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CN101973947

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Publication
CN101973947 B
number

Publication type Grant

Application
CN 201010289417
number

Publication date 9 Dec 2015

Filing date 25 Sep 2010

Priority date 25 Sep 2010

Also published as CN101973947A

Publication 201010289417.6,
number CN 101973947 B,
CN 101973947B,
CN 201010289417,
CN-B
B-101973947,
CN101973947 B,
 CN101973947B,
CN201010289417,
CN201010289417.6

Inventors , ,
, ,
,

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Export Citation BiBTeX, EndNote,

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Patent Citations (4), Classifications (1),

Legal Events (3)

External Links: SIPO, Espacenet

One technique for preparing spherodized RDX crystal

control method translated from Chinese
CN 101973947 B

ABSTRACT translated from Chinese

The present invention relates to a method for preparing spherical of RDX, including: (1)
adding a crystallization solvent and RDX kettle, heating temperature to dissolve, then add
crystal control agent methylene ammonium nitrate, nitro ethane or glycerol alcohol; (2) cooling
to 70 ~ 80 with or without seeding, holding 10-20min; (3) to cool to room temperature (20-
25 ). The resulting bulk density of RDX front 15-45% compared with the untreated increase
the viscosity paraffin mixed system fell 20-50% sensitivity (H50 value) fell 20-50%.

CLAIMS(6) translated from Chinese

1. A method of preparing RDX, which is characterized by: (1) the solvent cyclohexanone and
RDX crystal kettle was added, the solvent and the ratio of RDX 100mL: 200~300g, heated to
80~90 C so that RDX was completely dissolved, then add the weight of RDX 0.1-0.6% of
the initial amount of crystallization control agent nitroacetate burn or glycol; (2) at a rate of 3-5
C / minute cooling to 70~80 C when added to the initial amount of 5% by weight of RDX
seed, kept stirring speed 200~450r / min, insulation 10_20min; (3) at a rate of 1-5 C / minute
cooling to 20 ~25 C, stirring rate 200~450r / min, filtered, washed, and dried to obtain the
RDX products.

2. Preparation method according to claim 1, wherein the first step (2) was not
added RDX seed.

3. The method according to claim 1 or claim 2, wherein said crystallization control

agent is nitroethane.

4. The method according to claim 1 or claim 2, wherein the crystallization control

agent is added to the initial weight of RDX 0.2-0.3%

5. The method of claim 1 or claim 2, wherein the stirring rate is 200~250r / min.

6. The method according to claim 1 or claim 2, wherein the cooling rate in step (3)
is 3-5 C / min.

DESCRIPTION translated from Chinese

One technique for preparing spherodized RDX crystal control method

TECHNICAL FIELD

[0001] The present invention relates to a sphere of hexogen (RDX) preparation, particularly
relates to a method of preparing spherical crystal control technology RDX.

Background technique

[0002] The crystal ball with other shapes such as prismatic, acicular, rod-like crystals
compared, a better accumulation effect, has good processing flowability liquid polymer mixed
with a solvent or mucus, molding properties better.

[0003] Energetic compound shape affect the sensitivity of the crystals and bulk density,
spherical crystal having processed into the process of energetic materials in good processing
properties, and has good security, machined parts have more Good explosive performance
and low sensitivity. When spherical of RDX and other polymer adhesive materials, additives
and other ingredients made of energetic materials, can play a lift solids content can
compound to improve its energy, improve processing performance including energy materials
and so on.

[0004] Antoine EDMvan der Heijden ^ PRichard HBBouma (Crystallizat1n

andCharacterizat1n of RDX, HMX, and CL-20.CRYSTAL GROWTH & DESIGN, 2004, Vol.4,
N0.5: 999~1007) reported the use of an aqueous cyclohexanone recrystallized RDX RDX can
improve the effect of spherical crystals, and analyzed the amount of water for cyclohexanone
recrystallized RDX's influence. GB2156805A reported the use of - butyrolactone
recrystallized RDX with RDX method of preparing spherical. US4065529A reported the use
of RDX saturated cyclohexanone solution was prepared by ball of the RDX, the method by
controlling the temperature of the system, while observing the crystal shape RDX suspension,
when the ball reaches of the requirements, obtained by centrifugation spheroidizationwere
RDX. US20060272755A1 solvent and non-solvent method reports prepared by
recrystallization method RDX. JP2009051692A reported the use of organic solvents was
recrystallized RDX RDX in order to achieve improved crystal morphology approach. Feng et
al reported a cedar dimethyl sulfoxide as solvent, Twin-80 as crystal modifiers recrystallized
RDX method, but requires the preparation of RDX crystals screened through an optical
microscope having a good appearance and less crystal defects within the crystal The RDX
backup products, that is, the method does not effectively control the RDX crystal quality
(appearance and internal defects); however, the preparation of RDX products with better
crystalline particles with high apparent density, shock sensitivity reduced by 25%.

[0005] The present invention uses a crystalline RDX control agents on crystallization process
is controlled so that the resulting crystalline RDX crystals with controlled particle size and
distribution of the crystals have a spherical shape more regular, has a higher bulk density and
processing performance, At the same time fewer internal defects RDX crystal, which has a
lower sensitivity.

SUMMARY OF THE INVENTION

[0006] The present invention relates to a method for preparing spherical RDX technology
today, specifically including the following steps:

[0007] (I) will be added to the solvent and crystallization of RDX kettle, the solvent and the
ratio of RDX 100rnl: 200~300g, heated to 80-90 C so that RDX was completely dissolved,
then added to the weight of the initial amount of RDX 0.1 0.6% methylene ammonium nitrate
crystallization control agent, nitroethane or glycerol;

[0008] (2) at a rate of 3-5 C / minute cooling to 70~80 C with or without added weight of
RDX initial amount of 5% of the seed and keep stirring speed 200~450r / min, insulation
10_20min;

[0009] (3) at a rate of 1-5 C / min cooling to room temperature (20-25 C), stirring rate
200~450r / min, filtered, washed, and dried to obtain the product RDX.

[0010] The present invention RDX used in factory production in line with the use of standard
products, after treated, RDX shape becomes more regular, compared with and without crystal
control agents crystal, with less angular, with spherodized shape, with the same level of RDX
Particle Size and Distribution of the test, the measured bulk density of RDX front 15-45%
increase compared with the untreated, the viscosity of the liquid paraffin sphere of RDX mixed
system of relatively unprocessed RDX mixed with paraffin system The viscosity decreased
20-50%, sensitivity (H5. value) decreased 20-50%. RDX spherical crystal particles
characterized before and after treatment with an optical microscope morphology of its
appearance. RDX crystal particles before treatment as shown in the drawings, the crystal
particles are not very rule 1, showing massive, there are more angular. RDX crystals after
treatment almost no spherical angular shape also appears to rule, rendered spherical. RDX
treatment after having a spherical shape rules.

[0011] The present invention uses a small amount of crystal modifier to change the RDX
crystallization process, inhibiting the crystallization process RDX crystals during crystallization
defects (voids, dislocations, intergranular sandwich, etc.) reduced, thereby improving the
quality crystal, reducing the RDX mechanical sensitivity. However, measured by high
performance liquid around recrystallized RDX chemical purity is not reduced, the
crystallization control agent did not affect the chemical purity of RDX. Crystalline control
agents suitable crystallization process (solvent and RDX feed ratio, the cooling rate, stirring
speed, etc.) for RDX recrystallized RDX crystal shape can change not only to improve its
workability, bulk properties, but also improve its crystal quality reducing crystal defects,
reduce sensitivity.

Brief Description

[0012] Figure 1 is recrystallized RDX morphology of the particles before treatment.

[0013] FIG. 2 for the use of RDX particle crystal morphology control after treatment.

Specific embodiments

[0014] In one embodiment of the present invention, the solvent cyclohexanone and RDX join
crystallization reactor, the ratio of solvent and RDX 100ml: 200~300g, heated to 80-90 C
so that RDX is completely dissolved, The solvent is cyclohexanone, followed by addition of
0.1 to 0.6 wt% of the initial amount of RDX crystals controlling agent methylene ammonium
nitrate, nitro ethane or glycerol; then at a rate of 3-50C / min cooling to 70 ~80 C was
added when the weight of the initial amount of 5% RDX seed crystal, maintaining stirring
speed 200~250r / min, incubated 10_20min; Finally, stirring rate 200~250r / min, to 1-5 C /
min the rate of cooling to room temperature (20-25 C), filtered, washed, and dried to obtain
the RDX products. Testing with the same level before and after the recrystallized grain size
and size distribution of RDX, RDX measured the bulk density increase of 15-45% compared
with the untreated, the viscosity of the liquid paraffin RDX mixed system relative viscosity of
RDX and paraffin untreated mixed system fall 20-50%, sensitivity (H5. value) fell 20-50%.

[0015] In another embodiment of the present invention, the solvent cyclohexanone and RDX
join crystallization reactor, the ratio of solvent and RDX 100ml: 250~300g, heated to 85-90
C so that RDX is completely dissolved and then a weight of 0.2 to 0.3% of the initial amount
of RDX crystal control agent methylene ammonium nitrate or nitroethane; then at a rate of 3-5
C / minute cooling to 70~80 C when added weight of RDX 5% of the initial amount of
the seed crystal, maintaining stirring speed 200~250r / min, incubated 10-20min; and finally at
a rate of 2-5 C / min cooling to room temperature (20-25 C), stirring speed 200~ 250r /
min, filtered, washed, and dried to obtain the RDX products. The same level before and after
recrystallization size and size distribution of RDX test measured the bulk density before RDX
increase 25-45% over the untreated, the viscosity of the liquid paraffin RDX mixed system
relative viscosity of RDX and paraffin untreated mixed system decreased 30-50%, sensitivity
(H5. value) decreased 30-50%.

[0016] In one embodiment of the present invention, the solvent cyclohexanone and RDX join
crystallization reactor, the ratio of solvent and RDX 100ml: 200~300g, heated to 80-90 C
so that RDX is completely dissolved, then add the weight of RDX 0.l-0.6% of the initial
amount of crystal control agent methylene ammonium nitrate, nitro ethane or glycerol; and
then at a rate of 3-5 C / minute cooling to 70~80 C , maintaining agitation speed
200~450r / min, incubated 10_20min; finally at a rate of 1_5 C / min cooling to room
temperature (20-25 C), kept under stirring speed 200~450r / min, filtered, washed, and
dried i.e. I was RDX products. RDX measured the bulk density increase of 20-45% compared
with that before the untreated, the viscosity of the liquid paraffin RDX mixed system of
relatively untreated mixed system viscosity paraffin RDX and fell 30-50% sensitivity (H5.
Value) decreased 20- 50%.

[0017] In the present invention, a further particular embodiment, the solvent cyclohexanone
and RDX join crystallization reactor, the ratio of solvent and RDX 100ml: 200~300g, heated to
80-90 C so that RDX is completely dissolved and then a weight of 0.1 to 0.3% of the initial
amount of RDX crystal control agent methylene ammonium nitrate or nitroethane; then at a
rate of 3-5 C / minute cooling to 70~80 C, added weight of RDX 5% of the initial amount
of the seed crystal, maintaining stirring speed 200~450r / min, incubated 10-20min; and finally
at a rate of 1_5 C / min cooling to room temperature (20_25 C), kept under stirring
speed 200~450r / min , filtered, washed, and dried to obtain the RDX products. RDX
measured the bulk density increased compared with that before the untreated 20_45%, the
viscosity of the liquid paraffin RDX mixed system of relatively untreated mixed system
viscosity paraffin RDX and fell 30-50% sensitivity (H5q value) decreased 20-50%

[0018] The present invention is in the room temperature 20 C~25 C, stirring, filtration
processes are no special requirements, the use of conventional equipment and methods in
the art. The size of the present invention is measured by a laser particle size analyzer,
wherein the average particle size is a volume average particle size of the test results given.
The viscosity of the present invention is a rotary viscometer, the specific method is 50 g RDX
sample with 100 ml of liquid paraffin were mixed and the viscosity measured RDX and
paraffin mixed system, with the ball of wax mixed system viscosity RDX- relatively spherical
lowering of the viscosity of the mixed system before RDX- paraffin to quantitatively
characterize the effect spherodized after. Sensitivity testing methods GJB 772A-97 according
to the method prescribed by Cast drop weight lifting apparatus according to the
characteristics of the drop measured RDX high H5. . Hammer the quality of 5 0.005Kg,
medicines to 50 lmg. Measuring a temperature of 15~26 C, a humidity of 20% ~ 22%.
[0019] For a better understanding of the present invention, the following are a few specific
embodiments, and is not intended to limit the present invention.

[0020] Example

[0021] Example 1

[0022] 100ml solvent at room temperature and 200 g of cyclohexanone was added RDX
crystals kettle, heated to 80 C so that RDX was completely dissolved, then added to the
weight of glycerin RDX initial crystallization control agent is an amount of 0.2 g; and then
added weight at a rate of 3 C / min cooling to 70 C when 5% of the initial amount of
RDX RDX seed, kept stirring speed of 200rpm, insulation 1min; and finally at a rate of 5 C /
min cooling to room temperature 25 C, filtered, washed, and dried to obtain the RDX
products. Testing with the same level before and after the recrystallized grain size and size
distribution of RDX, RDX measured the bulk density increased by 15% compared with the
untreated, the viscosity of the liquid paraffin RDX mixed system relative viscosity of RDX and
paraffin untreated mixed system decreased by 20 % sensitivity (H5q value) decreased by
20%.

[0023] Example 2

[0024] 100ml solvent at room temperature and 200 g of cyclohexanone was added RDX
crystals kettle, heated to 80 C so that RDX was completely dissolved, then added to the
weight of the initial amount of 0.2 g RDX crystal control agent methylene ammonium nitrate ;
join again at a rate of 3 C / min cooling to 70 C at 10 g RDX seed, kept stirring speed of
200rpm, insulation 1min; and finally at a rate of 5 C / min cooling to room temperature, 25
C, filtered, washing, drying derived RDX products. Testing with the same level before and
after the recrystallized grain size and size distribution of RDX, RDX measured the bulk
density increased by 25% compared with the untreated, the viscosity of the mixed system
RDX and liquid paraffin and paraffin RDX relatively untreated mixed system viscosity
decreases 30 % sensitivity (H5. value) decreased by 30%.

[0025] Example 3

[0026] 100ml solvent at room temperature and 200 g of cyclohexanone was added RDX
crystals kettle, heated to 80 C so that RDX was completely dissolved, then added to the
weight of the initial amount of 0.2 g RDX crystal controlling agent nitroethane; and then at a
rate of 3 C / min cooling to 70 C, kept under stirring speed of 200rpm, insulation 1min;
and finally at a rate of 5 C / min cooling to room temperature, 25 C, filtered, washed,
and dried to obtain the product RDX. Testing with the same level before and after the
recrystallized grain size and size distribution of RDX, RDX measured the bulk density of the
former increased by 35% over the untreated, the viscosity of the liquid paraffin RDX mixed
system relative viscosity of RDX and paraffin untreated mixed system of drops 35 %
sensitivity (H5. value), down 40%.
[0027] Example 4

[0028] In a further embodiment of the present invention, the solvent is cyclohexanone and
RDX crystals kettle was added, and the amount of the solvent is RDX 1000ml, 250g, heated
to 90 C so that RDX was completely dissolved, then was added 0.5 g crystallization control
agent nitroethane; then at a rate of 4 C / min cooling to 75 C was added 20 g RDX
seed, kept stirring speed 250r / min, incubated 20min; finally at a rate of 2 C / min cool to
room temperature, 25 C, the phase stirring rate 250r / min, filtered, washed, and dried to
obtain the RDX products. RDX measured bulk density than before the untreated increased
by 45%, the viscosity of the liquid paraffin RDX mixed system relative viscosity of RDX and
paraffin untreated mixed system decreased by 50%, sensitivity (H5. Value) decreased by
50%.

[0029] Example 5

[0030] In a further embodiment of the present invention, the solvent is cyclohexanone and
RDX crystals kettle was added, and the amount of the solvent is RDX 1000ml, 250g, heated
to 90 C so that RDX was completely dissolved, then was added 0.5 g crystallization control
agent methylene ammonium nitrate; re at a rate of 5 C / min cooling to 80 C, keeping
stirring speed 450r / min, incubated 20min; finally at a rate of 20C / min cooling to room
temperature, 25 C, The phase stirring rate 450r / min, filtered, washed, and dried to obtain
the RDX products. RDX measured bulk density than before the untreated increased by 40%,
the viscosity of the liquid paraffin RDX mixed system relative viscosity of RDX and paraffin
untreated mixed system declined 45%, sensitivity (H5. Value), down 40%.

PATENT CITATIONS

Filin
Publicatio
Cited Patent g Applicant Title
n date
date
Title not
GB2156805A *
available
JP2009051692 Title not
A* available
The United
States Of
America As Process for
5 Jan 27 Dec Represente spheroidizatio
US4065529 *
1976 1977 d By The n of RDX
Secretary crystals
Of The
Army
Institut Particles of
US2006027275 2 Jun
7 Dec 2006 Franco- explosive of
5* 2006
Allemand low sensitivity
 Filin
Publicatio
Cited Patent g Applicant Title
n date
date
De to shock and
Recherches associated
De Saint- treatment
Louis process
* Cited by examiner

CLASSIFICATIONS

International Classification C07D251/06

LEGAL EVENTS

Date Code Event Description

16 Feb
C06 Publication
2011
Entry into substantive
3 Jul 2013 C10
examination
9 Dec 2015 C14 Grant of patent or utility model

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