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[5][_]
acid
(44)
[6][_]
sulphonates
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[7][_]
petroleum
(14)
[8][_]
sulphonic acid
(13)
[9][_]
sulphonic acids
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[10][_]
sulphonate
(8)
[11][_]
acids
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[12][_]
hydrocarbon
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[13][_]
alcohol
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[14][_]
alkali metal
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[15][_]
salts
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Sulphonic acid
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[17][_]
alcohols
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[18][_]
amines
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[19][_]
heavy petroleum
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[20][_]
inorganic salts
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[21][_]
organic solvent
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[22][_]
salt
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[23][_]
substituted amines
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[24][_]
Amines
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[25][_]
Heavy petroleum
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[26][_]
aromatic carboxylic acids
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[27][_]
free acid
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[28][_]
metal
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[29][_]
metals
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[30][_]
alkyl-aminocarbinols
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[31][_]
alkyl and cycloalkyl-esters
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[32][_]
aminosulphonates
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[33][_]
di- and tri-alkyl-amines
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oleum
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Water
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[37][_]
ammonia
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[38][_]
Ammonium
(11)
[39][_]
benzene
(4)
[40][_]
sodium
(4)
[41][_]
sodium chloride
(4)
[42][_]
naphthalene
(3)
[43][_]
ammonium sulphate
(2)
[44][_]
hydrochloric acid
(2)
[45][_]
hydroxide
(2)
[46][_]
isopropyl alcohol
(2)
[47][_]
phonic acid
(2)
[48][_]
sulphur
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[49][_]
SO3
(1)
[50][_]
SOS
(1)
[51][_]
asphalt
(1)
[52][_]
calcium
(1)
[53][_]
magnesium chloride
(1)
[54][_]
nitrogen
(1)
[55][_]
sodium sulphate
(1)
[56][_]
triethanolamine
(1)
[57][_]
Water Calcium chloride
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[58][_]
naphthalenesulphonic acid
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Physical
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[60][_]
15 percent
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[61][_]
50 percent
(3)
[62][_]
12 percent
(2)
[63][_]
1800 gallons
(2)
[64][_]
55 percent
(2)
[65][_]
700 gallons
(2)
[66][_]
about 10 percent
(2)
[67][_]
about 5 percent
(2)
[68][_]
one hour
(2)
[69][_]
one ton
(2)
[70][_]
-24 hours
(1)
[71][_]
10 percent
(1)
[72][_]
15 to 20 percent
(1)
[73][_]
16 hours
(1)
[74][_]
16 percent
(1)
[75][_]
1600 gallons
(1)
[76][_]
18 percent
(1)
[77][_]
2 pounds
(1)
[78][_]
2 to 15 percent
(1)
[79][_]
2550 gallons
(1)
[80][_]
26 percent
(1)
[81][_]
31 percent
(1)
[82][_]
3400 gallons
(1)
[83][_]
38 percent
(1)
[84][_]
4 gallons
(1)
[85][_]
4-1 percent
(1)
[86][_]
400,009 pounds
(1)
[87][_]
41 gallons
(1)
[88][_]
4700 gallons
(1)
[89][_]
5550 gallons
(1)
[90][_]
60 percent
(1)
[91][_]
6500 gallons
(1)
[92][_]
6ft
(1)
[93][_]
7 percent
(1)
[94][_]
725 gallons
(1)
[95][_]
8 percent
(1)
[96][_]
800 gallons
(1)
[97][_]
84 percent
(1)
[98][_]
about 1 to 4 pounds
(1)
[99][_]
about 2 to 3 gallons
(1)
[100][_]
about 40 percent
(1)
[101][_]
about 45 percent
(1)
[102][_]
about 70 percent
(1)
[103][_]
below 25 percent
(1)
[104][_]
four hour
(1)
[105][_]
four hours
(1)
[106][_]
not more than about 25 percent
(1)
[107][_]
one-half inch
(1)
[108][_]
room temperature
(1)
[109][_]
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[114][_]
Spra
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[115][_]
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[116][_]
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Publication
_________________________________________________________________
Number GB400009A
i»?
Title
_________________________________________________________________
EN Title Improvements in or relating to solid carbonaceous fuels
Abstract
_________________________________________________________________
Sulphonic acid compounds derived from heavy petroleum or hydrocarbon
oils, naphthalene , benzene , the higher alcohols , organic sulphur
compounds, and c. are applied, as by spraying aqueous or organic
solutions, to solid fuels such as coal, coke, or briquettes to form a
film thereover which retards surface disintegration or slacking and
formation of dust during transport and c.
A freezing point depressant such as sodium chloride or molasses and c.
may be added to aqueous solutions, or substances tending to lower the
pour point may be added to oil solutions.
A slightly acid 15 per cent solution of sodium sulphonate derived from
petroleum may be used, about \ba1/3\be-2 lbs. of solid compound being
necessary for each ton of coal.
For winter conditions, however, aqueous solutions of alkali metal
sulphonates obtained from petroleum oil acid sludge may not be stable
and ammonium sulphonates may be employed, examples of the preparation
of which are described.
Amines and substituted amines may
neutralize the sulphonated compounds.
be
used in place of ammonia to
The acid is preferably applied in a number of treatments, the first
sludge being discarded.
The sludge from remaining treatments is washed with water , sulphuric
acid separated and withdrawn and the remaining sludge neutralized with
ammonia ; or if the sludge emulsifies it is allowed to separate into
layers which are washed separately.
The washing water may contain an electrolyte to aid separation, such
as sodium chloride , ammonium sulphate or hydrochloric acid .
Oil soluble sulphonic compounds retained in the oil after the
treatment of oils with sulphuric acid may be removed by washing with a
solvent such as isopropyl alcohol which may then be used with or
without neutralizing the sulphonic acids as a fuel treating agent.
Or the sulphonic acids or salts may be separated and made up as a
solution in alcohol , water or a mixture thereof.
Low boiling oils such as gasoline, naphtha, and c. may also be used
when fire risk does not arise, otherwise the compounds may be
dissolved in gas oil and c.ALSO: Heavy petroleum or hydrocarbon oils,
naphthalene or benzene are sulphonated and applied to solid fuels to
form a film which retards surface disintegration or slacking.
Preferably
the hydrocarbon oils are subjected
treatments, the first sludge being discarded.
to
a
number
of
The sludge from remaining treatments is washed with water , sulphuric
acid separated and withdrawn and the remaining sludge neutralized with
ammonia or organic amines ; or if the sludge emulsifies it is allowed
to separate into layers which are washed separately.
The washing water may contain an electrolyte to aid separation.
Description
_________________________________________________________________
- - - r (V'
Ii __[Second Edition.]
PATENT SPECIFICATION
Convention Dates (United States) Dec. 12, 1931:
Nov. 8, 1932:
- 400,009 Corrcsponding Applications in United Kingdom No 34,788/32)
Dated Dec. 8, 1932.
No. 34,789 /32 f (One Complete Specificatic n Left) Accepted: Oct. 19,
1933.
COMPLETE SPECIFICATION.
Improvements in or relating to Solid Carbonaceous Fuels.
We, STANDARD OS; DYELI.OPMENT COMv.
PXsy,
a corporation duly organised and existing under the laws of the
State of - Delaware, United States of America, having offices at
Linden, Nlew Jersey, and 100, West 10th Street, Wilmington, Delaware,
both in the United States of America, do hereby declare the nature of
- this invention and in what manner the same is to be performed, to be
particularly described and ascertained in and by the following
statement:This invention relates to solid carbonaceous fuels (coal and coke in
lump form, briquettes, and the like) which have a tendency to form
dust or fines by surface disintegration or slacking, for example
during transport, and the said invention comprises a method of
treating
such
solid
carbonaceous
fuels whereby this surface
disintegration or slacking is inhibited.
The invention also comprises solid carbonaceous fuels when treated in
accord- ance with the said method.
It is known that various sulphonic acid compounds, for example, alkyl
and cycloalkyl esters of sulphonic acids derived from aromatic
carboxylic acids contain- ing more than one benzene ring, have wetting
properties, and it has been proposed to use such compounds to wet and
bind dust particles. It has also been. proposed to deacidify acid
sludge or acid resin - - obtained from the refining of mineral oils by
means of sulphuric acid or oleum , and to use the deacidified or
neutral sludge as a binder in the manufacture of briquettes.
- It has now been found, in accordance with the present invention,
that surface disintegration or slacking -of solid carbonaceous fuels
(coal and coke in lump form, - briquettes, and the like), may be inhibited and the fuel thus rendered relatively non-dusting, by
coating it with a sulphonic acid compound, such as a sulphonic acid
compound derived from petroleum or a naphthalene sulphonic acid
compound derived from petroleum or [Price 1[[s]]] Prll'eas S acid ,
either as such or in the form of a salt thereof.
Sulphonic acid compounds of the type described possess the following
properties which make them desirable for treating solid fuels which
have a tendency to form dust or fines by surface disintegration or
slacking.
These compounds form tenacious films over the fuel surface. They lay
any
dust that may be present at the time of treatment, and
substantially prevent or retard surface disintegration or slacking of
the fuel. They do not retard combustion.
They add slightly to the fuel value of the material and do not result
in objectionable smoke production. They are substantially without
odour and under normal conditions of use they do not corrode metals
nor cause any injury to those handling the fuel. They can be applied
in solution (aqueous or organic solvent ) by ordinary spray methods.
They are available in many oil refineries as waste materials which can
be obtained very cheaply. The aqueous solutions applied can be
sufficiently concentrated to prevent danger of freezing and binding of
the fuel lumps together, or suitable freezing point depressants may be
added, e[[g]] sodium chloride or molasses. When oil solutions are
used, substances tending to lower the pour point may be added.
When dried upon the fuel in presence of air the sulphonic compounds
are not readily dissolved by contact with water .
The blackness and lustre of the fuel are improved by treating with the
sulphonic compounds.
Coal, coke, briquettes or the like which have been discoloured on
storage may also be improved in appearance by treatment with the
sulphonic acids or sulphonates .
The sulphonic acid compounds when added to the discoloured coal or
other solid fuel, coat the fuel and conceal the discolouration. Coal
which has been previously artificially coloured may- also be treated
with these sulphonic acid comsklD, 400,009 pounds in greater than
order to prevent, dustig Inn this ease the amount of treating material
used
is not sufficient to cover completely all of the -coal
particles,. thus xleaving7 - -:-5 some - of.-the characteristic colouring material to abct as- a distinguishing feature, = -:
:: - - We are aware that -various- substances ha-ving -certain- of
the- above-mentioned _properties hlve been used heretofore to make
-soid:
fuels
= non-dusting, forexample, mineral- oilsas 7uch.
emlulsifledel mineral oils, - magnesium chloride - andt - calcium
cehl6ride. -: t15 f- lThe- improved treating agents- may- be - applied
by-= any usual spraying means.
This is in ge6aerdl -prefezed- although the i=fel- may 'be immersed
in- thed sontion for otherwise -brought intf dontact -with -it.
-20 Au advatgeiisu way of: carrying -out -the: - - minventtion is: toprepare a 5-15 O/D solution.- of the- sulphonic acid compound in
wzater: referring first, -to_ water -soluble lcom- poundsy and spray
it on- the coal-or other 25- fuIel as it passes through the rotary
sizing - screens.: For example,. a- solution of_ 15 percent of sodium - sulphonate derived from petroleum and slightly acid isdesirableGenerally-, about,- to 2 pounds -of sd: o0 sulphonic - acid
compounds in solution. arex necessary fox- treating one ton of coal
to- form- a satisfactory superficial layer over - -the lumps. greater
than A somewhat larger quantity_i required for treating coke or other
8 absorptive fuel. -The treating- agebM: 7-5 - most conveniently
-supplied to the trade in coincentrated -form, say- about 45 percent
sulphonic acid compounds and 55 percent water :
This material-L-espcciaily the neutralized =40 sulphonic - acids ,
imay alscQ be dried by a spray drieror -iihe like and the powderdissolved in-= the necessary amulmnt- of - water at the piace where
the fuelis--to be,treated. - 2 - 4-5 Ia the foregohi-o-descriptifox
reference has- been made-to -the waiter soluble sul-:: -gphonic acid
-comipounds - which are well known products of the treatment of h a-y
- petroleum fractions with --'uming or con0 - centrated- sulphuric
acid for the manu-fact-ure of-white- oiljs and certaini - lubricating oi-ls - These sulphonic acid compounds are separated in the
sludgeifron the - acid treatment. The sludge is washed- with water
with or without the addition - of live steam:- and -the. acids are
used as -such 'or after: neutraizinig theem-with a suitable basewhich- -may be - an alkali metal or allkaline earth metal compound:
or- a- basic nitrogen - compound - (all of:
- X - - which- are referredto: as alkalies). The - --preferredbases-- are - ammonia , sodinmn -: - - hydroxide - and -ealeiumh
hydroxide . It is - highly advantageous- to- regiove as much: SY.
sulphuric - acid --lv such. treatme.t: as greater than possible and,
not only because of the -corrosive action of the latter and- the
increase in viscosity which it gives the solution, but - also because
of the white colouration produced- by- the sodium sulphate -when a n
neutralized sludge is allowed to dry on the =fuel. Generally, the
sulphuric acid content should be controlled to -between 25 / 15
percent . zThe - water - soluble alkali metal sulphonates obtamed from
petroleum oil acid - sludge are-generally -suitable- as fuel treating
agents. However, aqueous solutions of these alkali metal sulphonates
may not be stable -at the low temperatures to be encountered in
transportation- and. use -nder - wineta - conditions. These solutions
often separate into two: dissimilar layers when, subjected for even a
short period of time to teimperatures of about O' to- 30 IF -The
solution i-s less efective as a=-fuel - - treating -agent -if -used in
this- separated or - polyphase:condition and can be -rendered again
homogeneous only with extreme -difficulty.- ---- - It has been - found
that aquieoua solutions of ammonium sulphonates may be prepared: which
poss -the- deeirable quality of being stable in the cold.for -exte ded
periodi of time.:
- Thand -following example illustrates one =preferred -method of:
preparing such - ammonum sulphonate treating composi- tions. 7 =-- XlglPvrXLE I. = A heavy viscuas petroleum oil fraction suitable for
the preparation of lubricat- ing oils or white oils was vigorously
agitated -with about 10 percent by - volume of- a 15 percent strength
finning. -sulphurie-- acid (i[[e]] sulphuric- acid containig- 15
percent free SO3 ). - - The acid sludge was allowed- to- settle and
was separately drawn off. -The oil was then slubjected to- vigorous
agitation -witha sec6nd- batch of-fresh acid of similar 110 - strength
- in - an amount about 5 percent -by volumne of-the original- oil.
Thetemperature 6ft the -oil and acid mixture -during these
treatments -:was maintaiined- prefer- ably below about 100 F., - say
from: 115:0--lAODGl-. The mixture. wat- passed to a sludge settling:
drum where, on sta.nd:-ing, the-- treated oil -separated - as atoplayer
andwas
withdrawn. 4700 gallons of this-" secohdn
treatment-- acid -sludge"' 120 - separated into - two, layers on
standing for -24 hours , the uppe1f layer -containing 3400 gallons
and- the bottom layer - 1300- gallons.
-The bottom layer and a part of the upper layer- were -forced by
compressed air into 125 a lead lined k:ettle containing:15o0 gallons
of watr zat 158 - F:.--This- sludge- charge amounted to 1800 gallons
and- contained fl30/ percent -- of sulphuric -acid . -- The c
eoncentrations of- sulphuric acid in acid sludge 130 used in place of
ammonia to neutralize the washed acid sludge - of the above example,
or to neutralize other suitable sulphonated compounds- Such products
are classified as amino sulphonates for, the 70 purpose of this
invention.
The methods and materials used in pteparing the ammonium sulphonates
from sulphonated products. will be found to affect the stability of
the resulting fuel 75 treating solutions very appreciably. It is
preferable that the sulphonic acids used should be substantially
free.of water -insQluble material, such as asphalt , and that they
should have a combining weight 80 below about 450, Say, from 300 to
450s It is accordingly preferred in obtaining the sulphonates by.:
acid treating, petroleum oil to apply the acid in a number of separate
treatments, and to discard 85 the sludge formed in the first acid
treatment. Sufficient acid is used in the first treatment to remove
substantially all asphaltic material from the oil. Usually the first
treatment will consist of about 10 percent 90 by volume of 15. percent
strength fuming acid ui[[e]] sulphuric acid containing 15 percent free
SOS ), and the amount of acid is decreased in each successive
treatment to a final -figure of about 5 percent . The sludges: from 95
the successive treatments are generally suitable, and may be- used
together - or separately for the preparation of thelherein described
ammonium sulphonates .
These successive treatments, excepting 100 the first are classified
together as " second treatment acid sludge " for the purpose of this
invention. It is preferred to conduct all- acid treatments at as low a
temperature as possible, say from 609 to 106 1000 F.
When the "second treatment acid . sludge" -is permitted to stand- it
may separate into. layers. For example, a lower- layer containing
about 70 percent sulphuric acid may separate from an upper layer
containing about 40 percent sulphuric acid .- A middle layer,
appearing to be an emulsion of upper and lower layers-, may also form.
The lower layer may be- 11'S: washed with water very easily and
permits a ready separation of the diluted acid from the washed
sludge,- as shown in the washing operations of the above example. The
middle and: upper layers 120' can often be washed in a similar manner,
but will be found to emulsify with water much more readily than the
bottom layer.
With some sludges a very stable "mayonnaise-like" emulsion may be 125
formed, but these emulsions can be separated by slow agitation or
"squeezing"out the sulphuric acid phase.
The most desirable way to produce the fuel treating agent is to wash
the commentioned in this application are actually the per cent by
weight of inorganic salts in the sludge after neutralization with
ammonia and drying- at. 220 F.). The sludge was transferred in one
hour , and at the end of this period the temperature of the kettle was
218 F.
The- mixture was settled for one hour .
An aqueous bottom layer' consisting of 1800 gallons of 4-1 percent
sulphuric acid (by weight, determined by titration of free acid )
separated and was then drawn off.
The remaining sludge containing 38 percent sulphuric acid was then.
washed with 700 gallons of water with agitation.by blowing with steam
and air at 1940 F. After settling, 700 gallons of a lower aqueous
layer containing 31 percent sulphuric acid was drawn off. The
remaining sludge then contained 26 percent sulphuric acid . A third
wash
with 725 gallons of water was conducted under the same
conditions. In this case the aqueous layer formed on settling
contained 16 percent sulphuric acid and -separated as a top layer
because of its low density. 800 gallons of this upper layer were
removed by decantation.
The -sludge then contained 18 percent sulphuric acid ; Aqua ammonia
was added to this sludge with agitation until the colour changed from
green to brown. Water was added to adjust the concentration of the
solution to 50 percent solids.
Both
the
50 percent solids (trade) concentra-35 tion of the
neutralized sludge, considered as amimonium sulphonates , and the 2 to
15 percent (treating) concentration will be found- to pass the
following " cold. test".
- This consists in; maintaining a sample. of the treating agent for
four hours at 00 F. and- then permitting it to warm up; gradually to
room temperature . The- material does not pass this test if. a bottom
layer: or sediment can be observed when the -45 bottle containing. the
sample is slowly - turned upside down either at the end of the four
hour . period at 00 F- or after warming up, to roomn temperature. It:
has not been found possible to prepare a sodium sulphonate treating.
agent from petroleum acid sludges which will pass this test. The
ammonium sulphonate treating agents, especially if prepared according to the above described process, will 55- generally be found to
pass the cold test satisfactorily.
The products of the reaction of nitrogenous bases with sulphonic acids
gener- ally may be used as fuel treating. agents and are considered
within the scope of this invention. For - example, amino bases such as
the amines , substituted amines such as the di- and tri-alkyl amines ,
the alkyl amino carbinols such as triethanolamine , and the like, may
be I, A j 1 1 i i 1 1 1 i I11 400,(309 1 1 1 i 1 i 1 i i i i i i I i i
i i t J _4 plete supply of sludge with water , separate and draw off
the sulphuric acid , and neutralize the remaining sludge with ammonia
. However, due to the varying nature of the sludge, in some cases the
total sludge cannot be washed successfully due to emulsification-- The
sludge may then be allowed to separate into layers, and the layers may
be washed separately. In such event it is advantageous_ to wash a
limited mixture of the layers, containing say all the lower layer and
as much of the upper layers as will permit a ready= separation of
sulphuric acid .
The conditions best suited for obtaining a washed acid sludge from any
given acid sludge are best determined by small scale tests involving
settling of the sludge and washing of the separate or mixed layers as
above described.
- The method described above is satisfactory for sulphonic acids
obtained by-treatmg lubricating- oil (white oil) fractions with
sulphuric acid , However, when 2and another fraction of petroleum oil,
such as bottoms stock (cylinder stock, etc.), is treated with
sulphuric acid , the- following procedure is adopted to make a suit,
able coal-treating material: The sludge is first washed with a small
amount of water to remove sulphuric acid . The sulphuric acid (bottom
layer)-is drawn off, additional water is added to the top layer and
the water soluble sulphonic acids are 36- extracted and may be used
directly as such or partially iieutralized to treat solid fuel.
:-In carrying out-the-separation of-the sulphuric acid , it is
essential that the - nature of the sulphonic acids be altered as
little as possible. If the -temperature is too high the combining
weight.of the acids rises markedly-- especially in the presence of
live steam and strong sulphuric- acid , causing instability and in-solubility. It is preferable to keep the combining weight below about - 450 byholding the temperature below. 225 - F. when -large
amounts of strong sulphuric 50-- acid -are present.- When all of the
top layeri sludge is not washed with the u bottom flayer, that
remaining may -be used for-the preparation of the desired fuel
treating agents as illustrated by the following example.
EXAaiPLE 2.
1600 gallons of the remaining top layer of the second treatment acid
sludge from - Example: 1, containing 55 percent - sulphuric acid ,
were added to 6500 gallons of water at 1760 F. and were stirred for
one hourTith live steam and air, the final temperature reaching 203 F.
After settling for 16 hours 5550 gallons of a top aqueous layer
containing 8 percent sulphuric acid were drawn off, leaving 2550
gallons of sludge containing 15 percent sulphuric acid . - This washed
sludge was neutralized with 28 B6 ammonia water and the concentration
of the neutralized sludge adjusted to 50 percent solids. On subjecting
a 15 percent solids aqueous solution of this product to the above
described cold test a viscous bottom layer appeared. - However, when
this product -was mixed with the product of Example 1, the mixtureshowed
no
separation
during the cold test and was entirely
satisfactory as a fuel treating agent.
The water used in all steps for washing the sludges in the above
examples mav contain a- suitable electrolyte or coagulating agent for
aiding the separation of the sludges from the sulphuric acid . Such
agents are sodium chloride , ammonium sulphate , hydrochloric acid ,
and the like.:
707580It is desirable to use as treating agents ammonium sulphonate
solutions containing not more than about 25 percent of inorganic 90
salts by weight, based on the total solids on drying. at 220 F., and
solutions containing less than 10 or 15 percent are preferred.;
Consequently, when preparing the ammonium r sulphonate from acid
sludge, 95 it is desirable to wash the sludge to below the.
corresponding content of - sulphuric acid , that is; to' below 25, 15,
or 10 percent .
The inorganic salts will be found to increase the viscosity of -the
-solution, to 100 havve an adverse effect on - the "cold tests and to
have a tende ncy to separate out in the form of a concentrated salt
solution on long standing. It is also desirable to use-the washed
sludge in a 105 substantially= neutral form in. order to avoid
corrosive effects, but compositions only partially neutralized withammonia are also stable and are effective as fueltreating agents. 110 An important property of the Sul-phonates which makes them highly
desirable for treating solid fuels is their exceptionally high wetting
power. This is illustrated in the following table, 115. which gives
results of comparative tests of the time required to wet one-half inch
of a strip of paper towel dipped vertically into the surface of an
aqueous solution, of the treating agent. The coal treating 120Q
agents" mentioned are samples of materials sold commercially for this
purpose.
400,009 Treating Agent.
Ammonium sulphonates Water - - Calcium chloride Coal treating agent A'
Coal
treating
sgent
BCoal treating, agent C 400,009 - j ConcentrationPer cent _ - - 2.5 - -. - - 2.5 - 2.5 _ - - - 2.5 - 2.5
Time Seconds.
240 315greater than 360 It has been found that a considerable
reduction
in fracture and dusting is obtained by the use of
sulphonates as fuel treating agents. The fuel (coal and coke in lump
form, briquettes, and the- like) may be sprayed with a solution of the
sulphonates or may be dipped into such solutions. This reduction in
fracture is especially important in the case of soft coal, which when
handled under ordinary conditions without treatment may show a
degradation to fines of even 15 to 20 percent .
The application as a spray of 4 gallons of a 12 percent sulphonate
solution per ton of nut size bituminous coal has been found to reduce
the normal fracture by 60 percent and the dust by 84 percent .
The best results are obtained if the fuel is treated with a sufficient
volume of the' solution to wet its entire surface and larger amounts
are not objectionable.
Generally, not less than: about 1 to 4 pounds of solid ammonium
sulphonates in solution are desired for treating one ton of most solid
fuels. For example, the use of 41 gallons of a' 7 percent solution of
sulphonates may be used to reduce the dusting of bituminous coal,
while for coke or anthracite coal about 2 to 3 gallons of a 12 percent
solution of sulphonates give satisfactory results.
The oil soluble sulphonic- acid compounds are also suitable for making
coal non-dusting. These compounds are retained by the oil after the
sulphuric acid treatment and are removed from the oil by washing with
an organic solvent such as isopropyl alcohol .
The alcohol solution containing sulphonic acids may be used either
with or without completely or partially neutralizing the sulphonic
acids , for treating coal and other fuels. Alternatively, the
sulphonic' acids or their salts may be separated and supplied as a
solution in alcohol or in water or in a mixture of alcohol and water .
An equivalent method is to dissolve the sulphonic acid compounds in
gas oil" or other hydrocarbon oil the use of which would not involve
an undue fire hazard when spraying solid fuel. When the fire hazard is
not a consideration, low boiling oils such as gasoline and naphtha may
be used as solvents for the sulphonic acid compounds.
-If necessary, the solvent for the sul. 65 phonic acid compounds may
be heated to any temperature short of its atmospheric boiling point,
or heated under pressure, to' bring the sulphonic- acid compounds
readily into solution. In general such 70 heating is ncot necessary.
The proportions of the oil soluble sulphonic' acid compounds to' be
used may be -the same as described for the water soluble compounds. In
both cases it will 75 be understood that considerable variation in the
concentration' is- permissible, a higher concentration being required
for fuels having a more pronounced tendency to form dust. The presence
of other substances 'is not precluded in the coating composition so
long as the sulphonic acid compounds exert the essential non-dusting
effect.
The sulphonic
various kinds
non-dusting.
acid compounds
and fuels may
are 85 capable of carrying dyes of
be simultaneously dyed and rendered
Although the water -soluble sulphonated 'products, and particularly
the 90 neutralized sulphonated products obtained in. the treatment of
heavy petroleum oils with concentrated or fuming - sulphuric acid are
preferred for the treatment of solid fuels in accordance with the
invention,
sulphonic acids and their salts , obtained by the
sulphonation of naphthalene , benzene , the higher alcohols , organic
sulphur compounds, hydrocarbon oils and the like are also effective in
decreasing 100 the tendency of solid fuels to form dust or to crack
into- fines, and aqueous solutions of such ammonium sulphonates may be
prepared which possess the desirable quality of being stable in the
cold for 105 extended periods of time.
It will be understood that the inventiou is not concerned with the
treatment of fuel dust per se, or with the formation of briquettes
from fuel particles. 110 Having now particularly described and
ascertained the nature of our said invention and in what manner the
same is to be performed, we declare that what we
Claims
_________________________________________________________________
claim is:-'' 115
1. The method of inhibiting surface disintegration or saleking of
solid carbonaceous fuels (coal and coke in lump form, briquettes, and
-the like), wherein _ -400,009 ii and u7i-s coate 7dWit a siponic cd
fr riqjettes, and -the eb),- werein COmpud -- tihe -fuel isoat-ed with
ammonium - sul2 .The method. of -inhibiting sufb phonates -derived
from: - petroleumn oil disintegration or slack-ing of' oldcar"seco5)dc tr6iiatinit acid sludge " i-4 bonacobus-fuiels-(coal and
cokand in lump _141. Phe inmetlio - of ihbtn uae7 7 form uhipettes,
and- the like), whri itegratinoip slackig of sldcr the fuel is
-sprayed _with -a solduion -of--a b-onace-ous Tiiels- (coal and coke
in lump sulphonio , acid - compound.- - Bm briqudettds, arid the
like),
wherein 3The method of i--nhibiting- surface thle fuel
is-coated with a sulphonic acid -disintegrto --or-slacking- oft -olid
car- compouind- -hich -has been, prepared by 75 - bonaceous _fuels
Ccosl and -oeinlm contacting acid -reactive - petroleum oil for in,
briquettes, and arid the lik6), - -whereirt
-Yvith--strong-sulphu-ric'a-cid, separating-the the fuel is -coatdi
-With a sdlphoiie - a.i entslde ahn sai -eara -- compohnildcei-ived
from petrole-m-. -- - f sludge-with- water to reduce its- sulphuric
-71 47 'The- method greater than '- of inhibiting - srfade acid content to below 25 percent / and -adding 80 diintegratin Or -csackn
of- solid a- ammonia to at -least partially neutralize --boaceous fuels (coal - and coke-Il lin hM-i} theS wvashed 'sludge.-form,
briquettes,- ahrd Th likeY, wherehn 15. The method of inhibiting
surface fhe fel i spraed wit a stolutiom, of- a, disintegration-- or
slacking
of
solid- carsulphpicacid. cporindl deti'ved- fro- k
bon-a-ce-ous- fuels- (coal and coke in lump 85 - - petroleum . - - - - - - form, briquettes,- and the like), wherein - 5, Temethod,
accordig -to -lit3 or the -fuel is--coated- with a sulphoric acid to
Cr6im AL iwhichli-the Loudiopud- whiobiha been- prepared -y - composed
essentially of -suilpjibonic-- acidst confacting heavey - petroleum oil with a 6. The methiod according-td- Claim 3- or sufficieiit
7amount of- stroifg sulphuric -acid 90 to ai 4 , n -which te' _compoud
is t6 bcause - eparation as shidge of -substaii--compsed sseniaU
of!parfsllneuta iallyr all --6spha;ltic mnatter'; separating hized
[suiphonic acids -- said sludge -from -the- oil teting- said- 7. Te
metod accrdingto Claim 3 ox--s- parat and d1 ilwith fuming sulphuric, acid , toCam4 nwic tecmo s - ep- ar-atig- the resulting-second -sludge, 95 compose essentially 6f alkaisllit washing-Tsaidsecond -sludge.with water - to 8. The ethodl -according toCat.3o educe
its -sulphuric acoid content to- below -tor- 31ai,- iii hici - the
-compound -is 29W percent -' and --adding - ammonia to at leasit
compos esd -il o- wae- dib- - - - rtially zneutrahize - the washed
sludge. sodium - sulphonalte. -16---jO The -m-ethod -according to
Claim 15, 100 fl9 The imthbd according to Claim 3 or in: which thfe sul- phonic acid -cornpound -- to Clam 4, iiiwhich the com ud- is has
-bee prepared - by settling the -second 6opsd - e iatially- -o6f
-Wasioimbe -treatmnttsig Oa opri eaa ammonjiun sulphonuie. --tion, ito
layers, and sujcigthloe l. Thie - method of inhibiting- - surface
laver- to- the - washin and -neutralizn 0 disinteatin fitlacing
76fsdlid.6arbn-steps----n - - - -0 aceousfuels(6oal ldbk and i luinip
fohi, -17. The- method according -to -Claim 15, -- - briuetts - nd he
-like, whrei Th nwihthe sulpionic- - acid -compound Thui i spay4 Or
therwie brouht -ito hasbeenprepared- by' settling the second 4-5 cbtc
wt oiini i raiitetetsludge so--as -to permit- separa- slvef f il-olule
supilnicacd crn-- ionint lyers, and subjecting to' the - - - pound
derid frfrt ptrolem. - washig ar - ntraliing seps - the lower 11.Tli
mehd:ofiTitig srfae -ytogthe wih olyso much of the ffiintgfatib. i
skkg- 6f oidc-uppe er r as-permit ready separation -50 bomibep - (c66i
-aid coke- in luiprofilptfi abid on iwtshing - -- fr;btiquett e nd the
like), wherein- - 8.Thrnihod -of - inhibiting surface the- fuui isspra 'ed- or otherwise bruh dsnbg toiI r -slaxoking --f solid carintocontact svith d solution of-b, sul? hondceous ftela_ (coal -and -cokein lump-, phonicai compoflnd iai a.substafice - formi -hriquettes,
-and 'h iesbtn whi-dh depresse s - the -ee---Riig or p1our tfa.lly
as'hiereinibefor6
described. pomnt-of-tle [solution. 19li. S6lid
carbonaceouts - fuels (coal and 12. The inethbd Of inhibiting surfaee
coke, ini Iump tcim, 'briquettes and the is -iltertoi or skiii -of
sold car- like), -whener treated in- accordac wth bolnaceods -fuels7
(e and o-al and -coke greater than i-- lump tbe inethod- claimided in
any -of the p'reced60-- form, bHrquettes, amid - -bhea like),wher6lb. fingoCiaimt 2 -- tile fuI- soated -withh an amin - sul"Datlid th-is 8th day of December, 1932. phonate. D-- -- DYOUNG and
CO., -- 13. The, meth od- of inhibiting surface -11 and 12,
Soiithamnpton:Buildings, London, disintegationi or saeing[ ofsldhlf
-XQ -65- boiiaceoii fuels -2((oal -nd - cbke fil luiap - -Agefrts-fdr
tile Applicants. Abingdon: Printed for His Majsi's Stationery-Office,
by Burgess and Son. - [Ut. 830}1B.-50/111/1936.]
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