CN1052484A - With cotton stalk is that raw material is made nitrocellulosic method - Google Patents
With cotton stalk is that raw material is made nitrocellulosic method Download PDFInfo
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- CN1052484A CN1052484A CN 90109489 CN90109489A CN1052484A CN 1052484 A CN1052484 A CN 1052484A CN 90109489 CN90109489 CN 90109489 CN 90109489 A CN90109489 A CN 90109489A CN 1052484 A CN1052484 A CN 1052484A
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Abstract
With cotton stalk is that raw material is made nitrocellulosic method, relates to the refining and soluble cotton manufacturing technology of cotton fibre surrogate.The present invention is that the water solubles and wax wherein removed in the hydrolysis of raw material employing plain boiled water with cotton stalk, produces the cotton stalk fiber element with ternary mixed alkali liquor saponification method again.Adopt the consumption of plain boiled water hydrolysis can minimizing alkali, reduce cost.Adopt Viscotrol C-rosin mixing saponifying agent can improve refined cellulose quality and product yield.Nitro-cotton stalk fiber element can replace nitro-cotton to make the various uses of pyroxylin(e)finish, zylonite, smokeless powder and other military products and artificial silk and regenerated fiber.
Description
The present invention relates to the refining and nitrocellulosic manufacturing technology of cotton fibre surrogate.
Cotton stalk fiber belongs to kind of a subclass stem fiber element, is made up of bast and cane two portions.Bast in the cane outside, fibre content are up to 70%, and the stipe part content of cellulose of removing after the bast is generally 40-45%, and the plain average content of whole stem fiber can reach between the 48-54%.China's cotton stalk resource is abundant, and in the cotton growing area, cotton stalk uses that generally just act as a fuel, high-load Mierocrystalline cellulose is burnt real in wasting greatly in the cotton stalk.
The objective of the invention is to, resourceful cotton stalk is processed, extract Mierocrystalline cellulose,, the depleted coarse raw materials is converted into the industrial chemicals with special purpose, promote the well-being of mankind as the civilian or military purposes.
Technical scheme of the present invention is: cotton stalk is placed on the screen cloth, remove dust and other impurity that cotton stalk is brought into by compressed-air actuated wind-force, compressed-air actuated pressure-controlling is at 3.2～3.5Kg/cm
2Can reach the purpose of impurity such as removing dust and leaf.The clean cotton stalk of removing impurity is to be cut into 40-60mm length after two roller machines about 2mm crush can feed intake through spacing.The cotton stalk of chopping is dropped in the stainless steel cauldron, with water heat altogether, is that 120-130 ℃, pressure are 2-2.5Kg/cm in temperature
2Condition under, kept 20-40 minute, make cotton stalk hydrolysis in water, removing the water solubles and the wax in the cotton stalk, and reduce the part macromolecular structure, make cotton stalk become loose.Drain hydrolysis not behind the liquid, will add the common hot digestion of loose cotton stalk after reactor and the hydrolysis again by the ternary mixed alkali liquor that sodium hydroxide, sodium sulphite and water glass are formed.The add-on of NaOH is the 3-3.5% of material gross weight in the mixed alkali liquor; The sodium sulphite add-on is the 1.5-1.9% of total weight of material; The water glass add-on is the 0.2-0.3% of total inventory, and heating up during boiling is controlled at 145-160 ℃, and pressure-controlling is at 2.8-3.2Kg/cm
2Keep after 70-90 minute, the mixing saponifying agent that adding is made up of Viscotrol C and rosin, this saponifying agent are in Viscotrol C: rosin=0.5～1.5: 9.5～8.5 ratio is mixed with Viscotrol C one rosin mixing saponifying agent, and its consumption is 0.25～0.35% of total weight of material.Be incubated 60-80 minute after adding saponifying agent, make it to take place saponification reaction.In the reaction process every exhaust in 30 minutes once, and circulation stirring reaction liquid.After reaction finishes, treat that temperature and pressure recovers the washing of discharging just often.Carry out chlorination, bleaching with sodium hypochlorite solution again through the cotton stalk fiber element after saponification and the washing.Through two, three sections rinsings (if as military nitrocotton raw material then only make second stage bleaching), reenter and be washed till no chlorion in the rinsing machine, when PH is 7.2～7.5, again with 0.025% sulfuric acid or pin acid neutralization, continue to wash to PH be 6.8～7.2, after deironing, desanding, concentrate and just get purified cotton rod fibers element, it can be shaped to the thick cloth of 0.85～1.20mm (like velveteen cloth two sides hairiness), also can directly extract by extracting machine.The above-mentioned Mierocrystalline cellulose that makes after shredding machine, the machine of shaking up tear up, mix pine, is given baking 5 minutes (make in the Mierocrystalline cellulose moisture content less than 3%) under 105～110 ℃ of temperature, carry out nitrated with nitre, sulphur nitration mixture again.Nitrated equipment adopts U type continuous nitrification device.Nitrated finish to drive to reenter in the rinsing machine after the acid with whizzer wash.Through the soluble cotton of washing with about 0.5% dilute sulphuric acid 110～115 ℃ boil wash after, water boils in 115～120 ℃ and is washed till neutrality and promptly finishes the stability processing again.The soluble cotton that the process stability is handled is preserved in the ethanol that contains 30% moisture content (neutrality) or 30% or is transported all safe and reliable.
Adopt production method of the present invention, refining with the mixed base saponification method again after cotton stalk is hydrolyzed in folding water, can make the cotton stalk fiber element.In hydrolytic process, remove after the water solubles and the wax, add mixed alkali liquor again, can reduce the consumption of alkali, alleviate the pollution in the refined cellulose process simultaneously.Add Viscotrol C-rosin saponifying agent and help the refining of cotton stalk fiber element, can improve refining quality, improve the product yield, help nitration reaction and carry out, shorten the production cycle thereby reduce production costs.Make soluble cotton with linters and compare, can reduce cost about 19.3%.The soluble cotton that purified cotton rod fibers element is produced can replace nitro-cotton to make pyroxylin(e)finish, zylonite, smokeless powder and other military products, also can be used as artificial silk and artificial cellulose's various uses.
Embodiment:
Can make nitrated nitro-cotton rod fibers element when operating with listed index in purified cotton rod fibers element and the table three as the listed index of table two by the listed process control condition of table one.
Table one: process control condition
Stage project control index remarks
Dedusting compressed air pressure 3.2～3.5Kg/cm
2
The roller spacing 2.0～3.2mm of two roller machines
Broken two roller machine working temperatures are lower than 35 ℃
Input speed 15～20 kg/minute
Cut off cotton stalk length 40～60mm
Input speed 40～55 kg/minute
128～130 ℃ of top temperatures
Pressure 2.2～2.3Kg/cm
2
Plain boiled water hydrolysis solid-to-liquid ratio 1: 7
35 minutes reaction times reached temperature
Calculate after 148～154 ℃ of the top temperatures
Pressure 2.8～3.2Kg/cm
2
1: 8 cotton stalk of boiling saponification solid-to-liquid ratio with
NaOH add-on 3.2% alkali lye it
Na
2S add-on 1.7% ratio
Na
2Sio
3Add-on 0.25%
The Viscotrol C add-on
Rosin add-on 0.32% is pressed 10% ratio
Example is in rosin
Add Viscotrol C
Total reaction time 240 minutes
Chlorination rinsing slurry concentration 6%
Chlorine dosage (to slurry) 1.8%
Nitration reaction H
2SO
468.44
HNO
321.87
Nitrogen oxide 1.22
Water 8.07
Rate of feeding 8 kg/minute are according to nitrated fibre
22～24 ℃ of plain nitrogen contents of dimension of nitration reaction temperature
The nitration reaction time can be adjusted reaction
Time
Stability treatment temp (1) acid is boiled 112 ℃
(2) poach is 115～120 ℃
0.7kg/cm is boiled in pressure (1) acid
2
(2) poach 1.25kg/cm
2
H
2SO
4Add-on 0.47%
Table two is nitrated with cotton stalk fiber quality figureofmerit (%)
Measured data
Project proposes index 123 remarks
Alpha-cellulose 95 96.72 97.22 97.89
Five-carbon sugar 3.5 2.72 2.11 1.50
12% NaOH 85 93.27 92.22 94.53 in the time of-5 ℃
Insolubles
Viscosity 15～40 33.5 34.2 31.9 unit centipoises
Sulfuric acid insolubles 0.5 0.12 0.15 0.11
Xylogen 0.5 0.23 0.29 0.26
Ash 0.5 0.18 0.23 0.24
Moisture content 8 3.82 3.90 3.70
Hydroscopicity is greater than 110 gram water 134.2 136.4 128.7
/ gram Mierocrystalline cellulose
Table three nitro-cotton rod fibers quality figureofmerit (%)
The WJ23-64 measured data
The project indicator 123
Nitrogen content 12.20～13.50 13.494 13.532 13.573
The alcohol ether solute is not more than 30 12.3 13.2 9.7
The dissolve with ethanol degree is not more than 4 1.4 1.2 1.1
Viscosity (E °) 3.0～15 4.8 5.2 4.4
140 ℃ of Beckman tests are not more than 3 1.87 2.01 1.96
Methyl-violet test 70-60 80-70 80-70 80-70
Ash is not more than 0.4 0.18 0.23 0.21
Yield 175.47 176.10 176.38
Claims (3)
1, be that raw material is made nitrocellulosic method with the cotton stalk, refining and the nitrocellulosic manufacturing technology that relates to the cotton fibre surrogate, be the hydrolysis saponification method to be given in deimpurity raw material employing produce the cotton stalk fiber element, the purified cotton rod fibers element after its chlorination, the rinsing is handled with mixed acid nitrification and through stability again and can be made nitro-cotton rod fibers element, technical characterictic of the present invention is:
A, employing pressurized air are removed the impurity in the cotton stalk, are total to heat with water in the chopping input reactor after it is crushed and carry out the plain boiled water hydrolysis, at 120～130 ℃ of temperature, pressure 2～2.5Kg/cm
2Keep under the condition draining after 20～30 minutes hydrolysis not liquid add the ternary mixed alkali liquor again and carry out boiling to remove the water solubles and wax, at 145～160 ℃ of temperature, pressure 2.8～3.2Kg/cm
2After keeping 70～90 minutes under the condition, add Viscotrol C-rosin mixing saponifying agent, be incubated 60-80 minute again, make it to take place saponification reaction;
B, the cotton stalk fiber element after refining may be molded to the Mierocrystalline cellulose cloth of two-sided hairiness, also availablely extract machine and directly extract;
C, purified cotton rod fibers element is torn up, carries out after shaking up nitrated again with (machine of shaking up) with shredding machine.
2, according to the described method of claim 1, it is characterized in that: the ternary mixed alkali liquor is made up of sodium hydroxide, sodium sulphite and water glass, and its consumption is respectively 3～3.5%, 1.5～1.9%, 0.2～0.3% of weight of material.
3, according to the described method of claim 1, it is characterized in that: Viscotrol C-rosin mixing saponifying agent is in Viscotrol C: rosin=0.5～1.5: 9.5～8.5 ratio is formulated, and its consumption is 0.25～0.35% of total weight of material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90109489 CN1052484A (en) | 1990-11-24 | 1990-11-24 | With cotton stalk is that raw material is made nitrocellulosic method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90109489 CN1052484A (en) | 1990-11-24 | 1990-11-24 | With cotton stalk is that raw material is made nitrocellulosic method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1052484A true CN1052484A (en) | 1991-06-26 |
Family
ID=4881457
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90109489 Pending CN1052484A (en) | 1990-11-24 | 1990-11-24 | With cotton stalk is that raw material is made nitrocellulosic method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1052484A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219862A (en) * | 2011-05-30 | 2011-10-19 | 四川北方硝化棉股份有限公司 | Method for preparing superhigh-viscosity energy-containing cellulose nitrate |
| CN103497076A (en) * | 2013-09-26 | 2014-01-08 | 白雪 | Preparation method of waste paper nitrocellulose blasting powder |
-
1990
- 1990-11-24 CN CN 90109489 patent/CN1052484A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219862A (en) * | 2011-05-30 | 2011-10-19 | 四川北方硝化棉股份有限公司 | Method for preparing superhigh-viscosity energy-containing cellulose nitrate |
| 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 |
| CN103497076A (en) * | 2013-09-26 | 2014-01-08 | 白雪 | Preparation method of waste paper nitrocellulose blasting powder |
| CN103497076B (en) * | 2013-09-26 | 2016-09-07 | 白雪 | Preparation method of waste paper nitrocellulose gunpowder |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |