CN110540484B - Continuous preparation process of nitrocotton for fireworks - Google Patents
Continuous preparation process of nitrocotton for fireworks Download PDFInfo
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- CN110540484B CN110540484B CN201910973403.7A CN201910973403A CN110540484B CN 110540484 B CN110540484 B CN 110540484B CN 201910973403 A CN201910973403 A CN 201910973403A CN 110540484 B CN110540484 B CN 110540484B
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
- C06B21/0066—Shaping the mixture by granulation, e.g. flaking
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
- C06B21/0075—Shaping the mixture by extrusion
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0083—Treatment of solid structures, e.g. for coating or impregnating with a modifier
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B25/00—Compositions containing a nitrated organic compound
- C06B25/18—Compositions containing a nitrated organic compound the compound being nitrocellulose present as 10% or more by weight of the total composition
- C06B25/20—Compositions containing a nitrated organic compound the compound being nitrocellulose present as 10% or more by weight of the total composition with a non-explosive or a non-explosive or a non-thermic component
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- Crystallography & Structural Chemistry (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The invention discloses a continuous preparation process of nitrocotton for fireworks, which comprises the steps of adding nitrocotton, a plasticizer, a stabilizer and a desensitizer into a kneader with a screw, stirring and plasticizing to obtain homogeneous nitrocotton, extruding the homogeneous nitrocotton through the screw at the bottom of the kneader and granulating to obtain nitrocotton particles; continuously inputting nitrocotton particles into a size mixing tank, and adding a plasticizer solution into the size mixing tank to obtain hardened nitrocotton; crushing the hardened nitrocotton in a wet crushing mode to obtain a powdery material; the solid-liquid separation is carried out on the powdery material, the separated solid is extracted, and the moisture content is controlled to be 26-40%, so that the nitrocotton for the fireworks is obtained.
Description
Technical Field
The invention belongs to the technical field of preparation processes of nitrocotton with special purposes, and particularly relates to a continuous preparation process of nitrocotton for fireworks.
Background
The indoor fireworks are also called cold light fireworks (also called cold fireworks and cold fireworks), belonging to micro (non) smoke spraying fireworks type environment protection fireworks, and are made up by using metal powder with low ignition point and adopting a certain preparation process, and the cold flame has low ignition point, its ignition point is 60-80 deg.C, external temperature is 30-50 deg.C, and is harmless to human body, so that it is applicable to stage performance and various moulding designs. The products mainly comprise stage fireworks, cake fireworks, handheld fireworks, ground fireworks, movie and television special effect fireworks and the like. The indoor fireworks on the market adopt novel formula, mainly replace black powder with the single base powder of retirement, can keep the ornamental effect of traditional fireworks, and smokeless production when setting off moreover, it is few to remain the dust, and security and stability are good.
The single base propellant contains only one high-molecular explosive base propellant. The main component of the nitrocotton is nitrocotton, which is also called nitrocotton single-base drug. The Chinese invention application with the publication number of CN103524278A discloses a processing method of single-base powder and double-base powder for fireworks, which comprises the following steps: (1) removing impurities from the single-base powder and double-base powder, preparing materials, and adding water for moistening; (2) processing the wet powder, putting the wet powder into a crusher for crushing, and centrifugally dewatering; (3) screening and grading; (4) processing dry powder to obtain single-base powder and double-base powder products for fireworks; (5) and (5) packaging the finished product, namely sealing and packaging the finished product by using an anti-static and damp-proof fiber woven bag to obtain the finished product and warehousing the finished product. The method is characterized in that single-base powder and double-base powder are used as raw materials and are processed to prepare the single-base powder and the double-base powder for fireworks, the used single-base powder is a product obtained by crushing the national storage retired single-base powder serving as a raw material, the single-base powder is military materials and is strictly controlled by the country, the quantity of the retired single-base powder put on the market is reduced year by year, the supply of the single-base powder is uncertain, the production requirement of indoor fireworks is difficult to meet, the preparation process of the single-base powder is complex, more equipment and devices are needed, the requirement on equipment is high, and the method is not suitable for the continuous development of the indoor firework industry.
The Chinese invention application with the publication number of CN109320387A discloses cellulose powder for cold light spraying fireworks and a preparation method thereof, the Chinese invention application with the publication number of CN109251116A discloses a production method of nitrocotton for indoor fireworks, and the Chinese invention application with the publication number of CN109438146A discloses a slurry method production process of the nitrocotton for the indoor fireworks; the process technology adopted by the invention application is an intermittent process; the Chinese invention application with the publication number of CN109251116A directly adds water to the kneading machine for hardening granulation after the nitrocotton is plasticized, the granulated material is not uniform in size and is not beneficial to subsequent crushing, the discharging mode after the kneading machine granulation is cylinder turning discharging, the safety risk exists, the production period is long, the field operation labor intensity is high, the automatic control cannot be realized, and the intrinsic safety is low.
Disclosure of Invention
The invention aims to provide a continuous preparation process of nitrocotton for fireworks, which solves the problem of long production period of the existing intermittent production equipment.
The technical scheme adopted by the invention is that a continuous preparation process of nitrocotton for fireworks is implemented according to the following steps:
step 1, mixing nitrocotton, plasticizer, stabilizer and desensitizer according to a mass ratio of 100: 40-200: 0.8-1.5: 1-10, adding the mixture into a kneader with a screw, stirring the mixture for 0.5-3h at the rotating speed of 36-45r/min to obtain homogeneous nitrocotton, and extruding and granulating the homogeneous nitrocotton through the screw at the bottom of the kneader to obtain continuously output nitrocotton particles;
step 2, continuously inputting nitrocotton particles into a size mixing tank, adding a plasticizer solution with the mass fraction of 0-15% into the size mixing tank, wherein the mass ratio of the nitrocotton particles to the plasticizer solution is 1:5-20, and soaking for 0.5-3h to obtain continuously hardened nitrocotton;
step 3, continuously crushing the hardened nitrocotton in a wet crushing mode to obtain a crushed material;
and 4, continuously feeding the crushed materials into a P60 pusher centrifuge, extracting the separated solids, and controlling the water content to be 26-40%, so as to obtain the nitrocotton for the fireworks.
The invention is also characterized in that:
the nitration degree of the nitrocotton in the step 1 is 190-205 ml/g.
In the step 1, the nitrocotton contains a mixed solution of water and alcohol with the mass fraction of 20-50% in any ratio, and the raw material of the nitrocotton is one of wood pulp cellulose, cotton pulp cellulose and bamboo pulp cellulose.
The plasticizer in the step 1 is one of ethyl acetate, methyl acetate, butyl acetate, methyl ethyl ketone, acetone, butanone, methyl ether, diethyl ether and propyl ether.
The stabilizer in the step 1 is one of diphenylamine, a No. I medium stabilizer and a No. II medium stabilizer.
The desensitizer in the step 1 is one of DBP, ATBC and ESO.
The continuous output nitrocotton particles obtained in the step 1 are achieved through interactive plasticization and granulation of two kneading machines, and the specific process is as follows: mixing nitrocotton, plasticizer, stabilizer and desensitizer according to a mass ratio of 100: 40-200: 0.8-1.5: 1-10 parts of the mixture is added into a first kneader with a screw, the kneader stirs for 0.5-3h at the rotating speed of 36-45r/min to plasticize the nitrocotton, a second kneader which firstly completes the plasticization of the nitrocotton extrudes and granulates during the plasticization of the first kneader, the rotating speed of an extruded discharging screw is 15-60r/min, the pelletizing frequency is 3-12 times/second, and the grain length is not more than 5 mm.
The crushed material in the step 3 has 60-90% of particle size of 80-100 meshes.
The continuously hardened nitrocotton obtained in the step 2 is finished by alternately hardening in two size mixing tanks, and the concrete process is as follows: continuously inputting nitrocotton particles into an empty size mixing tank, hardening for 0.5-3h to obtain hardened nitrocotton particles, then discharging, continuously inputting nitrocotton particles into another size mixing tank which is just discharged while discharging, and finishing material hardening and discharging in the previous size mixing tank when size mixing and hardening.
The invention has the beneficial effects that:
1) the invention relates to a continuous preparation process of nitrocotton for fireworks, wherein water is not added in the granulation process, a kneading machine is used for plasticizing and then extruding the plasticized nitrocotton into uniform strips through a bottom screw rod, granulating the strips, and then falling into a size mixing tank for hardening, the preparation process is continuously completed, and the problems that the granulated nitrocotton for fireworks is uneven in shape and difficult to crush to meet the requirement of particle size and the discharge of a cylinder-turning kneading machine is unsafe are solved;
2) the method can select the low-price nitrocotton raw material, has low control cost, is economical and practical in production process, improves the stability of the nitrocotton, reduces the sensitivity of the product, and ensures the storage and transportation safety performance; the prepared nitrocellulose for fireworks does not contain fibrous structures, is safe and stable to store, improves the stacking density of the nitrocellulose, meets the use requirements of indoor firework production in particle size, and meets the use requirements of indoor fireworks in application performance.
3) The main raw material of the invention is nitrocotton, which is used for manufacturing fireworks, the main gas generated after burning is nitrogen, and the gas has no smoke and sulfur in the combustion gas, thus meeting the environmental protection requirement of indoor fireworks.
4) The continuous preparation process of the nitrocotton for the fireworks, provided by the invention, overcomes the defects of an intermittent production process, reduces the labor intensity of operators, and improves the intrinsic safety of the process and the production efficiency.
Drawings
FIG. 1 is a flow chart of a continuous preparation process of nitrocotton for fireworks.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a continuous preparation process of nitrocotton for fireworks, which is implemented according to the following steps as shown in figure 1:
step 1, mixing nitrocotton, plasticizer, stabilizer and desensitizer according to a mass ratio of 100: 40-200: 0.8-1.5: 1-10, adding the mixture into a first kneader with a screw, stirring the mixture for 0.5-3h at the rotating speed of 36-45r/min by the kneader, plasticizing to obtain homogeneous nitrocotton, extruding and granulating by a second kneader which firstly completes the plasticizing of the nitrocotton in the plasticizing process of the first kneader, wherein the rotating speed of an extruded discharging screw is 15-60r/min, the granulating frequency is 3-12 times/second, and the particle length is not more than 5mm, so as to obtain continuously output nitrocotton particles;
the nitration degree of the nitrocotton is 190-205 ml/g.
The nitrocotton comprises a mixed solution of water and alcohol with the mass fraction of 20-50% in any ratio, and the raw material of the nitrocotton is one of wood pulp cellulose, cotton pulp cellulose and bamboo pulp cellulose.
The plasticizer is one of ethyl acetate, methyl acetate, butyl acetate, methyl ethyl ketone, acetone, butanone, methyl ether, ethyl ether and propyl ether.
The stabilizer is one of diphenylamine, a No. I medium stabilizer and a No. II medium stabilizer.
The desensitizer is one of DBP, ATBC and ESO.
Step 2, continuously inputting nitrocotton particles into empty size mixing tanks, adding a plasticizer solution with the mass fraction of 0-15% into one of the size mixing tanks, wherein the mass ratio of the nitrocotton particles to the plasticizer solution is 1:5-20, soaking for 0.5-3h, then discharging, continuously inputting the nitrocotton particles and the plasticizer solution into the other size mixing tank which is just discharged while discharging from the first size mixing tank, and finishing hardening and discharging in the previous size mixing tank when size mixing is hardened to obtain hardened nitrocotton;
step 3, crushing the hardened nitrocotton in a wet crushing mode to obtain a crushed material; the pulverized material has 60-90% of particle size of 80-100 mesh.
And 4, carrying out solid-liquid separation on the crushed materials, extracting the separated solids, and controlling the water content to be 26-40%, thus obtaining the nitrocotton for the fireworks.
Example 1
Adding 2000g of nitrocotton containing 20% of water and 190ml/g of nitration degree into a kneader, rotating for 1min and mixing uniformly; mixing 16g of diphenylamine, 20g of DBP20g and 800g of ethyl acetate, and dissolving the mixture by stirring continuously to obtain a uniform mixed solution; adding the mixed solution into a kneader at normal temperature, stirring at the rotating speed of 36r/min for 30min to complete plasticization; starting spiral discharging in a stirring state, wherein the spiral discharging rotating speed is 60r/min, the cutting speed of a cutter is 12 times/second, the same raw materials are added into a second kneading machine while the first kneading machine discharges, and the raw materials are plasticized under the same conditions, so that the two screw discharging kneading machines alternately plasticize and granulate, and uniform granular materials can be continuously obtained; continuously inputting the granulated nitrocotton into a size mixing tank, and continuously adding 10000g of aqueous solution into the size mixing tank for size mixing and hardening; and (3) wet-crushing the size-mixed material to obtain 80% of crushed material with the particle size of 80-100 meshes, and dehydrating to obtain nitrocotton with the water content of 26% to obtain the nitrocotton product for the indoor fireworks.
Example 2
Adding 37% of alcohol-containing solution and 2000g of nitrocotton with the nitration degree of 197ml/g into a kneader, and rotating positively for 1min to mix uniformly; dissolving 22g of a No. II medium fixing agent, ATBC100g and 2000g of acetone in a mixed manner, and dissolving the mixture by stirring continuously to obtain a uniform mixed solution; adding the mixed solution into a kneader at 15 ℃, and stirring at the rotating speed of 38r/min for 60min to complete plasticization; starting spiral discharging in a stirring state, rotating at the speed of 30r/min, simultaneously cutting the particles by a cutter at the speed of 6 times/second, adding the same raw materials into a second kneading machine while discharging the materials from a first kneading machine, and plasticizing under the same conditions, so that the two screw discharging kneading machines are alternately plasticized and granulated, and uniform granular materials can be continuously obtained; continuously inputting granulated nitrocotton into a size mixing tank, and continuously adding 22000g of acetone-containing aqueous solution into the size mixing tank for size mixing and hardening, wherein the concentration of a plasticizer in the aqueous solution is 7%; and (3) wet-crushing the size-mixed material, wherein the particle size is 80-100 meshes and accounts for 75%, and dehydrating to obtain nitrocotton with the water content of 35%, namely a nitrocotton product for fireworks.
Example 3
Adding 2000g of nitrocotton containing 50% of water and 205ml/g of nitration degree into a kneader, and rotating positively for 1min to mix uniformly; mixing 30g of a No. I medium reagent, 30g of ESO200g and 3000g of propyl ether, and dissolving the mixture by stirring continuously to obtain a uniform mixed solution; adding the mixed solution into a kneader at 60 ℃, and rotating positively for 90min to complete plasticization; starting spiral discharging in a stirring state, rotating at the speed of 15r/min, simultaneously cutting the grain by a cutter at the speed of 3 times/second, adding the same raw materials into a second kneading machine while discharging by a first kneading machine, and plasticizing under the same condition, so that the two screw discharging kneading machines are alternately plasticized and granulated, and uniform granular materials can be continuously obtained; continuously inputting the granulated nitrocotton into a size mixing tank, and continuously adding 40000g of clear water into the size mixing tank for size mixing and hardening; and (3) wet-crushing the size-mixed material, wherein the particle size is 80-100 meshes and accounts for 65%, and then dehydrating to obtain nitrocotton with the water content of 40%, namely a nitrocotton product for fireworks.
The raw materials related to the example 2 of the invention are prepared by a batch process, and the nitrocellulose product for fireworks with the same quality is prepared, and the results are shown in the table 1:
TABLE 1
The comparison of the table shows that the two kneaders are adopted in the invention, but the final granulation time and the time required by granulating the material to the time before the material enters the crusher are shortened by more than 2 times, and the particle size of the nitrocotton in the invention is relatively uniform, so that the working efficiency can be effectively improved.
Through the mode, the continuous preparation process of the nitrocotton for the fireworks, disclosed by the invention, has the advantages that no water is added in the granulation process, the nitrocotton is extruded into uniform strips through the bottom screw rod after the kneading machine is plasticized, the strips are cut into granules, and then the strips fall into the size mixing tank to be hardened, the preparation process is continuously completed, and the problems that the granulated nitrocotton for the fireworks is uneven in shape, difficult to crush and meets the requirement on particle size and the discharge of the cylinder-turning kneading machine is unsafe are solved; the method can select the low-price nitrocotton raw material, has low control cost, is economical and practical in production process, improves the stability of the nitrocotton, reduces the sensitivity of the product, and ensures the storage and transportation safety performance; the prepared nitrocotton for the fireworks does not contain fibrous structures, is safe and stable to store, improves the stacking density of the nitrocotton, meets the use requirements of indoor firework production in particle size, and meets the use requirements of indoor fireworks in application performance; in addition, the main raw material of the invention is nitrocotton, which is used for manufacturing fireworks, the main gas generated after burning is nitrogen, and the gas is smokeless and sulfur-free, thus meeting the environmental protection requirement of setting off indoor fireworks; the continuous preparation process of the nitrocotton for the fireworks, provided by the invention, overcomes the defects of an intermittent production process, reduces the labor intensity of operators, and improves the intrinsic safety of the process and the production efficiency.
Claims (5)
1. A continuous preparation process of nitrocotton for fireworks is characterized by comprising the following steps:
step 1, mixing nitrocotton, plasticizer, stabilizer and desensitizer according to a mass ratio of 100: 40-200: 0.8-1.5: 1-10, adding the mixture into a kneader with a screw, stirring the mixture for 0.5-3h at the rotating speed of 36-45r/min to obtain homogeneous nitrocotton, and extruding and granulating the homogeneous nitrocotton through the screw at the bottom of the kneader to obtain continuously output nitrocotton particles; the nitration degree of the nitrocotton in the step 1 is 190-205 ml/g;
the continuous output nitrocotton particles obtained in the step 1 are achieved through interactive plasticization and granulation of two kneading machines, and the specific process is as follows: mixing nitrocotton, plasticizer, stabilizer and desensitizer according to a mass ratio of 100: 40-200: 0.8-1.5: 1-10, adding the mixture into a first kneader with a screw, stirring the kneader for 0.5-3h at the rotating speed of 36-45r/min to plasticize the nitrocotton, extruding and granulating by a second kneader which firstly completes the plasticization of the nitrocotton in the plasticizing process of the first kneader, wherein the rotating speed of an extruded discharging screw is 15-60r/min, the granulating frequency is 3-12 times/second, and the particle length is not more than 5 mm;
the plasticizer is one of ethyl acetate, methyl acetate, butyl acetate, methyl ethyl ketone, acetone, butanone, methyl ether, ethyl ether and propyl ether;
step 2, continuously inputting nitrocotton particles into a size mixing tank, adding a plasticizer solution with the mass fraction of 0-15% into the size mixing tank, wherein the mass ratio of the nitrocotton particles to the plasticizer solution is 1:5-20, and soaking for 0.5-3h to obtain continuously hardened nitrocotton;
the step 2 of obtaining the continuously hardened nitrocotton is completed by alternately hardening in two size mixing tanks, and the specific process is as follows: continuously inputting nitrocotton particles into an empty size mixing tank, hardening for 0.5-3h to obtain hardened nitrocotton particles, then discharging, continuously inputting nitrocotton particles into another size mixing tank which is just discharged while discharging, and finishing material hardening and discharging in the previous size mixing tank when size mixing and hardening;
step 3, continuously crushing the hardened nitrocotton in a wet crushing mode to obtain a crushed material;
and 4, continuously feeding the crushed materials into a P60 pusher centrifuge, extracting the separated solids, and controlling the water content to be 26-40%, so as to obtain the nitrocotton for the fireworks.
2. The continuous preparation process of nitrocotton for fireworks according to claim 1, characterized in that in step 1, the nitrocotton contains a mixed solution of water and alcohol with mass fraction of 20-50% in any ratio, and the raw material of nitrocotton is one of wood pulp cellulose, cotton pulp cellulose and bamboo pulp cellulose.
3. The continuous preparation process of nitrocotton for fireworks according to claim 1, characterized in that the stabilizer in step 1 is one of diphenylamine, I-type stabilizer and II-type stabilizer.
4. The continuous preparation process of nitrocotton for fireworks according to claim 1, characterized in that the desensitizer in step 1 is one of DBP, ATBC, ESO.
5. The continuous preparation process of nitrocotton for fireworks according to claim 1, characterized in that the pulverized material of step 3 has 60-90% of particle size of 80-100 mesh.
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| CN113307708B (en) * | 2021-06-17 | 2022-06-03 | 张宏善 | Preparation method of single-base powder and single-base powder obtained by method |
| CN113980297A (en) * | 2021-11-18 | 2022-01-28 | 北方化学工业股份有限公司 | Method for preparing nitrocotton absorption plasticizer |
| CN114082492A (en) * | 2021-11-18 | 2022-02-25 | 北方化学工业股份有限公司 | Particle size control method for firework cotton |
| CN114394878B (en) * | 2022-01-25 | 2023-03-24 | 上栗县金圆花炮制造有限公司 | Mould pressing type combined firework ignition charge and laying process thereof |
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|---|---|---|---|---|
| US4051207A (en) * | 1974-12-27 | 1977-09-27 | Dynamit Nobel Aktiengesellschaft | Process for the production of propellant charge powders, especially nitroguanidine powders |
| CN1047072A (en) * | 1989-05-11 | 1990-11-21 | Wnc-氮化学有限公司 | The preparation method of triple-base propellant and device |
| CN109251116A (en) * | 2018-10-15 | 2019-01-22 | 四川北方硝化棉股份有限公司 | A kind of production method of interior fireworks nitrocotton |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4051207A (en) * | 1974-12-27 | 1977-09-27 | Dynamit Nobel Aktiengesellschaft | Process for the production of propellant charge powders, especially nitroguanidine powders |
| CN1047072A (en) * | 1989-05-11 | 1990-11-21 | Wnc-氮化学有限公司 | The preparation method of triple-base propellant and device |
| CN109251116A (en) * | 2018-10-15 | 2019-01-22 | 四川北方硝化棉股份有限公司 | A kind of production method of interior fireworks nitrocotton |
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