US3442766A - Distillation under vacuum with liquid protective seal - Google Patents

Distillation under vacuum with liquid protective seal Download PDF

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Publication number
US3442766A
US3442766A US472954A US3442766DA US3442766A US 3442766 A US3442766 A US 3442766A US 472954 A US472954 A US 472954A US 3442766D A US3442766D A US 3442766DA US 3442766 A US3442766 A US 3442766A
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United States
Prior art keywords
liquid
distillation
steam
water
vacuum
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Expired - Lifetime
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US472954A
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English (en)
Inventor
Charles D Smith
Bertram J Samuels
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Honeywell International Inc
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Allied Chemical Corp
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/10—Vacuum distillation
    • B01D3/103—Vacuum distillation by using a barometric column

Definitions

  • the invention relates to method and apparatus involving steam jet operated vacuum distillation systems especially for distillation of liquids reactive to Water and featuring a liquid seal device adapted to avoid contact between the distillate and water, said liquid seal comprising a chamber for receiving non-condensables between the steam jet and distillation column and condensers, said chamber connected to a barometric type tube which in turn is connected to a reservoir which contains an inert liquid having a density lower than water and immiscible therewith, said chamber adapted to collect liquids entering said chamber upon disruption of normal operation of the distillation system and divert said liquids into the tube and reservoir.
  • This invention relates to separation under vacuum of substances of different vapor pressures and more particularly refers to a liquid protective seal for use of vacuum distillation equipment.
  • a disadvantage of such distillation apparatus using steam jets to generate vacuum is that in the event of a sudden shut-down or failure of the steam-jets, condensed water from the steam jets and water from the intercondensers rushes rapidly into the evacuated distillation apparatus, thereby causing contamination of the contents of said apparatus with water. Water contamination is particularly undesirable when the material beingrectified in the apparatus is sensitive to moisture. Such is the case, for example, in the distillation of organic isocyanates, acid halides, and-anhydrides and the like.
  • a different form of contamination in vacuum distillation operations although less frequent sometimes results when for example due to sudden increase in the velocity of the steam-jets, such as may occur after a momentary failure, rapid boiling of the contents of the reboiler may occur, such that some hot distillate may be carried over, past the receivers, into the steam jets.
  • Interaction of distillate with the steamjets is undesirable and hazardous where the distillate is known to react with water exothermically, for example in the distillation of tolylene diisocyanates.
  • Such interaction of the distillate with the steam jets is equally undesirable where the distillate is known to react with water to form solid particles, for in such instances extremely hazardous conditions may develop due to plugging up of the steam paths.
  • An object of our invention is to provide apparatus and method which will overcome these disadvantages. Another object is to etfectively isolate the evacuation system, namely the steam-jets, from the remainder of the distillation apparatus, such that, in the event of a sudden 3,442,766 Patented May 6, 1969 failure of the steam-jets, contamination of the various parts of the distillation apparatus with condensed steam does '.not occur and also that in the event of a sudden over-loading of the receivers, interaction of the hot distillate with the steam-jets is avoided.
  • a typical distillation plant layout may comprise a fractionation column 1, a reboiler, which is not shown, a condenser 3, a liquid separator 6, a receiver18, steam jet conduit 10 leading to steam jets, not shown, and means for connecting these various components so as to render the apparatus operable.
  • Our liquid seal comprises the combination of chamber 8, tube 11, reservoir 12, overflow tank 23 and means for connecting these various components to each other and to a typical industrial distillation plant, as illustrated in the drawing.
  • vapors of the substance being purified by distillation pass from column 1 into condenser 3 through line 2. From condenser 3 distillate is withdrawn through lines 5 and 7 into receiver 18. Uncondensed vapors generally carrying entrained droplets from the top of condenser 3 pass through line 4 into a liquid separator 6 desirably equipped with a mist separator 25 such as a screen or spaced brickwork, Where the vapor velocity is reduced and any additional condensate collected in liquid separator 6, passes down through lines 19 and 7 into receiver 18 from the bottom of which distillate is discharged through line 14 and valve 26.
  • a mist separator 25 such as a screen or spaced brickwork
  • Non-condensables from the top of liquid separator 6 pass through line 20 into chamber 8 desirably at a point remote from vapor conduit 10 and preferably at one side of interposing baffle 9.
  • Reservoir 12 contains a volume of an inert liquid 21, which is immiscible with and whose density is less than water and desirably less than the substance being distilled.
  • the volume of liquid 21 is such that when a partial vacuum is generated in 8 through the operation of steam-jets 10 and the liquid 21 rises in tube 11 to counterbalance the vacuum that is created, the bottom of tube 11 will remain completely submerged in liquid 21.
  • Overflow line .13 is desirably situated so that the level of liquid 21 in reservoir 12 and in tube 11 will be at the same height as line 13 when steam jets 10 are not in operation.”
  • receiver 18, liquid separator 6 and other components of the distillation plant preceding or connecting receiver 18 and liquid separator 6 are protected against water contamination in the event of a sudden failure of steam jets 10.
  • liquid 21 is one which is inert, immiscible with and of lower density than water. Another requirement is that the liquid have a very low vapor pressure such that contamination of the apparatus by vapors of the liquid in reservoir 12 is avoided and such that loss of the liquid through evaporation, at the distillation conditions employed, is negligible. Any liquid material inert to water, immiscible with water, of lower density than water and having a low vapor pressure, i.e. a boiling point of at least 200 C., preferably above 275 C. may be employed. Hydrocarbons such as alkyl benzenes, e.g. dodecylbenzene, mineral oils, and diphenyl have been found satisfactory.
  • a vacuum distillation apparatus comprising a still and condenser means adapted in normal operation to condense substantially all desired condensables from the distillation and discharge therefrom substantially only non-condensables, a steam jet for producing a vacuum in said still and a liquid seal device separating the condenser means and steam jet, said liquid seal device comprising:

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
US472954A 1965-07-19 1965-07-19 Distillation under vacuum with liquid protective seal Expired - Lifetime US3442766A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US47295465A 1965-07-19 1965-07-19

Publications (1)

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US3442766A true US3442766A (en) 1969-05-06

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US472954A Expired - Lifetime US3442766A (en) 1965-07-19 1965-07-19 Distillation under vacuum with liquid protective seal

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US (1) US3442766A (cs)
BE (1) BE684283A (cs)
DE (1) DE1519609A1 (cs)
FR (1) FR1486937A (cs)
GB (1) GB1106738A (cs)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4043865A (en) * 1973-03-12 1977-08-23 Siemens Aktiengesellschaft Pressurized-water reactor coolant treatment system
WO1996016711A1 (fr) * 1994-11-29 1996-06-06 Valery Grigorievich Tsegelsky Installation de distillation sous vide d'un produit liquide
US6350352B2 (en) * 1996-08-27 2002-02-26 Basf Aktiengesellschaft Process for separating by distillation pure (meth)acrylic acid from mixtures
RU2477394C1 (ru) * 2011-07-08 2013-03-10 Министерство образования и науки Российской Федерации Государственное образовательное учреждение высшего профессионального образования "Московский автомобильно-дорожный государственный технический университет (МАДИ)" Многокомпонентная рабочая жидкость - имитатор скважинной жидкости для поверочного стенда

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1547893A (en) * 1921-09-03 1925-07-28 Bergius Friedrich Method of treating products of hydrolysis of cellulose
US1969793A (en) * 1931-08-10 1934-08-14 Chemical Construction Corp Concentrator apparatus
US1972157A (en) * 1928-12-04 1934-09-04 Barrett Co Vacuum distillation
US1982598A (en) * 1933-04-17 1934-11-27 William Garrigue & Co Distillation system
US1986165A (en) * 1932-07-14 1935-01-01 William Garrique & Company Inc Distillation apparatus
US2006985A (en) * 1926-03-13 1935-07-02 Claude George Method and apparatus for obtaining power from sea water
US2490659A (en) * 1944-04-24 1949-12-06 Robert E Snyder Solar heated vacuum still
US2573516A (en) * 1947-02-28 1951-10-30 Directie Staatsmijnen Nl Treatment of solutions

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1547893A (en) * 1921-09-03 1925-07-28 Bergius Friedrich Method of treating products of hydrolysis of cellulose
US2006985A (en) * 1926-03-13 1935-07-02 Claude George Method and apparatus for obtaining power from sea water
US1972157A (en) * 1928-12-04 1934-09-04 Barrett Co Vacuum distillation
US1969793A (en) * 1931-08-10 1934-08-14 Chemical Construction Corp Concentrator apparatus
US1986165A (en) * 1932-07-14 1935-01-01 William Garrique & Company Inc Distillation apparatus
US1982598A (en) * 1933-04-17 1934-11-27 William Garrigue & Co Distillation system
US2490659A (en) * 1944-04-24 1949-12-06 Robert E Snyder Solar heated vacuum still
US2573516A (en) * 1947-02-28 1951-10-30 Directie Staatsmijnen Nl Treatment of solutions

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4043865A (en) * 1973-03-12 1977-08-23 Siemens Aktiengesellschaft Pressurized-water reactor coolant treatment system
WO1996016711A1 (fr) * 1994-11-29 1996-06-06 Valery Grigorievich Tsegelsky Installation de distillation sous vide d'un produit liquide
US6350352B2 (en) * 1996-08-27 2002-02-26 Basf Aktiengesellschaft Process for separating by distillation pure (meth)acrylic acid from mixtures
RU2477394C1 (ru) * 2011-07-08 2013-03-10 Министерство образования и науки Российской Федерации Государственное образовательное учреждение высшего профессионального образования "Московский автомобильно-дорожный государственный технический университет (МАДИ)" Многокомпонентная рабочая жидкость - имитатор скважинной жидкости для поверочного стенда

Also Published As

Publication number Publication date
BE684283A (cs) 1967-01-03
FR1486937A (fr) 1967-06-30
GB1106738A (en) 1968-03-20
DE1519609A1 (de) 1970-03-12

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