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Патент USA US2136016

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2,136,016?
Patented Nov. 8, 1938
PATENT OFFICE-i;
‘2,136,016
METHOD’ FOR’ ‘*MANUFAGT’URING" SULPHUR r
COLORS
_} Simon :Norman,.-Providence, It. I.,. assignor to
‘Industrial Dyes‘tu?r‘: Company, East.Providence,.,
R.,.I.',_ acorporation of Rhode Island
No-Drawing. Application October '24,; 1935,
ScrialNo. 46,629.
14., Claims. (CL, 260F129)
phur-for two-hours. 501 parts waterare added;
'I'hiscihventionrelates to an improved manu
facturezofrsulphur colors bya new method which and then 10 parts-dinitro-para-hydroxy diphen»
can: be "used-‘on, alargesvariety of intermediates
ylamine are ‘added: The‘ whole (‘is refluxed- for
that :can ‘be. thionated.‘
twenty-four‘ hours, at 115° C;', the ~-mixture ‘is:
then poured-~intoel,000‘ partsewat-er, air iskblowrrr 5:;
in until all‘ the dyestuff'is @precipitateds The»
dyestuif’ is‘ thenl‘filteredi ‘and!’ dried andiiis ~nowe
.
Inmanufacturing sulphurwcolors from inter
mediates, . like >methyl-hydroxy-aminophenazine
and: substituted .diphenylaminesv and‘ paramido
phenoLand. their :homologs, it .has been-custom»
aryto; employ, as thionating agents, alkali metal,
10;. polysulphidesr- or: mixtures.‘ of».‘sod~a- ash, sodium
sulphide. and;sulphur.
I have . discovered that - by,
theguse'gofr aahottsolution ‘of certain-alkylene»
amines andusulphur‘ containing substances, sul~1
phurucolorsuare. produced .‘givingwdifferent shades
11):. andupropertiesaas compared with those; obtained
whenrusingath'e .=thionating< agents; which are at
ready for use, giving a blue black-shade;
‘
Example 3.——35:_v parts; byiv Weight,v ethyléne>~1
diamin‘e- are‘heated at 1409‘ C.‘ with 45“ parts sull- 10%;
phur for two hours. 50I'parts tglycerine are"
added and. thenlO. parts methyl‘—hydroxy-amino-~
phenazine are added: ‘ Thewhole is re?uxed for-J
two hours at 170° C.) thelmixture-isthen=pouredi
into 1,000 parts water, air/is blown vin?-untiill’yall’i 162;
the dyestuffiis precipitated; Thedyestu?‘iissthene
present; being; used 1 in the: manufacture of: ' sul- '
?ltered and dried and is now.t-rea'dy-‘fore-use}.
phur colors from thesesame intermediates. As‘
agspeci?c' instance, a; hot solution-of diethylene
giving a red brown. shade.
20,-. \diamines and:.sulphur,: or 'homologs' of; same and -
sulphunrwill produce the. above statedwshadesx
. In the,followingsexamples; itxsh'ould be‘under
stood vthat. lnaminot‘ restricted as to temperature; '
durationzofitime, or quantitieswused, as various
25;»,shades. oil-"colors result atv temperatures‘rangingv
from 110.? C‘., or even less, up to'200? C.
Itzshoulda: further‘ be: understood‘ thatuwhile
these-.11 examples‘ disclosev the. use: of water..- or‘
glycerine as the liquidimedium forithethionating,
.
Example 4~.-45 parts,,by weight; tetra-ethylene“
triamine are heatedfsatw 150° 0;‘? with‘.v 451i; parts'j 211s
sulphur for two hours, 50tparts' glycerirletarm
added and then 10F‘-parts.paramidopheno-l ‘base;
are added; The wholerisire?uxed‘l'for ‘two: hours=
at 180° 0;, the mixture is ‘then: poured into!‘
1,000 :parts' water,“ air is. blown in until-‘fall ‘the-?irt
dyestu? ’ is precipitated.v The dyestutf ‘fisw then:
?ltered and‘ dried and is znowrreadyzfonuse, give»
ing ' an olive < drab shade.
I claim:
.
1.‘ The process. of manufacturing. sulphurrcolev 311av
suchras ‘ ethylene glycol,‘. ethyl ‘ether oftzethylene. ors, which comprises gheating. .451. parts; byiweiglit,
gylcoL'; butyl ether ofaethylene ‘glycol, and, also, of tetra ethylene triamine with» 451 partsrby.
the. higher. boiling alcohols; such asbutyl, amyl;v weight; of J'sulphur': at¢a~ temperature of about‘:
and hexyl alcohols, or a mixture of anytwo. or 150° 0., for iasperiodofs about 'two‘ .hours,:.adding:.~:
thereto 50 parts,'..by'weight,' ofxglycerineiand then‘; 3.5;;v
more; thereo‘f;
Itzshould; also, beunderstoodathat 'a'wide range 10. parts; by. weight, ofiparaminophenol base};
ofstsulphur color intermediates can: be thionated. then. re?uxingrthe .whole. for about? two hours; at‘;
a temperature ofabout 180°:C., th'ennpouringi-the
by~ this :method; ,
The: alkylene‘ amines- . which .I‘. use ‘are of .1 the mixture into" 1,0100‘ parts; by~weightp ofzr'watergx
4;); higher:w boiling: types, such ' as; ethylene :-diamine, V blowingv air into the. mixture until all ‘the. dye-w 405i
d0.._other.~‘highervboiling point media canavbe used;
tetra-1.. ethylene“ triamine, penta -. ethylene = tetra.-.
stuffwis precipitated, . and: then.1 ?ltering-:andidryei
mine, propylene diamine, etc., and their homo»
ing the said dyestu?‘.
IOgStLf
.
Example 1.—35 parts, by weight, ethylene
4.3 diamine are heated at 140° C. with 45 parts sul
phur for two hours. 50 parts water are added
and then 10 parts phenazine are added. The
whole is re?uxed for twenty-four hours at 115°
C., the‘ mixture is then poured into 1,000 parts
50 water, air is blown in until the dyestu? is precipi
tated.
The dyestu?‘ is then ?ltered and dried
and is now ready for use, giving a red brown
shade.
‘Example 2.-35 parts, by weight, ethylene
55 diamine are heated at 140° C. with 45 parts sul
2. In .a .method‘ Ofii’PltBB?I‘lllgilSlilDh‘llI colors
from: dyestu? intermediates; :that :are thionateds
to produce dyes by means of thionating agents, 45
thionating such dyestuff intermediate selected
from a group consisting of amino phenols of the
benzene series, amines of the benzene series, and
phenazines, in a medium prepared from alkylene
amine and sulphur heated together for sub- 50
stantially two hours at substantially 140° to 150°
0., in which medium the said dyestuff intermedi
ate is actively converted into a sulphur color.
3. In a method of preparing sulphur colors
from dyestu? intermediates that are thionated to 55
2.,,
2,136,016
produce dyes by means of thionating agents,
thionating such dyestu? intermediate selected
group consisting of amino phenols of the benzene
series, amines of the benzene series, and phen
from a group consisting of amino phenols of the
benzene series, amines of the benzene series, and
phenazines, in a medium prepared from diethyl
ene diamine and sulphur heated together for
substantially two hours at substantially‘ 140° to
substantially 150° C., in which‘ medium the said
azines, thionated in a medium prepared from
alkylene amine and sulphur heated together for
substantially two hours at substantially the range
dyestuff intermediate is actively converted into
10 a sulphur color.
4. In a method of preparing sulphur colors
from dyestu? intermediates that are thionated
to produce dyes by means of thionating agents,
thionating such dyestuif intermediate selected
15 from a group consisting of amino phenols of the
benzene series, amines of the benzene series,
and phenazines, in a medium prepared from
tetra ethylene triamine and sulphur heated to‘
gether for substantially two hours at substanti
20 ally 140° to substantially 150° C., ‘in which
medium the said dyestu? intermediate is actively
converted into a sulphur color.
140° to 150° C.
I
9. In a dyestu?, a sulphur color prepared from
a sulphur color intermediate selected from a
group consisting of amino phenols of the benzene
series, amines of the benzene series, and phena 10
zines, thionated in a medium prepared from a
thionating agent and ethylene amine heated to
gether for substantially two hours at substantial
ly the range 140° to 150° C.
10. In a method of preparing sulphur colors 15
from dyestu? intermediates that are thionated to
produce dyes by means of thionating agents, thi
onating such dyestuff intermediate selected from
a group consisting of amino phenols of the ben
zene series, amines of the benzene series, and 20
phenazines, in a medium substantially identical
with that produced by heating together for sub
5. In a method of preparing sulphur colors from stantially two hours at substantially the range
dyestu? intermediates that are thionated to pro
140° to 150° C., alkylene amine and a thionating
25. duce dyes by means of thionating agents, thionat
agent, in which medium the said dyestu? inter
ing such dyestu? intermediate selected from a mediate is actively converted into a sulphur color.
group consisting of amino phenols of the benzene
11. In a method of preparing sulphur colors
series, amines of the benzene series, and phena
from dyestuff intermediates that are thionated to
zines, in a medium substantially identical with produce‘dyes by means of thionating agents, thi
30 that vproduced by heating together for substan
onating such dyestu? intermediate selected from 30
tially two hours at substantially the range 140° C. a group consisting of amino phenols of the ben
to 150° C., an alkylene amine, sulphur and a liq zene series, amines of the benzene series, and
uid selected from a group consisting of water, phenazines, in a medium substantially identical
glycerine, ethylene glycol, butyl alcohol, amyl al
.cohol, and hexyl alcohol, in which medium the
said dyestu? intermediate is actively converted
into a sulphur color.
'
6. In a method of preparing sulphur colors from
dyestuff intermediates that are thionated to pro
40 duce dyes by means of thionating agents, thionat
ing such dyestu? intermediate selected from a
group consisting of amino phenols of the benzene
series, amines of the benzene series, and phena
zines, in a medium substantially identical with
with that produced by heating together alkylene
amine and sulphur for substantially two hours 35
at substantially 140° to 150° C., in which medium
the said dyestuff intermediate is actively con
verted into a sulphur color.
12. In a dyestu?, a sulphur color prepared
from a sulphur color intermediate selected from 40
a group consisting of amino phenols of the ben
zene series, amines of the benzene series, and
phenazines, thionated in a medium substantially
identical with that produced by heating together
45 that produced by heating together for substan-" alkylene amine and sulphur for substantially two 45
tially two hours at substantially the range 140° to
150° C., an alkylene amine, sulphur and higher
aliphatic alcohol having more than three carbon
atoms, in which medium the said dyestuff inter
50 mediate is actively converted into a sulphur color.
7. In a method of preparing sulphur colors from
dyestuff intermediates that are thionated to pro
duce dyes by means of thionating agents, thionat
ing such dyestufl intermediate selected from a
55 group consisting of amino phenols of the benzene
series, amines of the benzene series, and phena
zines, in a medium prepared from propylene dia
mine and sulphur heated together for substan
tially two hours at substantially 140° to‘ substan
60 tially 150° C., in which medium the said dyestuff
intermediate is actively converted into a sulphur
color.
8. In a dyestuff, a sulphur color prepared from
a sulphur color intermediate selected from a
hours at substantially the range 140° to 150° C.
13. In a dyestuif, a sulphur color prepared from
a sulphur color intermediate selected from a
group consisting of amino phenols of the benzene
series, amines of the benzene series, and phen 50
azines, thionated in a medium prepared from tetra
ethylene 'triamine and sulphur heated together
for substantially two hours at substantially 140°
to 150° C.
'14. In a dyestu?, a sulphur color prepared from 55
a sulphur color intermediate selected from a
group consisting of amino phenols of the benzene
series, amines of the benzene series, and phena
zines, thionated in a medium prepared from pro
pylene diamine and sulphur heated together for 60
substantially two hours at substantially 140° to
150° C.
'
SIMON NORMAN.
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