CN102584783B - Method for preparing acetone peroxide trimer - Google Patents
Method for preparing acetone peroxide trimer Download PDFInfo
- Publication number
- CN102584783B CN102584783B CN 201110460164 CN201110460164A CN102584783B CN 102584783 B CN102584783 B CN 102584783B CN 201110460164 CN201110460164 CN 201110460164 CN 201110460164 A CN201110460164 A CN 201110460164A CN 102584783 B CN102584783 B CN 102584783B
- Authority
- CN
- China
- Prior art keywords
- acetone
- crude product
- peroxide
- stir
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- ZTLXICJMNFREPA-UHFFFAOYSA-N 3,3,6,6,9,9-hexamethyl-1,2,4,5,7,8-hexaoxonane Chemical compound CC1(C)OOC(C)(C)OOC(C)(C)OO1 ZTLXICJMNFREPA-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title abstract description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000003756 stirring Methods 0.000 claims abstract description 43
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000047 product Substances 0.000 claims abstract description 20
- 239000012043 crude product Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000001953 recrystallisation Methods 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003054 catalyst Substances 0.000 claims abstract 4
- 239000005457 ice water Substances 0.000 claims abstract 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- 239000000011 acetone peroxide Substances 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 13
- 235000019401 acetone peroxide Nutrition 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- 239000012065 filter cake Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims 2
- 238000004090 dissolution Methods 0.000 claims 1
- 229920001897 terpolymer Polymers 0.000 claims 1
- 230000002378 acidificating effect Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 150000002978 peroxides Chemical class 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 16
- 239000002360 explosive Substances 0.000 description 16
- 238000000967 suction filtration Methods 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- 235000011194 food seasoning agent Nutrition 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 239000003755 preservative agent Substances 0.000 description 4
- 230000002335 preservative effect Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- DAEAPNUQQAICNR-GFCOJPQKSA-N dadp Chemical compound C1=NC=2C(N)=NC=NC=2N1C1C[C@H](O)[C@@H](COP(O)(=O)OP(O)(O)=O)O1 DAEAPNUQQAICNR-GFCOJPQKSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000539 dimer Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000012453 solvate Substances 0.000 description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- MQCYJQMMCFDTRC-UHFFFAOYSA-N C1CCCCCCCC1.[O] Chemical compound C1CCCCCCCC1.[O] MQCYJQMMCFDTRC-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 241000883510 Kolla Species 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000010504 bond cleavage reaction Methods 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- JYYOBHFYCIDXHH-UHFFFAOYSA-N carbonic acid;hydrate Chemical compound O.OC(O)=O JYYOBHFYCIDXHH-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229960001701 chloroform Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
本发明涉及过氧化丙酮三聚物的制备方法，属于含能材料技术领域。将丙酮和过氧化物混合均匀，用滴液漏斗缓慢地向混合液中滴加入酸性介质催化剂，搅拌，直至反应器中出现大量白色沉淀，停止搅拌，然后静置；加入冰水，搅拌，抽滤；进行重结晶；重结晶所用溶剂为甲醇、丙酮或三氯甲烷，每克粗品用10～15ml溶剂进行溶解，在水浴上加热至45～50℃，缓慢搅拌使其完全溶解，再加入2～3ml溶剂/g粗品，溶解完毕自然冷却使其结晶，抽滤，自然干燥；精制后产品得率为粗产品的93％，纯度为99.3％～99.9％。本发明的方法简单、安全性好。The invention relates to a preparation method of acetone peroxide trimer, belonging to the technical field of energetic materials. Mix acetone and peroxide evenly, slowly add acidic medium catalyst dropwise to the mixture with a dropping funnel, stir until a large amount of white precipitates appear in the reactor, stop stirring, and then stand still; add ice water, stir, pump Filter; carry out recrystallization; the solvent used for recrystallization is methanol, acetone or chloroform, dissolve each gram of crude product with 10-15ml solvent, heat to 45-50°C on a water bath, stir slowly to make it dissolve completely, and then add 2 ～3ml solvent/g crude product, after dissolving, cool naturally to crystallize, filter with suction, and dry naturally; the yield of the refined product is 93% of the crude product, and the purity is 99.3%～99.9%. The method of the invention is simple and safe.
Description
Technical field
The present invention relates to the trimeric preparation method of acetone peroxide, belong to the energetic material technical field.
Background technology
Acetone peroxide tripolymer (Triacetone triperoxide TATP), formal name used at school: 3,3,6,6,9,9-vegolysen, 2,4,5,7,8-, six oxygen cyclononane are the products under acidic medium by acetone and hydrogen peroxide.Molecular formula is: C
9H
18O
6, molecular weight is 222.24.
Schulte-Ladbe.R in 2003, Kolla.p, Karst.U has delivered the trace analysis report of relevant acetone superoxide in Analytical Chemistry, propose to cause due to the reasons such as tension force of chemical bond the existence of acetone peroxide monomer, but dimer is more unstable than tripolymer.
Document record reports that the earliest event that TATP is used for the attack of terrorism is the pipe bomb event that Israel in 1980 occurs, and TATP sees Israel occupied area and Middle East repeatly for the manufacture of body bombs and car bomb subsequently.Typical case has shoes bomb event and Britain's subway explosive incident in 2005 of U.S.'s flight of calendar year 2001.In March, 2008 Beijing cracked China first TATP explosive manufacturing case be a School Students in Beijing.On March 28th, 2009, the one 14 years old middle school student in Hong Kong copy web material, have made TATP by oneself, grant the classmate, and its classmate lights when playing, and seriously wound hand, head and chest.
Although early stage due to the unstable unazotized characteristic of the easy distillation of TATP, very difficult to discerning of itself and Explosive Residues thereof, in recent years along with to the research of TATP deeply particularly to the in-depth of the understanding of its explosive decomposition characteristic, many explosive substances are discerned expert's development and are gone out the various methods of effectively discerning.
Because acetone peroxide tripolymer (TATP) structure is all unstable, therefore TATP is to warm, friction, impact is all very responsive, and slight friction or impact all can cause fierce blast, are once called for fun " Satan's mother " (Mother of Satan), character is similar with elementary priming explosive, brisance and TNT are suitable, and Meyer in 1977 have measured the gas comparison of TNT and TATP explosive decomposition, and the gas that the TATP blast of the quality such as discovery produces is equivalent to 80% of TNT.The people such as Jimmie C.Oxley in 2002 have studied the explosive combustion reaction of TATP, the TATP that discovery is less than two grams lights only burning at open space and does not explode, products of combustion is carbonic acid gas and water, a large amount of TATP can blast, a small amount of but also can produce blast at the TATP of enclosed space, after the TATP of complete drying places, distillation can be transformed into DADP, and this moment is than moistening TATP product explosive more.
but the most interesting is not the extreme susceptibility of TATP and DADP, but it is different from the explosive decomposition process of general explosive substance, usually the most of explosive substances known to us are all the oxidizing reaction decomposition coursees, and the explosive decomposition process of TATP is an Entropy Changes process, it is moment entropy increasing process, and there is no energy variation, this great discovery is that the people such as F.Dubnikova proposed in 2003, and delivered this achievement in research at Journal of the American Chemical Society, they point out that in article the combustion explosion process of TATP is different from general explosive, heat seldom or slight friction are clashed into just can cause the blast of TATP, this process is not oxidation reaction process but an entropy decomposition course, namely only has scission reaction, do not carry out oxidizing reaction.In this course, the TATP molecule first decomposes and discharges acetone, the Sauerstoffatom that connects together is scattered form oxygen and ozone molecule, and the energy that this process discharges is enough to make another TATP molecule generation chemical reaction, has kept the continuity of reaction.A TATP molecule finally can be decomposed into four molecules, and a small amount of TATP just can produce a large amount of gases, thereby produces powerful explosive power, therefore TATP is referred to as by " entropy explosive ".This result of study and the result of study of over nearly 60 years, various organo-peroxides being decomposed are coincide.
Acetone peroxide is to mix with hydrogen peroxide with acetone, carry out the product of catalyzed reaction under the acidic medium condition, product is white crystals, is dimer and trimerical compositions of mixtures by acetone peroxide, and the mixture of this composition and this mixture are dissolved in organic solvent and all have explosivity.Also till the present, do not see high purity TATP and TATP and how to separate with the DADP mixture.
The present invention reports the diverse a kind of very high TATP preparation method of purity for preparing of TATP preparation method before this.
Summary of the invention
The objective of the invention is in order to propose the trimeric preparation method of acetone peroxide.
The objective of the invention is to be achieved through the following technical solutions.
The trimeric preparation method of acetone peroxide of the present invention, concrete steps are:
1) acetone and superoxide are cooled to 2～-5 ℃; Superoxide is hydrogen peroxide, ozone or benzoyl peroxide;
2) acetone and superoxide are mixed, the mass ratio of acetone and superoxide is 1: 1.5～3; Then mixed solution is placed in water cooler, cooling 1～2h again, temperature is controlled at 2～-5 ℃;
3) be added dropwise to the acidic medium catalyzer lentamente in mixed solution with dropping funnel, stir, until occur a large amount of white precipitates in reactor, stop stirring then standing 24～48 hours; Control 20～50 of rate of addition per minutes; The volume of catalyzer is 10%～20% of mixeding liquid volume; The acidic medium catalyzer is HCl, H
2SO
4, HAe, HNO
3, or H
3PO
4
4) to step 3) add frozen water in the product that obtains, stir suction filtration; Then filter cake is washed 3～5 times with frozen water, the volume of frozen water is 3～4 times of filter cake volume, until washings pH value is 6～7; Drain rear drying, obtain the trimeric thick product of acetone peroxide, productive rate is 96.75%.
5) the thick product of acetone peroxide trimer is carried out recrystallization; The recrystallization solvent for use is methyl alcohol, acetone or trichloromethane, and every gram crude product dissolves with 10～15ml solvent, is heated to 45～50 ℃ in water-bath, slowly stirring is dissolved it fully, then adds 2～3ml solvent/g crude product, dissolves complete naturally cooling and makes its crystallization, suction filtration, seasoning; After refining, the product yield is 93% of thick product, and purity is 99.3%～99.9%.
The thick product of acetone peroxide trimer is the white solid powder, irritating smell slightly, water insoluble, be slightly soluble in methyl alcohol, be soluble in most of organic solvents, fusing point is 91.7～94.0 ℃, and after recrystallizing methanol, fusing point is 93.5～94.5 ℃, the acetone peroxide trimer is white rule crystallization after with recrystallizing methanol, with being colourless rule crystallization after acetone recrystallization.
Beneficial effect
Method of the present invention is simple, security good.
Description of drawings
Fig. 1 is the trimeric infrared spectrum of acetone peroxide of embodiment 1 preparation.
Embodiment
Add the cooling good acetone of 17.4g (0.3mol) and the hydrogen peroxide of 37.4g30% to mix 10 minutes in the 500ml beaker.After stirring, mixed solution is put into refrigerator cooling 1～2 hour again, control temperature at 2 ℃.Take out beaker, slowly be added dropwise to the concentrated hydrochloric acid of 10ml36% with dropper, rate of addition is 30 of per minutes; Stir while adding steadily; Until occur a large amount of white precipitates in beaker, stop stirring.Cover rim of a cup with preservative film, putting into water tank control temperature is 2 ℃, standing and reacting 30 hours.Add a small amount of frozen water in the beaker mixture, stir gently and make its suspension, use rapidly Bush's funnel suction filtration; Each frozen water washing with 3 times of gained solidss volumes left and right 5 times, to washings pH value be 6.8; Suction filtration, obtain acetone peroxide trimer crude product 21.9g after drying in the shade, productive rate is 98.47%.
Purify with the preparation-obtained crude product of 200ml dissolve with methanol, be heated to 47 ℃ in water-bath, stirring is dissolved it fully, then adds the methanol solvate into 10ml, and after stirring, naturally cooling makes its crystallization, suction filtration; Repeat above-mentioned recrystallization purification secondary again, obtain random crystalline product 20.87g after seasoning, productive rate is 93.91%, and purity is 98.57%.Its infrared spectrum following strong peak occurred as shown in Figure 1 in figure: 1180cm-strong peak, 947～786cm-quadruple strong peak, 3004～2948cm-double strong peak, 1360cm-strong peak.
Embodiment 2
Add the cooling good acetone of 26.1g (0.45mol) and 56.1g hydrogen peroxide (30%) to mix 10 minutes in the 500ml beaker.After stirring, mixed solution is put into refrigerator cooling 2 hours again, control temperature at 2 ℃.Take out beaker, slowly be added dropwise to 19ml acetic acid with dropper, rate of addition is 45 of per minutes; Stir while adding steadily; Until occur a large amount of white precipitates in beaker, stop stirring.Cover rim of a cup with preservative film, putting into water tank control temperature is 2 ℃, standing and reacting 36 hours.Add the 60ml frozen water in the beaker mixture, stir gently and make its suspension, use rapidly Bush's funnel suction filtration; The gained solids is with the washing of 200ml frozen water, until till washings pH value neutrality, suction filtration, obtains acetone peroxide trimer crude product 33g after drying in the shade, and productive rate is 98.99%.
Purify with the preparation-obtained crude product of 260ml acetone solution, be heated to 45 ℃ in water-bath, stirring is dissolved it fully, then adds the acetone solvent into 20ml, and after stirring, naturally cooling makes its crystallization, suction filtration; Repeat above-mentioned recrystallization again and purify three times, obtain random crystalline product 30.91g after seasoning, productive rate is 92.73%.Purity is 99.93%.
Embodiment 3
Add the cooling good acetone of 69.6g (1.2mol) and 149.6g hydrogen peroxide (30%) to mix 20 minutes in the 1000ml beaker.After stirring, mixed solution is put into refrigerator cooling 2 hours again, control temperature at 2 ℃.Take out beaker, slowly be added dropwise to 30ml phosphoric acid with dropper, rate of addition is 50 of per minutes; Stir while adding steadily; Until occur a large amount of white precipitates in beaker, stop stirring.Cover rim of a cup with preservative film, putting into water tank control temperature is 1 ℃, standing and reacting 24 hours.Add the 200ml frozen water in the beaker mixture, stir gently and make its suspension, use rapidly Bush's funnel suction filtration; The gained solids is with the washing of 400ml frozen water, until till washings pH value neutrality, suction filtration, obtains acetone peroxide trimer crude product 264g after drying in the shade, and productive rate is 99.0%.
Purify with the preparation-obtained crude product of 260ml dissolve with methanol, be heated to 45 ℃ in water-bath, stirring is dissolved it fully, then adds the methanol solvate into 20ml, and after stirring, naturally cooling makes its crystallization, suction filtration; Repeat above-mentioned recrystallization again and purify five times, obtain random crystal 2 42.9g after seasoning, productive rate is 91.08%.Purity is 99.96%.
In the recrystallization purification process, a product quality loss 2～5% of every recrystallization purification, purity improves 0.09～0.036%.When purity reaches 99.96%, further put forward highly purified possibility very little.
Embodiment 4
Add 34.8g (0.6mol)-5 ℃ acetone in the 500ml four-hole boiling flask, slowly add 32g ozone (0.65mol) to mix 22 minutes on the ice bath of-2 ℃.When controlling temperature at 2 ℃ on ice bath cooling 75 minutes, slowly be added dropwise to 15ml sulfuric acid, rate of addition is 38 of per minutes; Stir while adding steadily; Until occur a large amount of white precipitates in reaction flask, stop stirring.Controlling temperature is 2 ℃, standing and reacting 26 hours.Add the 90ml frozen water in the reaction flask mixture, stir gently and make its suspension, use rapidly Bush's funnel suction filtration; The gained solids is with the washing of 220ml frozen water, until till washings pH value neutrality, suction filtration, obtains crude product acetone peroxide trimer 42.45g after drying in the shade, and productive rate is 95.5%.
Purify with the preparation-obtained crude product of 300ml acetone solution, be heated to 42 ℃ in water-bath, stirring is dissolved it fully, and after stirring, naturally cooling makes its crystallization, obtains random crystalline product 39.87g after suction filtration, seasoning, and productive rate is 89.7%.Purity is 99.33%.
Embodiment 5
Add the cooling good acetone of 52.2g and the hydrogen peroxide of 110g30% to mix 10 minutes in the 1000ml beaker.After stirring, mixed solution is put into refrigerator cooling 45min again, control temperature at 2 ℃.Take out beaker, slowly be added dropwise to the concentrated nitric acid of 30ml with dropper, rate of addition is 30 of per minutes; Stir while adding steadily; Until occur a large amount of little yellow precipitates in beaker, stop stirring.Cover rim of a cup with preservative film, putting into water tank control temperature is 2 ℃, standing and reacting 24～48 hours.The water that adds 200ml2 ℃ in the beaker mixture stirs gently and makes its suspension, uses rapidly Bush's funnel suction filtration; With 1～2 ℃ of water washing, till reaching neutrality to the pH value, obtain white powder acetone peroxide trimer 65.8g after drying in the shade, productive rate is 98.7%, purity is 98.8%
Embodiment 6
Add the acetone of 2 ℃ of 1044g (18mol) at 10000ml in freezing reactor, slowly be added dropwise to the hydrogen peroxide with 2240g30%, mix 20 minutes, control 2 ℃ of temperature of reactor.Under the stirring at low speed state, slowly be added dropwise to 200ml acetic acid, rate of addition is 50～60 of per minutes; Until a large amount of precipitations appear in reactor, stop stirring.Standing and reacting 30 hours.
Mix the frozen water that adds 2 ℃ of 2000ml in reactor, blowing under the gentle agitation condition filters rapidly; Each with 1～2 ℃ of water washing of 5000ml 5～6 times, until till washings pH value reached neutrality, obtaining the acetone peroxide trimer after drying in the shade was white powder crude product 1314g, productive rate is 98.51%.
After thick product is used the 2000ml dissolve with methanol, be heated to 42 ℃, slow cooling under stirring state, controlling cooling rate 5min descends 1 ℃, stop stirring when dropping to 35 ℃, naturally cool to 5 ℃ and more than standing 5h after standing, suction filtration, obtain random trickle crystalline product 1216g after seasoning, productive rate is 91.2%.Purity is 99.59%.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110460164 CN102584783B (en) | 2011-12-31 | 2011-12-31 | Method for preparing acetone peroxide trimer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110460164 CN102584783B (en) | 2011-12-31 | 2011-12-31 | Method for preparing acetone peroxide trimer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102584783A CN102584783A (en) | 2012-07-18 |
| CN102584783B true CN102584783B (en) | 2013-06-05 |
Family
ID=46474107
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110460164 Expired - Fee Related CN102584783B (en) | 2011-12-31 | 2011-12-31 | Method for preparing acetone peroxide trimer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102584783B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795951B (en) * | 2012-08-20 | 2014-12-10 | 北京理工大学 | TATP full-range simulated explosive simulacrum |
| CN102838436B (en) * | 2012-09-12 | 2014-12-24 | 北京理工大学 | TATP (triacetone triperoxide) ray-level simulation explosive simulant |
| CN103214325B (en) * | 2013-04-01 | 2015-04-08 | 中国工程物理研究院化工材料研究所 | Preparation method of hexaazaisowurtzitane crystal |
| CN111606882A (en) * | 2020-06-29 | 2020-09-01 | 北京理工大学 | A kind of preparation method of per-deuterated tripperoxide triacetone |
| CN114957199A (en) * | 2022-04-29 | 2022-08-30 | 北京理工大学 | Method for safely synthesizing TATP |
| CN115043815A (en) * | 2022-05-31 | 2022-09-13 | 黄河三角洲京博化工研究院有限公司 | Novel peroxycycloalkane organic peroxide mixture and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10308891A1 (en) * | 2003-02-28 | 2004-09-09 | Peroxid-Chemie Gmbh & Co. Kg | Process for the preparation of trimeric cyclic cyclohexanone peroxide solutions |
| US20070111321A1 (en) * | 2005-08-31 | 2007-05-17 | Nomadics, Inc. | Detection of explosives and other species |
| CN101033220A (en) * | 2007-03-26 | 2007-09-12 | 浙江大学 | Method of preparing dihyperoxide with two rings |
-
2011
- 2011-12-31 CN CN 201110460164 patent/CN102584783B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102584783A (en) | 2012-07-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102584783B (en) | Method for preparing acetone peroxide trimer | |
| CA2858025C (en) | 5-[3-(2,5-dichloro-4,6-dimethyl-1-oxy-pyridin-3-yl)-[1,2,4]oxadiazol-5-yl]-2-hydroxy-3-methoxy-1-nitrobenzene as an intermediate to prepare a catechol-o-methyltransferase inhibitor | |
| CN101570459A (en) | Ethylenediamine perchlorate.triethylene diamine perchlorate eutectic initiating explosive and preparation method thereof | |
| CN101830858B (en) | Preparation method of 1H-1,2,4-tolyltriazole-3-methyl formate | |
| CN101891698A (en) | 3,4-di(3',5'-dinitryl-4'-methyl phenyl) furoxan compound | |
| CN115490698A (en) | A kind of 6-nitro-2-oxa-6-azaadamantane-4,8-diol dinitrate and its preparation method | |
| CN115894577A (en) | A kind of preparation method of modified nucleoside triphosphate | |
| CN103641670A (en) | Method for coating RDX cyclotrimethylene trinitramine and HMX cyclotetramethylene tetranitramine and coating material thereof | |
| AU2018266244B2 (en) | A method for producing potassium 1,1 -dinitramino-5,5-bistetrazolate and explosive compositions comprising said salt | |
| CN105541666B (en) | A kind of method for crystallising of triaminoguanidinium nitrate | |
| CN105566244A (en) | Synthetic method for 3-(4-aminofurazan-3-radical)-4-(4-nitrofurazan-3-radical) furazan | |
| CN104788502B (en) | The high nitrogen of ferrocene eutectic thing containing energy | |
| CN102532095B (en) | Preparation method for acetone peroxide dimer | |
| CN104610278A (en) | Safety production method of oxacephem antibiotic intermediate sulfoxide ester | |
| CN105367426A (en) | 2, 4-dinitrophenoxyethanol synthesizing method | |
| RU2449977C2 (en) | Method of producing oxidant for condensed energy systems | |
| CN110903261A (en) | Preparation method of high energy density material | |
| CN102627684A (en) | Synthesis method of 5-chloro-6beta, 19-epoxy-5alpha-androstane-3, 17-dione | |
| CN103880681A (en) | A new method for preparing nitroform | |
| CN115448879B (en) | Polynitro nitrogen-rich energy-containing compound and preparation method thereof | |
| CN117303989B (en) | Modified aluminum-lithium alloy fuel with excellent wet heat stability and compatibility and preparation method thereof | |
| CN102875557B (en) | Tetranitroglycoluril dipolymer, preparation method and application | |
| CN107266376B (en) | LLM-105 nitramine derivatives and preparation method thereof | |
| CN108586173A (en) | A kind of preparation method of the Subjective and Objective explosive of the embedded hydrogen peroxide molecule of structure cell | |
| CN102531909B (en) | Method for preparing ethyl nitrate by continuously nitrifying nitric acid steam |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130605 |