CN112321725B - Production method of 10000 second-degree nitrocotton - Google Patents
Production method of 10000 second-degree nitrocotton Download PDFInfo
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- CN112321725B CN112321725B CN202011330068.8A CN202011330068A CN112321725B CN 112321725 B CN112321725 B CN 112321725B CN 202011330068 A CN202011330068 A CN 202011330068A CN 112321725 B CN112321725 B CN 112321725B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B5/00—Preparation of cellulose esters of inorganic acids, e.g. phosphates
- C08B5/02—Cellulose nitrate, i.e. nitrocellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B5/00—Preparation of cellulose esters of inorganic acids, e.g. phosphates
- C08B5/02—Cellulose nitrate, i.e. nitrocellulose
- C08B5/04—Post-esterification treatments, e.g. densification of powders, including purification
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Abstract
The invention discloses a production method of 10000 seconds nitrocotton, which comprises the steps of uniformly mixing a proper amount of nitric acid, sulfuric acid and water to obtain mixed acid; sending the refined cotton into a nitrating machine through a carding machine and a fan, nitrating the refined cotton by adopting mixed acid to obtain acid nitrocotton, sending the acid nitrocotton into a centrifugal machine, adding a proper amount of water for replacement, then sending the acid nitrocotton into a water washing tank for water washing, and then sending the acid nitrocotton into a scouring pot; draining nitrocotton in a boiling and washing pot, thoroughly washing with water, adding water to submerge the nitrocotton, draining water after cold washing, adding water to submerge the nitrocotton, performing acid boiling, and draining water to obtain nitrocotton a; pumping the nitrocotton a into a centrifugal machine through a pump for dewatering, then continuously pumping the nitrocotton a into a cellucotton trough into the centrifugal machine for water displacement, and packaging the separated nitrocotton to obtain the 10000-second-degree nitrocotton. Solves the problems of low viscosity and high production cost of the nitrocotton in the prior art.
Description
Technical Field
The invention relates to the technical field of nitrocotton production, in particular to a method for producing 10000-second-degree nitrocotton.
Background
The nitrocellulose, also known as nitrocellulose and collodion, belongs to nitrate esters, and is white or yellowish flocculent, and is dissolved in acetone. The cellulose nitrate is prepared by esterification reaction of refined cotton, concentrated nitric acid and concentrated sulfuric acid. The cellulose nitrate has wide application range, is originally used in the military field and is an important raw material for manufacturing propellant powder, missile and rocket propellant; meanwhile, the method can also be used for manufacturing various products such as paint, typewriting wax paper, printing ink, varnished cloth, bottle mouth sealing sleeves, adhesives, leather oil, nail polish, ester soluble or water soluble coatings, table tennis, piano keys and the like. The viscosity of the conventional industrial nitrocotton is about 2000 seconds at most, the cost is high, and the viscosity of the nitrocotton is required to be higher along with the increase of the market demand of solid alcohol and glue.
Disclosure of Invention
The invention aims to provide a production method of 10000-second-degree nitrocotton, and solves the problems of low viscosity and high production cost of the nitrocotton in the prior art.
The technical scheme adopted by the invention is a 10000-second-degree nitrocotton production method, which is implemented according to the following steps:
step 1, preparing mixed acid
Taking a proper amount of nitric acid, sulfuric acid and water, and uniformly mixing to obtain mixed acid;
step 2, nitration
Sending the refined cotton into a nitrating machine through a carding machine and a fan, nitrating the refined cotton by adopting mixed acid to obtain acid nitrocotton, sending the acid nitrocotton into a centrifugal machine, adding a proper amount of water for replacement, then sending the acid nitrocotton into a water washing tank for water washing, and then sending the acid nitrocotton into a scouring pot;
step 3, acid cooking
Draining water from nitrocotton in a boiling-washing pot for 40min, thoroughly washing with water for 20min, adding water to submerge the nitrocotton, cold washing for 1h, draining water for 40min after cold washing, adding water to submerge the nitrocotton, performing acid boiling, and draining water to obtain nitrocotton a;
step 4, driving off water
Pumping the nitrocotton a into a centrifugal machine through a pump for dewatering, continuously pumping the dewatered nitrocotton a into a wine cotton tank into the centrifugal machine for water displacement, and packaging the separated nitrocotton to obtain the 10000-second-degree nitrocotton.
The invention is also characterized in that:
in the step 1, the mass percent of the nitric acid is 23.0 +/-0.5%, the mass percent of the water is 17.5 +/-0.15%, and the mass percent of the sulfuric acid is 59.5 +/-0.45%.
In the step 2, the nitrator is a 6-tube U-shaped nitrator, the temperature of the nitration treatment is 25-29 ℃, and the time is 30min.
In the step 2, the centrifugal machine is a double-stage piston pushing material P60 centrifugal machine, and the water adding amount is 925 to 975L/h.
In the step 3, the acid boiling temperature is 86 ℃ and the time is 2.5h.
In the step 3, the initial acidity of the nitrocotton is not more than 1g/L.
In the step 4, the volume concentration of the wine in the cellucotton groove is 70-75%, a wine adding pipe is arranged in a centrifugal machine, and the wine adding amount in the centrifugal machine is 1500-1650L/h.
The 10000-second-degree nitrocotton has the water content of not more than 4.5 percent, the nitrogen content of not more than 12.1 percent, the viscosity of not more than 22287 seconds and Abel of not less than 15min.
The refined cotton is M1000 grade refined cotton in GB/T9107, and the viscosity of the refined cotton is more than 800mpa & s.
The beneficial effects of the invention are:
the production method of the 10000-second-degree nitrocotton is mainly used for glue and solid alcohol, and has low production cost; the production method of the nitrocotton with the viscosity of 10000 seconds can realize the stable production of the nitrocotton with the viscosity of more than 10000 seconds, ensure that Abel of the nitrocotton is more than or equal to 15min, and the stability index qualification rate of the nitrocotton is 100 percent.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention provides a production method of 10000-second-degree nitrocotton, which is implemented according to the following steps:
step 1, preparing mixed acid
Taking a proper amount of nitric acid, sulfuric acid and water, and uniformly mixing to obtain mixed acid;
23.0 +/-0.5 percent of nitric acid, 17.5 +/-0.15 percent of water and 59.5 +/-0.45 percent of sulfuric acid;
the refined cotton is M1000 grade refined cotton in GB/T9107, and the viscosity of the refined cotton is more than 800mpa & s;
the nitrogen content of 10000 sec nitrocotton can be ensured to be 11.75-12.06% by the mixed acid, the dissolving effect under the high-viscosity state can be accelerated, and the dissolving time can be shortened;
step 2, nitration
Sending the refined cotton into a nitrator through a carding machine and a fan, nitrating the refined cotton by adopting mixed acid to obtain acid nitrocotton, sending the acid nitrocotton into a centrifuge, adding a proper amount of water for replacement, then sending the acid nitrocotton into a water washing tank for water washing, and then sending the acid nitrocotton into a scouring pot;
the nitrating machine is a 6-tube U-shaped nitrating machine, the temperature of the nitration treatment is 25-29 ℃, and the time is 30min;
the centrifugal machine is a double-stage piston material pushing P60 centrifugal machine, and the water adding amount is 925 to 975L/h;
the nitration reaction time is the retention time of the mixed acid and the refined cotton in the U-shaped nitrator, the nitration time is controlled within 30min, and at the moment, the nitration temperature is the most critical, and low-temperature nitration is adopted. But the nitration reaction temperature is too low, so that the reaction is not thorough, and the product contains unreacted refined cotton which cannot meet the requirement, so that the quality loss is caused; when the temperature is higher, side reactions of the refined cotton and the mixed acid are increased, the molecular chain of the nitrocellulose produced by the main reaction is easy to break, and the viscosity of the product is reduced; therefore, the optimal nitration temperature selected by the method is 25-29 ℃, the complete reaction of the product can be completely guaranteed, and the high-viscosity nitrocotton can be obtained. The data under the low temperature nitration process are shown in table 1:
TABLE 1 nitration Process data of the invention
Step 3, acid cooking
Draining water from nitrocotton in a boiling-washing pot for 40min, thoroughly washing with water for 20min, adding water to submerge the nitrocotton, cold washing for 1h, draining water after cold washing for 40min, adding water to submerge the nitrocotton, performing acid boiling, and draining water to obtain nitrocotton a;
the temperature of acid boiling is 86 ℃, and the time is 2.5h;
the initial acidity of the nitrocotton is not more than 1g/L;
the key point of the acid boiling process is to control the initial acidity of the nitrocotton, and because the nitrocotton is subjected to stability treatment during acid boiling and the residual acid in the cotton accelerates the decomposition of the nitrocotton, a low-acidity low-temperature washing process is adopted;
step 4, driving off water
Pumping the nitrocotton a into a centrifugal machine through a pump for dewatering, then continuously pumping the nitrocotton a into a cellucotton trough into the centrifugal machine for water displacement, and packaging the separated nitrocotton to obtain 10000-second-degree nitrocotton;
the volume concentration of the wine in the cellucotton groove is 70-75%, a wine adding pipe is arranged in the centrifugal machine, and the wine adding amount in the centrifugal machine is 1500-1650L/h;
the 10000-second-degree nitrocotton has the water content of not more than 4.5 percent, the nitrogen content of not more than 12.1 percent, the viscosity of not more than 22287 seconds and Abel of not less than 15min. The stability index yield is 100%.
The viscosity of the nitrocotton prepared by the refined cotton is 7000-20000 seconds.
Example 1
The production method of 10000 seconds nitrocotton is implemented according to the following steps:
step 1, preparing mixed acid
Taking a proper amount of nitric acid, sulfuric acid and water, and uniformly mixing to obtain mixed acid;
the mass percent of the nitric acid is 22.9 percent, the mass percent of the water is 17.6 percent, and the mass percent of the sulfuric acid is 59.5 percent;
the refined cotton is M1000 grade refined cotton in GB/T9107, and the viscosity of the refined cotton is more than 800mpa & s;
step 2, nitration
Sending the refined cotton into a nitrating machine through a carding machine and a fan, nitrating the refined cotton by adopting mixed acid to obtain acid nitrocotton, sending the acid nitrocotton into a centrifugal machine, adding a proper amount of water for replacement, then sending the acid nitrocotton into a water washing tank for water washing, and then sending the acid nitrocotton into a scouring pot;
the nitrifying machine is a 6-tube U-shaped nitrifying machine, the temperature of the nitrifying treatment is 26 ℃, and the time is 30min;
the centrifuge is a two-stage piston pusher P60 centrifuge, and the water addition amount is 950L/h;
step 3, acid cooking
Draining water from nitrocotton in a boiling-washing pot for 40min, thoroughly washing with water for 20min, adding water to submerge the nitrocotton, cold washing for 1h, draining water for 40min after cold washing, adding water to submerge the nitrocotton, performing acid boiling, and draining water to obtain nitrocotton a;
the temperature of acid cooking is 86 ℃, and the time is 2.5h;
the initial acidity of the nitrocotton is 1g/L;
step 4, driving off water
Pumping the nitrocotton a into a centrifugal machine through a pump for dewatering, then continuously pumping the nitrocotton a into a cellucotton trough into the centrifugal machine for water displacement, and packaging the separated nitrocotton to obtain 10000-second-degree nitrocotton;
the volume concentration of the wine in the cellucotton groove is 75%, a wine adding pipe is arranged in the centrifugal machine, and the wine adding amount in the centrifugal machine is 1600L/h;
the 10000-second-degree nitrocotton has the water content of 4.42 percent, the nitrogen content of 11.96 percent, the viscosity of 11139 seconds and Abel which is not less than 15min.
Example 2
The production method of 10000 seconds nitrocotton is implemented according to the following steps:
step 1, preparing mixed acid
Taking a proper amount of nitric acid, sulfuric acid and water, and uniformly mixing to obtain mixed acid;
the mass percent of the nitric acid is 22.80 percent, the mass percent of the water is 17.58 percent, and the mass percent of the sulfuric acid is 59.62 percent;
the refined cotton is M1000 grade refined cotton in GB/T9107, and the viscosity of the refined cotton is more than 800mpa & s;
step 2, nitration
Sending the refined cotton into a nitrating machine through a carding machine and a fan, nitrating the refined cotton by adopting mixed acid to obtain acid nitrocotton, sending the acid nitrocotton into a centrifugal machine, adding a proper amount of water for replacement, then sending the acid nitrocotton into a water washing tank for water washing, and then sending the acid nitrocotton into a scouring pot;
the nitrifying machine is a 6-tube U-shaped nitrifying machine, the temperature of the nitrifying treatment is 26 ℃, and the time is 30min;
the centrifugal machine is a double-stage piston material pushing P60 centrifugal machine, and the water adding amount is 975L/h;
step 3, acid boiling
Draining water from nitrocotton in a boiling-washing pot for 40min, thoroughly washing with water for 20min, adding water to submerge the nitrocotton, cold washing for 1h, draining water after cold washing for 40min, adding water to submerge the nitrocotton, performing acid boiling, and draining water to obtain nitrocotton a;
the temperature of acid cooking is 86 ℃, and the time is 2.5h;
the initial acidity of the nitrocotton is 1g/L;
step 4, driving off water
Pumping the nitrocotton a into a centrifugal machine through a pump for dewatering, then continuously pumping the nitrocotton a into a cellucotton trough into the centrifugal machine for water displacement, and packaging the separated nitrocotton to obtain 10000-second-degree nitrocotton;
the volume concentration of the wine in the cellucotton groove is 72 percent, a wine adding pipe is arranged in the centrifugal machine, and the wine adding amount in the centrifugal machine is 1500L/h;
the water content of the 10000 second nitrocotton is 4.41%, the nitrogen content is 11.94%, the viscosity is 11173 seconds, and Abel is not less than 15min.
Example 3
The production method of 10000 seconds nitrocotton is implemented according to the following steps:
step 1, preparing mixed acid
Taking a proper amount of nitric acid, sulfuric acid and water, and uniformly mixing to obtain mixed acid;
the mass percent of the nitric acid is 22.50 percent, the mass percent of the water is 17.55 percent, and the mass percent of the sulfuric acid is 59.95 percent;
the refined cotton is M1000 grade refined cotton in GB/T9107, and the viscosity of the refined cotton is more than 800mpa & s;
step 2, nitration
Sending the refined cotton into a nitrating machine through a carding machine and a fan, nitrating the refined cotton by adopting mixed acid to obtain acid nitrocotton, sending the acid nitrocotton into a centrifugal machine, adding a proper amount of water for replacement, then sending the acid nitrocotton into a water washing tank for water washing, and then sending the acid nitrocotton into a scouring pot;
the nitrifying machine is a 6-tube U-shaped nitrifying machine, the temperature of the nitrifying treatment is 29 ℃, and the time is 30min;
the centrifugal machine is a double-stage piston material pushing P60 centrifugal machine, and the water adding amount is 975L/h;
step 3, acid cooking
Draining water from nitrocotton in a boiling-washing pot for 40min, thoroughly washing with water for 20min, adding water to submerge the nitrocotton, cold washing for 1h, draining water for 40min after cold washing, adding water to submerge the nitrocotton, performing acid boiling, and draining water to obtain nitrocotton a;
the temperature of acid boiling is 86 ℃, and the time is 2.5h;
the initial acidity of the nitrocotton is 0.5g/L;
step 4, water driving
Pumping the nitrocotton a into a centrifugal machine through a pump for dewatering, then continuously pumping the nitrocotton a into a cellucotton trough into the centrifugal machine for water displacement, and packaging the separated nitrocotton to obtain 10000-second-degree nitrocotton;
the volume concentration of the wine in the cellucotton groove is 72 percent, a wine adding pipe is arranged in the centrifugal machine, and the wine adding amount in the centrifugal machine is 1550L/h;
the 10000-second-degree nitrocotton has the water content of 4.00 percent, the nitrogen content of 12.03 percent, the viscosity of 14423 seconds and Abel of more than or equal to 15min.
Example 4
The production method of 10000 sec nitrocotton is implemented according to the following steps:
step 1, preparing mixed acid
Taking a proper amount of nitric acid, sulfuric acid and water, and uniformly mixing to obtain mixed acid;
the mass percent of the nitric acid is 22.51 percent, the mass percent of the water is 17.58 percent, and the mass percent of the sulfuric acid is 59.91 percent;
the refined cotton is M1000 grade refined cotton in GB/T9107, and the viscosity of the refined cotton is more than 800mpa & s;
step 2, nitration
Sending the refined cotton into a nitrating machine through a carding machine and a fan, nitrating the refined cotton by adopting mixed acid to obtain acid nitrocotton, sending the acid nitrocotton into a centrifugal machine, adding a proper amount of water for replacement, then sending the acid nitrocotton into a water washing tank for water washing, and then sending the acid nitrocotton into a scouring pot;
the nitrifying machine is a 6-tube U-shaped nitrifying machine, the temperature of the nitrifying treatment is 26 ℃, and the time is 30min;
the centrifugal machine is a double-stage piston material pushing P60 centrifugal machine, and the water adding amount is 970L/h;
step 3, acid boiling
Draining water from nitrocotton in a boiling-washing pot for 40min, thoroughly washing with water for 20min, adding water to submerge the nitrocotton, cold washing for 1h, draining water after cold washing for 40min, adding water to submerge the nitrocotton, performing acid boiling, and draining water to obtain nitrocotton a;
the temperature of acid cooking is 86 ℃, and the time is 2.5h;
the initial acidity of the nitrocotton is 0.92g/L;
step 4, driving off water
Pumping the nitrocotton a into a centrifugal machine through a pump for dehydration, then continuously pumping the dewatered nitrocotton a into a wine cotton tank into the centrifugal machine for water displacement, and packaging the separated nitrocotton to obtain 10000-second-degree nitrocotton;
the volume concentration of the wine in the wine cotton groove is 75%, a wine adding pipe is arranged in the centrifugal machine, and the wine adding amount in the centrifugal machine is 1550L/h;
the 10000-second-degree nitrocotton has the water content of 4.16 percent, the nitrogen content of 11.83 percent, the viscosity of 11234 seconds and Abel of more than or equal to 15min.
Example 5
The production method of 10000 seconds nitrocotton is implemented according to the following steps:
step 1, preparing mixed acid
Taking a proper amount of nitric acid, sulfuric acid and water, and uniformly mixing to obtain mixed acid;
the mass percent of the nitric acid is 22.53 percent, the mass percent of the water is 17.60 percent, and the mass percent of the sulfuric acid is 59.87 percent;
the refined cotton is M1000 grade refined cotton in GB/T9107, and the viscosity of the refined cotton is more than 800mpa & s;
step 2, nitration
Sending the refined cotton into a nitrator through a carding machine and a fan, nitrating the refined cotton by adopting mixed acid to obtain acid nitrocotton, sending the acid nitrocotton into a centrifuge, adding a proper amount of water for replacement, then sending the acid nitrocotton into a water washing tank for water washing, and then sending the acid nitrocotton into a scouring pot;
the nitrifying machine is a 6-tube U-shaped nitrifying machine, the temperature of the nitrifying treatment is 25 ℃, and the time is 30min;
the centrifugal machine is a double-stage piston material pushing P60 centrifugal machine, and the water adding amount is 975L/h;
step 3, acid cooking
Draining water from nitrocotton in a boiling-washing pot for 40min, thoroughly washing with water for 20min, adding water to submerge the nitrocotton, cold washing for 1h, draining water after cold washing for 40min, adding water to submerge the nitrocotton, performing acid boiling, and draining water to obtain nitrocotton a;
the temperature of acid cooking is 86 ℃, and the time is 2.5h;
the initial acidity of the nitrocotton is 0.49g/L;
step 4, water driving
Pumping the nitrocotton a into a centrifugal machine through a pump for dewatering, then continuously pumping the nitrocotton a into a cellucotton trough into the centrifugal machine for water displacement, and packaging the separated nitrocotton to obtain 10000-second-degree nitrocotton;
the volume concentration of the wine in the cellucotton groove is 72 percent, a wine adding pipe is arranged in the centrifugal machine, and the wine adding amount in the centrifugal machine is 1650L/h;
the water content of the 10000 second nitrocotton is 4.50%, the nitrogen content is 12.06%, the viscosity is 22287 seconds, and Abel is not less than 15min.
Claims (3)
- The production method of 1.10000 seconds nitrocotton is characterized by comprising the following steps:step 1, preparing mixed acidTaking a proper amount of nitric acid, sulfuric acid and water, and uniformly mixing to obtain mixed acid;step 2, nitrationSending the refined cotton into a nitrating machine through a carding machine and a fan, nitrating the refined cotton by adopting mixed acid to obtain acid nitrocotton, sending the acid nitrocotton into a centrifugal machine, adding a proper amount of water for replacement, then sending the acid nitrocotton into a water washing tank for water washing, and then sending the acid nitrocotton into a scouring pot;step 3, acid boilingDraining water from nitrocotton in a boiling-washing pot for 40min, thoroughly washing with water for 20min, adding water to submerge the nitrocotton, cold washing for 1h, draining water after cold washing for 40min, adding water to submerge the nitrocotton, performing acid boiling, and draining water to obtain nitrocotton a;step 4, driving off waterPumping the nitrocotton a into a centrifugal machine through a pump for dewatering, then continuously pumping the nitrocotton a into a cellucotton trough into the centrifugal machine for water displacement, and packaging the separated nitrocotton to obtain the 10000-second-degree nitrocotton;in the step 1, the mass percent of the nitric acid is 23.0 +/-0.5%, the mass percent of the water is 17.5 +/-0.15%, and the mass percent of the sulfuric acid is 59.5 +/-0.45%;in the step 2, the nitrating machine is a 6-tube U-shaped nitrating machine, the temperature of the nitration treatment is 25-29 ℃, and the time is 30min; the centrifuge is a double-stage piston pusher P60 centrifuge, and the water addition amount is 925 to 975L/h;in the step 3, the acid cooking temperature is 80-90 ℃ and the time is 2.5h; the initial acidity of the nitrocotton is not more than 1g/L;in the step 4, the volume concentration of the wine in the cellucotton groove is 70-75%, a wine adding pipe is arranged in the centrifugal machine, and the wine adding amount in the centrifugal machine is 1500-1650L/h.
- 2. The method for producing the 10000 seconds degree nitrocotton according to claim 1, wherein the 10000 seconds degree nitrocotton has a water content of not more than 4.5%, a nitrogen content of not more than 12.1%, a viscosity of not more than 22287 seconds, and Abel ≥ 15min.
- 3. The method for producing 10000 seconds nitrocotton according to claim 1, wherein the purified cotton is GB/T9107M 1000 grade purified cotton, and the viscosity of the purified cotton is more than 800mPa s.
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Citations (2)
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GB781534A (en) * | 1955-09-20 | 1957-08-21 | Hercules Powder Co Ltd | Improvements in or relating to nitric acid esters of cellulose and process of preparing same |
CN102774524A (en) * | 2012-08-15 | 2012-11-14 | 四川北方硝化棉股份有限公司 | Continuous nitrocotton packaging production process |
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CN102219862B (en) * | 2011-05-30 | 2012-11-21 | 四川北方硝化棉股份有限公司 | Method for preparing superhigh-viscosity energy-containing cellulose nitrate |
CN103319611B (en) * | 2013-06-27 | 2015-06-24 | 南通泰利达化工有限公司 | Production process of 2000s/v nitrocotton |
CN105481617B (en) * | 2016-01-06 | 2017-11-07 | 中北大学 | A kind of Nanocomposite Energetic Materials and preparation method thereof |
CN106188312A (en) * | 2016-07-19 | 2016-12-07 | 南通泰利达化工有限公司 | A kind of production technology of 300 seconds degree nitrocottons |
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Publication number | Priority date | Publication date | Assignee | Title |
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GB781534A (en) * | 1955-09-20 | 1957-08-21 | Hercules Powder Co Ltd | Improvements in or relating to nitric acid esters of cellulose and process of preparing same |
CN102774524A (en) * | 2012-08-15 | 2012-11-14 | 四川北方硝化棉股份有限公司 | Continuous nitrocotton packaging production process |
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