CN105111316A - Nitro-cotton and method for producing same - Google Patents
Nitro-cotton and method for producing same Download PDFInfo
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- CN105111316A CN105111316A CN201510616171.1A CN201510616171A CN105111316A CN 105111316 A CN105111316 A CN 105111316A CN 201510616171 A CN201510616171 A CN 201510616171A CN 105111316 A CN105111316 A CN 105111316A
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Abstract
The invention belongs to the field of cellulose and novel chemical materials, and particularly relates to nitro-cotton and a method for producing the same. The method for producing the nitro-cotton includes steps of flocking wood pulp; nitrifying the wood pulp by the aid of mixed acid; cooking and washing the wood pulp, dehydrating the wood pulp and displacing water to obtain finished nitro-cotton products. The nitro-cotton and the method have the advantages that the method is low in cost and easy to implement, the nitro-cotton products are high in quality, and the effective method can be used for producing the nitro-cotton.
Description
Technical field
The invention belongs to Mierocrystalline cellulose and new chemical materials field, be specifically related to a kind of nitro-cotton and production method thereof.
Background technology
In nitro-cotton preparation, conventional raw material is purified cotton or wood pulp, and the physical aspect of these two kinds of raw materials is widely different, and this causes the preparation method's difference of the two very large.
Tradition nitro-cotton is produced and is adopted purified cotton to be starting material, and purified cotton is fluffy cotton-shaped form, and reaction is relatively easy, and processing condition require low, but due to raw material own characteristic, its colourity is high, impurity is many, quality is unstable, and on quality of finished, comparatively Wood pulp nitrocotton is poor.
Wood pulp nitrocotton has advantage usually in quality product, but causes its nitration reaction relative difficulty because of the form of the fine and close sheet of wood pulps, and the temperature of reaction of needs is high, long reaction time, concentration of nitric acid are high, and processing condition require higher.Current is that starting material production high-quality nitro-cotton mainly adopts slicing machine to carry out pre-treatment to starting material wood pulps with wood pulp, slicing machine is import equipment, cost is high, and wood pulps physical index (as: basic weight, density, thickness) is required strict, the work-ing life of cutting knife is short, and working service cost is high.
Chinese patent application 2011102234541 discloses a kind of Wood pulp nitrocotton production method.The method take timber as starting material, and the energy consumption of production is low, and production efficiency is high, and the colourity of product is low.Wood pulp nitrocotton production method comprises the following steps: when (1) Wood pulp nitrocotton is nitrated, nitration mixture used is the mixture of nitric acid, sulfuric acid and water, and by massfraction nitric acid 20.55%, moisture 10.18% in nitration mixture, surplus is sulfuric acid; (2) centrifugally acid wood pulp nitrocotton is driven after acid to obtain; (3) acid wood pulp nitrocotton is boiled and is washed, and the initial acidity of adjustment that adds water is 0.5-1.0g/L, boils and washes temperature 101-150 DEG C; (4) dewater; (5) expelling water.Step (5) expelling water process adds alcohol (the concentration >95% of alcohol) and controls Wood pulp nitrocotton wetting agent content 35%, wetting agent is the total amount of alcohol and water, wetting agent too high levels can raise customer using cost, and the too low national security that do not meet of wetting agent content stores and movement requirement.The manufacturing condition that this technology adopts requires high, and its temperature of reaction is high, long reaction time, concentration of nitric acid are high.
Summary of the invention
For the shortcoming existing for above-mentioned prior art, goal of the invention of the present invention is to provide a kind of nitro-cotton and production method thereof.The method adopts suede processing mode to wood pulps, makes it in physical aspect, be similar to purified cotton, thus remains that production method reaction conditions is low, preparation is easy to advantage, and obtains the advantage of gained nitro-cotton product high-quality.
First technical problem to be solved by this invention is to provide a kind of production method of nitro-cotton.The method comprises the following steps:
A, pre-treatment: carry out suede process to wood pulps, dry, obtain suede wood pulp;
B, nitration treatment: suede wood pulp is carried out nitration treatment with nitration mixture; Described nitration mixture is nitric acid 20 ~ 30% by mass percentage, water 15 ~ 19%, all the other are sulfuric acid;
C, subsequent disposal: boil wash, dewater, expelling water, obtain finished product nitro-cotton.
Preferably, in the method steps a of above-mentioned production nitro-cotton, described oven dry is dry 50 ~ 60min at 90 ~ 105 DEG C.
Preferably, in the method steps b of above-mentioned production nitro-cotton, the temperature of described nitration mixture is 30 ~ 40 DEG C.
Preferably, in the method steps b of above-mentioned production nitro-cotton, the condition of described nitration treatment is: nitrated temperature is 30 ~ 50 DEG C, nitrification coefficient is 60 ~ 100, the nitrated time is 10 ~ 30min; Described nitrification coefficient is the ratio of nitration mixture weight and suede wood pulp weight.
Preferably, in the method steps b of above-mentioned production nitro-cotton, described nitric acid massfraction is 98%; Described sulfuric acid massfraction is 98%.
Preferably, in the method steps b of above-mentioned production nitro-cotton, carry out in nitration treatment process breaing up process.
The production method that second technical problem to be solved by this invention is to provide above-mentioned nitro-cotton produces the nitro-cotton obtained.
The inventive method improves the manufacturing condition of wood pulp after carrying out suede process to wood pulps, not only improves nitro-cotton product quality, but also have reaction conditions low, preparation be easy to advantage.
Embodiment
A production method for nitro-cotton, comprises the following steps: carry out suede process to wood pulps, dries, obtains suede wood pulp; With nitration mixture, suede wood pulp is carried out nitration treatment, carry out while nitration treatment breaing up process; Boil again wash, dewater, expelling water, obtain finished product nitro-cotton.
In the method steps a of above-mentioned production nitro-cotton, described oven dry is dry 50 ~ 60min at 90 ~ 105 DEG C.
In the method steps b of above-mentioned production nitro-cotton, in order to reduce side reaction, before nitrated, nitration mixture temperature is controlled to 30 ~ 40 DEG C.
In the method steps b of above-mentioned production nitro-cotton, described nitration treatment condition is: nitrated temperature is 30 ~ 50 DEG C, nitrification coefficient is 60 ~ 100, the nitrated time is 10 ~ 30min; Described nitrification coefficient is the ratio of nitration mixture weight and suede wood pulp weight.
Wood pulps is the vegetable fibre pulp that trees are extracted through physical chemistry processing, and structure is finer and close, and nitration reaction is less likely to occur, and the temperature of reaction also needed during reaction is high, long reaction time, concentration of nitric acid are high.In order to overcome the defect of wood pulps itself, contriver finds through large quantity research, with suede machine, wood pulps is carried out suede process, can make it in physical aspect and be fluffy cotton-shaped form, be similar to purified cotton, thus reaction is relatively easy.So, step a of the present invention carries out suede process to wood pulps, and not only material quality is good, and after suede, the suede wood pulp of gained is similar to purified cotton, reaction conditions requires low, thus overcomes severe reaction conditions in prior art or the bad shortcoming of product quality.
Due to step a suede process has been carried out to wood pulps after the suede wood pulp of gained easily react, the fiber of wood pulp itself is also shorter than short velvet fiber simultaneously, the factor of these two aspects result in after suede wood pulp touches nitration mixture, cotton material and the nitration mixture on suede wood pulp surface shrink with regard to complete reaction, define the integument of the closeer cellulose ester of one deck, the parcel to inner processbearing astrocyte, thus may cause caking, finally makes raw material can not be fully nitrated.In order to overcome this defect, contriver finds through research, can carry out breaing up process in nitrated process, this breaks up process can break into staple fibre by macrofiber, also bulk can be broken into many fritters, wrapped part is come out, thus reach fully nitrated.Break up process and can adopt high speed dispersor, the blade of high speed dispersor also can replace with the blade of soybean milk maker, so, break up process and be not only only limited to employing high speed dispersor, as long as the equipment that can reach phase same-action can.
Boiling in the inventive method is washed, dewater, expelling water is by existing techniques in realizing.
Meanwhile, present invention also offers above-mentioned nitro-cotton production method and produce the nitro-cotton obtained.
The high speed dispersor that embodiment adopts is purchased from Tianjin Ke Lian material-testing machine factory, and model is Q3I type; The suede machine that embodiment adopts is purchased from Shanghai Zhilian Precision Machinery Co., Ltd., and model is ZLN (T)-II.
Embodiment 1
Wood pulps suede machine is carried out suede process, and baking oven put into by the suede wood pulp after process dries 1h, and temperature sets 104 DEG C.By mass percent preparation mixed acid solution, wherein nitric acid 22.80%, moisture 17.11%, all the other are sulfuric acid.Take 2400g nitration mixture and add beaker, the mixed acid solution heating in water bath weighed up is warmed up to 32 DEG C, takes suede wood pulp 30g and add mixed acid solution reaction, with high speed dispersor, the suede wood pulp in reaction is broken up simultaneously, control nitrated temperature at 38 DEG C, stop after reaction 15min.After stopping stirring, with filter screen take out nitrated in beaker after cotton material, the residual acid of extruding part, rinses with large water gaging, puts into miniature boiling again wash well-bucket and enter to boil and wash operation and boil wash with the large 1/4s that produces with sand net after wrapping.Boil after washing into, take out sample centrifuge dehydration 3min, then with alcohol-pickled twice, each 3min, more centrifugal expelling water 3min.
The present embodiment gained finished product Wood pulp nitrocotton index: nitrogen content 195.3mL/g, viscosity 2.8mpas, transmittance 93.1%, whiteness 94%, No. 140, colourity.
Comparative example 1
Wood pulp starting material are carried out slicing treatment.By massfraction nitric acid 52.16%, moisture 14.15%, all the other are the preparation mixed acid solution of sulfuric acid, take 2400g and add beaker.The mixed acid solution heating in water bath weighed up is warmed up to 42 DEG C, takes wood pulp section 80g and add mixed acid solution reaction, control nitrated temperature at 52 DEG C, stop after reaction 60min.After stopping stirring, with filter screen take out nitrated in beaker after cotton material, the residual acid of extruding part, rinses with large water gaging, puts into miniature boiling again wash well-bucket and enter to boil and wash operation and boil wash with the large 1/4s that produces with sand net after wrapping.Boil after washing into, take out sample centrifuge dehydration 3min, then with alcohol-pickled twice, each 3min, more centrifugal expelling water 3min.
This comparative example gained finished product Wood pulp nitrocotton index: nitrogen content 192.6mL/g, viscosity 2.8mpas, transmittance 92%, whiteness 93%, No. 150, colourity.
The slicing machine that this comparative example uses is import equipment, and cost is high, and requires strict to wood pulps physical index (as: basic weight, density, thickness), and the work-ing life of cutting knife is short, and working service cost is high.
The nitro-cotton quality product that this comparative example prepares compared to the inventive method is more or less the same, but high, the long reaction time of high, the nitrated temperature of nitric acid content in nitration mixture composition, therefore comparatively the present invention is high for cost.
Comparative example 2
Adopt purified cotton as nitrated starting material.By massfraction nitric acid 23.60%, moisture 18.33%, all the other are the preparation mixed acid solution of sulfuric acid, take 2400g and add beaker.The mixed acid solution heating in water bath weighed up is warmed up to 33 DEG C, takes purified cotton 40g and add mixed acid solution reaction, control nitrated temperature at 40 DEG C, stop after reaction 25min.After stopping stirring, with filter screen take out nitrated in beaker after cotton material, the residual acid of extruding part, rinses with large water gaging, puts into miniature boiling again wash well-bucket and enter to boil and wash operation and boil wash with the large 1/4s that produces with sand net after wrapping.Boil after washing into, take out sample centrifuge dehydration 3min, then with alcohol-pickled twice, each 3min, more centrifugal expelling water 3min.
This comparative example gained finished product C5 nitro-cotton index: nitrogen content 189.6mL/g, viscosity 3.2mpas, transmittance 88%, whiteness 85%, No. 180, colourity.
This comparative example compares embodiment 1, and processing condition are more or less the same, but the nitro-cotton quality of gained is not as the nitro-cotton quality of embodiment 1 gained.
Contrast known through embodiment and comparative example 1,2, the inventive method is simple to operate, cost is low, and the nitro-cotton quality prepared is good.So the inventive method is that the production of nitro-cotton provides a more efficiently approach.
Claims (7)
1. a production method for nitro-cotton, is characterized in that: comprise the following steps:
A, pre-treatment: carry out suede process to wood pulps, dry, obtain suede wood pulp;
B, nitration treatment: suede wood pulp is carried out nitration treatment with nitration mixture; Described nitration mixture is nitric acid 20 ~ 30% by mass percentage, water 15 ~ 19%, all the other are sulfuric acid;
C, subsequent disposal: boil wash, dewater, expelling water, obtain finished product nitro-cotton.
2. the production method of nitro-cotton according to claim 1, is characterized in that: in step a, and described oven dry is dry 50 ~ 60min at 90 ~ 105 DEG C.
3. the production method of nitro-cotton according to claim 1, is characterized in that: in step b, and the temperature of described nitration mixture is 30 ~ 40 DEG C.
4. the production method of nitro-cotton according to claim 1, is characterized in that: in step b, and the condition of described nitration treatment is: nitrated temperature is 30 ~ 50 DEG C, nitrification coefficient is 60 ~ 100, the nitrated time is 10 ~ 30min; Described nitrification coefficient is the ratio of nitration mixture weight and suede wood pulp weight.
5. the production method of nitro-cotton according to claim 1, is characterized in that: in step b, and described nitric acid massfraction is 98%; Described sulfuric acid massfraction is 98%.
6. the production method of nitro-cotton according to claim 1, is characterized in that: in step b, carries out breaing up process in nitration treatment process.
7. a nitro-cotton, is characterized in that: prepared by the production method of the nitro-cotton described in any one of claim 1 ~ 6.
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| CN201510616171.1A CN105111316B (en) | 2015-09-24 | 2015-09-24 | A kind of nitrocotton and its production method |
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| CN201510616171.1A CN105111316B (en) | 2015-09-24 | 2015-09-24 | A kind of nitrocotton and its production method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293992A (en) * | 2018-09-28 | 2019-02-01 | 四川北方硝化棉股份有限公司 | A kind of nitrocotton confuses technique |
| CN109504487A (en) * | 2018-10-18 | 2019-03-22 | 梅万伦 | A kind of method that plant cellulose and lignin mixture nitre esterification prepare fuel |
| CN111072785A (en) * | 2019-12-03 | 2020-04-28 | 北京理工大学 | Preparation method of high-nitrogen-content nitrified bamboo cellulose |
| CN112159481A (en) * | 2020-09-01 | 2021-01-01 | 北京理工大学 | Preparation method of special nitrating agent for bamboo fiber |
| CN115028745A (en) * | 2022-05-20 | 2022-09-09 | 北方化学工业股份有限公司 | Energy-containing nitrocotton and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108559103B (en) * | 2018-02-08 | 2020-11-06 | 潘小秋 | Preparation method of nitro-straw extract and product |
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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 |
| CN102321183A (en) * | 2011-08-05 | 2012-01-18 | 四川北方硝化棉股份有限公司 | Wood pulp nitrocotton production method |
| CN102926266A (en) * | 2011-08-09 | 2013-02-13 | 江苏五洲纸业有限公司 | Method for producing dissolving pulp by adopting wheat straw pulp as raw material |
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2015
- 2015-09-24 CN CN201510616171.1A patent/CN105111316B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN102321183A (en) * | 2011-08-05 | 2012-01-18 | 四川北方硝化棉股份有限公司 | Wood pulp nitrocotton production method |
| CN102926266A (en) * | 2011-08-09 | 2013-02-13 | 江苏五洲纸业有限公司 | Method for producing dissolving pulp by adopting wheat straw pulp as raw material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293992A (en) * | 2018-09-28 | 2019-02-01 | 四川北方硝化棉股份有限公司 | A kind of nitrocotton confuses technique |
| CN109504487A (en) * | 2018-10-18 | 2019-03-22 | 梅万伦 | A kind of method that plant cellulose and lignin mixture nitre esterification prepare fuel |
| CN111072785A (en) * | 2019-12-03 | 2020-04-28 | 北京理工大学 | Preparation method of high-nitrogen-content nitrified bamboo cellulose |
| CN111072785B (en) * | 2019-12-03 | 2020-12-01 | 北京理工大学 | Preparation method of high-nitrogen-content nitrified bamboo cellulose |
| CN112159481A (en) * | 2020-09-01 | 2021-01-01 | 北京理工大学 | Preparation method of special nitrating agent for bamboo fiber |
| CN115028745A (en) * | 2022-05-20 | 2022-09-09 | 北方化学工业股份有限公司 | Energy-containing nitrocotton and preparation method thereof |
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| CN105111316B (en) | 2017-06-09 |
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