GB1275232A - Improvements in or relating to sublimation processes - Google Patents

Improvements in or relating to sublimation processes

Info

Publication number
GB1275232A
GB1275232A GB1802570D GB1802570D GB1275232A GB 1275232 A GB1275232 A GB 1275232A GB 1802570 D GB1802570 D GB 1802570D GB 1802570 D GB1802570 D GB 1802570D GB 1275232 A GB1275232 A GB 1275232A
Authority
GB
United Kingdom
Prior art keywords
organic compound
vessel
solvent
slurry
vapours
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
GB1802570D
Inventor
Jay Young Welsh
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Diamond Shamrock Corp
Original Assignee
Diamond Shamrock Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Diamond Shamrock Corp filed Critical Diamond Shamrock Corp
Publication of GB1275232A publication Critical patent/GB1275232A/en
Expired legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D7/00—Sublimation
    • B01D7/02—Crystallisation directly from the vapour phase
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/685—Processes comprising at least two steps in series
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Paper (AREA)

Abstract

1275232 Sublimation separation of organic compounds from solutions DIAMOND SHAMROCK CORP 15 April 1970 [16 April 1969] 18025/70 Heading BIB [Also in Division C2] A sublimable organic compound, such as hydroquinone, naphthalene, p-dichlorobenzene or nicotinic acid, is separated from a slurry of finely-divided inert solids in a solution of the organic compound in a solvent having a boiling point lower than the melting point of the organic compound by heating the slurry, or filtered solution, under subatmospheric pressure to vaporize the solvent at a temperature below the melting point of the organic compound, then heating the dry solid residue to a higher temperature at a lower pressure to sublime the organic compound, and condensing the vapours of the organic compound in the form of a crystalline deposit. One manner of carrying out the process is to boil off some of the solvent from the slurry in a heated agitated tank, and then distribute the concentrate on the hollow trays 10" of drier-sublimer unit, wherein it is heated under vacuum so that the remaining solvent is first removed, and then the organic compound is sublimed, the sublimed vapours being condensed on a hollow plate 25 from which the crystalline sublimate is transferred by a rotary scraper 28 into cooler 30. Heating fluid (e.g. oil) is pumped through jacket 12, trays 10" and jackets 15, 16, 17. Another heat-transfer medium is pumped through hollow plate 25. The evaporation vessel 10 is covered with thermal-insulation material 10'; and the vapours pass from vessel 10 to vessel 20 through thermally-insulated conduit 22. Solvent-vapour is removed from vessel 10 to an aspirator through valved-coupling 39; but when sublimation is to be effected, coupling 39 is closed, and a two-stage vacuum pump, connected to vessel 20 at 32, is actuated. Plate 25 may be replaced by a rotary drum condenser.
GB1802570D 1969-04-16 1970-04-15 Improvements in or relating to sublimation processes Expired GB1275232A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US81664269A 1969-04-16 1969-04-16

Publications (1)

Publication Number Publication Date
GB1275232A true GB1275232A (en) 1972-05-24

Family

ID=25221235

Family Applications (1)

Application Number Title Priority Date Filing Date
GB1802570D Expired GB1275232A (en) 1969-04-16 1970-04-15 Improvements in or relating to sublimation processes

Country Status (4)

Country Link
JP (1) JPS526979B1 (en)
DE (1) DE2018047B2 (en)
FR (1) FR2043368A5 (en)
GB (1) GB1275232A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2032515B1 (en) * 2006-06-29 2017-03-29 Rhodia Opérations New form of hydroquinone and process for obtaining it
CN106748702A (en) * 2017-01-17 2017-05-31 湖北开元化工科技股份有限公司 The equipment that a kind of sublimed method produces 1,4-benzoquinone
CN109107213A (en) * 2018-10-24 2019-01-01 爱发科真空技术（沈阳）有限公司 A kind of integrated structure of sublimating structural and solidification recyclable device
CN111530118A (en) * 2020-05-21 2020-08-14 郑州大学 External heating device used in vacuum environment and ultrahigh vacuum equipment
WO2022122029A1 (en) * 2020-12-11 2022-06-16 安徽金禾实业股份有限公司 Cooling device and cooling method for maltol sublimation section

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2032515B1 (en) * 2006-06-29 2017-03-29 Rhodia Opérations New form of hydroquinone and process for obtaining it
CN106748702A (en) * 2017-01-17 2017-05-31 湖北开元化工科技股份有限公司 The equipment that a kind of sublimed method produces 1,4-benzoquinone
CN106748702B (en) * 2017-01-17 2023-09-01 湖北开元化工科技股份有限公司 Equipment for producing p-benzoquinone by sublimation method
CN109107213A (en) * 2018-10-24 2019-01-01 爱发科真空技术（沈阳）有限公司 A kind of integrated structure of sublimating structural and solidification recyclable device
CN111530118A (en) * 2020-05-21 2020-08-14 郑州大学 External heating device used in vacuum environment and ultrahigh vacuum equipment
WO2022122029A1 (en) * 2020-12-11 2022-06-16 安徽金禾实业股份有限公司 Cooling device and cooling method for maltol sublimation section

Also Published As

Publication number Publication date
FR2043368A5 (en) 1971-02-12
DE2018047B2 (en) 1973-06-20
DE2018047C3 (en) 1974-02-07
DE2018047A1 (en) 1970-10-22
JPS526979B1 (en) 1977-02-26

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Legal Events

Date Code Title Description
PS Patent sealed [section 19, patents act 1949]
PLNP Patent lapsed through nonpayment of renewal fees