KR830007536A - Separation and Purification Method of Olto-Toluene Sulfonamide - Google Patents

Separation and Purification Method of Olto-Toluene Sulfonamide Download PDF

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Publication number
KR830007536A
KR830007536A KR1019810004624A KR810004624A KR830007536A KR 830007536 A KR830007536 A KR 830007536A KR 1019810004624 A KR1019810004624 A KR 1019810004624A KR 810004624 A KR810004624 A KR 810004624A KR 830007536 A KR830007536 A KR 830007536A
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KR
South Korea
Prior art keywords
crystals
added
amount
water
primary
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KR1019810004624A
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Korean (ko)
Inventor
이건형
구대환
이창원
곽동혁
Original Assignee
노상두
주식회사 금양
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Priority to KR1019810004624A priority Critical patent/KR830007536A/en
Publication of KR830007536A publication Critical patent/KR830007536A/en

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    • 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
    • C07C303/42—Separation; Purification; Stabilisation; Use of additives
    • C07C303/44—Separation; Purification

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

Abstract

내용 없음No content

Description

올토-톨루엔 술폰 아미드의 분리정제 방법Separation and Purification Method of Olto-Toluene Sulfonamide

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

Claims (4)

조(粗) 올토-톨루엔 술폰아미드와 이것에 약 6-11배량의 물과 소량의 활성탄을 넣어 95∼100℃에서 완전히 용해 시킨후 여과기(보온형)를 사용하여 열여과 한후 60∼80℃로 냉각시켜 결정화하여 일차 결정을 얻은후 상징액을 분리하고 생성된 결정물에 약2.5∼3.5배의 물과 소량의 수산화나트륨을 넣은후 95∼100℃에서 충분히 용해시킨후 산으로 pH를 7∼7.5로 조정한후 60∼70℃로 냉각 결정하여 고순도 올토 톨루엔 술폰 아미드의 제조방법.Crude allo-toluene sulfonamide and about 6-11 times of water and a small amount of activated carbon are completely dissolved at 95 ~ 100 ℃, and then filtered by heat using a filter (heat insulation type) to 60 ~ 80 ℃. After crystallization by cooling to obtain the primary crystals, the supernatant was separated, and about 2.5 to 3.5 times of water and a small amount of sodium hydroxide were added to the resulting crystals. Method of producing high-purity oltotoluene sulfone amide by crystallization after cooling to 60-70 ° C. 제1항에 있어서 사용되는 물의 양이 조올토 톨루엔 술폰 아미드에 대해 8∼10배이고 열여과의 온도가 100℃이며 일차 결정화 온도가 70∼75℃인 것이 특징인 방법.The method according to claim 1, characterized in that the amount of water used is 8 to 10 times with respect to the zolto toluene sulfone amide, the temperature of heat filtration is 100 ° C and the primary crystallization temperature is 70 to 75 ° C. 제1항에 있어서, 일차 결정물에 첨가하는 물의 양이 결정물에 대해 3배 이고 첨가된 수산화나트룸의 양이 1차 결정에 대해서 6∼8중량%이고 결정화 냉각온도가 65℃인것이 특징인 방법.The method of claim 1, wherein the amount of water added to the primary crystals is three times the amount of the crystals, the amount of added sodium hydroxide is 6 to 8% by weight relative to the primary crystals, and the crystallization cooling temperature is 65 ° C. How to be. 제1항에 있어서 일차 결정시 분리된 상징액을 산으로 5.5∼6.5되게 조정하고 30℃이하에서 결정화하여 정제된 잔사를 얻은후 여기에 2.5∼3.5배의 물과 소량의 수산화나트륨을 넣어 가하고 95∼100℃까지 가열하에 완전히 용해한후 70∼80℃까지 냉각하여 결정물을 회수하여 이를 다시 원료 올토-톨루엔 술폰아미드에 가함을 특징으로 하는 방법.The method of claim 1, wherein the supernatant separated at the time of primary determination is adjusted to 5.5 to 6.5 with acid and crystallized at 30 ° C. or lower to obtain a purified residue. 2.5 to 3.5 times of water and a small amount of sodium hydroxide are added thereto and then 95 to Dissolving completely under heating to 100 ° C. and then cooling to 70-80 ° C. to recover the crystals, which are then added to the raw material olto-toluene sulfonamide. ※참고사항:최초출원 내용에 의하여 공개하는 것임.※ Note: This is to be disclosed based on the first application.
KR1019810004624A 1981-11-28 1981-11-28 Separation and Purification Method of Olto-Toluene Sulfonamide KR830007536A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
KR1019810004624A KR830007536A (en) 1981-11-28 1981-11-28 Separation and Purification Method of Olto-Toluene Sulfonamide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1019810004624A KR830007536A (en) 1981-11-28 1981-11-28 Separation and Purification Method of Olto-Toluene Sulfonamide

Publications (1)

Publication Number Publication Date
KR830007536A true KR830007536A (en) 1983-10-21

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KR1019810004624A KR830007536A (en) 1981-11-28 1981-11-28 Separation and Purification Method of Olto-Toluene Sulfonamide

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