylene glycol, butyl ether of ethylene glycol,
and, also, the higher boiling alcohols, such as
butyl, amyl, and hexyl alcohols, or a mixture or
45 any two or more thereof.
It should, also, be understood that a wide
range of sulphur color intermediates can be
thionated by this method.
The alkylene amines which I use are of the
50 higher boiling types, such as ethylene diamine,
tetra ethylene triamine, penta ethylene tetra
mine, propylene diamine, etc., and their
homologs.
Example 1.—-35 parts, by weight, ethylene
65 ‘diamine are heated at 140° C. with 45 parts sul
phur for two hours. 50 parts‘v water arev added
and then, 10' parts v‘methyl-hydroxy-aminof
phenazine are added. The whole is re?uxedfor
twenty-four hours at 115°.’ C., the mixturefis
then poured into 1,000 parts water, air is blown
in until the dyestuii- is precipitated. The dye
stuff is then ?ltered and dried and is now ready
for use, givingl a'.red.brown ‘shade.
1
-
,
Example 2.—35 parts, by weight,’ ethylene
diamine are'heated ail-I40‘? C. with 4__5 parts su1-. 10
phur for two hours. 50 parts water are‘ added
and ‘then 10 parts dinitro-para-hydroxy diphenyl
amine are added.
The whole is re?uxed for
twenty-four hours at 115° C., the mixture is
then poured into 1,000 parts water, air is blown 15
in until all the dyestuff is precipitated.
The
dyestuii is then ?ltered and dried and is now
ready for use, giving a blue black shade.
Example 3.—-35 parts, by weight, ethylene
diamine are heated at 140° C. with 45 parts sul 20
phur for two hours. 50 parts glycerine are added
and
then
10
parts
methyl-hydroxy-amino
phenazine are added. The whole is re?uxed for
two hours at 170° C., the mixture is then poured
into 1,000 parts water, air is blown in until all
the dyestuff is precipitated.
The dyestu? is
then ?ltered and dried and is now ready for use,
giving a red brown shade.
Example 4.-—45 parts, by weight, tetra ethyl
ene triamine are heated at 150° C. with 45 30
parts sulphur for two hours. 50 parts glycerine
are added and then 10 parts paramidophenol
base are added. The whole is re?uxed for two
hours at 180° C., the mixture is then poured into
1,000 parts water, air is blown in until all the
dyestuif is precipitated.
The dyestu? is then
?ltered and dried and is now ready for use, giv
ing an olive drab shade.
I claim:
1. In a method of preparing sulphur colors 40
from dyestuff intermediates that are thionated
to- produce dyes by means of thionating agents,
thionating a dyestu? intermediate selected from
a group consisting of amino phenols of the ben
zene series, amines of the benzene series, and 45
phenazines, in a medium prepared from ethylene
diamine and sulphur heated together for sub
stantially two hours at substantially the range
140° to 150° C‘., in which medium the said inter
50
mediate is converted into a sulphur color.
2. In a method of preparing sulphur colors
from phenazines that are thionated to- produce
dyes by means of thionating agents, thionating
a phenazine in a medium prepared from ethylene
diamine and sulphur heated together for substan
2 V
2,136,017
tially two hours at substantially 140° to substan
tially 150° C., in which medium the phenazine
is actively converted into a sulphur color.
3. The process of manufacturing sulphur
colors, which consists in heating 35 parts, by
weight, of ethylene diamine with 45 parts, by
weight, of sulphur to a temperature of about 140°
C.', for a period of about two hours, adding there
to 50 parts, by weight, of water and then 10
10 parts, by weight, of methyl-hydroxy-amino
phenazine, refluxing the whole for a period of
about twenty-four hours, at a temperature of
about 115°’ C., pouring the mixture into 1,000
parts, by weight, of water, then blowing air into
15 the mixture until the dyestuif is precipitated,
and then ?ltering and drying the said dyestu?.
4. The process of manufacturing sulphur colors,
which consists in heating 35 parts, by Weight, of
ethylene diamine with 45 parts, by weight, of sul
20 phur to a temperature of about 140° C., for a
period ‘of about two hours, adding thereto 50
parts, by weight, of water and then 10 parts, by
weight, of dinitro-para-hydroxy diphenylamine,
re?uxing the whole for a period of about twenty
so
four *hours, at a temperature of about 115° C.,
then pouring the mixture into 1,000 parts, by
weight, of water, then blowing air into the mix?
ture until all the dyestuff'is precipitated, and
then ?ltering and drying the said dyestu?“.
35. The process of manufacturing sulphur colors,
which consists in heating 35 parts, by weight, of
ethylene diamine with 45 parts, by Weight, of
sulphur to a temperature of about 140° C., for a
period of about two hours, adding thereto 50
parts, by weight, of glycerine and then 10 parts,
by weight, of methyl-hydroxy-amino-phenazine,
re?uxing the who-1e for a period of about two
hours, at a temperature of about 170° C., then
pouring the mixture into 1,000 parts, by weight,
of water, then blowing air into the mixture until
all the dyestuff is precipitated, and then ?lter
ing and drying the said dyestu?.
6. In a method of preparingrsulphur colors,
thionating methyl hydroxy-amino-phenazine in
a medium prepared from ethylene diamine and
sulphur heated together for substantially two
hours at substantially 140° to 150° C., in which
medium methyl hydroxy-amino-phenazine is
converted into a sulphur color.
'7. In a method of preparing sulphur colors,
thionating para-aminophenol in a medium pre
pared from ethylene diamine and sulphur heated
together for substantially two hours at substan
tially 140° to 150° C., in which medium parae
amino-phenol is converted into a sulphur color.
8. In a method of preparing sulphur colors,
thionating dinitro-para-hydroxydiphenyl-amine
in a medium prepared from ethylene diamine
and sulphur heated together forsubstantially two
hours at substantially 140° to 150° .C., in which
medium dinitro~para-hydroxydiphenyl-amine is
converted into a sulphur color.
SIMON NORMAN.
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