公开(公告)号：KR100251343B1

公开(公告)日：2000-05-01

申请号：KR1019970074900

申请日：1997-12-27

Applicant: 국방과학연구소

Inventor： 박방삼 ,  고은미 ,  정원복

IPC: C07D249/10

Abstract: PURPOSE: Provided is a preparation method of 3-nitro- 1,2,4-triazol-5-one (NTO) which shows stability against impact or heat and has high-explosive energy. The method simplifies a process by eliminating the process for filtration, drying, crushing of NTO and reproviding it, thus increases its yield. CONSTITUTION: A preparation method of NTO is composed of the following steps of; (a) preparing 1,2,4-triazol-5-one (TO) by condensation reaction of semicarbazide·HCl and formic acid and then distillation of formic acid; (b) synthesizing NTO by adding high concentration sulfuric acid, water and nitric acid in high concentration preferably at 60 deg.C without process of filtration, drying and crush of the prepared TO.

Abstract translation: 目的：提供3-硝基-1,2,4-三唑-5-酮（NTO）的制备方法，其显示出对冲击或热量的稳定性，并具有高爆炸能量。 该方法通过消除过滤，干燥，破碎NTO并重新制备的方法简化了工艺，从而提高了产率。 构成：NTO的制备方法由以下步骤组成： （a）通过氨基脲·HCl和甲酸的缩合反应制备1,2,4-三唑-5-酮（TO），然后蒸馏甲酸; （b）通过加入高浓度硫酸，高浓度的水和硝酸，优选在60℃下合成NTO，无需过滤，干燥和粉碎所制备的TO。

公开(公告)号：KR100495677B1

公开(公告)日：2005-06-16

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: 본 발명은 글라이시딜 디나이트로프로필 카보네이트 및 폴리(글라이시딜 디나이트로프로필 카보네이트)에 관한 것이다. 본 발명은 고성능 둔감 화약용 고에너지 결합제로 사용되는 예비중합체(prepolymer)인 폴리(글라이시딜 디나이트로프로필 카보네이트)를 제공한다. 본 발명에서는 나이트레이트기 대신 나이트로기를 에너지기로 도입함으로써 기존의 에너지 결합제에 비하여 열적 안정성이 월등히 개선된 예비중합체를 제공한다.

公开(公告)号：KR1020010095504A

公开(公告)日：2001-11-07

申请号：KR1020000018626

申请日：2000-04-10

Applicant: 국방과학연구소

Inventor： 김진석 ,  조진래 ,  이근득 ,  박방삼

IPC: C06B25/00

CPC classification number: C06B45/105

Abstract: PURPOSE: An energetic formal plasticizer for explosive formulations comprises bis(2,2-dinitropropyl)formal(BDNPF), and especially comprises bis(2,2-dinitropropyl)diformal(BDNPDF) as anti-crystalline agent. The energetic formal plasticizer exhibits superior thermal/chemical properties with less production cost. CONSTITUTION: The mole ratio of BDNPDF is desirable controlled to be 8-44mol.% of a mixture of BDNPF and BDNPDF. The preparation method of this plasticizer comprises the steps of (i) dissolving 2,2-dinitropropanol and formaldehyde source such as paraformaldehyde and s-trioxane in an organic solvent like methylene chloride; (ii) adding sulfuric acid solution while controlling the temperature of a reactor in the range of -30 to 20deg.C (iii) refining obtained mixture.

Abstract translation: 目的：用于爆炸性制剂的高能型正型增塑剂包括双（2,2-二硝基丙基）甲醛（BDNPF），特别是作为抗结晶剂的双（2,2-二硝基丙基）异构体（BDNPDF）。 能量的正式增塑剂具有优异的热/化学性能，生产成本更低。 构成：BDNPDF的摩尔比被控制为BDNPF和BDNPDF的混合物的8-44mol％。 该增塑剂的制备方法包括以下步骤：（i）将2,2-二硝基丙醇和甲醛源如多聚甲醛和s-三恶烷溶解在有机溶剂如二氯甲烷中; （ii）加入硫酸溶液，同时将反应器的温度控制在-30至20℃范围内。（iii）精炼所得混合物。

公开(公告)号：KR100255359B1

公开(公告)日：2000-05-01

申请号：KR1019970074893

申请日：1997-12-27

Applicant: 국방과학연구소

Inventor： 박방삼 ,  김현수 ,  채주승

IPC: C06B45/18

Abstract: PURPOSE: Provided is a compressed complex gunpowder composition of which charging density is increased and which is insensitive to an external shock. CONSTITUTION: The compressed complex gun powder comprises: (i) 90-96 wt.% of raw material powder(H.M.X); (ii) 1-3 wt.% of acrylate elastic copolymer(HyTemp-4404) as a crosslinking monomer having reactive hydroxy group; and (iii) 3-9 wt.% of D.O.A. The method comprises steps of: (i) dissolving 15-20 wt.% of the acrylate elastic copolymer(HyTemp-4404) in ethyl acetate at a temperature of 50-60 deg.C to prepare a liquid polymer solution; (ii) dispersing 8.0-11.0 wt.% of H.M.X in water to prepare a slurry solution; and (iii) after injecting the polymer solution into the slurry solution at a temperature of 60-70 deg.C to form a granular body, distilling the granular body.

Abstract translation: 目的：提供一种压缩复合火药组合物，其充电密度增加，对外部冲击不敏感。 构成：压缩复合枪粉末包括：（i）90-96重量％的原料粉末（H.M.X）; （ii）作为具有反应性羟基的交联单体的丙烯酸酯弹性共聚物（HyTemp-4404）1-3重量％ 和（iii）3-9重量％的D.O.A. 该方法包括以下步骤：（i）将15-20重量％的丙烯酸酯弹性共聚物（HyTemp-4404）在50-60℃的温度下溶解在乙酸乙酯中以制备液体聚合物溶液; （ii）将8.0-11.0重量％的H.M.X分散在水中以制备浆液; 和（iii）在60-70℃的温度下将聚合物溶液注入浆液中以形成粒状体，蒸馏出粒状体。

公开(公告)号：KR1019990054997A

公开(公告)日：1999-07-15

申请号：KR1019970074900

申请日：1997-12-27

Applicant: 국방과학연구소

Inventor： 박방삼 ,  고은미 ,  정원복

IPC: C07D249/10

Abstract: 본 발명은 충격이나 열 등에 안정하면서 고폭 에너지를 함유한 니트로 트리오졸론(NTO)의 제조방법에 관한 것으로, NTO 합성의 중간체인 TO를 사용하여 NTO를 제조하는 공정에 있어서 TO가 생성된 반응기에 진한 질산을 공정중에 바로 투입하여 질산의 공급을 제거하는 방법을 제공하여, 제조된 TO를 여과, 건조, 분쇄 후 다시 공급하는 공정을 생략함으로써, 기존 공정과 비교하여 생산 공정의 간소화 및 생산 수율의 증가가 가능하다.

公开(公告)号：KR1019990054990A

公开(公告)日：1999-07-15

申请号：KR1019970074893

申请日：1997-12-27

Applicant: 국방과학연구소

Inventor： 박방삼 ,  김현수 ,  채주승

IPC: C06B45/18

Abstract: 본 발명은 에이치.엠.엑스(HMX) 90∼96 중량%에 아크릴레이트 탄성공중합수지(HyTemp) 1∼5 중량%와 디.오.에이.(DOA) 0∼10 중량%를 함유한 결합제를 피복 응집시킨 압축형 복합 화약에 관한 것이며, 또한 그 제조 방법이 제공된다.

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：KR100282224B1

公开(公告)日：2001-02-15

申请号：KR1019970074894

申请日：1997-12-27

Applicant: 국방과학연구소

Inventor： 박방삼 ,  김현수 ,  이정민 ,  김광주 ,  김민준 ,  김선환

IPC: C07D249/10

Abstract: 본 발명은 니트로트리오졸론(NTO) 결정의 형상 및 크기를 조절하는 재결정 방법에 있어서, 첨가제를 사용하지 않는 결정화 방법을 이용하여 다각형 형태를 갖는 다양한 크기의 입자를 조절하여 제조하는 방법에 관한 것인데, 특히, 용매로서 물, 알콜류 및 그의 혼합물로 이루어진 군 중에서 선택된 것을 사용하는 것을 특징으로 하는 NTO의 형상 및 입도 조절 방법을 제공한다.

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。