公开(公告)号：KR1020030087341A

公开(公告)日：2003-11-14

申请号：KR1020020025361

申请日：2002-05-08

Applicant: 국방과학연구소

Inventor： 김진석 ,  조진래 ,  이근득 ,  박방삼

IPC: C07D303/16

CPC classification number: C08G65/22 ,  C07D303/16

Abstract: PURPOSE: Glycidyl dinitropropyl carbonate and poly(glycidyl dinitropropyl carbonate) are provided. Prepolymer having improved thermal stability is cheaply prepared by substituting a nitrate group by a nitro group as an energy group. CONSTITUTION: Glycidyl dinitropropyl carbonate represented by the formula(I) is provided. Poly(glycidyl dinitropropyl carbonate) represented by the formula(II) and having molecular weight of 2,000 to 3,500 is provided. A process for preparing the glycidyl dinitropropyl carbonate of the formula(I) comprises the steps of: dissolving 2,2-dinitropropanol in methylenechloride; adding pyridine into the mixture; adding allylchloroformate in methylene chloride to the mixture and reacting them; adding methylenechloride and distilled water into the mixture; dehydrating the methylenechloride extract with anhydrous magnesium sulfate; filtering the dehydrated solution to prepare allyl dinitropropyl carbonate; dissolving allyl dinitropropyl carbonate in methanol; adding hydrogen peroxide and NaOH into the mixture and reacting them; adding methylenechloride and distilled water into the mixture; dehydrating the methylenechloride extract with anhydrous magnesium sulfate; and filtering the dehydrated solution. A process for preparing the poly(glycidyl dinitropropyl carbonate) of the formula(II) comprises the steps of: mixing boron trifluoride etherate with 1,4-butanediol and removing ether under reduced pressure; dissolving the glycidyl dinitropropyl carbonate of the formula(I) in the boron trifluoride etherate solution; adding methylenechloride and distilled water into the mixture; dehydrating the mixture with anhydrous magnesium sulfate; adding ethanol into the dehydrated solution; and removing volatile compounds under reduced pressure.

Abstract translation: 目的：提供碳酸缩水甘油基二硝基丙酯和聚（缩水甘油基二硝基丙基碳酸酯）。 具有改善的热稳定性的预聚物通过用硝基代替硝基作为能量来廉价地制备。 构成：提供由式（I）表示的缩水甘油基二硝基丙基碳酸酯。 提供由式（II）表示的分子量为2,000至3,500的聚（缩水甘油基二硝基丙基碳酸酯）。 制备式（I）的缩水甘油基二硝基丙基碳酸酯的方法包括以下步骤：将2,2-二硝基丙醇溶解在二氯甲烷中; 向混合物中加入吡啶; 将二氯甲烷中的氯甲酸烯丙酯加入到混合物中并使它们反应; 向混合物中加入二氯甲烷和蒸馏水; 用无水硫酸镁脱水二氯甲烷萃取液; 过滤脱水溶液制备碳酸烯丙酯二硝基丙酯; 将烯丙基二硝基丙酸酯溶于甲醇中; 向混合物中加入过氧化氢和NaOH，使它们反应; 向混合物中加入二氯甲烷和蒸馏水; 用无水硫酸镁脱水二氯甲烷萃取液; 并对脱水溶液进行过滤。 制备式（II）的聚（缩水甘油基二硝基丙基碳酸酯）的方法包括以下步骤：将三氟化硼醚合物与1,4-丁二醇混合并在减压下除去乙醚; 将式（I）的缩水甘油基二硝基丙酸酯溶解在三氟化硼乙醚溶液中; 向混合物中加入二氯甲烷和蒸馏水; 用无水硫酸镁脱水混合物; 将乙醇加入脱水溶液中; 并在减压下除去挥发性化合物。

公开(公告)号：KR1020010095503A

公开(公告)日：2001-11-07

申请号：KR1020000018625

申请日：2000-04-10

Applicant: 국방과학연구소

Inventor： 조진래 ,  김진석 ,  이근득 ,  전용구 ,  박방삼

IPC: C06B25/00

CPC classification number: C06B45/105

Abstract: PURPOSE: An energetic nitro-formal plasticizer for explosive formulations comprises eutectic mixture mixed with bis(2,2-dinitropropyl)formal(BDNPF), 2,2-dinitropropyl 2,2-dibutyl formal(DNPBF) and bis(2,2-dinitrobutyl)formal(BDNPF). The energetic nitro-formal plasticizer exhibits superior thermal/chemical properties with less production cost. CONSTITUTION: The molecular ratio of BDNPF/DNPBF/BDNPF in formulation of this plasticizer is in the range 20-68%/28-50%/4-30%. The plasticizer is allowed to contain diformal, however its content is desirable controlled to be not more than 3%. The preparation method of this plasticizer comprises the steps of (i) dissolving 2,2-dinitropropanol and 2,2-dinitrobutanol in the mole ratio of 3 to 6:1 at 0 to 30deg.C in an organic solvent like methylene chloride; (ii) at 20deg.C or lower, adding sulfuric acid solution in which formaldehyde sources such as paraformaldehyde and s-trioxane is dissolved; (iii) refining obtained mixture.

Abstract translation: 目的：用于爆炸性制剂的高能硝基形式增塑剂包括与双（2,2-二硝基丙基）甲醛（BDNPF），2,2-二硝基丙基2,2-二丁基甲醛（DNPBF）和双（2,2-二硝基丙基） dinitrobutyl）正式（BDNPF）。 精力充沛的硝基形式增塑剂具有优异的热/化学性能，生产成本较低。 构成：该增塑剂配方中BDNPF / DNPBF / BDNPF的分子比在20-68％/ 28-50％/ 4-30％的范围内。 允许增塑剂含有不均匀性，但其含量优选控制在不超过3％。 该增塑剂的制备方法包括以下步骤：（i）在有机溶剂如二氯甲烷中，在0至30℃下，以3-6:1的摩尔比溶解2,2-二硝基丙醇和2,2-二硝基丁醇; （ii）在20℃以下，加入溶解有多聚甲醛和s-三恶烷等甲醛源的硫酸溶液; （iii）精制所得混合物。

公开(公告)号：KR101150156B1

公开(公告)日：2012-05-24

申请号：KR1020100041972

申请日：2010-05-04

Applicant: 국방과학연구소

Inventor： 김진석 ,  김승희 ,  조진래 ,  고은미

IPC: C07D233/91 ,  C07D233/92

CPC classification number: C07D233/92

Abstract: The present invention provides a method for preparing 2,4-dinitroimidazole, wherein separation of 1,4-donitroimidazole in powder form is avoided so that it is possible to eliminate allergy problems in workers and simplify the process, thereby improving process economy.

公开(公告)号：KR100890936B1

公开(公告)日：2009-04-02

申请号：KR1020080096262

申请日：2008-09-30

Applicant: 국방과학연구소

Inventor： 고은미 ,  김진석 ,  조진래 ,  김현수

IPC: C07D239/24 ,  C07D239/42

CPC classification number: C07D239/553

Abstract: Provided is a nitrification method of 4,6-dihydroxy-2-methylpyrimidine used as a precursor of 1,1-diamino-2,2-dinitro ethylene which is a kind of gunpowder by using an organic solvent to secure a high yield. A nitrification method of 4,6-dihydroxy-2-methylpyrimidine comprises the following steps of: melting the 4,6-dihydroxy-2-methylpyrimidine in concentrated sulfuric acid in a first step; adding dichloromethane to a solution of the first step in a second step; and adding concentrated nitric acid to the solution of the second step and stirring the obtained solution in a third step.

Abstract translation: 提供用作1,1-二氨基-2,2-二硝基乙烯的前体的4,6-二羟基-2-甲基嘧啶的硝化方法，其是通过使用有机溶剂确保高产率的一种火药。 4,6-二羟基-2-甲基嘧啶的硝化方法包括以下步骤：在第一步骤中使4,6-二羟基-2-甲基嘧啶在浓硫酸中熔融; 在第二步骤中将二氯甲烷加入到第一步骤的溶液中; 并向第二步骤的溶液中加入浓硝酸，并在第三步骤中搅拌所得溶液。

公开(公告)号：KR100490339B1

公开(公告)日：2005-05-17

申请号：KR1020020025362

申请日：2002-05-08

Applicant: 국방과학연구소

Inventor： 이근득 ,  김진석 ,  조진래 ,  김정국

IPC: C08F220/10

CPC classification number: C08F220/36 ,  C06B45/105

Abstract: 본 발명은 신규물질인 2,2-디나이트로프로필 아크릴레이트와 2,2-디나이트로부틸 아크릴레이트의 공중합체를 제공한다. 상기 공중합체는 기존의 에너지 함유 결합제보다 기계적 강도가 우수할 뿐 아니라, 상기 공중합체를 복합 화약에 적용하는 경우 기존의 에너지 함유 결합제에 비하여 복합 화약을 둔감시키는 효과가 있다.

公开(公告)号：KR100381133B1

公开(公告)日：2003-04-23

申请号：KR1020000018625

申请日：2000-04-10

Applicant: 국방과학연구소

Inventor： 조진래 ,  김진석 ,  이근득 ,  전용구 ,  박방삼

IPC: C06B25/00

CPC classification number: C06B45/105

Abstract: An energetic plascitizer comprising bis(2,2-dinitropropyl) formal, 2,2-dinitropropyl 2,2-dinitrobutyl formal and bis 2,2-dinitrobutyl) formal in a molar ratio of 20~68%/28~50%/4~30% is, described. It is also provided a method for synthesizing the plasticizer comprising: dissolving 2,2-dinitropropanol and 2,2-dinitrobutanol into an organic solvent to form an organic solution, in which the molar ratio of 2,2-dinitropropanol to 2,2-dinitrobutanol is 3:1-6:1; adding to the organic solution a sulfuric acid solution where formaldehyde source was dissolved, wherein the temperature of reaction medium is maintained below 20° C.; and separating and purifying the product from the reaction mixture.The plascitizer according to the present invention has an excellent thermal and chemical properties while incurring a low production cost. Especially, the energy content of the plasticizer of the present invention is heightened by minimizing the content of the diformal generated as a side product, so that it is favorably adapted for use in an insensitive high performance explosive and a propellant.

Abstract translation: 包含摩尔比为20〜68％/ 28〜50％/ 4的双（2,2-二硝基丙基）缩甲醛，2,2-二硝基丙基2,2-二硝基丁基缩甲醛和二（2,2-二硝基丁基）缩甲醛的高能增塑剂 描述了〜30％。 还提供了合成增塑剂的方法，包括：将2,2-二硝基丙醇和2,2-二硝基丁醇溶解在有机溶剂中以形成有机溶液，其中2,2-二硝基丙醇与2,2-二硝基丙醇的摩尔比 二硝基丁醇为3：1-6：1; 向有机溶液中加入溶解有甲醛源的硫酸溶液，其中反应介质的温度保持在20℃以下; C。; 并从反应混合物中分离和纯化产物。根据本发明的增溶剂具有优异的热和化学性质，同时降低生产成本。 尤其是，通过使作为副产物产生的二甲酸二甲酯的含量最小化，本发明增塑剂的能量含量得到提高，因此它适合用于不敏感的高性能炸药和推进剂。

公开(公告)号：KR100365648B1

公开(公告)日：2002-12-26

申请号：KR1020000018626

申请日：2000-04-10

Applicant: 국방과학연구소

Inventor： 김진석 ,  조진래 ,  이근득 ,  박방삼

IPC: C06B25/00

Abstract: 본 발명은 비스(2,2-디니트로프로필)포름알(BDNPF)과 결정화 방지제를 함유하는 고에너지 가소제에 있어서, 상기 결정화 방지제가 비스(2,2-디니트로프로필)디포름알(BDNPDF)인 것을 특징으로 하는 가소제 및 그 제조 방법에 관한 것이다.
BDNPF의 결정화 방지를 위해 BDNPDF를 사용할 경우, -20℃의 온도에서 6개월 이상 방치하더라도 결정화되지 아니하며, 열적/화학적 특성도 우수한 것으로 밝혀졌다. 그리고 반응 부산물로 간주되어온 BDNPDF를 결정화 방지제로 사용함에 의해 BDNPDF를 제거하기 위한 부차적 공정이 불필요하고, 생산비가 저렴하다는 이점이 있다.

公开(公告)号：KR100186287B1

公开(公告)日：1999-05-01

申请号：KR1019950000267

申请日：1995-01-09

Applicant: 국방과학연구소

Inventor： 정용구 ,  조진래 ,  김진석

IPC: C07D301/27 ,  C07D303/36

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.

公开(公告)号：KR1019960030500A

公开(公告)日：1996-08-17

申请号：KR1019950000267

申请日：1995-01-09

Applicant: 국방과학연구소

Inventor： 정용구 ,  조진래 ,  김진석

IPC: C07D301/27 ,  C07D303/36

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.