GB401612

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Molecule
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Sodium Chloride
(46)
[6][_]
NH3
(34)
[7][_]
sodium
(5)
[8][_]
calcium
(3)
[9][_]
magnesium
(3)
[10][_]
chloride
(2)
[11][_]
sodium bicarbonate
(2)
[12][_]
water
(2)
[13][_]
NaCl
(1)
[14][_]
ammonium
(1)
[15][_]
magnesium chloride
(1)
[16][_]
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Generic
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salt
(9)
[18][_]
salts
(2)
[19][_]
ammonia Sulphates
(1)
[20][_]
chlorides
(1)
[21][_]
sulphates
(1)
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Physical
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reduced pressure
(3)
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an hour
(2)
[25][_]
greater than atmospheric pressure
(2)
[26][_]
0.6 percent
(1)
[27][_]
5 percent
(1)
[28][_]
87 percent
(1)
[29][_]
99 percent
(1)
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Gene Or Protein
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Cl 2
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Publication
_________________________________________________________________
Number GB401612A
i»?
Title
_________________________________________________________________
EN Title Improvements in or relating to the extraction of purification
of sodium chloride
Abstract
_________________________________________________________________
Sodium chloride is recovered from substances containing it, such as
rock or sea salt , by extracting with liquid ammonia , separating
insoluble substances, and evaporating the solution obtained.
The whole of the sodium chloride may be recovered by evaporating the
solution to dryness, or a part may be recovered by heating to 30 DEG
C. and the mother liquor be used to extract more sodium chloride .
Extraction is preferably effected at a temperature between 0 and -- 10
DEG C., as below -- 10 DEG C. a less soluble ammonium compound of
sodium chloride , NaCl [[x]] NH3 , is formed.
The recovered salt is completely freed from ammonia by heating to
150-200 DEG C. under reduced pressure .
The solution of sodium chloride in liquid ammonia after evaporation to
remove excess ammonia may be treated with water to obtain a solution
for use in the production of sodium bicarbonate .
Description
_________________________________________________________________
r -i,I '; PATENT SPECIFICATION
Application Date: June 14, 1933 No 17,029/33.
Coplete Accepted: Nov 16, 7983.
COMPLETE SPECIFICATION.
401,612 Improvements in or relating to the Extraction or Purification
of Sodium Chloride .
I, RYOSABVRO HARA, of 43, Tsunogorocho, Sendai, Japan, an Engineer and
Subject of the Emperor of Japan, 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 Iby the following
statement:This invention relates
sodium chloride .
to
a process for Jo extracting or purifying
Sodium chloride in its naturally occurring state, such, for example,
as rock salt or sea salt is usually associated with other salts such
as the sulphates of sodium , calcium and magnesium and the chlorides
of magnesium and calcium as well as other impurities.
It is an object of the present invention to provide a new and improved
process for separating sodium chloride from other substances usually
associated with it in the naturally occurring salt .
The invention is based upon the discovery that sodium chloride is
soluble in liquid ammonia or forms with ammonia a compound which is
soluble in liquid ammonia Sulphates of sodium , calcium and magnesium
and all other impurities usually associated with sodium Bichloride in
the naturally occurring salt are found to be insoluble in liquid
ammonia and form no compounds with ammonia which are soluble in liquid
ammonia .
According
to
the
present
invention a process for obtaining
substantially pure sodium chloride from a mixture of sodium chloride
and other substances consists in treating the mixture with liquid
ammonia in order to dissolve the sodium chloride , separating the
solution thus formed from insoluble substances and extracting the
sodium chloride from the solution hby evaporating -the ammonia
Preferably 4,5 the mixture to be treated is added to liquid ammonia
and stirred therewith under a pressure greater than atmospheric
pressure and at a temperature below 00 Cl.
The sodium chloride either dissolves in t; the ammonia or forms
therewith a compound which dissolves in the ammonia , whilst the other
materials present in the mixture are insoluble and can easily be
fprice 1 '1-1 separated from the solution by a process of filtering or
decanting The filtrate, 55 which contains only pure sodium chloride in
solution, is then evaporated whereupon the salt crystallises out, and
the evaporated ammonia may lbe recovered without any loss and
liquified for further use 60 As the solubility curve of sodium
chloride in liquid ammonia has a negative co-efficient at temperatures
above minus C the filtered solution (the primary filtrate) may be
heated to a temperature 65 above this level in order to recrystallise
the greater part of sodium chloride , and the liquid (the secondary
filtrate) separated from the crystals by filtering or decanting This
secondary filtrate '0 contains only a small quantity of sodium
chloride and, therefore, can ibe used as the initial solvent in the
process.
The crystallised salt absorbs some ammonia and in order to remove all
traces 7,5 thereof from the crystals, the latter are heated to
150-2000 C under reduced pressure for an hour or two.
If it is -desired to utilise an ammonical solution of pure sodium
chloride , in 80 some manufacturing process, the orimarn filtrate
obtained as above may be prepared for use.
For 'example, the above method of purification may be easily applied
to the 85 Solvay process of manufacturing soda ash from sodium
chloride by proceeding as follows The primary filtrate is evaporated
to some extent, in order to remove excess 9 o ammonia The calculated
quantity of water is then introduced and stirring is continued to
dissolve all sodium chloride and ammonia at the temperature employed
in the process This solution 95 is used directly for the precipitation
of sodium bicarbonate in fhe Solvay dppafatus in the well known
manner.
Thus,
with
the simple processes of dissolving, filtering and
evaporating, sub loo stantially pure sodium chloride may be obtained.
The insoluble residue which remains after filteringz or decanting the
solution, contains impure, but useful substances i 05 The residue may
be heated to drive away 4 (c 1 401,612 ammonia and may then Ibe used
for the preparation of salts such as magnesium chloride .
The invention
examples:-
will
be
more particularly described in the following
EXAMPLE I. parts of raw solar salt ( 87 percent Na Cl 2 .
0.6 percent Mg SOQ, 0 5 percent Ca SO 4) is introduced into 1,000
parts of liquid ammonia under pressure, cooled to about minus 70 C and
stirred for an hour About 99 percent of sodium chloride in the raw
material can be easily dissolved in the solution, and then all
impurities are separated from the solution by filtration through a
suitable filtering medium At this temperature, sodium chloride is
dissolved in liquid ammonia as Na Cl, and if this operation is carried
out at a temperature below minus 100 C an ammonia compound of sodium
chloride , Na Cl x Nll,, is formed As this compound is less soluble in
liquid ammonia than sodium chloride , it is preferable to carry out
the operation above minus 100 C.
The filtrate thus obtained is evaporated to dryness finally leaving
160 parts of pure solid sodium chloride The evaporated ammonia is
recovered without loss and liquefied by means of an ammonia compressor
for further use.
EXAMPLE II.
The clear filtrate as obtained in the process described in Examule I
is heated to about 300 C to recrystallise the greater portion of
sodium chloride It has been found that at this temperature the
solubility of sodium chloride in liquid ammonia is 32 c'rammes per
kilogramme of ammonia Therefore, lbv separating the crystals from the
solution, it is possible to obtain about 130 parts of solid sodium
chloride in the form of fine crystals free from moisture The crystals
are separated from the weak solution by filtration or decanting and
the weak solution is employed for digesting fresh quantities of raw
material.
W 50 Having now particularly described and ascertained the nature of
my said invention and in what manner the same is to
Claims
_________________________________________________________________
1 be performed, I declare that what I claim is:1 A process for
obtaining substantially 55 pure sodium chloride from a mixture of
sodium chloride and other materials which consists in treating the
mixture with liquid ammonia in order to dissolve the sodium chloride ,
separating the 60 solution so formed from insoluble substances and
extracting the sodium chloride from the solution by evaporating the
ammonia .
2 A process for obtaining substantially 65 pure sodium chloride from a
mixture of sodium chloride and other substances which consists in
dissolving the sodium chloride in liquid ammonia under a pressure
greater than atmospheric pressure 70 and preferably at a temperature
below 00 C, removing insoluble substances bv' filtration or by
decanting and evaporating the clear solution to drayness.
3 A process for obtaining substantially 75 pure sodium chloride from a
mixture of sodium chloride and other substances which consists in
dissolving the sodium chloride in liquid ammonia under a pressure
greater than atmospheric and 80 preferably at a temperature below 0 C,
removing insoluble substances by filtra tion or by decanting and
heating the clear solution to about 30 C in order to recrystallise a
part of the sodium chloride , 85 and separating the recrystallised
sodium ' chloride from the remaining solution by filtration or
decanting.
4 A process for
claimed in Claim
obtaining
go 1 or
substantially pure sodium chloride as
Claim 2 or Claim 3, wherein the sodium
chloride is finally heated to 150-2000 C under reduced pressure in
order to remove all traces of ammonia .
5 A process for obtaining pure sodium if chloride substantially as
hereinbef ore described.
6 Sodium chloride when prepared 'bv the process claimed in any of the
preceding Claims O OO Dated this 14th day of June, 1933. G F REDFERN
and Co, Chartered Patent Agents, 15, South Street, London, E C 2,
Agents
for
the Applicant. Redhill: Printed for His Majesty's
Stationery Office, 'by Love and Malcomson, Ltd -1933.
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