fractional distillation (1903)

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FRACTIONALDISTILLATIONBY

SYDNEY YOUNG,

D.Sc., F.R.S.

PROFESSOR OF CHEMISTRY IN UNIVERSITY COLLEGE, BRISTOL.

WITH SEVENTY-TWO ILLUSTRATIONS

ILonbon

MACMILLAN ANDNEW YORK:

CO.,

LIMITED

THE MACMILLAN COMPANY

1903All rights reservtd

RICHARD CLAY AND SONS, LIMITED, BREAD STREET HILL, B.C., ANDBUNGAV, SUFFOLK.

PREFACEDURING the past eighteen years I have been engaged in investigations which necessitated the preparation of chemical materials in the purest possible state, and as theof fractional distillation had, in

great majority of these substances were liquids, the process most cases, to be resortedto for their purification.

The

difficulties I

met with

in

some

of the separations led

meand

toI

make a careful investigation of the whole subject, was thus enabled to devise some new methods and

forms of apparatus which have been described from time to time in various scientific journals.

hope that the solution of the which so often occur in carrying out a fractional

It is in the

difficulties

distillation

may

be rendered easier, and that the value and economy of

highly efficient still-heads in laboratory work

may come

to

be more widely recognised than is generally the case at present, that this book has been written.

Browntaken

J. Campbell works by Libavius and Ulstadius, from which Figures 2 and 34 have been

My

sincere

thanks are due to Professor

for the loan of valuable ancient

;

to

myfor

proofs,

and

colleague, Dr. F. E. Francis, for reading the much valuable assistance in compiling the

vi

PREFACE;

index

and

to

Professor R. A. Gregory andfor

Mr. A. T,

Simmons,proofs.

B.Sc.,

many

useful

the arrangement of the

MS. and

for

suggestions regarding the perusal of the

inin

In the description and illustration of the stills employed commerce I have derived much assistance from articlesThorpe's

"Dictionary

of

Applied

Chemistry"

and

" Precis de Chimie Industrielle." Payen's I have made much use of the experimental data of

Brown, Konowaloff, Lehfeldt, Zawidski and other observers, and have, as far as possible, made due acknowledgment, but in some of the tables this has not been practicable.Several fractional distillations and numerous experiments have been carried out while the book was being written and the results have in many cases not been publishedelsewhere.S.

Y.

BRISTOL,Anyn.it 1903.

CONTENTSCHAPTERINTRODUCTIONI

PAF,

APPARATUS REQUIRED

1

CHAPTERTHE BOILING POINT OF A PURE LIQUID

II

22III

CHAPTERVAPOUR PRESSURES OF MIXED LIQUIDS

32-

CHAPTER IVBOILING POINTS OF MIXED LIQUIDS

51

CHAPTER VCOMPOSITIONOFLIQUID AND VAPOUR PHASES;

EXPERIMENTAL71

DETERMINATIONS

CHAPTER VICOMPOSITION OF LIQUID AND VAPOUR PHASES, CONSIDERED THEORETICALLY89

CHAPTERCHAPTER

VII. .

DIRECTIONS FOR CARRYING OUT A FRACTIONAL DISTILLATION

114

VIII144

THEORETICAL RELATIONS BETWEEN THE WEIGHT AND COMPOSITION OF DISTILLATE

CHAPTER IXRELATION BETWEEN THE BOILING POINTS OF RESIDUE AND DISTILLATE 150

CONTENTSCHAPTER XMODIFICATIONS OF THE STILL-HEADPAGE 154

CHAPTER XIMODIFICATIONS OF THE STILL-HEAD (continued)',

DEPHLEGMATORS

.

171

CHAPTER

XII180

MODIFICATIONS OF THE STILL-HEAD (continued); "REGULATED" OR "CONSTANT TEMPERATURE" STILL-HEADS

CHAPTERCONTINUOUS DISTILLATION

XIII186

CHAPTER X[VFRACTIONAL DISTILLATION WITH AN IMPROVED STILL-HEAD.

.

.

191

CHAPTER XVDISTILLATION ON THE MANUFACTURING SCALE196

CHAPTER XVIFRACTIONAL DISTILLATION ANALYSISAS .A

METHOD

OF

QUANTITATIVE204

CHAPTER XVHMETHODS BY WHICH THE COMPOSITION OF MIXTURES OF CONSTANT BOILING POINT MAY BE DETERMINED223

CHAPTER XVIIIINDIRECT METHOD OF SEPARATING THE COMPONENTS OF A MIXTURE OF CONSTANT BOILING POINT 231.

.

CHAPTER XIXGENERALPURPOSES FOR WHICH FRACTIONAL DISTILLATION IS REQUIRED. INTERPRETATION OF EXPERIMENTAL RESULTS. CHOICE OF STILL-HEAD, NUMBER OF FRACTIONS, ETC. 239

REMARKS.

APPENDIX INDEX.

269-27.-)

LISTFIG.1.2.

OF ILLUSTRATIONSPAGE 33

employed by the Alexandrian Chemists Water condenser described by Libavius (1611)Still

3.

4.

5.6.

Ordinary modern apparatus for distillation Another ordinary form of apparatus Inner tube of condenser, bad and good forms (a and b). Guard for Bunsen burnerStill

456

8 817

7.8.

heated by steamvolatile liquids

Condenser for

9.

10.11.

Distillation under reduced pressure Modified receiver for above (Thome's),, ,,

18 19 19

(Bredt's)(Brtthl's)

12.13. 14.

20 22

Vapour pressure curve Vapour pressures of mixturesMixtures ofAnilineStill

of alcohols with water

.

.

4647

15.16. 17.

maximum vapour

pressure

56

Boiling points of mixtures of chlorobenzene and bromo-

benzene18.

57 58

Apparatus for determining the boiling points of mixturesDeviation of boiling point-molecular composition curve

19.

20.

Composition

from straightness (methyl and propyl acetates) ... Brown's of liquid and vapour phases.6

61

apparatus

73

xFIG.

LIST OF ILLUSTRATIONSPAGKComposition of liquid and vapour phases.apparatus Composition of liquid and vapour phases.apparatus Composition ofLehfeldt's

21.

75Zawidski's77

22.

23.

liquid

and

vapour

phases.

Gahl's

apparatus24.

81liquid

Composition ofapparatus Variation ofc

and vapour phases.

Carveth's

82with molecular percentage of

25.

A

(ethyl

alcohol and benzene)26.

103molecular fractional

Partial

andof

total pressures against

amount27.

A (ethylene dichloride

and benzene)

.

.

.

109

Fractional distillation of mixture of benzene and toluene.

Total weight of distillate plotted against temperature28. (a

.

122

and

Fractional distillation of mixture of methyl, Total weight of distillate ethyl and propyl acetates.b).

plotted against temperature29.30.

137 and 138 139

Separation of pentanes from petroleum Relation between weight of liquid distilled and compositiontillation

of

distillate

Two

components.

First dis-

145

31 and 32.

Relation between weight of liquid distilled and composition of distillate Two components. Laterdistillations

146

33 (a to/).34.

between weight of liquid distilled and composition of distillate Three componentsRelation.

.

147 154 163165

Modified still-heads6).

;

Ulstadius'"

still

35. (a and

" Rod aad Discstill-head

still-heads

36.37.

"Pear"

"Evaporator"

still-heads; original,,;

form(one section).

166 166 168171

38. 39.

;

modified

,,

(

,,

)

.

40.41.

Linnemann dephlegmatorGlinsky

172

LIST OF ILLUSTRATIONSFIG.

xi

42.43.

Le Bel-Henninger dephlegmator (, 6, c). Young and Thomas dephlegmator" Brown's " regulated temperature still-head Combined dephlegmator and regulated temperaturestill-

PAGE 172173181

44.45.

head46.47.

183distillation,,

Continuous,,

Carveth's apparatus

187

Lord Rayleigh's apparatus, modicomponents189197

fied so as to separate three

48.49.

Mansfield's

still

Coupler's

still still

198

50. 51.

French column

199

52. (a

Section of dephlegmator Dubrunfaut's and 6). Section of dephlegmator Egrot's,, ,, ,,

200

200201 201

53 and 54.55.56.57.

Savalle'sCofFey's

Section of Pistorius still-head(modified)

201201

58.

The " Coffey

"

still

202

59.

Specific gravities of distillates

from mixtures of ethyl226;

alcohol and water60.

Vapour pressure-molecular composition curvedisulphide and methylalDistillation of

carbon227

61.

62.

aqueous hydrochloric acid. Composition of liquid and vapour Carbon disulphide and methylal. Relative weights inliquid and vapour Carbon disulphide and methylal.

228229

63.

Logarithms

of relative

weights64.

229

Carbon disulphide and methylal. Relation between c (Brown) and molecular percentage of carbon disulphide 230CurveCurveillustrating the distillation of a substance

65.

which240

contains only66.

much

less volatile impurities

illustrating the distillation of a substance

which243

contains only

much more

volatile impurities

xii

LIST OF ILLUSTRATIONSPAGE

FIG.

67.

Cu

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