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Патент USA US2110879

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2,110,879
Patented Mar. 1?, 1938
UNITED STATES
PATENT OFFICE :
2,110,879,
CATALYTIC HYDRATION' ory'omrmns 'ro
'
ALCOHOLS
iWalter Philip Joshua, Cheam, Herbert Muggleton Stanley, Tadworth, and John Blair Dymock,
Sutton, England
' _ No Drawing.
Application January 19, 1934, Se
rial No. 707,416. In Great Britain February 8,
1933
'
9 Claims. (01. 260-456)
Example I v
The present invention relates to the combina
' tion of ole?nes and water vapour to form the
corresponding alcohols with the aid of suitable
catalysts. The mechanical stability of such cata
5 lysts is of considerable importance when high
partial pressures of steam are used.
According to the present invention the hydra
tion of the ole?nes is e?ected with the aid of a
1O
catalyst rendered mechanically stable without
its activity being impaired by incorporating with
the active catalytic material during the prepara
tion of the catalysts organic ‘substances capable
of forming'true or colloidal solutions‘ in water,
A catalyst comprising one gram‘ molecule of
manganese carbonate, half a gram molecule of
boric anhydride and four gram molecules of
phosphoric acid was evaporated down to dryness 5
on an air bath in the presence of 35 grams of
sucrose. The resulting product was ground and
baked at 200° :C. until no odor. of caramel was
perceptible. The dry'friable product was ground
up with 2 per cent of linseed oil as binder and L10
tabletted. The tablets were baked at 200° C;
’
This catalyst when employed at a temperature
of 280° C. for the catalytic conversion of ethylene
into ethyl alcohol by means of steam, using a
and which when subjected to relatively elevated
15 temperatures in admixture with the ‘catalytic total pressure of 40 atmospheres, i'. e. 10 at'mos- 15
material will leave as residue in the catalyst sub
pheres of steam and 30 atmospheres‘ of ethylene,
stantially carbon only. The subjection'of the remained mechanically stable, and produced a
mixture to the elevated temperature may be ef
yield of ethyl alcohol of 248 grams per litre of
fected in the presence of oxygen containing gases.
The amount of added organic substances is‘pref
20 erably riot more than 20 per cent by weight of.
the catalytic material employed in the prepara
catalyst per hour.
-
'
‘ A catalyst of similar composition but without 20
the inclusion of sucrose could not have been
produced in a form sufficiently friable to allow‘oi
tion of the catalyst.
'
tabletting and would under the above pressure
As examples of suitable organic substances ca- . conditions have changed to a mud within about
2r pable of forming true solutions or colloidal solu
" tions/in water and of leaving substantially noth
ing but carbon in the catalyst ?nally obtained
for use, .we may mention the fgallowingz-sucrose,
starch and other carbohydrates such as glucose,
fructose, and molasses; also gelatine, pectin and
30 _ the like, and higher alcohols such as glycerol and.
mannitol.
,
a
‘
The incorporation of the organic material is
particularly applicable to catalysts consisting of
phosphates of active elements and containing an
excess of phosphoric acid over and above the
amount required to form the orthophosphate or
the element or elements employed. When at
tempt is made to use catalytic material con
taining relatively large amounts of phosphoric
4O
‘acid under conditions of high partial steam pres
sure such as is required at total working pres
sures between 20 and 100 atmospheres without
?rst preparing the material as above described,
it tends to break down mechanically. The me
as CH
chanical stability oi.’ such material could be im
proved by decreasing the amount of phosphoric
acid present in it, but we have found that this
reduces materially the activity of the material
-0 and diminishes the amount of alcohol which can
be produced per unit volume of such ‘material.
The following examples illustrate the manner
in which the invention may be carried into effect
two ‘hours and would not have given suchv high 25
yields of alcohol.
‘
'
Example II
A catalyst comprising one gram molecule of
calcium oxide, half a gram molecule of boric an 30
hydride, and four gram molecules of phosphoric
acid was evaporated down to dryness on an air
bath in the presence'of 30 gram molecules of
sucrose. The mass was treated in the same way
as in Example I, but tabletted with 3 per cent
of linseed oil as binder.
35
When used under the same temperature and
pressure conditions as in Example I, the catalyst
remained mechanically stable and yielded, per
litre oi catalyst, 25?. grams of ethyl alcohol per 40
Example III
A catalyst comprising one gram molecule man
ganese carbonate, halt a gram molecule of boric
anhydride and 3.6 gram molecules of phosphoric
acid was evaporated‘down to dryness in the pres
ence of 5 per cent glycerine,‘ calculated on the dry
weight of catalyst.‘ The mass was treated as in
Example 11, being 'tabletted with 3 per cent 01' 50
linseed oil as binder.
,
.
The output of ethyl alcohol from ethylene and
steam under similar temperature and pressure
and the results obtained by using the catalysts conditions to those used in Examples I and II
was 110.7 grams per hour.
55
described.
>
_
_
‘
55
~ 2
2,1 10,879
What we claim is:—
1. The process of catalytically converting ole
?nes and water vapor into alcohols which com
prises passing said ole?nes and water vapor over
a phosphate catalyst wherein excess phosphoric
acid is incorporated, said catalyst being made by
incorporating with the active catalytic material
I an organic material leaving when heated sub- '
stantially only a carbon skeleton without dete
10 ‘riorating the catalyst and capable 01» forming a
?nes and water vapor into alcohols which com
prises passing said ole?nes and water vapor over
a phosphate catalyst wherein excess phosphoric
acid is incorporated, said catalyst being made by
incorporating with the active catalytic material
a carbohydrate and then subjecting said catalyst
to an elevated temperature so that said carbo
hydrate will leave in the catalyst as a residue
substantially, only carbon whereby a carbona;
ceous skeleton is formed in situ which will give 10
true or colloidal solution in water and then sub
the necessary mechanical stability for withstand
jecting said catalyst to an elevated temperature ing the conditions of said process.
so that said-organic material will leave in the
6. The process of catalytically converting ole
catalyst as a residue substantially'only carbon ?nes and water vapor into alcohols which coni
v15 whereby a carbonaceous skeleton is formed in > prises passing said ole?nes and water vapor over
situ which will give the necessary mechanical a phosphate catalyst wherein excess phosphoric 15
stability for withstanding the conditions of said
process.
2. The process of catalytically converting ole
20 ?nes and ‘water vapor into alcohols which com
prises passing said ole?nes and water vapor over
‘ a hydration catalyst wherein an excess of a min
eral acid is incorporated, said catalyst being made
by incorporating with the active catalytic mate,
25 rial an organic material leaving when heated
substantially only a carbon skeleton without de
teriorating the catalyst and capable of forming
a true or colloidal solution in water and then sub~
jecting said catalyst to an elevated temperature
30 so that said organic material will leave in the
catalyst as a residue .substantially only carbon
whereby a carbonaceous skeleton is formed in
situ which willgive the necessary mechanical
acid is incorporated, said catalyst being made by‘
'incorporating with the active catalytic material
a higher alcohol and then subjecting said cata
lyst :to an elevated temperature so that said 20
higher alcohol will leave in the catalyst as a resi-'
due’substantially' only carbon whereby a car
bonaceous skelton is formed_in situ which will
give the necessary mechanical stability for with
standing the conditions of said process.
25
7. .The process of catalytically converting ole
?nes and water vapor into alcohols which com
prises passing said ole?nes and water vapor over
a phosphate catalyst wherein excess phosphoric
acid is incorporated, said catalyst being made by 30
incorporating with the active catalytic material
gelatin and then subjecting said catalyst‘ to an el
evated temperature so that said gelatin will leave
stability for withstanding the conditions of said . in the catalyst as a residue substantially only car- ,
process.
bon whereby a carbonaceous skeleton is formed 35
3. The process of catalytically converting :‘e
in situ which will give the necessary mechanical
fines and water vapor into alcohols which com
stability for withstanding the conditions of said
prises passing said ole?nes and water vapor over
a phosphate catalyst wherein excess phosphoric
8. The process of catalytically converting ole
acid is incorporated, said catalyst being made by . v?nes and water vapor into alcohols which com
incorporating with the active catalytic material prises passing said ole?nes and water vapor over‘ 40
an organic material leaving when heated sub ' a phosphate catalyst wherein excess phosphoric
stantially only a, carbon skeleton without de-' acid is incorporated, said catalyst being made by
process.
teriorating the catalyst and capable of- forming a
45 true or colloidal solution in water and then sub—
jecting said catalyst to an elevated temperature
in the presence of an oxygen containing gas so
that said organic material will leave in the cat
alyst as a residue substantially only carbon
50 whereby a carbonaceous skeleton is formed in
situ which will give the necessary mechanical
stability for withstanding the conditions of said
process.
i
4. The process of catalytically converting ole
55 ?nes and water vapor into alcohols which coin
pris'es passingv said ole?nes and water vapor over
a phosphate catalyst wherein excess phosphoric
acid is incorporated, said catalyst being made
by incorporating with the active catalytic ma
60 terial an organic material leaving when heated
substantially only a carbon skeleton without de
.
'
incorporating with the active catalytic material
glycerol and then subjecting said catalyst to an 45
elevated temperature so that said glycerol will
leave in the catalyst as a residue substantially
only carbon whereby a carbonaceous skeleton is
formed in situ which will give the necessary me
chanical stability for withstanding the conditions 50
of said process.
9. The process of catalytically converting ole
?nes and water vapor into alcohols which com
prises passing said ole?nes and water vapor over
a» basic radical wherein phosphoric acid is in 55
corporated in excess of that required to form the
ortho phosphate of said radical, said catalyst
being made by incorporatingwith the active cat
alytic material an organic material leaving when
heated substantially only a carbon skeleton with 60
out deteriorating the catalyst and capable of
teriorating the catalyst and capable of forming
forming a true or colloidal solution in water and
a true or colloidal solution in water, the amount
then'subjecting said catalyst to an elevated tem
perature so that said organic material will leave
of said'organic material being up to 20% of the
65 weight of the active catalytic material used and
thensubjecting said catalyst to an elevated tem
perature so that said organic} material will leave
in the catalyst as a residue substantially only
carbon whereby a carbonaceous skeleton is
70 formed in situ which will give‘ the necessary me
chanical vstability for withstanding the condi
tions of said process.
‘
5. The process of catalytically converting "ole
in the catalyst as a residue substantially only car
bon whereby a carbonaceous skeleton is formed
in situ which will give the necessary mechanical
stability 'for withstanding the conditions of said
process.
WALTER PHILIP JOSHUA.
-
HERBERT MUGGLETON STANLEY.
JOHN BLAIR DYMOCK.
v
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