CN101973950A - Method for preparing HMX by dynamic material ratio technology - Google Patents

Method for preparing HMX by dynamic material ratio technology Download PDF

Info

Publication number
CN101973950A
CN101973950A CN2010102846948A CN201010284694A CN101973950A CN 101973950 A CN101973950 A CN 101973950A CN 2010102846948 A CN2010102846948 A CN 2010102846948A CN 201010284694 A CN201010284694 A CN 201010284694A CN 101973950 A CN101973950 A CN 101973950A
Authority
CN
China
Prior art keywords
aceticanhydride
section
nitre
acetic acid
hmx
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.)
Pending
Application number
CN2010102846948A
Other languages
Chinese (zh)
Inventor
陈树森
金韶华
李丽洁
李燕月
刘云飞
陈华雄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Institute of Technology BIT
Original Assignee
Beijing Institute of Technology BIT
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Beijing Institute of Technology BIT filed Critical Beijing Institute of Technology BIT
Priority to CN2010102846948A priority Critical patent/CN101973950A/en
Publication of CN101973950A publication Critical patent/CN101973950A/en
Pending legal-status Critical Current

Links

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a process for preparing HMX, which comprises raw material preparation, nitration and pyrolysis processes, and also relates to dynamic material ratio technology for a HMX preparation process. By a material ratio adjusting method, a practical material ratio is kept relatively stable by adjusting the material ratio when the mass of a raw material changes greatly, so that a production process, product yield and product quality are kept stable. In an intermittent process, the HMX yield is up to 75 percent on the premise of lowering the using amount of acetic anhydride by 30 percent and the consumption of the raw material is far lower than that of the same type of foreign process. When the method is applied to a continuous production line, the HMX yield is up to 65 percent on the premise of lowering the using amount of the acetic anhydride by 25 percent, which surpasses that of domestic and foreign intermittent processes.

Description

A kind of usefulness dynamically expects to prepare than technology the method for HMX
Technical field
The present invention relates to the manufacture method of a kind of octogen (HMX), also relate to a kind of HMX manufacturing process and dynamic material thereof, belong to the energetic material field than technology.
Background technology
There is the technology stability problem in the HMX production process, the outstanding behaviours of technology stability is that process temperature is wayward, crude product yield instability, crude product composition and spent acid are formed unstable, and above-mentioned labile factor will cause changeing brilliant technology instability, finished product yield instability and spent acid and handle unstable.
Causing the unsettled important factor of technology is the actual material ratio imbalance that the raw material quality fluctuation brings.Change to adopt corresponding dynamic material ratio according to raw material quality, it is stable that actual material ratio in the system is remained, thereby the HMX yield is remained on the higher level, and reduce and hang wax, prolong the equipment washing cycle, reduces discharge of wastewater.
So-called dynamically material makes the main material ratio in the system keep the constant material ratio control method in principal reaction path in stable and then the maintenance system than being the add-on of adjusting relevant raw materials when raw material quality changes.Dynamic material is to adjust the material ratio at any time than not, just when main raw material(s) such as the bigger variation of acetic acid quality generation, can't bring very burden to operation, but may produce good economic benefit and social benefit than the adjustment of carrying out expecting when driving.Dynamically the core of material ratio is to determine the aceticanhydride consumption according to raw material quality.
Summary of the invention
HMX manufacturing process of the present invention comprises that mainly starting material are prepared, operations such as nitre is separated, pyrolysis, and the starting material of use comprise urotropine, acetic acid, aceticanhydride, nitric acid, ammonium nitrate etc.:
(1) starting material are prepared
Load weighted nitric acid (NA) is joined in the batching still, start and stir, add load weighted ammonium nitrate (AN) under whipped state, the reinforced back of finishing continues to stir, and fully is dissolved in salpeter solution up to AN, obtains ammonium nitrate-salpeter solution,
Load weighted acetic acid (HAc) is joined in the batching still, start and stir, add load weighted urotropine (HA) under whipped state, the reinforced back of finishing continues to stir, and fully is dissolved in the HAc solution up to HA, obtains urotropine-acetum;
(2) nitre is separated
One section nitre is separated: separate to nitre and add acetic acid (HAc) and acetic anhydride (Ac in the reactor 2O) as end liquid, under agitation condition, end liquid slowly is warmed up to 40-50 ℃, in 30min, evenly drip whole urotropine-acetums of burden process gained, 40% left and right sides ammonium nitrate-salpeter solution and total Ac continuously 2About 40% of O consumption, this moment, the adularescent solid was separated out.Carry out one section insulation behind reinforced the end, one section nitre is separated liquid under 40-50 ℃ of temperature, be incubated 15～30min;
Two sections nitre are separated: after one section insulation finishes, under 40-50 ℃ of temperature condition, evenly drip remaining ammonium nitrate-salpeter solution and Ac continuously in 30min 2O behind reinforced the end, separates liquid with two sections nitre and is incubated about 50-110min down at 40-55 ℃;
(3) pyrolysis
Under stirring condition, separate a certain amount of 65～75 ℃ water or dilute acetic acid (from the spent acid treatment process) of adding in the liquid to nitre, the acetic acid content that nitre is separated in the liquid is controlled at about 80%, slowly is warmed up to 100 ± 2 ℃, backflow 60min, pyrolysis byproducts.Pyrolysis finishes, and cools to 70 ± 2 ℃, filters, and washes, gets the HMX crude product.
The dynamic material that the invention still further relates to the HMX manufacturing process promptly when bigger variation takes place raw material quality, than adjusting, keeps actual material than relatively stable by material, and then guarantees that the material that generates technology, product yield and constant product quality compares inflation method than technology; In being interrupted method technology, under reduction aceticanhydride consumption 30% prerequisite, make the HMX yield reach 75%, raw materials consumption is also far below the level of external similar technology, described method is applied to tinuous production, reducing under aceticanhydride consumption 25% prerequisite, make the HMX yield reach 65%, surpass domestic and international interruption method state of the art.
Specific embodiments
In one embodiment of the invention, prepare HMX by following steps, (1) nitric acid is joined in the batching still, under whipped state, add ammonium nitrate, ammonium nitrate fully is dissolved in salpeter solution and obtains ammonium nitrate-salpeter solution, to claim acetic acid to join in another batching still, and add urotropine under whipped state, urotropine fully is dissolved in and obtains urotropine-acetum in the acetum; (2) one sections nitre are separated: separate to nitre and add acetic acid and acetic anhydride in the reactor as end liquid, be warmed up to 40-50 ℃, evenly drip whole urotropine-acetums of burden process gained, 40% left and right sides ammonium nitrate-salpeter solution and total Ac continuously in 30min 2About 40% of O consumption is separated liquid with one section nitre and be incubated 15～80min under 40-50 ℃ of temperature; Two sections nitre are separated: after one section insulation finishes, under 40-50 ℃ of temperature condition, evenly drip remaining ammonium nitrate-salpeter solution and Ac continuously in 30min 2O behind reinforced the end, separates liquid with two sections nitre and is incubated 40-100min down at 40-55 ℃; (3) pyrolysis: under stirring condition, separate to nitre and to add entry or dilute acetic acid in the liquid, the acetic acid content that nitre is separated in the liquid is controlled at about 80%, be warmed up to 80-110 ℃, backflow 50-80min, pyrolysis byproducts, cool to 50-70 ℃, filter, wash, get the HMX crude product, wherein the weight ratio of each raw material is a urotropine and the material ratio of nitric acid, ammonium nitrate and acetic acid, aceticanhydride is 1: 2～2.5: 2～2.5: 7～10: 5～7, and ammonium nitrate-salpeter solution and aceticanhydride are 37.5～40: 62.5～60 one, two section dispensed weight ratio.
In another embodiment of the present invention, the HMX manufacturing process adopts urotropine to separate matrix as nitre, uses nitro, acetic acid and aceticanhydride mixture to separate agent as nitre, and ammonium nitrate is that nitre is separated catalyzer, synthetic HMX.The processing condition of its preparation and material are 1: 2～2.5: 2～2.5: 7～9.5: 5.5: 6.5 than the material ratio for urotropine and nitric acid, ammonium nitrate and acetic acid, the salpeter solution of ammonium nitrate and the aceticanhydride allocation proportion in one, two section nitre is separated is 37.5～40: 62.5～60, urotropine is separated under the base and the effect of catalyzer through two sections pyrogenically prepared HMX at nitre, one section pyrolysis temperature is controlled at 80～85 ℃, and two sections pyrolysis temperatures are controlled at 105 ℃.
One section nitre is separated mechanism:
Figure BSA00000274000800031
Two sections nitre are separated mechanism:
Figure BSA00000274000800032
Intermediate 2
In the HMX manufacture method that the present invention relates to, the main effect of aceticanhydride has three aspects, and the one, main composition and the nitric acid of separating agent as nitre generate the acetic acid nitric ether; The one, the small amount of moisture that may generate in moisture of bringing into as starting material in the dewatering agent elimination system and the reaction, the existence of separating agent for activation nitre creates conditions; The 3rd, assist methylene radical to generate the acetyl-o-methyl of leaving away easily as esterifying agent.Its side effect is esterification and the acylation reaction that by product takes place to generate.The common impurity that exists also is that the impurity that nitre is separated the technogenic influence maximum is moisture in the various starting material; It is acetic acid that nitre is separated the maximum starting material of technogenic influence.On the basis to aceticanhydride demand demand, dynamic material ratio method has been proposed at quantitative examination moisture and acetic acid quality.Promptly at raw material quality, mainly be water content in the acetic acid and nitric acid content when bigger variations takes place, adjust aceticanhydride and separate consumption in the process, thereby guarantee the stability of HMX generation technology, product yield and quality product at end liquid and nitre.
(1) at the dynamic material ratio of moisture in the end liquid acetic acid
When not conforming to nitric acid in the end liquid when only moisture, can add the reaction of aceticanhydride and water, eliminate the water in the end liquid.Aceticanhydride hydrolysis rate at normal temperatures is very little, but but reacts under temperature condition more than 40 ℃ and finish within a short period of time.Add excessive aceticanhydride in end liquid, the hydrolysis reaction of aceticanhydride can be eliminated moisture in end liquid temperature-rise period, generates acetic acid.Adding the aceticanhydride amount in the end liquid can be calculated as follows:
Figure BSA00000274000800033
W AceticanhydrideFor adding the weight of aceticanhydride, W in the end liquid Ester acidBe the acetic acid add-on in the end liquid, C is the acetic acid water content.As the acetic acid water content is 2% o'clock, whenever in the moisture 20g of gram acetic acid, should add the 113g aceticanhydride at least in the end liquid in the end liquid.
Figure BSA00000274000800041
Can together consider that for the moisture that brings that acetic acid in the reinforced process brings this partly discusses at the aceticanhydride consumption with the moisture that other starting material bring.
(2) at the dynamic material ratio of nitric acid and water in the end liquid acetic acid
Nitric acid in the end liquid has two kinds of treatment processs.A kind of is to add aceticanhydride, makes the reaction of nitric acid and aceticanhydride generate nitrating agent acetic acid nitric ether, and a kind of is to add urotropine, makes it generate the nitrate of urotropine.
A) end liquid adding urotropine is eliminated excessive nitric acid
Because contain water and nitric acid in the end liquid, water must be removed with aceticanhydride.Add the aceticanhydride of entry needs this moment earlier, end liquid begins to heat up, and the reaction of aceticanhydride and water generates acetic acid in the process of intensification.Nitric acid also can generate the acetic acid nitric ether with the aceticanhydride reaction in the temperature-rise period, but the acetic acid nitric ether is met the water hydrolysis, generates acetic acid and nitric acid again.In fact be equivalent to water elder generation and aceticanhydride reaction, after water is eliminated fully, just generate the acetic acid nitric ether.Add urotropine and add the aceticanhydride and the ammonium nitrate of metering in end liquid, the nitre that promptly utilizes nitric acid in the end liquid in advance to carry out a urotropine mononitrate is separated.This method complicated operation should not adopt.
B) the adding aceticanhydride is removed water and the nitric acid in the end liquid simultaneously
It is more reasonable to add aceticanhydride, reaction in the system at this moment has aceticanhydride and nitric acid reaction to generate acetic acid nitric ether, the hydrolysis reaction of acetic acid nitric ether and the hydrolysis reaction of aceticanhydride, when adding the metering aceticanhydride, the water in the system all generates acetic acid, and the nitric acid in the system then generates the acetic acid nitric ether.Consider ammonium nitrate in the nitre enzymatic hydrolysis system nitrated catalyst action and the effect of stable ring compound, also should add in the end liquid with end liquid in the ammonium nitrate of quality such as nitric acid.
Respectively need a part aceticanhydride because generate a part acetic acid nitric ether and remove a part water, then the add-on of aceticanhydride can be calculated by following formula in the end liquid.
Figure BSA00000274000800042
W in the formula AceticanhydrideBe the aceticanhydride weight that should add in the end liquid, W Acetic acidBe the acetic acid weight that adds in the end liquid, C WaterBe the water content of acetic acid, C Nitric acidBe the nitric acid content in the acetic acid.
When containing the nitric acid of 2% water and 2% in the acetic acid simultaneously, the acetic acid in every kilogram of end liquid contains 20g water and 20g nitric acid, needs aceticanhydride respectively, and the aceticanhydride add-on is at least in the end liquid
Figure BSA00000274000800043
Figure BSA00000274000800044
(3) simplification of aceticanhydride consumption is calculated
The HMX production technique is bigger to one section aceticanhydride add-on influence, and after employing was dynamically expected ratio, one section major and minor reaction did not change, and the aceticanhydride consumption is only relevant with the moisture total amount in the starting material, can draw the calculation formula of one section aceticanhydride consumption thus:
Figure BSA00000274000800052
W in the formula One section aceticanhydrideBe the aceticanhydride weight that adds in the one-stage nitration, 1-C HNBe the water content of the urotropine that adds in the end liquid, 1-C NABe the water content in the nitric acid, 1-C AcOHWater content for acetic acid.
Discuss as can be known by the front, the water content of nitric acid, ammonium nitrate, urotropine is very little to one section aceticanhydride consumption influence, so, can raw-materially allow that the water yield gets common numerical value with these three kinds, its required aceticanhydride amount is 107g, and it is 2363g that the demand of these data and reaction pair aceticanhydride is merged into a constant.It is as follows to obtain formula thus:
Figure BSA00000274000800053
C: the moisture content percentage in the acetic acid is 1% as the acetic acid water content, C=1 then, and the acetic acid water content is 0.9 o'clock, C=0.9 etc.
The aceticanhydride total amount still is
With traditional method, in described HMX manufacturing process, starting material are than HA (urotropine): HAc (acetic acid): Ac 2O (aceticanhydride): NA (nitric acid): AN (ammonium nitrate)=1: 98: 8.9: 24: 2.4.
In embodiment preferred of the present invention, the adoptable starting material of method of the present invention are than HA: HAc: Ac 2O: NA: AN=1: 9.8: 6.23: 2.3: 2.3.
This testing data is compared with the starting material ratio of traditional technology, and the HA consumption of unit mass HMX reduces by 37%, and the HAc consumption reduces by 37%, Ac 2The O consumption reduces by 56%, and nitric acid dosage reduces by 38%, and the AN consumption reduces by 39%.The spent acid growing amount of HMX per ton is reduced to about 15 tons by about 25 tons of former technology, reduces about 40%.
The industrial hexamethylenetetramine that the present invention uses (urotropine HA) should meet GB/T 9015-1998 standard-required, and quality index is as follows:
Figure BSA00000274000800055
The industrial ammonium nitrate (AN) that the present invention uses should meet GB 2945-1989 standard-required:
Figure BSA00000274000800062
The industrial nitric acid (NA) that the present invention uses should meet GB/T 3371-2002 standard-required:
The project quality standard
The outward appearance light yellow transparent liquid does not have visible mechanical impurity
Nitric acid content 〉=990%
Sulfuric acid content≤008%
Ignition residue content≤002
Nitrous acid content≤015%
Embodiment one
Selecting the urotropine charging capacity is 1000g, selecting material is urotropine than (mass ratio): nitric acid: ammonium nitrate: acetic acid=1: 2.2: 2.2: 9.8, when urotropine, nitric acid, three kinds of starting material water content of ammonium nitrate are 0.5%, the acetic acid water content is 0.4% o'clock, and one section aceticanhydride actual amount is calculated as follows:
Figure BSA00000274000800063
The aceticanhydride consumption is 2556g, and two sections aceticanhydride consumptions are 5623～7668g, are preferably 6134～6390g.Urotropine is 1: 2～25: 2～25～7～10 with the material ratio of nitric acid, ammonium nitrate and acetic acid; It is 42～46 ℃ that the nitre of one section and two sections is separated temperature; The one nitre period of separating is 30～60min, and two nitre periods of separating are 40～100min; Pyrolysis temperature is 50～110 ℃, and the filtration temperature of crude product HMX is 50～80 ℃.The result is interrupted the yield that legal system is equipped with HMX and reaches 70～78%, and the yield that continuous processing prepares HMX reaches 65-76%.
Embodiment two
Selecting the urotropine charging capacity is 1000g, selecting material is urotropine than (mass ratio): nitric acid: ammonium nitrate: acetic acid=1: 22: 22: 9.8, when urotropine, nitric acid, three kinds of starting material water content of ammonium nitrate are 0.5%, the acetic acid water content is 0.4% o'clock, calculates by following formula of reduction:
Figure BSA00000274000800071
The one section aceticanhydride consumption that calculates is 2587g, and two sections aceticanhydride consumptions are 5691～7761g, are preferably 6208～6467g.Urotropine is 1: 2～2.5: 2～2.5～7～10 with the material ratio of nitric acid, ammonium nitrate and acetic acid; It is 42～46 ℃ that the nitre of one section and two sections is separated temperature; The one nitre period of separating is 30～60min, and two nitre periods of separating are 40～100min; Pyrolysis temperature is 50～110 ℃, and the filtration temperature of crude product HMX is 50～80 ℃.The result is interrupted the yield that legal system is equipped with HMX and reaches 70～78%, and the yield that continuous processing prepares HMX reaches 65-75%.
Embodiment three
Selecting the urotropine charging capacity is 1000g, selecting material is urotropine than (mass ratio): nitric acid: ammonium nitrate: acetic acid=1: 2.2: 2.2: 9.8, when urotropine, three kinds of starting material water content of ammonium nitrate are 0.5%, the nitric acid water content is 1.5%, the acetic acid water content is 1% o'clock, and one section aceticanhydride actual amount is calculated as follows:
The one section aceticanhydride consumption that calculates is 2939g, and two sections aceticanhydride consumptions are 6465～8817g, are preferably 7053～7347g.Urotropine is 1: 2～25: 2～2.5～7～10 with the material ratio of nitric acid, ammonium nitrate and acetic acid; It is 42～46 ℃ that the nitre of one section and two sections is separated temperature; The one nitre period of separating is 30～60min, and two nitre periods of separating are 40～100min; Pyrolysis temperature is 50～110 ℃, and the filtration temperature of crude product HMX is 50～80 ℃.The result is interrupted the yield that legal system is equipped with HMX and reaches 68～73%, and the yield that continuous processing prepares HMX reaches 63-72%.

Claims (9)

1. HMX manufacturing process comprises that starting material are prepared, nitre is separated, pyrogenic processes:
(1) starting material are prepared: nitric acid is joined in the batching still, add ammonium nitrate under whipped state, ammonium nitrate fully is dissolved in salpeter solution and obtains ammonium nitrate-salpeter solution,
To claim acetic acid to join in another batching still, and add urotropine under whipped state, urotropine fully is dissolved in and obtains urotropine-acetum in the acetum;
(2) nitre is separated
One section nitre is separated: separate to nitre and add acetic acid and acetic anhydride in the reactor as end liquid, be warmed up to 40-50 ℃, evenly drip whole urotropine-acetums of burden process gained, 40% left and right sides ammonium nitrate-salpeter solution and total Ac continuously in 30min 2About 40% of O consumption is separated liquid with one section nitre and be incubated 15～80min under 40-50 ℃ of temperature,
Two sections nitre are separated: after one section insulation finishes, under 40-50 ℃ of temperature condition, evenly drip remaining ammonium nitrate-salpeter solution and Ac continuously in 30min 2O behind reinforced the end, separates liquid with two sections nitre and is incubated 40-100min down at 40-55 ℃;
(3) pyrolysis
Under stirring condition, separate to nitre and to add entry or dilute acetic acid in the liquid, the acetic acid content that nitre is separated in the liquid is controlled at about 80%, is warmed up to 80-110 ℃, backflow 50-80min, pyrolysis byproducts cools to 50-70 ℃, filters, wash, HMX product mutually,
Wherein the weight ratio of each raw material is a urotropine and the material ratio of nitric acid, ammonium nitrate and acetic acid, aceticanhydride is 1: 2～2.5: 2～25: 7～10: 5～7, and ammonium nitrate-salpeter solution and aceticanhydride are 37.5～40: 62.5～60 one, two section dispensed weight ratio.
2. according to right 1 described HMX manufacturing process, wherein urotropine is 1: 2～2.5: 2～2.5: 7～9.5: 55: 65 with the material ratio of nitric acid, ammonium nitrate and acetic acid, the salpeter solution of ammonium nitrate and the aceticanhydride allocation proportion in one, two section nitre is separated is 37.5～40: 62.5～60, urotropine is through two sections pyrogenically prepared HMX, one section pyrolysis temperature is controlled at 80～85 ℃, and two sections pyrolysis temperatures are controlled at 105 ℃.
3. according to right 1 described HMX manufacturing process, wherein the acetic acid moisture content is not more than 2%, and preferred acetic acid moisture content is not more than 0.5%; Nitric acid content is not more than 2% in the acetic acid, and nitric acid content is not more than 0.5% in the preferred acetic acid, and wherein moisture content is not more than 1.5% in the nitric acid, and moisture is not more than 1% in the preferred nitric acid.
4. one kind according to the described HMX manufacturing process of claim 1, it has adopted dynamic material than technology, and the urotropine charging capacity is 1000 gram equivalents, and the benchmark consumption of one section aceticanhydride is 2256 gram equivalents, actual amount is regulated according to the starting material water content, and one section aceticanhydride actual amount is calculated as follows:
Figure FSA00000274000700021
W in the formula One section aceticanhydrideBe one section aceticanhydride actual amount, 1-C HNBe the water content of the urotropine that adds in the end liquid, 1-C NABe the water content in the nitric acid, 1-C AcOHBe the water content of acetic acid, one, two section aceticanhydride total amount is 2.0～4.0 times of one section aceticanhydride consumption, is preferably 2.4～3.0 times of one section vinegar amount.
5. one kind according to the described HMX manufacturing process of claim 1, and it has adopted dynamic material than technology, when nitric acid ammonium nitrate and urotropine water content all less than 0.5% the time, one section aceticanhydride actual amount can be calculated by following formula of reduction:
Figure FSA00000274000700022
One, two sections aceticanhydride total amounts are 22～4.0 times of one section aceticanhydride consumption, are preferably 2.4～3.0 times of one section vinegar amount.
6. according to right 1 described method, it is 42～46 ℃ that the nitre of one section and two sections is separated temperature.
7. according to right 1 described method, the one nitre period of separating is 30～60min, and two nitre periods of separating are 50～80min.
8. according to the method for right 1 record, pyrolysis temperature is 80～100 ℃.
9. according to the method according to right 1 record, the filtration temperature of crude product HMX is 65～70 ℃.
CN2010102846948A 2010-09-17 2010-09-17 Method for preparing HMX by dynamic material ratio technology Pending CN101973950A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010102846948A CN101973950A (en) 2010-09-17 2010-09-17 Method for preparing HMX by dynamic material ratio technology

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010102846948A CN101973950A (en) 2010-09-17 2010-09-17 Method for preparing HMX by dynamic material ratio technology

Publications (1)

Publication Number Publication Date
CN101973950A true CN101973950A (en) 2011-02-16

Family

ID=43573868

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010102846948A Pending CN101973950A (en) 2010-09-17 2010-09-17 Method for preparing HMX by dynamic material ratio technology

Country Status (1)

Country Link
CN (1) CN101973950A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103524443A (en) * 2013-09-29 2014-01-22 山西北化关铝化工有限公司 Specific HMX (cyclotetramethylene tetranitramine)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3770721A (en) * 1956-02-09 1973-11-06 Us Army Direct production of beta hmx
US4086228A (en) * 1976-10-22 1978-04-25 The United States Of America As Represented By The Secretary Of The Army Process for preparing cyclotetramethylenetetranitramine
US5391736A (en) * 1990-01-29 1995-02-21 Gencorp Aerojet Preparation of 2,4,6-trinitro-2,4,6-triaza-cyclohexanone
CN1716136A (en) * 2004-07-02 2006-01-04 天津鼎成高新技术产业有限公司 Dynamic compounding controller and method
CN101624394A (en) * 2009-08-12 2010-01-13 北京理工大学 Sphericized hexanitrohexaazaisowurtzitane (HNIW) crystal and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3770721A (en) * 1956-02-09 1973-11-06 Us Army Direct production of beta hmx
US4086228A (en) * 1976-10-22 1978-04-25 The United States Of America As Represented By The Secretary Of The Army Process for preparing cyclotetramethylenetetranitramine
US5391736A (en) * 1990-01-29 1995-02-21 Gencorp Aerojet Preparation of 2,4,6-trinitro-2,4,6-triaza-cyclohexanone
CN1716136A (en) * 2004-07-02 2006-01-04 天津鼎成高新技术产业有限公司 Dynamic compounding controller and method
CN101624394A (en) * 2009-08-12 2010-01-13 北京理工大学 Sphericized hexanitrohexaazaisowurtzitane (HNIW) crystal and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
曹端林等: "醋酐法制备HMX工艺改进研究", 《兵工学报（火化工分册）》 *
李伟明: ""醋酐法生产HMX工艺研究"", 《中国优秀硕士学位论文全文数据库工程科技I辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103524443A (en) * 2013-09-29 2014-01-22 山西北化关铝化工有限公司 Specific HMX (cyclotetramethylene tetranitramine)
CN103524443B (en) * 2013-09-29 2015-05-13 山西北化关铝化工有限公司 Specific HMX (cyclotetramethylene tetranitramine)

Similar Documents

Publication Publication Date Title
CN102070457B (en) Method for continuously preparing dinitrochlorobenzene
CN104649910B (en) Method capable of recycling acids for preparing 2,5-dichloronitrobenzene (DCNB) through continuous nitration
CN100457701C (en) Method for separating and preparing mono, bis-pentaerythritol and its by-product using high temperature condensation and concatenate recrystallization
CN100430384C (en) Method for the production of 4-(4-aminophenyl)-3-morpholinon
CN102827038B (en) Preparation process for nitroguanidine
CN101648866A (en) Preparation technology of p-tert-butyl benzoic acid
CN111848406B (en) Preparation method of 2-chloro-4-fluoro-5-nitrobenzaldehyde
CN101830859B (en) Production method of isocyanuric acid
KR100812622B1 (en) Process for the preparation of nitric esters of monohydric alcohols
CN101475487B (en) Recycling use method of nitration acid
CN107793328A (en) A kind of production method of N, N cyanoethyl benzylaniline
CN101973950A (en) Method for preparing HMX by dynamic material ratio technology
CN102875435A (en) Organic thiosulfuric acid derivative preparation method
CN106699591A (en) Clean production process of glycine and co-produced ammonium chloride
CN104788389A (en) Preparation method of 5-bromouracil
CN101219958A (en) Method for producing 5-nitryl isophthalic acid
CN102746692B (en) Preparation method for disperse blue 2BLN
CN101066929B (en) Process of preparing 4-amino-3-nitro phenol
CN107986971A (en) A kind of preparation method of cyclohexyl nitrate
CN100593540C (en) Method for preparing 5-amido-1-(2,6-dichlorin-4-trifluoro methylbenzene)-3-cyano pyrazole
CN102718632B (en) Method for preparing terpin hydrate by virtue of continuous hydration
CN101823986A (en) Preparation method for tert-butyl carbazate
CN108911999B (en) Synthesis method of 1-aminoanthraquinone
CN103086969B (en) Synthesis method of iminostilbene carbonyl chloride
CN101225069A (en) Method for synthesizing meropenem intermediate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C53 Correction of patent of invention or patent application
CB03 Change of inventor or designer information

Inventor after: Jin Shaohua

Inventor after: Chen Shusen

Inventor after: Li Lijie

Inventor after: Li Yanyue

Inventor after: Liu Yunfei

Inventor after: Chen Huaxiong

Inventor after: Shu Qinghai

Inventor before: Chen Shusen

Inventor before: Jin Shaohua

Inventor before: Li Lijie

Inventor before: Li Yanyue

Inventor before: Liu Yunfei

Inventor before: Chen Huaxiong

COR Change of bibliographic data

Free format text: CORRECT: INVENTOR; FROM: CHEN SHUSEN JIN SHAOHUA LI LIJIE LI YANYUE LIU YUNFEI CHEN HUAXIONG TO: JIN SHAOHUA CHEN SHUSEN LI LIJIE LI YANYUE LIU YUNFEI CHEN HUAXIONG SHU QINGHAI

C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20110216