CN103709255B - Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives - Google Patents
Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives Download PDFInfo
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- CN103709255B CN103709255B CN201310721933.5A CN201310721933A CN103709255B CN 103709255 B CN103709255 B CN 103709255B CN 201310721933 A CN201310721933 A CN 201310721933A CN 103709255 B CN103709255 B CN 103709255B
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Abstract
The invention belongs to the preparing technical field of cellulose esters, be specifically related to Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives.The technical problem to be solved in the present invention is that traditional method COD wastewater discharge is high, boils that to wash technological operation loaded down with trivial details, and energy resource consumption is big, and production efficiency is low.The present invention solves the scheme of above-mentioned technical problem and is to provide a kind of Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, including: by through nitric-sulfuric acid nitrification, drive acid and washing after nitrocellulose, carry out boiling the explosive wastewater nitrocellulose washing, being carefully met after disconnected, fine purifiation requirement successively.The technique that the present invention provides, operates easier, and the production cycle has shortened, and greatly reduces production cost, decreases the discharge of high COD alkalescence cooking water, plays a role in energy saving.
Description
Technical field
The invention belongs to the preparing technical field of cellulose esters, be specifically related to explosive wastewater nitrocellulose viscosity reduction and stable treatment
Technique.
Technical background
Cellulose through nitric-sulfuric acid nitrification, drive acid and washing after, in its capillary tube, be also adsorbed with a number of free sulphur
Acid and nitric acid.Impurity in the some fibre element sulfuric ester, nitric-sulfuric acid ester and the cellulose that generate when these residual acid and nitration reaction
(such as many contracting penta candy, lignins etc.) are become the unease impurity such as nitrification carbohydrate by nitrification.These unease impurity can cause nitrification
The decomposition of cellulose, burn and explode.Therefore, the nitrocellulose after washing must carry out viscosity reduction and stable treatment.
Traditional explosive wastewater nitrocellulose viscosity reduction and stable treatment method be: by the nitrocellulose after washing finite concentration,
The water of temperature carries out boiling wash, boil and after washing, sour water is drained, thoroughly wash with neutral water；Add water and add alkali so that nitrocellulose exists
Certain basicity, at a temperature of boil and wash, boil and also alkaline water is drained after washing, thoroughly wash with neutral water, reach viscosity reduction and remove unease
The purpose of impurity, meanwhile, alkalescence is boiled to wash and also can be improved the follow-up thin disconnected effect of nitrocellulose；But boil the nitrocellulose after washing its
In capillary tube, residual acid can not eliminate completely, and the stability index obtaining product does not reaches requirement yet, it is necessary to carefully breaks through follow-up
Stable treatment further with fine purifiation process；Thin breaking is to wash, by boiling, the nitrocellulose that rear fiber is longer, by the mechanical thing of shredder
Reason effect, by fibre cutting with grind, increases the specific surface area of fiber, and the residual acid in fiber capillary is easier to leach, and carefully breaks
Process is carried out in water, and need to keep the alkalescence of thin disconnected water by adding alkali；The nitrocellulose carefully having no progeny also needs
In alkaline medium, carry out thermal washing and cold wash, remove the unease impurity such as residual acid further.
Above-mentioned traditional processing technology uses alkali to remove the unease impurity in nitrocellulose, can produce substantial amounts of spent lye (about
7m3/ t product), and COD(COD) high (about 2000mg/L), meanwhile, boil that to wash technological operation loaded down with trivial details, the energy
Consuming big, production efficiency is low.
Summary of the invention
The technical problem to be solved in the present invention is that traditional method COD wastewater discharge is high, boils that to wash technological operation loaded down with trivial details, energy resource consumption
Greatly, production efficiency is low.
The present invention solves the scheme of above-mentioned technical problem and is to provide a kind of explosive wastewater nitrocellulose viscosity reduction and the work of stable treatment
Skill.
Above-mentioned Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives includes: will through nitric-sulfuric acid nitrification, drive acid and water
Nitrocellulose after washing, carries out boiling the explosive wastewater nitrocellulose washing, being carefully met after disconnected, fine purifiation requirement successively.
Wherein, in above-mentioned Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, it is to boil in acid water that described boiling is washed
Wash.Boiling the operation washed in described acid water is: in acid solution, boils prior to 70 DEG C～130 DEG C and washes 1～15h, it is preferred that first
Boil in 90～120 DEG C and wash 5～10h；Then heat to 80 DEG C～140 DEG C boil again and wash 1～15h, it is preferred that be warming up to 100～
125 DEG C are boiled and wash 2～8h.The concentration of described acid solution is calculated as 0.1～5g/L with sulphuric acid, wherein contains in sulphuric acid or nitric acid at least
A kind of.
Wherein, in above-mentioned Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, described thin breaking is to boil washed nitre
The fibre cutting of cellulose and grinding.
Wherein, in above-mentioned Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, described thin disconnected during need to add
Alkali.Described alkali is any one in sodium hydroxide, sodium carbonate, sodium bicarbonate.The addition of described alkali is 2.5～5kg/t nitre
Cellulose.The Adding Way of described alkali is that after being dissolved by solid base, gradation adds.Wherein, aqueous slkali is formed after solid base dissolves
Concentration >=90g/L.
Wherein, in above-mentioned Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, described fine purifiation is first to use hot water fine purifiation,
Room temperature cold wash again.The temperature of described hot water fine purifiation is 50～100 DEG C；It is preferably 80～97 DEG C.The time of described hot water fine purifiation is
0.5～15h；It is preferably 1～8h.The time of described room temperature cold wash is 0.25～2h, preferably 0.5～1h.
Wherein, in above-mentioned Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, need during described hot water fine purifiation
Alkali to be added.Described alkali is any one in sodium hydroxide, sodium carbonate, sodium bicarbonate.The addition of described alkali is
0.25～3kg/t nitrocellulose.The Adding Way of described alkali is to add in poacher after solid base dissolving.
The beneficial effects of the present invention is: the technique that the present invention provides is to boil nitrocellulose in acid water to wash, and reduces
Washed journey of soda boiling, decreases number of times material and water heated up, and technological operation is easier, and the production cycle has contracted
Short, greatly reduce production cost.Meanwhile, decrease the discharge of high COD alkalescence cooking water, play a role in energy saving.
Detailed description of the invention
Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, comprises the following steps:
A, by through nitric-sulfuric acid nitrification, drive acid and washing after nitrocellulose boil in acid water and wash；Described acid decocting in water is washed
Operation be:: in acid solution, boil prior to 70 DEG C～130 DEG C and wash 1～15h, it is preferred that boil in 90～120 DEG C and wash 5～10h；
Then heat to 80 DEG C～140 DEG C boil again and wash 1～15h, it is preferred that boil in 100～125 DEG C and wash 2～8h；Described acid solution
Concentration is calculated as 0.1～5g/L with sulphuric acid, wherein contains at least one in sulphuric acid or nitric acid；
B, and grind boiling washed nitrocellulose shredder fibre cutting；Described thin disconnected during need to add alkali；
Described alkali is any one in sodium hydroxide, sodium carbonate, sodium bicarbonate；
C, the nitrocellulose elder generation hot water fine purifiation that will carefully have no progeny, then room temperature cold wash, be met the explosive wastewater nitrocellulose of requirement
Element；The temperature of described hot water fine purifiation is 50～100 DEG C, preferably 80～97 DEG C；The time of described hot water fine purifiation is 0.5～15h, excellent
Elect 1～8h as；The time of room temperature cold wash is 0.25～2h, preferably 0.5～1h；Need during described hot water fine purifiation to add alkali.
Wherein, in above-mentioned Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, described requirement is GJB3204-1998
" military products nitrocotton general specification ", is specifically shown in Table 1.
Table 1 explosive wastewater nitrocellulose viscosity reduction and the requirement of stable treatment
| Article Number index | B level is cotton | C level is cotton | D level is cotton |
| The degree of nitration (mL/g) | ≥210.3 | 190.0～198.3 | 188.0～193.5 |
| Alcohol ether dissolubility (%) | ≤15 | ≥97 | ≥98 |
| Ethanol dissolubility (%) | ≤4.0 | ≤7.0 | ≤12.0 |
| Permanence (mL/g) | ≤3.5 | ≤2.5 | ≤2.5 |
| Basicity (%) | ≤0.25 | ≤0.25 | ≤0.2 |
| Ash (%) | ≤0.5 | ≤0.5 | ≤0.5 |
| Viscosity (mm2/S) | ≥20.5 | ≥20.5 | 10.0～17.4 |
| Thin disconnected degree (mL) | ≤90 | ≤90 | ≤70 |
Wherein, in above-mentioned Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, the addition of alkali described in step b is
2.5～5kg/t nitrocelluloses.The Adding Way of described alkali is that after being dissolved by solid base, gradation adds.Wherein, after solid base dissolves
Form the concentration >=90g/L of aqueous slkali.
Wherein, in above-mentioned Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, the alkali described in step c be sodium hydroxide,
Any one in sodium carbonate, sodium bicarbonate.The addition of described alkali is 0.25～3kg/t nitrocellulose.The addition of described alkali
Method is to add in poacher after solid base dissolving.
In step a, along with the raising of the concentration of acid solution, byproduct of reaction will be hydrolyzed, and the stability of product is improved,
But can aggravate macromolecules degradation, therefore the concentration of acid solution can not be too high simultaneously.
In step a, if it is too short to boil the time washed in acid water, by-product can be made to remove clean, product stability is bad；If time
Between long production cycle length and viscosity reduction serious.If it is too low to boil the temperature washed in acid water, by-product also can be made to remove unclean, product
Stability is bad；If temperature is too high, to will also result in viscosity reduction serious.Generally boiling and washing operation is to boil in cask washing what a kind of carrying vapour circulated
Carry out.
In step b, thin breaking is the specific surface area in order to increase fiber, makes the residual acid in fiber capillary be easier to leach.Thin disconnected
Process need to add the basicity that alkali remains certain, removes residual acid further, increases product stability.The main alkali position that adds is in charging
Groove and thin disconnected during concentration groove in.
COD detection in embodiment uses the dichromate titration that GB/T11914-1989 water chemical oxygen demand measures, remaining
Index presses the method detection of GJB3204-1998 " military products nitrocotton general specification ".
Embodiment 1
500g nitrification, the nitrocellulose washed being added in digester, carry out acid decocting in water, the acid solutions that acid is boiled is
2.0g/L(is with sulphur acid meter), temperature controls at 80 DEG C～85 DEG C, time 8h, after the most directly heat up acid decocting in water, temperature controls
90 DEG C～95 DEG C, time 6h.Carefully breaking through shredder, adding sodium bicarbonate amount is 0.2g again.The poacher fine purifiation stirred by band again,
Hot water fine purifiation twice, fine purifiation temperature is 85～90 DEG C for the first time, and the time is 4h, adds sodium bicarbonate 0.1g, then draining add water into
The row hot fine purifiation of second time, fine purifiation temperature is 80～85 DEG C, and the time is 3h, adds sodium bicarbonate 0.05g, then draining, uses cold water
Washing 0.5h i.e. prepares explosive wastewater nitrocellulose.
8.6 ° of E of the viscosity of explosive wastewater nitrocellulose obtained by the present embodiment, thin disconnected degree 95mL, 140 soundness tests
2.02mL/g, basicity 0.17%(is with calcium carbonate), alcohol ether dissolubility, nitrogen content, ash index of grading all meets the requirements；Boil and wash
Water COD:355mg/L.
Embodiment 2
500g nitrification, the nitrocellulose washed being added in digester, carry out acid decocting in water, the acid solutions that acid is boiled is
3.5g/L(is with sulphur acid meter), temperature controls at 90 DEG C～95 DEG C, time 7h, after the most directly heat up acid decocting in water, temperature controls
100 DEG C～105 DEG C, time 7h, carefully break through shredder, adding sodium carbonate amount is 0.35g, then the poacher fine purifiation stirred by band,
Hot water fine purifiation twice, fine purifiation temperature is 82～85 DEG C for the first time, and the time is 4h, adds sodium carbonate 0.15g, and then draining adds water and carries out
The hottest fine purifiation, fine purifiation temperature is 86～91 DEG C, and the time is 4h, adds sodium carbonate 0.10g then draining, washs 1h with cold water
I.e. prepare explosive wastewater nitrocellulose.
7.2 ° of E of the viscosity of explosive wastewater cellulose obtained by the present embodiment, thin disconnected degree 100mL, 140 soundness tests
2.32mL/g, basicity 0.37%(is with calcium carbonate), alcohol ether dissolubility, nitrogen content, ash index of grading all meets the requirements；Boil and wash
Water COD:286mg/L.
Embodiment 3
500g nitrification, the nitrocellulose washed being added in digester, carry out acid decocting in water, the acid solutions that acid is boiled is
2.8g/L(is with sulphur acid meter), temperature controls at 100 DEG C～105 DEG C, time 6h, after the most directly heat up acid decocting in water, temperature controls
At 105 DEG C～108 DEG C, time 7h, carefully to break through shredder, hydro-oxidation sodium amount is 0.18g, then the poacher stirred by band
Fine purifiation, hot water fine purifiation twice, fine purifiation temperature is 86～89 DEG C for the first time, and the time is 2h, hydro-oxidation sodium 0.15g, then draining
Adding water and carry out the hot fine purifiation of second time, fine purifiation temperature is 83～86 DEG C, and the time is 2h, hydro-oxidation sodium 0.10g then draining, uses
Cold water washing 0.5h i.e. prepares explosive wastewater nitrocellulose.
6.5 ° of E of the viscosity of explosive wastewater cellulose obtained by the present embodiment, thin disconnected degree 92mL, 140 soundness test 1.95mL/g,
Basicity 0.22%(is with calcium carbonate), alcohol ether dissolubility, nitrogen content, ash index of grading all meets the requirements；Boil wash water COD:
303mg/L。
Embodiment 4
500g nitrification, the nitrocellulose washed being added in digester, carry out acid decocting in water, the acid solutions that acid is boiled is
2.8g/L(is with sulphur acid meter), temperature controls at 110 DEG C～115 DEG C, time 6h, after the most directly heat up acid decocting in water, temperature controls
At 113 DEG C～116 DEG C, time 5h, carefully break through shredder, adding sodium carbonate amount is 0.15g, then the poacher essence stirred by band
Washing, hot water fine purifiation twice, fine purifiation temperature is 90～94 DEG C for the first time, and the time is 3h, adds sodium carbonate 0.13g, and then draining adds water
Carrying out the hot fine purifiation of second time, fine purifiation temperature is 93～96 DEG C, and the time is 2h, adds sodium carbonate 0.10g then draining, washes with cold water
Wash 1h and i.e. prepare explosive wastewater nitrocellulose.
4.1 ° of E of the viscosity of explosive wastewater cellulose obtained by the present embodiment, thin disconnected degree 86mL, 140 soundness test 1.63mL/g,
Basicity 0.16%(is with calcium carbonate), alcohol ether dissolubility, nitrogen content, ash index of grading all meets the requirements；Boil wash water COD:
333mg/L。
Embodiment 5
500g nitrification, the nitrocellulose washed being added in digester, carry out acid decocting in water, the acid solutions that acid is boiled is
2.8g/L(is with sulphur acid meter), temperature controls at 115 DEG C～120 DEG C, time 5h, after the most directly heat up acid decocting in water, temperature controls
At 122 DEG C～125 DEG C, time 4h, carefully break through shredder, adding sodium bicarbonate amount is 0.20g, then the poacher stirred by band
Fine purifiation, hot water fine purifiation twice, fine purifiation temperature is 90～94 DEG C for the first time, and the time is 4h, adds sodium bicarbonate 0.10g, then draining
Adding water and carry out the hot fine purifiation of second time, fine purifiation temperature is 93～96 DEG C, and the time is 2h, adds sodium bicarbonate 0.05g then draining, uses
Cold water washing 2h i.e. prepares explosive wastewater nitrocellulose.
2.8 ° of E of the viscosity of explosive wastewater cellulose obtained by the present embodiment, thin disconnected degree 84mL, 140 soundness test 1.77mL/g,
Basicity 0.09%(is with calcium carbonate), alcohol ether dissolubility, nitrogen content, ash index of grading all meets the requirements；Boil wash water COD:
364mg/L。
Embodiment 6
500g nitrification, the nitrocellulose washed being added in digester, carry out acid decocting in water, the acid solutions that acid is boiled is
2.3g/L(is with sulphur acid meter), temperature controls at 110 DEG C～115 DEG C, time 7h, after the most directly heat up acid decocting in water, temperature controls
At 115 DEG C～118 DEG C, time 5h, carefully break through shredder, adding sodium carbonate amount is 0.15g, then the poacher essence stirred by band
Washing, hot water fine purifiation twice, fine purifiation temperature is 90～92 DEG C for the first time, and the time is 4h, adds sodium carbonate 0.10g, and then draining adds water
Carrying out the hot fine purifiation of second time, fine purifiation temperature is 88～90 DEG C, and the time is 2h, adds sodium carbonate 0.05g then draining, washes with cold water
Wash 0.75h and i.e. prepare explosive wastewater nitrocellulose.
4.5 ° of E of the viscosity of explosive wastewater cellulose obtained by the present embodiment, thin disconnected degree 88mL, 140 soundness test 1.85mL/g,
Basicity 0.12%(is with calcium carbonate), alcohol ether dissolubility, nitrogen content, ash index of grading all meets the requirements；Boil wash water COD:
267mg/L。
The technique that the present invention provides, operates easier, and the production cycle has shortened, and greatly reduces production cost, reduces
The discharge of high COD alkalescence cooking water, plays a role in energy saving.
Claims (3)
1. Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives, its step includes: will through nitric-sulfuric acid nitrification, drive
Nitrocellulose after acid and washing, carries out boiling the explosive wastewater nitrocellulose washing, being carefully met after disconnected, fine purifiation requirement successively
Element；Described thin disconnected during need to add alkali, described alkali is any one in sodium hydroxide, sodium carbonate, sodium bicarbonate；
Described boiling that to wash be to boil to wash in acid water, the operation that described acid decocting in water is washed is: in acid solution, boil prior to 90～120 DEG C
Wash 5～10h, then heat to 100～125 DEG C and boil and wash 5～8h；The concentration of described acid solution is calculated as 0.1～5g/L with sulphuric acid,
Wherein contain at least one in sulphuric acid or nitric acid；Described fine purifiation is first to use hot water fine purifiation, then room temperature cold wash；Described hot water essence
The temperature washed is 50～100 DEG C, and the time of described hot water fine purifiation is 0.5～15h；The time of described room temperature cold wash is 0.25～2h；Institute
Needing during stating hot water fine purifiation to add alkali, described alkali is any one in sodium hydroxide, sodium carbonate, sodium bicarbonate,
The addition of described alkali is 0.25～3kg/t nitrocellulose.
Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives the most according to claim 1, it is characterised in that: institute
Stating the addition of alkali during carefully breaking is 2.5～5kg/t nitrocelluloses.
Technique for performing viscosity reduction and stabilization treatment on nitrocellulose for propellants and explosives the most according to claim 1, it is characterised in that: institute
The temperature stating hot water fine purifiation is 80～97 DEG C；The time of described hot water fine purifiation is 1～8h；The time of described room temperature cold wash is 0.5～1h.
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| CN104003825B (en) * | 2014-05-30 | 2016-08-24 | 泸州北方化学工业有限公司 | Wood pulp nitrocellulose single-base gun propellant and preparation method thereof |
| CN109504487B (en) * | 2018-10-18 | 2022-02-22 | 梅万伦 | Method for preparing fuel by nitrating mixture of plant cellulose and lignin |
| CN111763265A (en) * | 2020-07-14 | 2020-10-13 | 北京理工大学 | Method for refining nitration bamboo cellulose crude product |
| CN112409497A (en) * | 2020-11-09 | 2021-02-26 | 北方化学工业股份有限公司 | Preparation method of low-ash energy-containing nitrocotton |
| 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 |
| CN113969513B (en) * | 2021-10-28 | 2023-07-25 | 北方化学工业股份有限公司 | Method for breaking nitrocellulose |
| 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 |
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| CN102219861A (en) * | 2011-05-30 | 2011-10-19 | 四川北方硝化棉股份有限公司 | Method for preparing cellulose nitrate for explosive from wood pulp |
| CN102351955A (en) * | 2011-08-05 | 2012-02-15 | 四川北方硝化棉股份有限公司 | Nitrocotton boiling and washing method |
| CN102807623A (en) * | 2012-08-17 | 2012-12-05 | 四川北方硝化棉股份有限公司 | Acid removal process for nitrocotton |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219861A (en) * | 2011-05-30 | 2011-10-19 | 四川北方硝化棉股份有限公司 | Method for preparing cellulose nitrate for explosive from wood pulp |
| CN102351955A (en) * | 2011-08-05 | 2012-02-15 | 四川北方硝化棉股份有限公司 | Nitrocotton boiling and washing method |
| CN102807623A (en) * | 2012-08-17 | 2012-12-05 | 四川北方硝化棉股份有限公司 | Acid removal process for nitrocotton |
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