CN106478323A - Automatically controlled solid propellant of a kind of high-performance and preparation method thereof - Google Patents
Automatically controlled solid propellant of a kind of high-performance and preparation method thereof Download PDFInfo
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- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B31/00—Compositions containing an inorganic nitrogen-oxygen salt
- C06B31/28—Compositions containing an inorganic nitrogen-oxygen salt the salt being ammonium nitrate
- C06B31/32—Compositions containing an inorganic nitrogen-oxygen salt the salt being ammonium nitrate with a nitrated organic compound
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Abstract
The invention discloses automatically controlled solid propellant of a kind of high-performance and preparation method thereof.With HAN, ammonium nitrate, ethylenediamine nitrate, in ethanolamine nitrate a kind of or both be oxidant, polyvinyl alcohol, one of polyvinylamine nitrate or two kinds are as binding agent, 2, 2 ' bipyridyls, one of dihydrogen phosphate or two kinds are as buffer agent, 5 aminotetrazoles are stabilizer, 1, 2, 4 triazoles, 1, 3, one of 5 s-triazine or two kinds make ballistic modifying agent, additional crosslink agent, plasticizer, mix at room temperature, directly irrigate after stirring under vacuum condition or vacuum pouring is in combustor or mould, curing molding at 50 DEG C.Prepared solid propellant has good flame and feels characteristic immediately, nonflammable under high temperature, but can be burnt under the conditions of certain voltage, and there is preferable combustibility, treat that power-off after-combustion stops immediately, also can adjust its burn rate by adjusting voltage swing.
Description
Technical field
The present invention relates to automatically controlled solid propellant field, the automatically controlled solid propellant of specifically a kind of high-performance and its preparation side
Method.
Background technology
Rail control electromotor, as a kind of energy flight attitude of effective control aircraft and the non-conventional engine in direction, passes through
The ignition of precise control propellant, burn rate size and characteristic of extinguishing are used for realizing spacecraft, guided missile or satellite are flown
The orbital exponent of row trajectory and flight attitude correction.
Electric ignition propellant with its fast response time, control accuracy is high and be applied to rail control and start.Electric ignition propellant
It is a kind of new energetic material, can burn under conditions of applied voltage generation high-temperature fuel gas jet, can be divided into liquid and consolidate
Body two class.
Electrically-fired electromotor is carried out with liquid type there is ratio regulation of leaping high, be easy to, but it is multiple to there is structure
Miscellaneous, architecture quality is big, propellant is difficult storage, be difficult to safeguard, the shortcoming of poor stability.
Microminiature solid propellant rocket group has the advantages that structure is simple, it is fast to respond, and its technology maturation, reliability are high,
Can long term storage, greatly shorten the combat readiness time, but only applied on small-sized spacecraft and Guided Weapons.
Additionally, traditional electric ignition propellant exists, ignition voltage is high, and energy resource consumption is big, and after power-off propellant combustion is not
Can stop at once, extinguish poor performance, the energy of whole propulsion system provides mainly by power supply.
Therefore, research and development to obtain a kind of cheap, environmental protection, safety and stability, ignition power force down, combustibility
Good, extinguish that performance is good and controllability of burning is high solid propellant propulsion has great importance.
Content of the invention
Present invention aim to address in prior art, solid push agent is expensive, be difficult storage, poor stability, combustion
The problems such as burning performance is not enough, applicable scope is little.
Employed technical scheme comprise that such for realizing the object of the invention, a kind of automatically controlled solid propellant of high-performance and its
Preparation method is it is characterised in that include following raw material and its parts by weight：
Load weighted above-mentioned raw materials are followed the steps below：
1) at ambient temperature, oxidant, stabilizer, binding agent, cross-linking agent, ballistic modifying agent are added sequentially to react
In device, vacuum stirring, obtain the medicine slurry stirring；
Described stir speed (S.S.) scope is 100～380 revs/min；Described mixing time scope is 0.4～3 hour；
2) by step 1) in the medicine slurry stirring that obtains under normal pressure or vacuum condition, irrigate to combustor or mould
Tool, under the conditions of 35～50 DEG C, standing, after 5～8 days, obtains product.
Further, described oxidant be HAN, ammonium nitrate, hydrazine nitrate, ethanolamine nitrate, ethylenediamine nitrate,
One or more of Triethanolamine nitrate, sodium nitrate or potassium nitrate.
Further, described binding agent is polyvinyl alcohol, polyvinylamine nitrate, polyvinyl alcohol polyvinylamine copolymer
One or more of nitrate, end hydroxy butadiene, polyacrylamide or polyethylene.
Further, described stabilizer is disodium edta, 8-hydroxyquinoline, 5- aminotetrazole, 1- hydroxyl
One or more of ethylidene -1,1- di 2 ethylhexyl phosphonic acid, 2,2 '-bipyridyl, ammonium dihydrogen phosphate or ATMP.
Further, described ballistic modifying agent is 1,2,4- triazoles or 1, one of 3,5- s-triazine or two kinds.
Further, the preparation of described ethanolamine nitrate comprises the following steps：
1) at ambient temperature ethanolamine is added in reaction vessel, adds ammonium nitrate, machine while hand operated mixing
Tool stirs 12～48 hours, obtains mixture A；
The molal quantity of described ammonium nitrate and ethanolamine is equal；
Described churned mechanically speed range is 100～250 revs/min；
2) mixture A is heated to 30～50 DEG C, isothermal reaction was cooled to room temperature after 1～3 hour；
It is subsequently adding isopyknic absolute methanol, after stirring mixing, be placed in 12～48 hours in refrigerator；There is white in solution
Crystal generate, to be crystallized filter to obtain crude product completely afterwards, crude product is carried out mistake after recrystallization with the absolute methanol of two volumes
Filter, is vacuum dried under room temperature, obtains final product ethanolamine nitrate.
Further, the preparation of described ethylenediamine nitrate comprises the following steps：
1) at ambient temperature ethylenediamine is added in reaction vessel, adds ammonium nitrate, machine while hand operated mixing
Tool stirs 12～48 hours, obtains mixture B；
The molal quantity of described ammonium nitrate and ethylenediamine is equal；
Described churned mechanically speed range is 100～250 revs/min；
2) to step 1) in the mixture B that obtains, add isopyknic dehydrated alcohol, produce white precipitate I, filter,
After being dried 12～48 hours under the conditions of white precipitate I is placed in 35～60 DEG C, obtain ethylenediamine nitrate.
Further, the preparation of described polyvinylamine nitrate comprises the following steps：
1) polyvinylamine is dissolved in equipped with the container of distilled water, stirring to being completely dissolved；
Described polyvinylamine is 1 20～50 with w/v (g mL) scope of distilled water；
2) to step 1) in polyvinylamine solution in, under stirring Deca concentration be 2～6mol/L salpeter solution；
Produce white precipitate II during Deca nitric acid, obtain mixture C；
Described stir speed (S.S.) scope is 300～500 revs/min；
The volume range of described salpeter solution and polyvinylamine solution is 1 4～6；
3) by step 2) in the mixture C that obtains filtered, the white precipitate II that will obtain after filtering is placed in no water beetle
In alcohol, stand 0.5～2 hour, filter again, obtain white precipitate III；
4) at ambient temperature, by step 3) in after the white precipitate II that obtains is dried 1～2 hour, then by white precipitate
III is placed in and is dried in hot air circulation drying oven at 40 DEG C, until being dried completely；
5) by step 4) in the dried product exhibited that obtains pulverized, sieve, obtain product.
Further, the preparation of described polyvinyl alcohol polyvinylamine copolymer nitrate comprises the following steps：
1) polyvinyl alcohol and polyvinylamine are mixed according to the mol ratio of (80～90) (10～20), after mixing
Product be dissolved in methanol aqueous solution, obtain mixture D；
Described polyvinyl alcohol is 1 10～20 with w/v (g mL) scope of methanol aqueous solution；
2) to step 1) in the mixture D that obtains, add the methanol solution dissolved with the bicyclic oxygenated butadiene of 1,3-, in room
Stir 12～48 hours under the conditions of temperature, obtain mixture E；
The speed range of described stirring is 100～300 revs/min；
The concentration range of the bicyclic oxygenated butadiene methanol solution of described 1,3- is 1～20%；The bicyclic oxidation fourth of described 1,3-
The volume range of diene methanol solution and mixture D is 1 10～40；
3) add concentration to be 10%～50% salpeter solution in mixture D, the pH regulator of mixture E to 1～2 obtains
To mixture F；
4) under stirring, isopropanol is added step 3) in the mixture G that obtains, obtain white precipitate IV；
The volume range of described mixture F and isopropanol is 1 2～6；
5) at ambient temperature, by step 4) in after the white precipitate IV that obtains washs with absolute methanol, then will be heavy for white
Shallow lake IV is placed in and is dried in hot air circulation drying oven at 35～45 DEG C, after 12～48 hours, then the vacuum being placed in 30～50 DEG C
Condition is complete down to being dried；
6) by step 5) in the dried product exhibited that obtains pulverized, sieve, obtain product.
The solution have the advantages that mathematical, the present invention has advantages below：
1) use the automatically controlled solid propellant that the method for the present invention makes to flame, mechanical impact, electrostatic and abrasive feel
Degree all has the property felt immediately well；
2) using the automatically controlled solid propellant that the method for the present invention makes, there is higher energy in itself, greatly reduce outer
The offer of portion's energy, it is low to overcome traditional automatically controlled solid propellant energy itself, the high shortcoming of required ignition voltage；
3) using the automatically controlled solid propellant that the method for the present invention makes, there is automatically controlled characteristic well, that is, in applied voltage
Under conditions of can catching fire, energising continue, its combustion continuation is carried out, and power-off after-combustion can be extinguished immediately, and can by adjust
Applied voltage size is come speed when regulating and controlling its burning；
4) the automatically controlled solid propellant that the method for the present invention makes is used to be non-metal kind propellant, combustion product granule contains
Amount is few, no toxic gas such as hydrogen chloride in the gas of generation, has preferable environmental protection characteristic；
5) use the automatically controlled solid propellant preparation process is simple that the method for the present invention makes it is easy to operation, safe,
The form of different shape combustor or mould can be carried out in levelability medicine slurry state, there is good adaptability, in appearance
There is in precise tracking and gas generator good application prospect.
Brief description
Fig. 1 be polyvinyl alcohol DTG curve；
Fig. 2 is the DTG curve of polyvinylamine nitrate；
Fig. 3 is the DTG curve of polyvinyl alcohol-polyvinylamine copolymer thing nitrate；
Fig. 4 is the propellant DTG curve with polyvinyl alcohol as binding agent；
Fig. 5 is with polyvinyl alcohol-DTG curve as binding agent for the polyvinylamine copolymer thing nitrate.
Specific embodiment
With reference to embodiment, the invention will be further described, but only should not be construed the above-mentioned subject area of the present invention
It is limited to following embodiments.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and used
With means, make various replacements and change, all should include within the scope of the present invention.
Embodiment 1：
Automatically controlled solid propellant of a kind of high-performance and preparation method thereof, it is characterised in that including several formula, described is joined
Side is as shown in table 1；
Table 1
Prepare following raw material：
1) preparation of oxidant ethanolamine nitrate
1.1) at ambient temperature 24.44g (0.4mol) ethanolamine is added in reaction vessel, same in hand operated mixing
When add 32.68g (0.4mol) ammonium nitrate, mechanical agitation 48 hours, obtain mixture A；
The molal quantity of described ammonium nitrate and ethanolamine is equal；
Described churned mechanically speed range is 100 revs/min；
1.2) mixture A is heated to 35 DEG C, isothermal reaction was cooled to room temperature after 2 hours；
It is subsequently adding isopyknic absolute methanol, after stirring mixing, be placed in 24 hours in refrigerator；There is white crystal in solution
Generate, to be crystallized filter to obtain crude product completely afterwards, crude product is carried out with the absolute methanol of two volumes after recrystallization filter, room
Temperature is lower to be vacuum dried, and obtains final product ethanolamine nitrate.
2) preparation of oxidant ethylenediamine nitrate
2.1) at ambient temperature 18.12g (0.6mol) ethylenediamine is added in 250ml reaction vessel, is stirring manually
Add ammonium nitrate, mechanical agitation 24 hours while mixing, obtain mixture B；
The molal quantity of described ammonium nitrate and ethylenediamine is equal；
Described churned mechanically speed range is 250 revs/min；
2.2) to step 2.1) in the mixture B that obtains, add isopyknic dehydrated alcohol, produce white precipitate I, mistake
Filter, after being dried 48 hours, obtains ethylenediamine nitrate under the conditions of white precipitate I is placed in 50 DEG C.
3) preparation of adhesive polyethylene amine nitrate
3.1) 20.0g polyvinylamine is dissolved in the container equipped with 600mL distilled water, stirs to being completely dissolved；
3.2) to step 3.1) in polyvinylamine solution in, under stirring Deca 200ml concentration be 4mol/L nitre
Acid solution；Produce white precipitate II during Deca nitric acid, obtain mixture C；
Described stir speed (S.S.) scope is 300 revs/min；
3.3) by step 3.2) in the mixture C that obtains filtered, the white precipitate II that will obtain after filtering is placed in
In 160mL absolute methanol, stand 2 hours, filter again, obtain white precipitate III；
3.4) at ambient temperature, by step 3.3) in after the white precipitate II that obtains is dried 2 hours, then by white precipitate
III is placed in and is dried in hot air circulation drying oven at 40 DEG C, until being dried completely；
3.5) by step 3.4) in the dried product exhibited that obtains pulverized, sieve, obtain product.
4) preparation of adhesive polyethylene alcohol polyvinylamine copolymer nitrate
4.1) 10g polyvinyl alcohol and polyvinylamine are mixed according to 85 15 mol ratio, will be molten for mixed product
(volume ratio in 200ml methanol aqueous solution：Methanol/water=35/65), obtain mixture D；
4.2) to step 4.1) in the mixture D that obtains, add 5ml dissolved with the bicyclic oxygenated butadiene of 1,3- of 0.5g
Methanol solution, stirs 48 hours at ambient temperature, obtains mixture E；
The speed range of described stirring is 300 revs/min；
4.3) add concentration to be 35% salpeter solution in mixture D, the pH regulator of mixture E to 1～2 is mixed
Compound F；
4.4) under stirring, 1L isopropanol is added step 4.3) in the mixture G that obtains, obtain white precipitate
Ⅳ；
4.5) at ambient temperature, by step 4.4) in after the white precipitate IV that obtains washs with 50ml absolute methanol, then
White precipitate IV is placed at 40 DEG C and is dried in hot air circulation drying oven, after 24 hours, then the vacuum condition being placed in 50 DEG C
Complete down to being dried；
4.6) by step 4.5) in the dried product exhibited that obtains pulverized, sieve, obtain product.
Raw material in load weighted table 1 is followed the steps below：
1) at ambient temperature, oxidant, stabilizer, binding agent, cross-linking agent, ballistic modifying agent are added sequentially to react
In device, vacuum stirring, obtain the medicine slurry stirring；
Described stir speed (S.S.) scope is 380 revs/min；Described mixing time scope is 0.4 hour；
2) by step 1) in the medicine slurry stirring that obtains under normal pressure or vacuum condition, irrigate to combustor or mould
Tool, under the conditions of 50 DEG C, standing, after 8 days, obtains product.
Embodiment 2：
Automatically controlled solid propellant of a kind of high-performance and preparation method thereof, it is characterised in that including several formula, described is joined
Side is as shown in table 2；
Table 2
Raw material in load weighted table 2 is followed the steps below：
1) at ambient temperature, oxidant, stabilizer, binding agent, cross-linking agent, ballistic modifying agent are added sequentially to react
In device, vacuum stirring, obtain the medicine slurry stirring；
Described stir speed (S.S.) scope is 100 revs/min；Described mixing time scope is 3 hours；
2) by step 1) in the medicine slurry stirring that obtains under normal pressure or vacuum condition, irrigate to combustor or mould
Tool, under the conditions of 50 DEG C, standing, after 5 days, obtains product.
Embodiment 3：
Automatically controlled solid propellant of a kind of high-performance and preparation method thereof, it is characterised in that including several formula, described is joined
Side is as shown in table 3；
Table 3
1) preparation of oxidant ethanolamine nitrate
1.1) at ambient temperature 12.22g (0.2mol) ethanolamine is added in reaction vessel, same in hand operated mixing
When add 16.34g (0.2mol) ammonium nitrate, mechanical agitation 48 hours, obtain mixture A；
The molal quantity of described ammonium nitrate and ethanolamine is equal；
Described churned mechanically speed range is 250 revs/min；
1.2) mixture A is heated to 40 DEG C, isothermal reaction was cooled to room temperature after 2 hours；
It is subsequently adding isopyknic absolute methanol, after stirring mixing, be placed in 48 hours in refrigerator；There is white crystal in solution
Generate, to be crystallized filter to obtain crude product completely afterwards, crude product is carried out with the absolute methanol of two volumes after recrystallization filter, room
Temperature is lower to be vacuum dried, and obtains final product ethanolamine nitrate.
2) preparation of adhesive polyethylene alcohol polyvinylamine copolymer nitrate
2.1) 10g polyvinyl alcohol and polyvinylamine are mixed according to 88 12 mol ratio, will be molten for mixed product
(volume ratio in 200ml methanol aqueous solution：Methanol/water=35/65), obtain mixture D；
2.2) to step 2.1) in the mixture D that obtains, add 5ml dissolved with the bicyclic oxygenated butadiene of 1,3- of 0.3g
Methanol solution, stirs 36 hours at ambient temperature, obtains mixture E；
The speed range of described stirring is 300 revs/min；
2.3) add concentration to be 35% salpeter solution in mixture D, the pH regulator of mixture E to 1～2 is mixed
Compound F；
2.4) under stirring, 1L isopropanol is added step 2.3) in the mixture G that obtains, obtain white precipitate
Ⅳ；
2.5) at ambient temperature, by step 2.4) in after the white precipitate IV that obtains washs with 50ml absolute methanol, then
White precipitate IV is placed at 40 DEG C and is dried in hot air circulation drying oven, after 24 hours, then the vacuum condition being placed in 50 DEG C
Complete down to being dried；
2.6) by step 2.5) in the dried product exhibited that obtains pulverized, sieve, obtain product.
Raw material in load weighted table 3 is followed the steps below：
1) at ambient temperature, oxidant, stabilizer, binding agent, cross-linking agent, ballistic modifying agent are added sequentially to react
In device, vacuum stirring, obtain the medicine slurry stirring；
Described stir speed (S.S.) scope is 100 revs/min；Described mixing time scope is 3 hours；
2) by step 1) in the medicine slurry stirring that obtains under normal pressure or vacuum condition, irrigate to combustor or mould
Tool, under the conditions of 50 DEG C, standing, after 8 days, obtains product.
Embodiment 4：
Automatically controlled solid propellant of a kind of high-performance and preparation method thereof, it is characterised in that including several formula, described is joined
Side is as shown in table 4；
Table 4
1) preparation of oxidant ethylenediamine nitrate
1.1) at ambient temperature 9.06g (0.3mol) ethylenediamine is added in 250ml reaction vessel, in hand operated mixing
While add 24.59g (0.3mol) ammonium nitrate, mechanical agitation 48 hours, obtain mixture B；
Described churned mechanically speed range is 250 revs/min；
1.2) to step 1.1) in the mixture B that obtains, add isopyknic dehydrated alcohol, produce white precipitate I, mistake
Filter, after being dried 48 hours, obtains ethylenediamine nitrate under the conditions of white precipitate I is placed in 50 DEG C.
2) preparation of adhesive polyethylene alcohol polyvinylamine copolymer nitrate
2.1) 10g polyvinyl alcohol and polyvinylamine are mixed according to 90 10 mol ratio, will be molten for mixed product
(volume ratio in 200ml methanol aqueous solution：Methanol/water=35/65), obtain mixture D；
2.2) to step 2.1) in the mixture D that obtains, add 5ml dissolved with the bicyclic oxygenated butadiene of 1,3- of 1.0g
Methanol solution, stirs 48 hours at ambient temperature, obtains mixture E；
The speed range of described stirring is 300 revs/min；
2.3) add concentration to be 35% salpeter solution in mixture D, the pH regulator of mixture E to 1～2 is mixed
Compound F；
2.4) under stirring, 1L isopropanol is added step 2.3) in the mixture G that obtains, obtain white precipitate
Ⅳ；
2.5) at ambient temperature, by step 2.4) in after the white precipitate IV that obtains washs with 50ml absolute methanol, then
White precipitate IV is placed at 40 DEG C and is dried in hot air circulation drying oven, after 24 hours, then the vacuum condition being placed in 50 DEG C
Complete down to being dried；
2.6) by step 2.5) in the dried product exhibited that obtains pulverized, sieve, obtain product.
Raw material in load weighted table 4 is followed the steps below：
1) at ambient temperature, oxidant, stabilizer, binding agent, cross-linking agent, ballistic modifying agent are added sequentially to react
In device, vacuum stirring, obtain the medicine slurry stirring；
Described stir speed (S.S.) scope is 100 revs/min；Described mixing time scope is 3 hours；
2) by step 1) in the medicine slurry stirring that obtains under normal pressure or vacuum condition, irrigate to combustor or mould
Tool, under the conditions of 50 DEG C, standing, after 8 days, obtains product.
Claims (9)
1. automatically controlled solid propellant of a kind of high-performance and preparation method thereof is it is characterised in that include following raw material and its weight portion
Number：
Load weighted above-mentioned raw materials are followed the steps below：
1) at ambient temperature, oxidant, stabilizer, binding agent, cross-linking agent, ballistic modifying agent are added sequentially to reactor
In, vacuum stirring, obtain the medicine slurry stirring；
Described stir speed (S.S.) scope is 100～380 revs/min；Described mixing time scope is 0.4～3 hour；
2) by step 1) in the medicine slurry stirring that obtains under normal pressure or vacuum condition, irrigate to combustor or mould,
Under the conditions of 35～50 DEG C, standing, after 5～8 days, obtains product.
2. automatically controlled solid propellant of a kind of high-performance according to claim 1 and preparation method thereof it is characterised in that：Described
Oxidant is HAN, ammonium nitrate, hydrazine nitrate, ethanolamine nitrate, ethylenediamine nitrate, Triethanolamine nitrate, nitric acid
One or more of sodium or potassium nitrate.
3. automatically controlled solid propellant of a kind of high-performance according to claim 1 and preparation method thereof it is characterised in that：Described
Binding agent be polyvinyl alcohol, polyvinylamine nitrate, polyvinyl alcohol polyvinylamine copolymer nitrate, terminal hydroxy group polybutadiene
One or more of alkene, polyacrylamide or polyethylene.
4. automatically controlled solid propellant of a kind of high-performance according to claim 1 and preparation method thereof it is characterised in that：Described
Stabilizer be disodium edta, 8-hydroxyquinoline, 5- aminotetrazole, 1- hydroxy ethylene -1,1- di 2 ethylhexyl phosphonic acid, 2,
One or more of 2 '-bipyridyl, ammonium dihydrogen phosphate or ATMP.
5. automatically controlled solid propellant of a kind of high-performance according to claim 1 and preparation method thereof it is characterised in that：Described
Ballistic modifying agent be one of 1,2,4- triazole or 1,3,5- s-triazine or two kinds.
6. automatically controlled solid propellant of a kind of high-performance according to claim 2 and preparation method thereof is it is characterised in that described
The preparation of ethanolamine nitrate comprise the following steps：
1) at ambient temperature ethanolamine is added in reaction vessel, adds ammonium nitrate while hand operated mixing, machinery stirs
Mix 12～48 hours, obtain mixture A；
The molal quantity of described ammonium nitrate and ethanolamine is equal；
Described churned mechanically speed range is 100～250 revs/min；
2) mixture A is heated to 30～50 DEG C, isothermal reaction was cooled to room temperature after 1～3 hour；
It is subsequently adding isopyknic absolute methanol, after stirring mixing, be placed in 12～48 hours in refrigerator；There is white crystal in solution
Generate, to be crystallized filter to obtain crude product completely afterwards, crude product is carried out with the absolute methanol of two volumes after recrystallization filter, room
Temperature is lower to be vacuum dried, and obtains final product ethanolamine nitrate.
7. automatically controlled solid propellant of a kind of high-performance according to claim 2 and preparation method thereof is it is characterised in that described
The preparation of ethylenediamine nitrate comprises the following steps：
1) at ambient temperature ethylenediamine is added in reaction vessel, adds ammonium nitrate while hand operated mixing, machinery stirs
Mix 12～48 hours, obtain mixture B；
The molal quantity of described ammonium nitrate and ethylenediamine is equal；
Described churned mechanically speed range is 100～250 revs/min；
2) to step 1) in the mixture B that obtains, add isopyknic dehydrated alcohol, produce white precipitate I, filter, will be white
After color precipitation I is dried 12～48 hours under the conditions of being placed in 35～60 DEG C, obtain ethylenediamine nitrate.
8. automatically controlled solid propellant of a kind of high-performance according to claim 3 and preparation method thereof it is characterised in that：Described
The preparation of polyvinylamine nitrate comprises the following steps：
1) polyvinylamine is dissolved in equipped with the container of distilled water, stirring to being completely dissolved；
Described polyvinylamine is 1 20～50 with w/v (g mL) scope of distilled water；
2) to step 1) in polyvinylamine solution in, under stirring Deca concentration be 2～6mol/L salpeter solution；Dripping
Plus produce white precipitate II during nitric acid, obtain mixture C；
Described stir speed (S.S.) scope is 300～500 revs/min；
The volume range of described salpeter solution and polyvinylamine solution is 1 4～6；
3) by step 2) in the mixture C that obtains filtered, the white precipitate II that will obtain after filtering is placed in absolute methanol,
Standing 0.5～2 hour, filters again, obtains white precipitate III；
4) at ambient temperature, by step 3) in after the white precipitate II that obtains is dried 1～2 hour, then white precipitate III is put
It is dried in hot air circulation drying oven at 40 DEG C, until being dried completely；
5) by step 4) in the dried product exhibited that obtains pulverized, sieve, obtain product.
9. automatically controlled solid propellant of a kind of high-performance according to claim 3 and preparation method thereof is it is characterised in that described
The preparation of polyvinyl alcohol polyvinylamine copolymer nitrate comprises the following steps：
1) polyvinyl alcohol and polyvinylamine are mixed according to the mol ratio of (80～90) (10～20), by mixed product
Thing is dissolved in methanol aqueous solution, obtains mixture D；
Described polyvinyl alcohol is 1 10～20 with w/v (g mL) scope of methanol aqueous solution；
2) to step 1) in the mixture D that obtains, add the methanol solution dissolved with the bicyclic oxygenated butadiene of 1,3-, in room temperature bar
Stir 12～48 hours under part, obtain mixture E；
The speed range of described stirring is 100～300 revs/min；
The concentration range of the bicyclic oxygenated butadiene methanol solution of described 1,3- is 1～20%；The bicyclic oxygenated butadiene of described 1,3-
The volume range of methanol solution and mixture D is 1 10～40；
3) add concentration to be 10%～50% salpeter solution in mixture D, the pH regulator of mixture E to 1～2 is mixed
Compound F；
4) under stirring, isopropanol is added step 3) in the mixture G that obtains, obtain white precipitate IV；
The volume range of described mixture F and isopropanol is 1 2～6；
5) at ambient temperature, by step 4) in after the white precipitate IV that obtains washs with absolute methanol, then by white precipitate IV
It is placed in and be dried in hot air circulation drying oven at 35～45 DEG C, after 12～48 hours, then the vacuum condition being placed in 30～50 DEG C
Complete down to being dried；
6) by step 5) in the dried product exhibited that obtains pulverized, sieve, obtain product.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106905091A (en) * | 2017-03-15 | 2017-06-30 | 重庆大学 | It is a kind of based on perchlorate can automatically controlled burning solid propellant and preparation method thereof |
| CN109851457A (en) * | 2019-03-22 | 2019-06-07 | 湖北航天化学技术研究所 | A kind of automatically controlled solid propellant and preparation method thereof containing metal fuel |
| CN109942356A (en) * | 2019-03-29 | 2019-06-28 | 湖北航天化学技术研究所 | A kind of automatically controlled solid propellant and preparation method thereof |
| CN110054537A (en) * | 2019-03-22 | 2019-07-26 | 湖北航天化学技术研究所 | A kind of automatically controlled solid propellant and preparation method thereof |
| CN110759800A (en) * | 2018-07-27 | 2020-02-07 | 南京理工大学 | High-energy high-mechanical-property electronic control solid propellant |
| CN112979395A (en) * | 2021-04-12 | 2021-06-18 | 中北大学 | Gas generating agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106905091A (en) * | 2017-03-15 | 2017-06-30 | 重庆大学 | It is a kind of based on perchlorate can automatically controlled burning solid propellant and preparation method thereof |
| CN106905091B (en) * | 2017-03-15 | 2019-05-07 | 重庆大学 | It is a kind of based on perchlorate can automatically controlled burning solid propellant and preparation method thereof |
| CN110759800A (en) * | 2018-07-27 | 2020-02-07 | 南京理工大学 | High-energy high-mechanical-property electronic control solid propellant |
| CN109851457A (en) * | 2019-03-22 | 2019-06-07 | 湖北航天化学技术研究所 | A kind of automatically controlled solid propellant and preparation method thereof containing metal fuel |
| CN110054537A (en) * | 2019-03-22 | 2019-07-26 | 湖北航天化学技术研究所 | A kind of automatically controlled solid propellant and preparation method thereof |
| CN109942356A (en) * | 2019-03-29 | 2019-06-28 | 湖北航天化学技术研究所 | A kind of automatically controlled solid propellant and preparation method thereof |
| CN112979395A (en) * | 2021-04-12 | 2021-06-18 | 中北大学 | Gas generating agent and preparation method thereof |
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