KR960030500A - Synthesis and Polymerization Method of Glycidyl Nitrate, a Monomer for Synthesis of High Energizers - Google Patents

Synthesis and Polymerization Method of Glycidyl Nitrate, a Monomer for Synthesis of High Energizers Download PDF

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Publication number
KR960030500A
KR960030500A KR1019950000267A KR19950000267A KR960030500A KR 960030500 A KR960030500 A KR 960030500A KR 1019950000267 A KR1019950000267 A KR 1019950000267A KR 19950000267 A KR19950000267 A KR 19950000267A KR 960030500 A KR960030500 A KR 960030500A
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South Korea
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nitrate
monomer
glycidyl
synthesis
polyglycidyl
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KR1019950000267A
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Korean (ko)
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KR100186287B1 (en
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전용구
조진래
김진석
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황해웅
국방과학연구소
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Priority to KR1019950000267A priority Critical patent/KR100186287B1/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
    • C07D303/02—Compounds containing oxirane rings
    • C07D303/08—Compounds containing oxirane rings with hydrocarbon radicals, substituted by halogen atoms, nitro radicals or nitroso radicals
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D301/00—Preparation of oxiranes
    • C07D301/27—Condensation of epihalohydrins or halohydrins with compounds containing active hydrogen atoms
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/04—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers only
    • C08G65/22—Cyclic ethers having at least one atom other than carbon and hydrogen outside the ring

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Epoxy Resins (AREA)

Abstract

복합화약에서 고분자 결합제로 사용되는 폴리글리시딜 나이트레이트 합성용 모노머인 글리시딜 나이트레이트의 개선된 제조방법 및 이를 중합함으로써 폴리글리시딜 나이트레이트를 제조하는 방법이 제공된다. 본 발명의 방법에 따라 글리시딜 나이트레이트 제조시 질산염 존재하에 반응을 시키고 폴리글리시딜 나이트레이트 제조시 활성화 모노머 중합법을 사용함으로써 종래방법보다 더 높은 수율로 부생성물 없이 목적생성물을 얻을 수 있다.Provided are an improved method for preparing glycidyl nitrate, a monomer for synthesizing polyglycidyl nitrate, which is used as a polymer binder in a composite powder, and a method for preparing polyglycidyl nitrate by polymerizing the same. According to the method of the present invention, by reacting in the presence of nitrate in the preparation of glycidyl nitrate and using the activated monomer polymerization method in the production of polyglycidyl nitrate, the desired product can be obtained without a by-product in a higher yield than the conventional method. .

Description

고에너저 선폴리머 합성용 모노머인 글리시딜 나이트레이트(Glycidyl Nitrate)의 합성 및 그의 중합방법Synthesis and Polymerization Method of Glycidyl Nitrate, a Monomer for Synthesis of High Energizers

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

Claims (4)

다음 구조식(I)의 글리시딜 나이트레이트의 제조방법에 있어서, -10∼20℃의 반응 온도에서 에피클로로히드린을 질산염 존재하에 50∼100%의 질산과 반응시킨 20∼40%의 수산화나트륨으로 고리화시키는 단계로 되는 글리시딜 나이트레이트의 제조방법.In the method for preparing glycidyl nitrate of the following formula (I), 20-40% sodium hydroxide obtained by reacting epichlorohydrin with 50-100% nitric acid in the presence of nitrate at a reaction temperature of -10-20 占 폚. Method for preparing glycidyl nitrate which is a step of cyclization. 제1항에 있어서, 질산염이 다음 구조식(Ⅱ)The method of claim 1, wherein the nitrate is represented by the following structural formula (II) MaM´b(NO3)c(Ⅱ)M a M´ b (NO 3 ) c (II) (식 중 M과 M´은 알칼리금속, 알칼리토금속, 회토류금속 및 1가의 양이온 원자단에서 선택된 a는 1 또는 2의 정수, b는 0,1 또는 2의 정수이며 c는 1,2 또는 6의 정수임)로 표시되는 군 중에서 선택되고 에피클로로히드린과 질산염은 1 : 0.5 내지 1 : 0.6의 몰비로 사용하는 것이 특징인 방법.(Wherein M and M 'are selected from alkali metal, alkaline earth metal, rare earth metal and monovalent cation atom group, a is an integer of 1 or 2, b is an integer of 0, 1 or 2 and c is 1,2 or 6 And epichlorohydrin and nitrate are used in a molar ratio of 1: 0.5 to 1: 0.6. 제2항에 있어서, 질산염이 질산칼륨, 질산나트륨, 질산암모늄, 질산바륨, 세릭암모늄나이트레이트 중에서 선택되는 것이 특징인 방법.The method of claim 2 wherein the nitrate is selected from potassium nitrate, sodium nitrate, ammonium nitrate, barium nitrate, and ceric ammonium nitrate. 모노머로서 다음 구조식(I)의 글리시딜 나이트레이트를 중합시켜 다음 구조식(∏)의 폴리글리시딜 나이트레이트를 합성하는 방법에 있어서, 개시제로서 1,4-부타디올과 루이스 산 촉매로서 보른트리플루오라이드에테레이트를 먼저 혼합하여 촉매 중의 에테르를 감압에 의해 완전히 제거한 다음 여기에 활성화된 모노머가 알코올과 반응하는 속도와 동일하게 되도록 모노머인 글리시딜 나이트레이트를 서서히 주입하여 0내지 30℃에서 반응시키는 것이 특징인 폴리글리시딜 나이트 레이트의 합성방법.In the method of polymerizing the glycidyl nitrate of the following structural formula (I) as a monomer, and synthesizing the polyglycidyl nitrate of the following structural formula (B), 1,4-butadiol and Lewis acid catalyst as an initiator Fluoride etherate was first mixed to completely remove the ether in the catalyst by depressurization, and then slowly injected with glycidyl nitrate as a monomer so that the activated monomer reacts with the alcohol at 0 to 30 ° C. A method for synthesizing polyglycidyl nitrate, characterized by reacting. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019950000267A 1995-01-09 1995-01-09 A preparation method of glycidyl nitrate as a monomer for synthesizing energetic pre-polymer KR100186287B1 (en)

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KR1019950000267A KR100186287B1 (en) 1995-01-09 1995-01-09 A preparation method of glycidyl nitrate as a monomer for synthesizing energetic pre-polymer

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Application Number Priority Date Filing Date Title
KR1019950000267A KR100186287B1 (en) 1995-01-09 1995-01-09 A preparation method of glycidyl nitrate as a monomer for synthesizing energetic pre-polymer

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KR960030500A true KR960030500A (en) 1996-08-17
KR100186287B1 KR100186287B1 (en) 1999-05-01

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KR100495677B1 (en) * 2002-05-08 2005-06-16 국방과학연구소 Glycidyl dinitropropyl carbonate and poly(glycidyl dinitropropyl carbonate)

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