CN102219861A - Method for preparing cellulose nitrate for explosive from wood pulp - Google Patents
Method for preparing cellulose nitrate for explosive from wood pulp Download PDFInfo
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- CN102219861A CN102219861A CN 201110141936 CN201110141936A CN102219861A CN 102219861 A CN102219861 A CN 102219861A CN 201110141936 CN201110141936 CN 201110141936 CN 201110141936 A CN201110141936 A CN 201110141936A CN 102219861 A CN102219861 A CN 102219861A
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Abstract
The invention relates to a method for preparing cellulose nitrate for an explosive from wood pulp, in particular relates to a preparation method of cellulose nitrate for an explosive and belongs to the technical field of cellulose preparation. The method is characterized by comprising the following steps: adding 20-30 parts by weight of wood pulp in 500 parts by weight of mixed acid, carrying out middle-low temperature nitration reaction and then washing; and then successively carrying out boil washing, shredding and refine washing so as to obtain the cellulose nitrate for the explosive. In the preparation method of the cellulose nitrate, the wood pulp is used as a raw material, which is not a precedent in the field of military cellulose nitrate, thereby broadening the use range of the raw material in nitrated cellulose production, and simultaneously, the wood pulp is cheaper than cotton linter and can be used as the raw material of energy-containing nitrated cotton for production, thereby greatly solving the cost problem of the raw material; and at the same time, the environmental protection pressure problem brought by a large amount of cotton dust, black liquid and acidic wastewater which are generated in the processes of cotton opening, boiling, bleaching and drying refined cotton when a nitrated cotton product is prepared by utilizing the cotton linter as the raw material is solved.
Description
Technical field
The present invention relates to a kind of is the method for feedstock production cellulose nitrate with the wood pulp, particularly relates to the preparation method of a kind of fiery explosive with cellulose nitrate, belongs to the preparing technical field of cellulose ester.
Background technology
Cellulose nitrate is commonly called as nitro-cotton or nitrocotton, is the product of Mierocrystalline cellulose and nitric acid reaction, is the important source material of making propelling charge, guided missile, rocket propellant.
The main raw material(s) of cellulose nitrate production is a linters.1. contain impurity such as cellulosic concomitant product and the cotton seed hulls of in the cotton ginning process, bringing into, cotton boll skin and dust in the linters, these materials are not driven away to a certain degree, all can bring detrimentally affect for the nitrated production safety of the quality of nitro-cotton and nitric-sulfuric acid and quality of gunpowder etc.2. in addition, the nitration product of pectin, xylogen, pentosan remains in the nitro-cotton, can reduce the chemical stability of nitro-cotton, can also reduce the nitrogen content and the yield of nitro-cotton.3. the fat of linters, wax and content of lignin height can be by vigorous oxidations in nitrifying process, produce local superheating and nitro-cotton decomposed catch fire.4. inorganic salts is non-energy ingredient, and content can cause the energy of gunpowder to reduce too much in the nitro-cotton, and the cigarette during shooting increases.Owing to above reason, must make with extra care as the cotton fibre of making the nitro-cotton raw material, and can use after meeting the certain quality index.Owing to the fast development of chemical fibre industry and derivatived cellulose industry, the main raw material(s) linters price of cellulose nitrate production went up always in recent years.The purified effect is to remove the non-cellulose composition, reduces viscosity simultaneously, the homogeneity of ensuring the quality of products.But, the purified cotton production process from opener, boiling, bleach the oven dry will produce a large amount of cotton dirt, black liquor and acid waste water, the environmental protection pressure problem of bringing.
Therefore, this area need seek new starting material replace cotton short flannel be used to contain can nitro-cotton production.So far, do not see that adopting wood pulp is the method for feedstock production fire explosive with cellulose nitrate.
Summary of the invention
The object of the present invention is to provide a kind of is the method for raw material preparing cellulose nitrate with the wood pulp, save the purified cotton production process, avoided the generation of a large amount of cotton dirt, waste water, the preparing product index satisfies GJB3204-1998 " military products nitro-cotton general specification " requirement.
Technical scheme of the present invention:
Prepare the method for fiery explosive by wood pulps, it is characterized in that through following steps with cellulose nitrate:
The wood pulp that adds 20～30 weight parts in the nitration mixture of 500 weight parts, middle low temperature nitration reaction is finished after washing, boil successively then wash, carefully disconnected, fine purifiation is promptly; Wherein, described nitration mixture is the mixture of nitric acid, sulfuric acid and water, and wherein the mass percent of nitric acid, sulfuric acid and water is: nitric acid 30.00%～60.00%, sulfuric acid 33.50%～64.00%, moisture 5.00%～16.50%.
Wherein, nitrated temperature is no more than 60 ℃.
15～45 ℃ of preferably nitrated temperature.
As preferably, the mass percent of nitric acid, sulfuric acid and water is in the described nitration mixture: nitric acid 40%～50%, sulfuric acid 45%～55%, moisture 5%～12%.
Digestion time is advisable with 30-60min.
As preferably, describedly boil that to wash be to boil and soda boiling through peracid successively, wherein, the zero degree acid that acid is boiled is counted 0～5g/l with sulfuric acid, and the basicity of soda boiling is controlled at below the 0.5g/l in yellow soda ash.
The temperature that acid is boiled is controlled at 80 ℃～120 ℃, and the temperature of soda boiling is controlled at 80 ℃～120 ℃.
Preferably sour temperature of boiling is controlled at 90-115 ℃, and the temperature of soda boiling is controlled at 100-110 ℃.
The cellulose nitrate index of the inventive method preparation meets GJB3204-1998 " military products nitro-cotton general specification " requirement.
Beneficial effect of the present invention:
The preparation method of cellulose nitrate of the present invention is to be starting material with the wood pulp, and raw-material use range in the soluble cotton production has been expanded also beyond example in this military at home cellulose nitrate field.Simultaneously, high-quality wood pulp as containing energy nitro-cotton production starting material, solves the problem of material cost with the advantage of and price steadiness cheap than linters greatly.Overcome simultaneously in the prior art when being raw material preparing nitro-cotton product, purified cotton opener, boiling, bleached oven dry and produce a large amount of cotton dirt, black liquor and acid waste water, the environmental protection pressure problem of bringing with the linters.
Embodiment
With the wood pulp is starting material,, save the purified cotton production process, avoided the generation of a large amount of cotton dirt, waste water.
Concrete, one of embodiment: the nitration mixture of 500 weight parts is preheating to 15～45 ℃, the wood pulp that adds 20～30 weight parts then, the low temperature nitration reaction is 30～60 minutes in carrying out, after washing is finished in reaction, boils the cellulose nitrate of washing, carefully obtaining degree of nitrification 188ml/g～216ml/g behind disconnected, the fine purifiation successively.
Nitrated temperature is no more than 60 ℃, and the too high starting material of temperature can be carbonized.Usually carry out nitratedly at 15～60 ℃, temperature is low excessively, and reactive behavior is low.
At nitration mixture described in the above-mentioned reaction is the mixture of nitric acid, sulfuric acid and water, wherein the mass percent of nitric acid, sulfuric acid and water is: nitric acid 30.00%～60.00%, sulfuric acid 33.50%～64.00%, moisture 5.00%～16.50% also contains the unavoidable impurities oxynitride in addition in the nitration mixture.Preferably nitric acid 40%～50%, sulfuric acid 45%～55%, moisture 5%～12%.
Digestion time should be greater than 30 minutes, and the time is too short nitrated not saturating, and the nitrogen amount is low.Overlong time is uneconomical.
In above-mentioned reaction, described low temperature boils to wash and respectively is that acid is boiled and soda boiling: the zero degree acid that acid is boiled is 0～5g/l (with sulphur acid meter), and temperature is controlled at 80 ℃～120 ℃ (preferred 90-115 ℃), time 1～7h (preferred 3-5h); The basicity of soda boiling is controlled at 0.5g/l following (in yellow soda ash), 80 ℃～120 ℃ of temperature (preferred 100-110 ℃), time 1～7h (preferred 4-7 hour).
Described zero degree acid is to boil the acidity of washing before the beginning, and zero degree acid is 0 to be poach.Along with the raising of zero degree acid concentration, byproduct of reaction will be hydrolyzed, and the stability of product is improved, but can aggravate macromolecules degradation simultaneously, so the zero degree acid concentration can not be too high.
The too high product of the basicity of soda boiling can be by saponification, and nitrogen content reduces.
Acid boil or the soda boiling time too short, it is unclean that by product removes, product stability is bad; The overlong time production cycle is long and viscosity reduction is serious.Acid boil or the soda boiling temperature low excessively, it is unclean that by product removes, product stability is bad; The too high meeting of temperature causes viscosity reduction serious.
The present invention selects first acid to boil the reason of back soda boiling, is to be acid because the back system is boiled in acid, and is acid by the soda boiling reduction, to improve product stability.In addition, increase the fiber rigidity, be beneficial to the carrying out of thin disconnected process by further soda boiling.
Usually boiling and washing operation is to boil in the cask washing at a kind of carrying vapour round-robin to carry out.
The present invention is described in further detail below in conjunction with embodiment, but the working of an invention mode is not limited thereto.
Embodiment 1
Nitration mixture 500g is added one to be equipped with in the churned mechanically 1000ml beaker, wherein each composition quality mark is respectively nitric acid 35.23% in the nitration mixture, sulfuric acid 56.87%, moisture 7.98%, and heating in water bath is to 15 ℃ of temperature, then the wood pulp 25g of water ratio after the drying below 10% joined in the beaker, stir and nitration reaction was taken out after 45 minutes, carry out successively that acid is boiled and soda boiling, the zero degree acid that acid is boiled is 3.5g/l (with sulphur acid meter), temperature is controlled at 105 ℃～115 ℃, time 3h, the basicity of soda boiling is controlled at 0.79g/l (in yellow soda ash), 100 ℃～110 ℃ of temperature, time 5h promptly makes fiery explosive cellulose nitrate behind thin disconnected fine purifiation.
The nitrogen content of the prepared cellulose nitrate of present embodiment is 199.8ml/g (measures according to the interferometer mode method, down with), 8.6 ° of E of viscosity (measure, down with) according to capillary viscosimeter method method, and alcohol ether solubleness, thin disconnected degree and stability all meet the requirements.
Embodiment 2
Nitration mixture 500g is added one to be equipped with in the churned mechanically 1000ml beaker, wherein each composition quality mark is respectively nitric acid 42.11% in the nitration mixture, sulfuric acid 50.36%, moisture 6.71%, and heating in water bath is to 15 ℃ of temperature, then the wood pulp 30g of water ratio after the drying below 10% joined in the beaker, stir and nitration reaction was taken out after 45 minutes, carry out successively that acid is boiled and soda boiling, the zero degree acid that acid is boiled is 4.5g/l (with sulphur acid meter), temperature is controlled at 105 ℃～115 ℃, time 3h, the basicity of soda boiling is controlled at 0.68g/l (in yellow soda ash), 100 ℃～110 ℃ of temperature, time 5h is through carefully disconnected, promptly make fiery explosive cellulose nitrate behind the fine purifiation.
The nitrogen content of the prepared cellulose nitrate of present embodiment is 211.4ml/g, 5.2 ° of E of viscosity, and alcohol ether solubleness, thin disconnected degree and stability all meet the requirements.
Embodiment 3
Nitration mixture 500g is added one to be equipped with in the churned mechanically 1000ml beaker, wherein each composition quality mark is respectively nitric acid 45.86% in the nitration mixture, sulfuric acid 39.34%, moisture 13.85%, and heating in water bath is to 20 ℃ of temperature, join in the beaker after then the wood pulp 25g of water ratio after the drying below 10% being broken up, stir and nitration reaction was taken out after 45 minutes, carry out successively that acid is boiled and soda boiling, the zero degree acid that acid is boiled is 2.2g/l (with sulphur acid meter), temperature is controlled at 90 ℃～100 ℃, time 3h, the basicity of soda boiling is controlled at 0.77g/l following (in yellow soda ash), 102 ℃～110 ℃ of temperature, time 6h is through thin, have no progeny and promptly make fiery explosive cellulose nitrate.
The nitrogen content of the prepared cellulose nitrate of present embodiment is 195.4ml/g, 6.2 ° of E of viscosity, and alcohol ether solubleness, thin disconnected degree and stability all meet the requirements.
Embodiment 4
Nitration mixture 500g is added one to be equipped with in the churned mechanically 1000ml beaker, wherein each composition quality mark is respectively nitric acid 46.11% in the nitration mixture, sulfuric acid 37.58%, moisture 15.32%, and heating in water bath is to 25 ℃ of temperature, then the wood pulp 30g of water ratio after the drying below 10% joined in the beaker, stir and nitration reaction was taken out after 45 minutes, carry out successively that acid is boiled and soda boiling, the zero degree acid that acid is boiled is 4.1g/l (with sulphur acid meter), temperature is controlled at 105 ℃～115 ℃, time 3h, the basicity of soda boiling is controlled at 0.82g/l (in yellow soda ash), 100 ℃～110 ℃ of temperature, time 5h is through carefully disconnected, promptly make fiery explosive cellulose nitrate behind the fine purifiation.
The nitrogen content of the prepared cellulose nitrate of present embodiment is 188.3ml/g, 4.6 ° of E of viscosity, and alcohol ether solubleness, thin disconnected degree and stability all meet the requirements.
Embodiment 5
Nitration mixture 500g is added one to be equipped with in the churned mechanically 1000ml beaker, wherein each composition quality mark is respectively nitric acid 40.86% in the nitration mixture, sulfuric acid 48.00%, moisture 10.21%, and heating in water bath is to 20 ℃ of temperature, join in the beaker after then the wood pulp 25g of water ratio after the drying below 10% being broken up, stir and nitration reaction was taken out after 45 minutes, carry out successively that acid is boiled and soda boiling, the zero degree acid that acid is boiled is 3.2g/l (with sulphur acid meter), temperature is controlled at 90 ℃～100 ℃, time 3h, the basicity of soda boiling is controlled at 0.75g/l following (in yellow soda ash), 102 ℃～110 ℃ of temperature, time 6h promptly makes fiery explosive cellulose nitrate through carefully having no progeny.
The nitrogen content of the prepared cellulose nitrate of present embodiment is 205.3ml/g, 6.6 ° of E of viscosity, and alcohol ether solubleness, thin disconnected degree and stability all meet the requirements.
Embodiment 6
Nitration mixture 500g is added one to be equipped with in the churned mechanically 1000ml beaker, wherein each composition quality mark is respectively nitric acid 42.36% in the nitration mixture, sulfuric acid 49.62%, moisture 6.71%, and heating in water bath is to 18 ℃ of temperature, then the wood pulp 25g of water ratio after the drying below 10% joined in the beaker, stir and nitration reaction was taken out after 45 minutes, carry out successively that acid is boiled and soda boiling, the zero degree acid that acid is boiled is 3.2g/l (with sulphur acid meter), temperature is controlled at 105 ℃～115 ℃, time 4h, the basicity of soda boiling is controlled at 0.55g/l (in yellow soda ash), 100 ℃～110 ℃ of temperature, time 5h is through carefully disconnected, promptly make fiery explosive cellulose nitrate behind the fine purifiation.
The nitrogen content of the prepared cellulose nitrate of present embodiment is 215.4ml/g, 5.2 ° of E of viscosity, and alcohol ether solubleness, thin disconnected degree and stability all meet the requirements.
Claims (8)
1. prepare the method for fiery explosive by wood pulps, it is characterized in that through following steps with cellulose nitrate:
The wood pulp that adds 20～30 weight parts in the nitration mixture of 500 weight parts, middle low temperature nitration reaction is finished after washing, boil successively then wash, carefully disconnected, fine purifiation is promptly; Wherein, described nitration mixture is the mixture of nitric acid, sulfuric acid and water, and wherein the mass percent of nitric acid, sulfuric acid and water is: nitric acid 30.00%～60.00%, sulfuric acid 33.50%～64.00%, moisture 5.00%～16.50%.
2. according to claim 1ly prepare the fiery explosive method with cellulose nitrate by wood pulps, it is characterized in that: nitrated temperature is no more than 60 ℃.
3. according to claim 2ly prepare fiery explosive method, it is characterized in that: 15～45 ℃ of nitrated temperature with cellulose nitrate by wood pulps.
4. according to each described method for preparing fiery explosive usefulness cellulose nitrate by wood pulps of claim 1～3, it is characterized in that: the mass percent of nitric acid, sulfuric acid and water is in the described nitration mixture: nitric acid 40%～50%, sulfuric acid 45%～55%, moisture 5%～12%.
5. each describedly prepares the fiery explosive method with cellulose nitrate by wood pulps according to claim 1～4, it is characterized in that: digestion time 30-60min.
6. according to each described method for preparing fiery explosive usefulness cellulose nitrate by wood pulps of claim 1-5, it is characterized in that: describedly boil that to wash be to boil and soda boiling through peracid successively, wherein, the zero degree acid that acid is boiled is counted 0～5g/l with sulfuric acid, the basicity of soda boiling is controlled at below the 0.5g/l in yellow soda ash.
7. according to claim 6ly prepare the fiery explosive method with cellulose nitrate by wood pulps, it is characterized in that: the temperature that acid is boiled is controlled at 80 ℃～120 ℃, and the temperature of soda boiling is controlled at 80 ℃～120 ℃.
8. according to claim 7ly prepare the fiery explosive method with cellulose nitrate by wood pulps, it is characterized in that: the temperature that acid is boiled is controlled at 90-115 ℃, and the temperature of soda boiling is controlled at 100-110 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110141936 CN102219861B (en) | 2011-05-30 | 2011-05-30 | Method for preparing cellulose nitrate for explosive from wood pulp |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110141936 CN102219861B (en) | 2011-05-30 | 2011-05-30 | Method for preparing cellulose nitrate for explosive from wood pulp |
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| CN102219861A true CN102219861A (en) | 2011-10-19 |
| CN102219861B CN102219861B (en) | 2012-12-19 |
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| CN 201110141936 Expired - Fee Related CN102219861B (en) | 2011-05-30 | 2011-05-30 | Method for preparing cellulose nitrate for explosive from wood pulp |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709255A (en) * | 2013-12-24 | 2014-04-09 | 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 |
| CN104003825A (en) * | 2014-05-30 | 2014-08-27 | 泸州北方化学工业有限公司 | Wood pulp nitrocellulose single-base propellant and preparation method thereof |
| CN105111316A (en) * | 2015-09-24 | 2015-12-02 | 四川北方硝化棉股份有限公司 | Nitro-cotton and method for producing same |
| CN105175556A (en) * | 2015-10-20 | 2015-12-23 | 四川北方硝化棉股份有限公司 | Wood pulp cellulose nitrate and preparation method thereof |
| CN111647090A (en) * | 2020-07-14 | 2020-09-11 | 北京理工大学 | Method for nitrifying bamboo cellulose by using waste acid |
| 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 |
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| GB347169A (en) * | 1929-12-14 | 1931-04-14 | Henry Conrad Heide | Improvements in the production of nitro cellulose |
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| US3337532A (en) * | 1962-06-05 | 1967-08-22 | France Etat | Preparation of mixed cellulose polyol ether nitrates |
| CN85106196A (en) * | 1985-08-14 | 1987-03-04 | 刘吉平 | With the Herba Poae Sphondylodis is that raw material is made soluble cotton |
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2011
- 2011-05-30 CN CN 201110141936 patent/CN102219861B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB347169A (en) * | 1929-12-14 | 1931-04-14 | Henry Conrad Heide | Improvements in the production of nitro cellulose |
| GB355492A (en) * | 1930-08-11 | 1931-08-27 | Henry Conrad Heide | Improvements in the manufacture of nitro cellulose |
| GB808609A (en) * | 1956-05-15 | 1959-02-04 | Hercules Powder Co Ltd | Improvements in or relating to process and apparatus for the continuous manufacture of nitrocellulose |
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Non-Patent Citations (1)
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709255A (en) * | 2013-12-24 | 2014-04-09 | 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 |
| 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 |
| CN104003825A (en) * | 2014-05-30 | 2014-08-27 | 泸州北方化学工业有限公司 | Wood pulp nitrocellulose single-base propellant and preparation method thereof |
| 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 |
| CN105111316A (en) * | 2015-09-24 | 2015-12-02 | 四川北方硝化棉股份有限公司 | Nitro-cotton and method for producing same |
| CN105175556A (en) * | 2015-10-20 | 2015-12-23 | 四川北方硝化棉股份有限公司 | Wood pulp cellulose nitrate and preparation method thereof |
| CN111647090A (en) * | 2020-07-14 | 2020-09-11 | 北京理工大学 | Method for nitrifying bamboo cellulose by using waste acid |
| 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 |
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