CN105130716A - Preparation method of 602 little smoke agent through mechanical mixing - Google Patents
Preparation method of 602 little smoke agent through mechanical mixing Download PDFInfo
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- CN105130716A CN105130716A CN201510471970.4A CN201510471970A CN105130716A CN 105130716 A CN105130716 A CN 105130716A CN 201510471970 A CN201510471970 A CN 201510471970A CN 105130716 A CN105130716 A CN 105130716A
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Abstract
The invention discloses a preparation method of 602 little smoke agent through mechanical mixing. The preparation method comprises the following steps: processing raw materials, selecting raw materials, weighing raw materials, preparing a nitro-cotton adhesive, dry-mixing a tertiary mixture, controlling the grinding time, wet-drying the tertiary mixture, increasing density, granulating, polishing, drying, batching, mixing, and screening qualified particles. The 602 little smoke agent is composed of 78.5 to 81.5% of lead chromate, 14 to 16% of antimony sulfide, 4.5 to 5.5% of potassium perchlorate, and 0.3 to 0.7% of weak cotton additive. The particle size of the agent is in a range of 9 pores/cm (screen underflow) and 19 pores/cm (oversize product). By adjusting the raw materials and dry-mixing and grinding time, the agent can meet the special time requirements of grenade-6 fuze (5.5 to 9 seconds), 83 artificial rainfall fuze (13 to 17 seconds), 07 artificial rainfall fuze (12 to 17 seconds) and the like. The provided agent can be mixed uniformly, the reliability and stability of the agent are high, and the agent is safe to manufacture.
Description
Technical field
The invention belongs to many component mixing Loading Materials for Initiating Explosive Devices manufacturing technologies, be specifically related to a kind of method that mechanically mixing prepares the micro-cigarette medicine of many components.
Background technology
602 micro-cigarette medicine production process technical sophistications, difficulty are large, and key control technology is by production technology experience for many years.This technology can because of the density of each component, granularity, be dry mixed polishing time, wet mixing time, rush the difference of density hours, operator, affect the reliability and stability of powder performance, cause a large amount of manpower and materials wastes.
Summary of the invention
The object of the invention is to the shortcoming for 602 micro-cigarette medicine production technique, a kind of 602 micro-cigarette medicine pharmaceutical technique methods are provided, make it have following advantage: medicament mixes, medicament unfailing performance and agent stability can improve.
The present invention relates to the method for the micro-cigarette medicine of the many components of a kind of mechanically mixing, be prepared according to the following steps:
The first step: raw-material process
1, the process of potassium perchlorate
Take chemical reagent potassium perchlorate 10kg, put into vibration mill, add the copper ball 60kg of ∮ 10 ~ 20mm, carry out vibration polishing and take out after 3 ~ 10 hours, under being sieved by 60 ~ 65 holes/cm bolting silk is qualified particle.Dried by qualified particle, moisture content is not more than 0.15%, for subsequent use for chronological classification by different polishing after drying.
2, the process of sulfuration ladder
Take the sulfuration ladder 10kg after refining pulverizing, put into vibration mill, add the steel ball 60kg of ∮ 15 ~ 25mm, carry out vibration polishing and take out after 5 ~ 20 hours, under being sieved by 60 ~ 65 holes/cm bolting silk is qualified particle.Qualified particle oven dry is not more than 0.2% to moisture content.Survey the specific surface area of sulfuration ladder, specific surface area difference is less than 500g/cm
2to mix be one barrel.For subsequent use by different specific surface area classification.
3, the process of lead chromate
Dry chemical reagent lead chromate and be not more than 0.2% to moisture content, survey specific surface area for subsequent use.
4, the washing of nitro-cotton
Get about 2kg nitro-cotton to load in calico pocket, put into the basin filling distilled water and clean, soak, repeat 3 ~ 4 times.After washing with alcohol-pickled dehydration once, dehydration post-drying be not more than 1% to moisture content.
Second step: raw-material selection
Starting material specific surface area is larger, and the finished product medicament time is shorter, thus chooses corresponding starting material by product requirement.Because the specific surface area of potassium perchlorate, sulfuration ladder can process on request, and lead chromate controls by supplied materials, so first choose the suitable lead chromate of specific surface area according to product requirement, then join get corresponding sulfuration ladder, potassium perchlorate makes sample, carrys out selection material according to the loose sintering fruit of sample.(all loose burning time is the loose sintering fruit of 83 people's rain batch pans herein.)
Raw-material specific surface area needed for 602 micro-cigarette medicine different sortses, the sample burning time approximate range that falls apart is as follows:
3rd step: raw-materially to take
Calculate by a small quantities of 40kg, lead chromate is containing 80%, and antimony sulfide is containing 15%, and potassium perchlorate, containing 5%, takes the starting material lead chromate 32kg chosen, sulfuration ladder 6kg, potassium perchlorate 2kg.
4th step: the preparation of nitro-cotton tackiness agent
Take the nitro-cotton 260g after washing and drying to put into and dissolve bucket, separately get chemical reagent acetone (8000 ~ 10000) ml pour in bucket stir make it to dissolve completely for subsequent use.
5th step: be dry mixed tertiary mixture
Add the copper ball 50kg of ∮ (10 ~ 20) mm in vibrations mill, take 1 small quantities of medicament is added in vibration mill, polishing (3 ~ 15) h.The time of sample grasp medicine, stability and polishing time is done in vibration processes.The required sample time approximate range controlled of 602 micro-cigarette medicine different sorts products is as follows:
| Kind | Sample is fallen apart burning time (s) |
| 602 micro-cigarette medicines (pomegranate-6 fuse is used) | 13.5～14.2 |
| 602 micro-cigarette medicines (83 people's rain fuses are used) | 14.7～15.5 |
| 602 micro-cigarette medicines (07 people's rain fuse is used) | 16.5～17.5 |
6th step: wet mixing tertiary mixture
By the nitrocellulose solution prepared, pouring in post-type mixer, adding in stirrer by being dry mixed the tertiary mixture of having polished, drive to stir 3.5h.
7th step: granulation
The tertiary mixture getting wet mixing good is about 8kg, puts into enamel basin and is kneaded into dry thick shape, be placed on rush density machine pot in, punching press 7 ~ 15 minutes, then be placed on tablets press and carry out granulation by double-deck 5 holes/cm copper screen cloth.Be top sieve with 9 holes/cm bolting silk after granulation, 19 holes/cm bolting silk is that the vibratory screening apparatus of lower sieve screens qualified particle.
8th step: light medicine
Every small quantities of qualified particle is about 40kg to pour in light medicine drum, light medicine is about 30min.
9th step: dry
By micro-cigarette medicine good for light, spread in drip pan, its thickness is 10 ~ 15mm, drip pan is put into baking cabinet and dries, and baking medicine temperature 65 ~ 75 DEG C, is dried to moisture content and volatile content is less than 0.15%.
Tenth step: batching is mixed greatly
Large mixed do not allow from the examination average burning time in bulk to exceed each in small batches ± 0.8 second, respectively do not allow from examination fluctuation range combustion time in bulk to exceed in small batches ± 0.1 second.Poured into by each small quantities of medicine mixed greatly in large mixed cylinder simultaneously, drive mixed greatly, once mixed greatly amount is 50 ~ 250 kilograms, mixed 30 ~ 50 minutes greatly.
11 step: screen qualified particle
Qualified particle size is between 9 holes/cm bolting silk screen underflow and 19 holes/cm bolting silk screen overflow.
The invention belongs to many components mechanically mixing Loading Materials for Initiating Explosive Devices manufacturing technology, its advantage is as follows:
(1) the present invention effectively ensure that many components medicament mixing uniformity, improves medicament unfailing performance and stability.
(2) the present invention can produce qualified medicament according to the requirement of different 602 micro-cigarette pharmacopoeia classes.
Embodiment:
The present invention relates to the method for the micro-cigarette medicine of the many components of a kind of mechanically mixing, be prepared according to the following steps:
The first step: raw-material process
1, the process of potassium perchlorate
Take chemical reagent potassium perchlorate 10kg, put into vibration mill, add the copper ball 60kg of ∮ 10 ~ 20mm, carry out vibration polishing to take out after 3 ~ 10 hours, under being sieved by 60 ~ 65 holes/cm bolting silk is qualified particle, dried by qualified particle, moisture content is not more than 0.15%, for subsequent use for chronological classification by different polishing after drying;
2, the process of sulfuration ladder
Take the sulfuration ladder 10kg after refining pulverizing, put into vibration mill, add the steel ball 60kg of ∮ 15 ~ 25mm, carry out vibration polishing and take out after 5 ~ 20 hours, under being sieved by 60 ~ 65 holes //cm bolting silk is qualified particle.Qualified particle is dried and is not more than 0.2% to moisture content, survey the specific surface area of sulfuration ladder, specific surface area difference is less than 500g/cm
2to mix be one barrel, for subsequent use by different specific surface area classification;
3, the process of lead chromate
Dry chemical reagent lead chromate and be not more than 0.2% to moisture content, survey specific surface area for subsequent use;
4, the washing of nitro-cotton
Get about 2kg nitro-cotton to load in calico pocket, put into the basin filling distilled water and clean, soak, repeat 3 ~ 4 times.After washing with alcohol-pickled dehydration once, dehydration post-drying be not more than 1% to moisture content;
Second step: raw-material selection
Starting material specific surface area is larger, and the finished product medicament time is shorter, thus chooses corresponding starting material by product requirement.Because the specific surface area of potassium perchlorate, sulfuration ladder can process on request, and lead chromate controls by supplied materials, so first choose the suitable lead chromate of specific surface area according to product requirement, then join get corresponding sulfuration ladder, potassium perchlorate makes sample, carrys out selection material according to the loose sintering fruit of sample;
Raw-material specific surface area needed for 602 micro-cigarette medicine different sortses, the sample burning time approximate range that falls apart is as follows:
3rd step: raw-materially to take
Calculate by a small quantities of 40kg, lead chromate is containing 80%, and antimony sulfide is containing 15%, and potassium perchlorate, containing 5%, takes the starting material lead chromate 32kg chosen, sulfuration ladder 6kg, potassium perchlorate 2kg '
4th step: the preparation of nitro-cotton tackiness agent
Take the nitro-cotton 260g after washing and drying to put into and dissolve bucket, separately get chemical reagent acetone 8000ml ~ 10000ml pour in bucket stir make it to dissolve completely for subsequent use;
5th step: be dry mixed tertiary mixture
The copper ball 50kg of ∮ 10mm ~ 20mm is added in vibrations mill, the medicament taken is added in vibration mill, polishing 3 ~ 15h, does the time of sample grasp medicine, stability and polishing time in vibration processes, 602 micro-cigarette medicine variant productions required control sample time approximate range is as follows:
| Kind | Sample is fallen apart burning time (s) |
| 602 micro-cigarette medicines (pomegranate-6 fuse is used) | 13.5～14.2 |
| 602 micro-cigarette medicines (83 people's rain fuses are used) | 14.7～15.5 |
| 602 micro-cigarette medicines (07 people's rain fuse is used) | 16.5～17.5 |
6th step: wet mixing tertiary mixture
By the nitrocellulose solution prepared, pouring in post-type mixer, adding in stirrer by being dry mixed the tertiary mixture of having polished, drive to stir 3.5h;
7th step: granulation
The tertiary mixture getting wet mixing good is about 8kg, puts into enamel basin and is kneaded into dry thick shape, be placed on rush density machine pot in, punching press 7 ~ 15 minutes, then be placed on tablets press and carry out granulation by double-deck 5 holes/cm copper screen cloth; Be top sieve with 9 holes/cm bolting silk after granulation, 19 holes/cm bolting silk is that the vibratory screening apparatus of lower sieve screens qualified particle;
8th step: light medicine
Every small quantities of qualified particle is about 40kg to pour in light medicine drum, light medicine is about 30min;
9th step: dry
By micro-cigarette medicine good for light, spread in drip pan, its thickness is 10 ~ 15mm, drip pan is put into baking cabinet and dries, and baking medicine temperature 65-75 DEG C, is dried to moisture content and volatile content is less than 0.15%;
Tenth step: batching is mixed greatly
Large mixed do not allow from the examination average burning time in bulk to exceed each in small batches ± 0.8 second, respectively do not allow from examination fluctuation range combustion time in bulk to exceed in small batches ± 0.1 second.Poured into by each small quantities of medicine mixed greatly in large mixed cylinder simultaneously, drive mixed greatly, once mixed greatly amount is 50 ~ 250 kilograms, mixed 30 ~ 50 minutes greatly;
11 step: screen qualified particle
Qualified particle size is between 9 holes/cm bolting silk screen underflow and 19 holes/cm bolting silk screen overflow;
The physico-chemical analysis of many components 602 micro-cigarette medicine should meet following requirement:
Combustionproperty requires to meet following requirement:
Embodiment 1:
Produce 602 micro-cigarette medicine 50kg pomegranate-6 fuse (5.5 ~ 9) s
The first step: raw-material process
1, the process of potassium perchlorate
Take chemical reagent potassium perchlorate 10kg, put into vibration mill, add the copper ball 60kg of ∮ 10 ~ 20mm, carry out vibration polishing and take out after 3 ~ 10 hours, under being sieved by 60 ~ 65 holes/cm bolting silk is qualified particle.Dried by qualified particle, moisture content is not more than 0.15%, for subsequent use for chronological classification by different polishing after drying;
2, the process of sulfuration ladder
Take the sulfuration ladder 10kg after refining pulverizing, put into vibration mill, add the steel ball 60kg of ∮ 15 ~ 25mm, carry out vibration polishing and take out after 5 ~ 20 hours, under being sieved by 60 ~ 65 holes/cm bolting silk is qualified particle.Qualified particle oven dry is not more than 0.2% to moisture content; Survey the specific surface area of sulfuration ladder, specific surface area difference is less than 500g/cm
2to mix be one barrel, for subsequent use by different specific surface area classification;
3, the process of lead chromate
Dry chemical reagent lead chromate and be not more than 0.2% to moisture content, survey specific surface area for subsequent use;
4, the washing of nitro-cotton
Get about 2kg nitro-cotton to load in calico pocket, put into the basin filling distilled water and clean, soak, repeat 3 ~ 4 times.After washing with alcohol-pickled dehydration once, dehydration post-drying be not more than 1% to moisture content;
Second step: raw-material selection
Be 2824g/cm according to Production requirement Selection radio surface-area
2lead chromate, sample before feeding intake from different specific surface area sulfuration ladder, potassium perchlorate, its result is as follows:
| Sequence number | Lead chromate (g/cm 2) | Antimony sulfide (g/cm 2) | Potassium perchlorate | Sample is fallen apart burning time (s) |
| 1 | 2824 | 4300 | The polishing time 6 (h) | 16.2 |
| 2 | 2824 | 5000 | The polishing time 6 (h) | 15.9 |
| 3 | 2824 | 5700 | The polishing time 6 (h) | 15.50 |
According to above result, 1,2 is all passable, but No. 2 times are better, and thus Selection radio surface-area is 2824g/cm
2lead chromate, specific surface area is 5000g/cm
2sulfuration ladder, the potassium perchlorate of polishing time 6 (h) feeds intake production.
3rd step: raw-materially to take
By a small quantities of 40kg, take the starting material lead chromate 32kg chosen, sulfuration ladder 6kg, potassium perchlorate 2kg, totally 2 small quantities of.
4th step: the preparation of nitro-cotton tackiness agent
Take the nitro-cotton 260g after washing and drying to put into and dissolve bucket, separately get acetone 10000ml and pour in bucket to stir and make it to dissolve completely for subsequent use, prepare two samples.
5th step: be dry mixed tertiary mixture
Add the copper ball 50kg of ∮ (10 ~ 20) mm in vibrations mill, the medicament taken is added in vibration mill and polishes.Its polishing time and sample changing conditions as follows:
| Polishing time (h) | Loose burning time (s) | Average loose burning time (s) |
| 3 | 15.2、14.4、14.8、14.1、14.6、X、14.8 | 14.65 |
| 7 | 14.5、14.2、14.3、14.7、14.1、14.3、13.7 | 14.26 |
| 10 | 13.8、13.9、14.5、13.9、14.4、13.5、14 | 14 |
Find out from above result, polish and within 3 hours, have misfire situation to occur, 7 hours, 10 hours more stable, the 10 hours medicament time of polishing is more suitable, and thus each polishing time in small batches of this batch of medicament is 6 hours.
6th step: wet mixing tertiary mixture
By the nitrocellulose solution prepared, pouring in post-type mixer, adding in stirrer by being dry mixed the tertiary mixture of having polished, drive to stir 3.5h.
7th step: granulation
The tertiary mixture getting wet mixing good is about 8kg, puts into enamel basin and is kneaded into dry thick shape, be placed on rush density machine pot in, punching press 10 minutes, then be placed on tablets press and carry out granulation by double-deck 5 holes/cm copper screen cloth.Be top sieve with 9 holes/cm bolting silk after qualified granulation, 19 holes/cm bolting silk is that the vibratory screening apparatus of lower sieve screens qualified particle.
8th step: light medicine
Every small quantities of qualified particle being about 40kg pours in light medicine drum, light medicine about 30 minutes.
9th step: dry
By micro-cigarette medicine good for light, spread in drip pan, its thickness is 10 ~ 15mm, drip pan is put into baking cabinet and dries, and baking medicine temperature 65-75 DEG C, is dried to moisture content and volatile content is less than 0.15%.
Tenth step: batching is mixed greatly
Large mixed do not allow from the examination average burning time in bulk to exceed each in small batches ± 0.8 second, respectively do not allow from examination fluctuation range combustion time in bulk to exceed in small batches ± 0.1 second.
By above step continuous dosing 2, it is as follows from test result:
| Sequence number | Loose burning time (s) | Mean time (s) | Fluctuation range (s) |
| 1 | 13.4、14.2、14、14.4、13.8、14、14.3、13.5 | 13.95 | ±0.55 |
| 2 | 13.8、13.8、13.1、13.7、13、13.7、14.1、13.9 | 13.64 | ±0.64 |
1,2 all meet large mixed requirements in small batches, are total to about 70kg in small batches and pour in large mixed cylinder simultaneously, drive mixed greatly, large mixed 40 minutes by 1,2.
11 step: screen qualified particle
Qualified particle size is between 9 holes/cm bolting silk screen underflow and 19 holes/cm bolting silk screen overflow.
Many components 602 micro-cigarette pharmacology fractional analysis result is:
Combustionproperty result is:
Physico-chemical analysis and combustionproperty all meet the demands.
Embodiment 2;
Produce 602 micro-cigarette medicine 200kg83 people rain fuse (13 ~ 17) s
The first step: raw-material process
1, the process of potassium perchlorate
Take chemical reagent potassium perchlorate 10kg, put into vibration mill, add the copper ball 60kg of ∮ 10 ~ 20mm, carry out vibration polishing and take out after 3 ~ 10 hours, under being sieved by 60 ~ 65 holes/cm bolting silk is qualified particle.Dried by qualified particle, moisture content is not more than 0.15%, for subsequent use for chronological classification by different polishing after drying.
2, the process of sulfuration ladder
Take the sulfuration ladder 10kg after refining pulverizing, put into vibration mill, add the steel ball 60kg of ∮ 15 ~ 25mm, carry out vibration polishing and take out after 5 ~ 20 hours, under being sieved by 60 ~ 65 holes/cm bolting silk is qualified particle.Qualified particle oven dry is not more than 0.2% to moisture content.Survey the specific surface area of sulfuration ladder, specific surface area difference is less than 500g/cm
2to mix be one barrel.For subsequent use by different specific surface area classification.
3, the process of lead chromate
Dry chemical reagent lead chromate and be not more than 0.2% to moisture content, survey specific surface area for subsequent use.
4, the washing of nitro-cotton
Get about 2kg nitro-cotton to load in calico pocket, put into the basin filling distilled water and clean, soak, repeat 3 ~ 4 times.After washing with alcohol-pickled dehydration once, dehydration post-drying be not more than 1% to moisture content.
Second step: raw-material selection
Be 2391g/cm according to Production requirement Selection radio surface-area
2lead chromate, sample before feeding intake from different specific surface area sulfuration ladder, potassium perchlorate, its result is as follows:
| Sequence number | Lead chromate (g/cm 2) | Antimony sulfide (g/cm 2) | Potassium perchlorate | Sample is fallen apart burning time (s) |
| 1 | 2391 | 3500 | The polishing time 6 (h) | 19.1 |
| 2 | 2391 | 4300 | The polishing time 6 (h) | 18.3 |
| 3 | 2391 | 5000 | The polishing time 6 (h) | 17.5 |
According to above result, 2,3 is all passable, and No. 2 times are better, and thus Selection radio surface-area is 2391g/cm
2lead chromate, specific surface area is 4300g/cm
2sulfuration ladder, the potassium perchlorate of polishing time 6 (h) feeds intake production.
3rd step: raw-materially to take
Calculate by a small quantities of 40kg, take the starting material lead chromate 32kg chosen, sulfuration ladder 6kg, potassium perchlorate 2kg, nominal gets 6 in small batches.
4th step: the preparation of nitro-cotton tackiness agent
Take the nitro-cotton 260g after washing and drying to put into and dissolve bucket, separately get acetone 10000ml and pour in bucket to stir and make it to dissolve completely for subsequent use, prepare 6 solution.
5th step: be dry mixed tertiary mixture
Add the copper ball 50kg of ∮ (10 ~ 20) mm in vibrations mill, the medicament taken is added in vibration mill and polishes.Its polishing time and sample changing conditions as follows:
| Polishing time (h) | Loose burning time (s) | Average loose burning time (s) |
| 3 | 16.4、16.7、X、15.5、16.4、X、15.3、 | 16.06 |
| 7 | 15.3、15.7、15.9、16.3、14.7、16.1、15.5 | 15.64 |
| 10 | 14.9、15.3、14.7、15.9、15.4、15.5、15.6 | 15.33 |
Find out from above result, polish and within 3 hours, have misfire situation to occur, 7 hours, 10 hours more stable, the 10 hours medicament time of polishing is more suitable, and thus each polishing time in small batches of this batch of medicament is 10 hours.
6th step: wet mixing tertiary mixture
By the nitrocellulose solution prepared, pouring in post-type mixer, adding in stirrer by being dry mixed the tertiary mixture of having polished, drive to stir 3.5h.
7th step: granulation
The tertiary mixture getting wet mixing good is about 8kg, puts into enamel basin and is kneaded into dry thick shape, be placed on rush density machine pot in, punching press 10 minutes, then be placed on tablets press and carry out granulation by double-deck 5 holes/cm copper screen cloth.Be top sieve with 9 holes/cm bolting silk after granulation, 19 holes/cm bolting silk is that the vibratory screening apparatus of lower sieve screens qualified particle.
8th step: light medicine
Every small quantities of qualified particle being about 40kg pours in light medicine drum, light medicine about 30 minutes.
9th step: dry
By micro-cigarette medicine good for light, spread in drip pan, its thickness is (10 ~ 15) mm, and drip pan is put into baking cabinet and dry, baking medicine temperature (65-75) DEG C, is dried to moisture content and volatile content is less than 0.15%.
Tenth step: batching is mixed greatly
Large mixed do not allow from the examination average burning time in bulk to exceed each in small batches ± 0.8 second, respectively do not allow from examination fluctuation range combustion time in bulk to exceed in small batches ± 0.1 second.
Small quantities of by above step continuous dosing 6, it is as follows from test result:
| Sequence number | Loose burning time (s) | Mean time (s) | Fluctuation range (s) |
| 1 | 15.5、14.9、15.2、15.6、15.7、16、15.3 | 15.46 | ±0.64 |
| 2 | 16.2、15.4、16.2、15.1、15.3、14.9、14.9 | 15.43 | ±0.77 |
| 3 | 15.5、15、15、15.7、14.6、15.4、14.7 | 15.13 | ±0.53 |
| 4 | 15.3、14.7、15.5、15.3、15.5、15.7、15.2 | 15.31 | ±0.61 |
| 5 | 14.8、14.7、15.2、15.3、15、14.8、15.5 | 15.04 | ±0.46 |
| 6 | 14.7、14.9、15.7、15.3、14.8、15.5、14.9 | 15.11 | ±0.59 |
Each all satisfied large mixed requirement in small batches, is total to about 200kg in small batches and pours in mixed greatly cylinder simultaneously, drive mixed greatly, large mixed 40 minutes by 6.
11 step: screen qualified particle
Qualified particle size is between 9 holes/cm bolting silk screen underflow and 19 holes/cm bolting silk screen overflow.
Many components 602 micro-cigarette pharmacology fractional analysis result is:
Combustionproperty result is:
Physico-chemical analysis and combustionproperty all meet the demands.
Embodiment 3;
Produce 602 micro-cigarette medicine 200kg07 people rain fuse (12 ~ 17) s
The first step: raw-material process
1, the process of potassium perchlorate
Take chemical reagent potassium perchlorate 10kg, put into vibration mill, add the copper ball 60kg of ∮ (10 ~ 20) mm, take out after carrying out vibration polishing (3 ~ 10) hour, by being qualified particle under (60 ~ 65) hole/cm bolting silk sieve.Dried by qualified particle, moisture content is not more than 0.15%, for subsequent use for chronological classification by different polishing after drying.
2, the process of sulfuration ladder
Take the sulfuration ladder 10kg after refining pulverizing, put into vibration mill, add the steel ball 60kg of ∮ (15 ~ 25) mm, take out after carrying out vibration polishing (5 ~ 20) hour, by being qualified particle under (60 ~ 65) hole/cm bolting silk sieve.Qualified particle oven dry is not more than 0.2% to moisture content.Survey the specific surface area of sulfuration ladder, specific surface area difference is less than 500g/cm
2to mix be one barrel.For subsequent use by different specific surface area classification.
3, the process of lead chromate
Dry chemical reagent lead chromate and be not more than 0.2% to moisture content, survey specific surface area for subsequent use.
4, the washing of nitro-cotton
Get about 2kg nitro-cotton to load in calico pocket, put into the basin filling distilled water and clean, soak, repeat 3 ~ 4 times.After washing with alcohol-pickled dehydration once, dehydration post-drying be not more than 1% to moisture content.
Second step: raw-material selection
Be 2030g/cm according to Production requirement Selection radio surface-area
2lead chromate, sample before feeding intake by proportioning from the sulfuration of different specific surface area ladder, potassium perchlorate, its result is as follows:
| Sequence number | Lead chromate (g/cm 2) | Antimony sulfide (g/cm 2) | Potassium perchlorate | Sample is fallen apart burning time (s) |
| 1 | 2030 | 3500 | The polishing time 6 (h) | 20.2 |
| 2 | 2030 | 3000 | The polishing time 6 (h) | 21.3 |
| 3 | 2030 | 3000 | The polishing time 3 (h) | 22.1 |
According to above result, 1,3 is all passable, and Selection radio surface-area is 2030g/cm
2lead chromate, specific surface area is 3000g/cm
2sulfuration ladder, the potassium perchlorate of polishing time 3 (h) feeds intake production.
3rd step: raw-materially to take
Calculate by a small quantities of 40kg, take the starting material lead chromate 32kg chosen, sulfuration ladder 6kg, potassium perchlorate 2kg, totally 6 small quantities of.
4th step: the preparation of nitro-cotton tackiness agent
Take the nitro-cotton 260g after washing and drying to put into and dissolve bucket, separately get acetone 10000ml and pour in bucket to stir and make it to dissolve completely for subsequent use, prepare 6 solution.
5th step: be dry mixed tertiary mixture
Add the copper ball 50kg of ∮ (10 ~ 20) mm in vibrations mill, the medicament taken is added in vibration mill and polishes.Its polishing time and sample changing conditions as follows:
| Polishing time (h) | Loose burning time (s) | Average loose burning time (s) |
| 3 | 17.3、17.6、X、18、16.9、18.3、X | 17.62 |
| 6 | 17.1、16.8、17.5、17.5、16.9、17.3、17.3 | 17.20 |
Find out from above result, polish and within 3 hours, have misfire situation to occur, 6 hours also suitable compared with steady time, and thus each polishing time in small batches of this batch of medicament is 6 hours.
6th step: wet mixing tertiary mixture
By the nitrocellulose solution prepared, pouring in post-type mixer, adding in stirrer by being dry mixed the tertiary mixture of having polished, drive to stir 3.5h.
7th step: granulation
The tertiary mixture getting wet mixing good is about 8kg, puts into enamel basin and is kneaded into dry thick shape, be placed on rush density machine pot in, punching press 10 minutes, then be placed on tablets press and carry out granulation by double-deck 5 holes/cm copper screen cloth.Be top sieve with 9 holes/cm bolting silk after granulation, 19 holes/cm bolting silk is that the vibratory screening apparatus of lower sieve screens qualified particle.
8th step: light medicine
Every small quantities of qualified particle being about 40kg pours in light medicine drum, light medicine about 30 minutes.
9th step: dry
By micro-cigarette medicine good for light, spread in drip pan, its thickness is (10 ~ 15) mm, and drip pan is put into baking cabinet and dry, baking medicine temperature (65-75) DEG C, is dried to moisture content and volatile content is less than 0.15%.
Tenth step: batching is mixed greatly
Large mixed do not allow from the examination average burning time in bulk to exceed each in small batches ± 0.8 second, respectively do not allow from examination fluctuation range combustion time in bulk to exceed in small batches ± 0.1 second.
By above step continuous dosing 6, it is as follows from test result:
| Sequence number | Loose burning time (s) | Mean time (s) | Fluctuation range (s) |
| 1 | 17.5、16、17.2、16.9、16.2、16.6、17 | 16.77 | ±0.77 |
| 2 | 16.8、16.8、16.3、16.5、17.5、17、16.8 | 16.81 | ±0.69 |
| 3 | 17.5、17.5、17.7、17.1、17、17.2、16.9 | 17.27 | ±0.43 |
| 4 | 16.7、17.2、17.8、17.2、17.8、16.8、17.8 | 17.33 | ±0.63 |
| 5 | 16.7、16.9、16.7、16.1、16.8、16.8、16.6 | 16.66 | ±0.56 |
| 6 | 16.5、17.3、16.7、17.7、16.5、16.9、17.1 | 16.96 | ±0.74 |
Each all satisfied large mixed requirement in small batches, is total to about 200kg in small batches and pours in mixed greatly cylinder simultaneously, drive mixed greatly, large mixed 40 minutes by 5.
11 step: screen qualified particle
Qualified particle size is between 9 holes/cm bolting silk screen underflow and 19 holes/cm bolting silk screen overflow.
Many components 602 micro-cigarette pharmacology fractional analysis result is:
Combustionproperty result is:
Physico-chemical analysis and combustionproperty all meet the demands.
Claims (1)
1. a method for the micro-cigarette medicine of the many components of mechanically mixing, is characterized in that the method adopts following steps to be prepared:
The first step: raw-material process
1, the process of potassium perchlorate
Take chemical reagent potassium perchlorate 10kg, put into vibration mill, add the copper ball 60kg that diameter is ∮ 10 ~ ∮ 20mm, carry out vibration polishing to take out after 3 ~ 10 hours, under being sieved by 60 ~ 65 holes/cm bolting silk is qualified particle, dried by qualified particle, moisture content is not more than 0.15%, for subsequent use for chronological classification by different polishing after drying;
2, the process of sulfuration ladder
Take the sulfuration ladder 10kg after refining pulverizing, put into vibration mill, add the steel ball 60kg that diameter is ∮ 15mm ~ ∮ 25mm, carry out vibration polishing to take out after 5 ~ 20 hours, under being sieved by 60 ~ 65 holes/cm bolting silk is qualified particle, qualified particle is dried and is not more than 0.2% to moisture content, survey the specific surface area of sulfuration ladder, specific surface area difference is less than 500g/cm
2to mix be one barrel, for subsequent use by different specific surface area classification;
3, the process of lead chromate
Dry chemical reagent lead chromate and be not more than 0.2% to moisture content, survey specific surface area for subsequent use;
4, the washing of nitro-cotton
Get about 2kg nitro-cotton to load in calico pocket, put into fill distilled water basin cleaning, soak, repeats 3 ~ 4 times, after washing with alcohol-pickled dehydration once, post-drying of dewatering is not more than 1% to moisture content;
Second step: raw-material selection
Starting material specific surface area is larger, and the finished product medicament time is shorter, thus chooses corresponding starting material by product requirement.Because the specific surface area of potassium perchlorate, sulfuration ladder can process on request, and lead chromate controls by supplied materials, so first choose the suitable lead chromate of specific surface area according to product requirement, then join get corresponding sulfuration ladder, potassium perchlorate makes sample, carrys out selection material according to the loose sintering fruit of sample;
Raw-material specific surface area needed for 602 micro-cigarette medicine variant productions, the sample burning time approximate range that falls apart is as follows:
3rd step: raw-materially to take
Calculate by a small quantities of 40kg, lead chromate is containing 80%, and antimony sulfide is containing 15%, and potassium perchlorate, containing 5%, takes the starting material lead chromate 32kg chosen, sulfuration ladder 6kg, potassium perchlorate 2kg;
4th step: the preparation of nitro-cotton tackiness agent
Take the nitro-cotton 260g after washing and drying to put into and dissolve bucket, separately get chemical reagent acetone 8000 ~ 10000ml pour in bucket stir make it to dissolve completely for subsequent use;
5th step: be dry mixed tertiary mixture
The copper ball 50kg of ∮ 10 ~ 20mm is added in vibrations mill, the medicament taken is added in vibration mill, polish 3 ~ 15 hours, do the time of sample grasp medicine, stability and polishing time in vibration processes, 602 micro-cigarette medicine variant productions required control sample time approximate range is as follows:
6th step: wet mixing tertiary mixture
By the nitrocellulose solution prepared, pouring in post-type mixer, adding in stirrer by being dry mixed the tertiary mixture of having polished, drive to stir 3.5h;
7th step: granulation
The tertiary mixture getting wet mixing good is about 8kg, puts into enamel basin and is kneaded into dry thick shape, be placed on rush density machine pot in, punching press 7 ~ 15 minutes, then be placed on tablets press and carry out granulation by double-deck 5 holes/cm copper screen cloth; Be top sieve with 9 holes/cm bolting silk after granulation, 19 holes/cm bolting silk is that the vibratory screening apparatus of lower sieve screens qualified particle;
8th step: light medicine
Every small quantities of qualified particle is about 40kg to pour in light medicine drum, light medicine is about 30min;
9th step: dry
By micro-cigarette medicine good for light, spread in drip pan, its thickness is 10 ~ 15mm, drip pan is put into baking cabinet and dries, and baking medicine temperature 65-75 DEG C, is dried to moisture content and volatile content is less than 0.15; .
Tenth step: batching is mixed greatly
Large mixed do not allow from the examination average burning time in bulk to exceed each in small batches ± 0.8 second, respectively small quantities of do not allow from examination fluctuation range combustion time in bulk to exceed ± 0.1 second, each small quantities of medicine mixed is greatly poured into simultaneously in large mixed cylinder, drive large mixed, once mixed greatly amount is 50 ~ 250 kilograms, mixed 30 ~ 50 minutes greatly;
11 step: screen qualified particle
Qualified particle size is between 9 holes/cm bolting silk screen underflow and 19 holes/cm bolting silk screen overflow.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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