FR2387947A1 - PROCESS FOR PREPARING NAPHTHALENE-1,3,6-TRISULPHONIC ACID - Google Patents

PROCESS FOR PREPARING NAPHTHALENE-1,3,6-TRISULPHONIC ACID

Info

Publication number
FR2387947A1
FR2387947A1 FR7811944A FR7811944A FR2387947A1 FR 2387947 A1 FR2387947 A1 FR 2387947A1 FR 7811944 A FR7811944 A FR 7811944A FR 7811944 A FR7811944 A FR 7811944A FR 2387947 A1 FR2387947 A1 FR 2387947A1
Authority
FR
France
Prior art keywords
naphthalene
degrees
reaction mixture
added per
per mole
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.)
Withdrawn
Application number
FR7811944A
Other languages
French (fr)
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.)
Bayer AG
Original Assignee
Bayer AG
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 Bayer AG filed Critical Bayer AG
Publication of FR2387947A1 publication Critical patent/FR2387947A1/en
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
    • C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
    • C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un procédé de préparation d'acide naphtalène-1,3,6-trisulfonique par sulfonation de naphtalène à température élevée, l'acide sulfurique et l'oléum étant chacun introduits en deux fois. Selon ce procédé, on effectue successivement les étapes suivantes : a. on introduit préalablement le naphtalène sous forme liquide à 80-120 degrés C; b. on ajoute, par mole de naphtalène introduit, 1,0 à 3,0 moles d'acide sulfurique à 80-120 degrés C; c. on maintient le mélange réactionnel à 80-120 degrés C pendant 0,1 à 5h; d. on porte le mélange réactionnel à 130-170 degrés C et on le maintient à cette température pendant 0,2 à 5 h; e. on refroidit le mélange réactionnel à 20-120 degrés C et on ajoute, par mole de naphtalene introduit, 0 à 2,0 moles d'acide sulfurique ; f. on ajoute, par mole de naphtalène introduit, 2,5 à 2,9 moles de SO3 , sous forme d'un oleum, à 40-100 degrés C; g. on chauffe le mélange réactionnel à 140-160 degrés C et on le maintient à cette température pendant 1 à 4 h; h. on ajoute, par mole de naphtalène introduit, 0,01 à 1,0 mole de SO 3 , sous forme d'un oléum, à 60-160 degrés C; i. on agite ensuite le mélange réactionnel pendant 0,5 à 4 h à 140-160 degrés C. Le rendement en acide naphtalène-1,3,6 trisulfonique est plus élevé et la formation de produits secondaires moins importante que dans les procédés connus jusqu'à présent.Disclosed is a process for the preparation of naphthalene-1,3,6-trisulfonic acid by sulfonation of naphthalene at elevated temperature, with sulfuric acid and oleum each being introduced in two stages. According to this method, the following steps are carried out successively: a. the naphthalene is introduced beforehand in liquid form at 80-120 degrees C; b. 1.0 to 3.0 moles of sulfuric acid at 80-120 degrees C are added per mole of naphthalene introduced; vs. the reaction mixture is maintained at 80-120 degrees C for 0.1 to 5 hours; d. the reaction mixture is brought to 130-170 degrees C and maintained at this temperature for 0.2 to 5 h; e. the reaction mixture is cooled to 20-120 ° C. and 0 to 2.0 moles of sulfuric acid are added per mole of naphthalene introduced; f. 2.5 to 2.9 moles of SO 3, in the form of an oleum, at 40-100 degrees C, are added per mole of naphthalene introduced; g. the reaction mixture is heated to 140-160 degrees C and maintained at this temperature for 1 to 4 hours; h. 0.01 to 1.0 mole of SO 3, in the form of an oleum, at 60-160 degrees C, is added per mole of naphthalene introduced; i. the reaction mixture is then stirred for 0.5 to 4 h at 140-160 degrees C. The yield of naphthalene-1,3,6 trisulfonic acid is higher and the formation of side products less important than in the processes known up to now.

FR7811944A 1977-04-23 1978-04-21 PROCESS FOR PREPARING NAPHTHALENE-1,3,6-TRISULPHONIC ACID Withdrawn FR2387947A1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE2718207A DE2718207C3 (en) 1977-04-23 1977-04-23 Process for the preparation of naphthalene-1,3,6-trisulfonic acid

Publications (1)

Publication Number Publication Date
FR2387947A1 true FR2387947A1 (en) 1978-11-17

Family

ID=6007133

Family Applications (1)

Application Number Title Priority Date Filing Date
FR7811944A Withdrawn FR2387947A1 (en) 1977-04-23 1978-04-21 PROCESS FOR PREPARING NAPHTHALENE-1,3,6-TRISULPHONIC ACID

Country Status (8)

Country Link
JP (1) JPS53132548A (en)
BE (1) BE866223A (en)
BR (1) BR7802456A (en)
CH (1) CH634044A5 (en)
DE (1) DE2718207C3 (en)
FR (1) FR2387947A1 (en)
GB (1) GB1596897A (en)
IT (1) IT1104816B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0012260A1 (en) * 1978-12-09 1980-06-25 Bayer Ag Sulphurisation compounds of naphthalene, process for their preparation and their use
EP0013558A1 (en) * 1979-01-13 1980-07-23 Bayer Ag Process for the preparation of naphthalene-1,3,5-trisulphonic acid

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5096552A (en) * 1973-12-28 1975-07-31

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5096552A (en) * 1973-12-28 1975-07-31

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
CA1975 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0012260A1 (en) * 1978-12-09 1980-06-25 Bayer Ag Sulphurisation compounds of naphthalene, process for their preparation and their use
EP0013558A1 (en) * 1979-01-13 1980-07-23 Bayer Ag Process for the preparation of naphthalene-1,3,5-trisulphonic acid

Also Published As

Publication number Publication date
JPS53132548A (en) 1978-11-18
BE866223A (en) 1978-10-23
IT7849013A0 (en) 1978-04-21
BR7802456A (en) 1979-04-03
DE2718207B2 (en) 1980-09-11
DE2718207A1 (en) 1978-11-02
JPS5645909B2 (en) 1981-10-29
IT1104816B (en) 1985-10-28
CH634044A5 (en) 1983-01-14
DE2718207C3 (en) 1981-11-05
GB1596897A (en) 1981-09-03

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Legal Events

Date Code Title Description
RE Withdrawal of published application