公开(公告)号：KR1020010011940A

公开(公告)日：2001-02-15

申请号：KR1019990031560

申请日：1999-07-31

Applicant: 국방과학연구소

Inventor： 이본수 ,  정규현 ,  전용구

IPC: C07D259/00

Abstract: PURPOSE: The polyacylhexaazaisowurtzitane(AIW) derivatives, their production method and a method for producing hexanitro hexaazaisowurtzitane(HNIW) using the same are provided, thereby HNIW can be effectively produced in higher yield by using AIW easily produced. CONSTITUTION: The polyacylhexaazaisowurtzitane(AIW; polyacyl-2,4,6,8,10,12- hexaaza-tetracyclo £5.5.0.0(5.9).0(3.11)|dodecane) derivatives represented by the formula (I), in which X is RCO, wherein R is H or C1 to C10 alkyl, X' is H or R'CO, wherein R' is H or C1 to C10 alkyl, X'' is H or R''CO, wherein R'' is H or C1 to C10, and R, R' and R'' are the same or different, is produced by reacting hexaarylmethylhexaazaisowurtzitane(HArlW) with (R1CO)2O in the presence of metal catalyst, H2 and organic solvent; removing the solvent; and mixing the remnant with (R1CO)2O, (R2CO)2O, R2COX or R2COOH. The HNIW is produced by reacting AIW derivatives and their isomers with nitrogenating agents such as (R1CO)2O, (R2CO)2O, R2COX or R2COOH.

Abstract translation: 目的：提供多酰基六氮杂异纤锌矿型结构烷烃（AIW）衍生物，其制备方法和使用其制备六氮杂异纤锌矿型结构烷烃（HNIW）的方法，从而通过使用容易制备的AIW可以更高的产率有效地制备HNIW。 构成：由式（I）表示的聚酰基六氮杂异纤锌矿型结构烷烃（AIW;聚酰基-2,4,6,8,10,12-六氮杂 - 四环五十五.0.0.0（5.9）.0（3.11）|十二烷）衍生物，其中 X为RCO，其中R为H或C 1至C 10烷基，X'为H或R'CO，其中R'为H或C 1至C 10烷基，X“为H或R”CO，其中R“为 通过六芳基甲基六氮杂异纤锌矿型结构烷烃（HArlW）与（R1CO）2O在金属催化剂，H 2和有机溶剂的存在下反应制备R，R'和R“相同或不同。 除去溶剂; 并将剩余物与（R1CO）2O，（R2CO）2O，R2COX或R2COOH混合。 HNIW通过使AIW衍生物及其异构体与氮化剂如（R 1 CO）2 O，（R 2 CO）2 O，R 2 COX或R 2 COOH反应而生成。

公开(公告)号：KR100281825B1

公开(公告)日：2001-02-15

申请号：KR1019980055431

申请日：1998-12-16

Applicant: 국방과학연구소

Inventor： 이본수 ,  정규현 ,  전용구

IPC: C07C205/02

Abstract: 본 발명은 쉽게 구할 수 있으며, 보관 및 제조상에서 안정한, 다음 화학식 1을 갖는 N-니트로-4-아자헵탄산 유도체:
화학식 1
O
2 NN(CH
2 CH
2 Z)
2
(식 중에서, Z는 CN, CO
2 R 및 COR로 이루어진 군 중에서 선택된 전자 받게 작용기이며, 상기 R은 탄소수 1-10의 알킬기임)로부터 N,N-디니트로아미드염을 제조하는 방법, 및 상기 화학식 1의 N-니트로-4-아자헵탄산 유도체의 개선된 제조 방법을 제공한다.

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：KR1020000039933A

公开(公告)日：2000-07-05

申请号：KR1019980055431

申请日：1998-12-16

Applicant: 국방과학연구소

Inventor： 이본수 ,  정규현 ,  전용구

IPC: C07C205/02

Abstract: PURPOSE: A dinitroamide salt is provided which is made from N-nitro-4-azaheptanic acid derivative having stability on preparation and safe-keeping. CONSTITUTION: A method for the preparation of a dinitroamide salt being improved comprises the steps of: adding a base as an ammonia, RNH2, (RR')NH, (RR'R)N, N2H4, N1-N10 amine organic base, (wherein, R, R', R are equal or different C1-C20 alkyl group) or metal hydroxylation, to a N-nitro-4-azaheptanic acid derivative followed chemical formula 1(O2N-N(CH2CH2Z)2); reacting a nitrating agent being selected from HNO3, NO3¬3AlCl4¬-, N2O5, NO2BF, NO2Cl, NO2Br, NO2F or (NO2+)2(S2O7¬2-); reacting a base being equal the base as a ammonia, RNH2, (RR')NH, (RR'R)N, N2H4, N1-N10 amine organic base, (wherein, R, R', R are equal or different C1-C20 alkyl group) or metal hydroxylation, or not, again. Wherein the following chemical formula 1 is O2N-N(CH2CH2Z)2(wherein, Z is selected of CN, CO2R or COR, R is alkyl group of C1-C10).

Abstract translation: 目的：提供由N-硝基-4-氮杂庚酸衍生物制备的二硝基酰胺盐，其在制备和保存时具有稳定性。 构成：改进的二硝基酰胺盐的制备方法包括以下步骤：加入碱作为氨，RNH2，（RR'）NH，（RR'R）N，N2H4，N1-N10胺有机碱，（ 根据化学式1（O 2 N-N（CH 2 CH 2 Z）2）的N-硝基-4-氮杂庚酸衍生物，其中R，R'，R等于或不同的C 1 -C 20烷基）或金属羟基化。 使选自HNO3，NO3_3AlCl4-，N2O5，NO2BF，NO2Cl，NO2Br，NO2F或（NO2 +）2（S2O7-2-）的硝化剂反应; 使碱作为氨，RNH2，（RR'）NH，（RR'R）N，N2H4，N1-N10胺有机碱（其中，R，R'，R等于或不同的C1- C20烷基）或金属羟基化反应。 其中以下化学式1是O 2 N-N（CH 2 CH 2 Z）2（其中，Z选自CN，CO 2 R或COR，R是C 1 -C 10的烷基）。

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。