CN102351955B - Nitrocotton boiling and washing method - Google Patents
Nitrocotton boiling and washing method Download PDFInfo
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- CN102351955B CN102351955B CN 201110223462 CN201110223462A CN102351955B CN 102351955 B CN102351955 B CN 102351955B CN 201110223462 CN201110223462 CN 201110223462 CN 201110223462 A CN201110223462 A CN 201110223462A CN 102351955 B CN102351955 B CN 102351955B
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Abstract
The invention belongs to the technical field of nitrocotton production methods, and in particular relates to a nitrocotton boiling and washing method, aiming to provide the nitrocotton boiling and washing method. By using the method, the quality of a product is improved, the consumption of water and steam in a boiling and washing process is reduced, and the production period is shortened. The nitrocotton boiling and washing method comprises the following steps of: after nitration, boiling and washing nitrocotton for 1-4 hours at the temperature of 101-110 DEG C in a 0.5-10g/l diluted sulfuric acid aqueous solution; raising the temperature to 111-150 DEG C and further boiling and washing for 1-5 hours; and thoroughly discharging the aqueous solution and then adding water for washing. According to the invention, boiling and washing starting acidity is controlled, acid water discharge and cold washing are not carried out after an acid boiling process is finished, and impurities in nitrocotton are removed by fully utilizing the strong oxidizability of diluted acid water at a high temperature; temperature is directly raised and then high-temperature boiling and washing is carried out; and a large amount of production practices prove that by using a new process, water-saving and gas-saving effects are obvious, production period is short, and the discharge amount of acid water in the boiling and washing production process is reduced.
Description
Technical field
The invention belongs to nitro-cotton production method technical field, particularly nitro-cotton boils washing method.
Background technology
At present, the technique that domestic nitro-cotton manufacturer produces nitro-cotton be mainly purified cotton nitrated, centrifugal drive after the acid acid nitro-cotton, acid nitro-cotton boil and wash, dehydration, expelling water step, acid nitro-cotton boil the process of washing generally adopt first acid to boil to drain the sour water cold wash after the mode of production of poach two-step approach again, initial acidity sulfuric acid 2～6g/l is boiled in acid, temperature: 100～110 ℃, the time is boiled in acid: 1～4h, the acid of draining is to boil water, again add entry, and intensification poach: 103～150 ℃, the poach time: 1～5h.Non-persistent composition in the nitro-cotton is removed in acting as that acid is boiled, and the effect of poach is the polymerization degree that reduces nitro-cotton.The nitro-cotton product index that such technique obtains is generally transmittance 92～93%, No. 230～250, colourity, whiteness 87～89%.Whole acid nitro-cotton boils to be washed the production cycle and is about 16 hours, and production process steam and water consumption are high, and steam consumption 1.8t/t.NC boils and washes production process sour water quantity discharged large (about 40t/t.NC), causes the nitro-cotton production cost to remain high.
Summary of the invention
Technical problem to be solved by this invention provides a kind of nitro-cotton and boils washing method, and the method can improve the nitro-cotton product quality, reduces to boil and washes the consumption of production process water and steam, shortens the production cycle.
Nitro-cotton boils washing method: after purified cotton is nitrated in the dilute sulfuric acid aqueous solution of 0.5～10g/l 101～110 ℃ boil and wash 1～4 hour, be warming up to 111～150 ℃ and continue to boil and wash 1～5 hour, add water washing after draining the aqueous solution.
The nitrated rear filtration of purified cotton namely gets acid nitro-cotton; Nitro-cotton boils to be washed sour water and connects and to boil rear dehydration, expelling water and namely get the nitro-cotton finished product.
Preferably, it is that purified cotton is boiled in 101～109 ℃ after nitrated and washes 1.2～3.5 hours that nitro-cotton boils washing method, is warming up to 116～146 ℃ and continues to boil and wash 1.6～4.6 hours.
Dilute sulfuric acid aqueous solution concentration is 0.6～9.1g/l.When dilute sulfuric acid aqueous solution concentration was 7.5～9.1g/l, the product transmittance that makes was high.When dilute sulfuric acid aqueous solution concentration was 0.6～0.9g/l, the product whiteness that makes was high, colourity is low.
Adding the water washing time is 0.5～2h, makes nitro-cotton finished acid content be no more than 0.08%, spends height to prevent the nitro-cotton product acid.
Nitro-cotton boils to be washed when temperature is adjusted into 111～150 ℃, according to product viscosity to wash temperature higher in order to wash temperature and time according to adjusting to boil, to boil, it is longer to boil the time of washing, the product viscosity that obtains is lower.
Nitro-cotton is washed production process and must be flooded with boiling wash water whole boiling, and prevents from that nitro-cotton from boiling to wash the process lack of water and decompose.
It is the high-temperature-hot-water more than 100 ℃ to be boiled later in every batch of nitro-cotton acid drain that the tradition nitro-cotton boils washing method, then use the tap water cold wash, poach again again, this production technique water and steam consumes high, production cycle is long, product whiteness is low, colourity is high, and the present invention's control is boiled and washed beginning acidity, and not cold wash of the complete not acid discharge water of process is boiled in acid, take full advantage of the impurity in the diluted acid water strong oxidizing property removal nitro-cotton at high temperature, directly intensification is carried out hot stage again and is boiled and wash, and the quality product that a large amount of production practice proof novel procesies are not only produced is high, and water saving joint vapour effect is remarkable, with short production cycle, reduce and boil the quantity discharged of washing the production process sour water.
Embodiment
Embodiment 1
Nitro-cotton is added in the diluted acid that concentration is 0.6g/l, and control is boiled the cask washing liquid level water level gauge center line (water floods nitro-cotton, prevent nitro-cotton from boiling wash the process lack of water and decompose), 105 ℃ of temperature are boiled in acid, 1.2 hours time is boiled in acid, and temperature is adjusted into 126 ℃, is incubated 3 hours.Get rid of to boil and wash waste water, the discharging in 80 minutes of water cold wash.
The nitro-cotton product index that obtains: nitrogen content 193.2ml/g, No. 180, transmittance 94.2% (top grade product 〉=93%), colourity (top grade≤No. 230), whiteness 91% (top grade 〉=88%)
Steam consumption 1.3t/tNC boils and washes production process sour water quantity discharged 28t/tNC.
Embodiment 2
Nitro-cotton is added in the diluted acid that concentration is 7.5g/l, control is boiled the cask washing liquid level and (nitro-cotton is flooded at the water level gauge center line, preventing that nitro-cotton from boiling washes the process lack of water and decomposes), 109 ℃ of temperature are boiled in acid, and 3.4 hours time is boiled in acid, and temperature is adjusted into 146 ℃, be incubated 1.6 hours, after the poach insulation is finished, get rid of to boil and wash waste water, the discharging in 96 minutes of water cold wash.
The nitro-cotton product index that obtains: nitrogen content 190.4ml/g, No. 210, transmittance 95.0% (top grade product 〉=93%), colourity (top grade≤No. 230), whiteness 89% (〉=88%)
Steam consumption 1.1t/tNC boils and washes production process sour water quantity discharged 25t/tNC.
Embodiment 3
It is in the dilute sulphuric acid of 9.1g/l that the purified cotton nitro-cotton is added concentration, control is boiled the cask washing liquid level and (nitro-cotton is flooded at the water level gauge center line, preventing that nitro-cotton from boiling washes the process lack of water and decomposes), 101 ℃ of temperature are boiled in acid, and 3.2 hours time is boiled in acid, and temperature is adjusted into 116 ℃, be incubated 4.6 hours, after the poach insulation is finished, get rid of to boil and wash waste water, the discharging in 120 minutes of water cold wash.
The nitro-cotton product index that obtains: nitrogen content 194.6ml/g, No. 200, transmittance 94.8% (top grade product 〉=93%), colourity (top grade≤No. 230), whiteness 90% (〉=88%)
Steam consumption 1.4t/tNC boils and washes production process sour water quantity discharged 106t/tNC.
Claims (7)
1. nitro-cotton boils washing method, it is characterized in that: after purified cotton is nitrated in the dilute sulfuric acid aqueous solution of 0.5～10g/l 101～110 ℃ boil and wash 1～4 hour, be warming up to 111～150 ℃ and continue to boil and wash 1～5 hour, add water washing after draining the aqueous solution.
2. nitro-cotton according to claim 1 boils washing method, it is characterized in that: boil in 101～109 ℃ after purified cotton is nitrated and wash 1.2～3.5 hours, be warming up to 116～146 ℃ and continue to boil and wash 1.6～4.6 hours.
3. nitro-cotton according to claim 1 and 2 boils washing method, it is characterized in that: dilute sulfuric acid aqueous solution concentration is 0.6～9.1g/l.
4. nitro-cotton according to claim 1 and 2 boils washing method, it is characterized in that: dilute sulfuric acid aqueous solution concentration is 7.5～9.1g/l.
5. nitro-cotton according to claim 1 and 2 boils washing method, it is characterized in that: adding the water washing time is 0.5～2h.
6. nitro-cotton according to claim 3 boils washing method, it is characterized in that: adding the water washing time is 0.5～2h.
7. nitro-cotton according to claim 4 boils washing method, it is characterized in that: adding the water washing time is 0.5～2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110223462 CN102351955B (en) | 2011-08-05 | 2011-08-05 | Nitrocotton boiling and washing method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110223462 CN102351955B (en) | 2011-08-05 | 2011-08-05 | Nitrocotton boiling and washing method |
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| CN102351955A CN102351955A (en) | 2012-02-15 |
| CN102351955B true CN102351955B (en) | 2013-03-20 |
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| CN 201110223462 Expired - Fee Related CN102351955B (en) | 2011-08-05 | 2011-08-05 | Nitrocotton boiling and washing method |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102774524B (en) * | 2012-08-15 | 2014-04-16 | 四川北方硝化棉股份有限公司 | Continuous nitrocotton packaging production process |
| CN103709255B (en) * | 2013-12-24 | 2016-08-17 | 四川北方硝化棉股份有限公司 | Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives |
| 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 |
| CN112321726B (en) * | 2020-11-23 | 2022-11-25 | 北方化学工业股份有限公司 | Boiling and washing process of low-viscosity high-nitration-degree energy-containing B cotton |
| CN116120471A (en) * | 2022-11-30 | 2023-05-16 | 北方化学工业股份有限公司 | Nitrocotton boiling and washing method |
| CN116621996A (en) * | 2023-04-27 | 2023-08-22 | 北方化学工业股份有限公司 | Industrial nitrocotton stability treatment method |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| DE2727553C2 (en) * | 1977-06-18 | 1983-11-10 | Wolff Walsrode Ag, 3030 Walsrode | Continuous process for the pre-stabilization of pre-deacidified nitrocellulose |
| DE10220270B4 (en) * | 2002-05-07 | 2017-01-26 | Dow Global Technologies Inc. | Continuous process for the preparation and / or processing of polysaccharide derivatives |
| RU2241716C1 (en) * | 2003-06-06 | 2004-12-10 | Федеральное государственное унитарное предприятие "Государственный научно-исследовательский институт химических продуктов" | Method for stabilization of nitrocellulose |
| CN101343329A (en) * | 2008-08-04 | 2009-01-14 | 北京理工大学 | Multi-hydroxyalkyl cellulose ether nitrate and preparation thereof |
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