CN102807623B - Acid removal process for nitrocotton - Google Patents
Acid removal process for nitrocotton Download PDFInfo
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- CN102807623B CN102807623B CN201210295139.4A CN201210295139A CN102807623B CN 102807623 B CN102807623 B CN 102807623B CN 201210295139 A CN201210295139 A CN 201210295139A CN 102807623 B CN102807623 B CN 102807623B
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Abstract
The invention discloses an acid removal process for nitrocotton capable of improving the waste acid recovery rate and reducing the production cost, and belongs to the technical field of nitrocotton production. The acid removal process comprises the following steps: a, continuously conveying the acidic nitrocotton into an acid removal machine for solid-liquid separation and washing; b, continuously conveying the nitrocotton into a first washing groove, continuously conveying a subsequently returned washing solution into the first washing groove, and continuously adding water or diluted acid solution for mixing at the same time; c, continuously conveying the nitrocotton and the solution into a buffer tank through a cotton conveying pump, continuously returning part of the solution in the buffer tank into the acid removal machine for washing the nitrocotton, conveying the nitrocotton and the rest solution in the buffer tank into a centrifugal washing machine for washing, spraying the water or the diluted acid solution while washing, and continuously conveying washing water obtained after washing into the first washing tank; and d, conveying the nitrocotton into a second washing tank, and conveying the nitrocotton to the boiling and washing processes through the cotton conveying pump. According to the acid removal process, the recovery rate of nitric acid and sulfuric acid is increased, the acidity of wastewater is reduced, the production cost of the nitrocotton is reduced, and the economic benefit is increased.
Description
Technical field
The invention belongs to nitro-cotton production technical field, be specifically related to a kind of nitro-cotton and drive sour technique.
Background technology
At present, the sour mode that generally adopts centrifuge washing is driven to acid nitro-cotton by nitro-cotton manufacturer both at home and abroad, and driving sour machine is to drive requisite equipment in sour technique.Drive sour machine and be whizzer, because it uses in the sour operation of driving of nitro-cotton production process, therefore this area is all referred to as the sour machine that drives.In prior art, to drive sour technique conventionally as follows for nitro-cotton: as shown in Figure 1, acid cotton (being acid nitro-cotton, the nitro-cotton obtaining for nitrated operation and sour mixture) joins the first half section of driving sour machine screen frame, first carries out solid-liquid separation, and liquid enters acid tank; Solid is subject to the thrust of material-pulling device, moves to gradually the second half section of screen frame, carries out displacement washing with the acid solution of driving adding, and the liquid after washing enters acid tank equally, completes the sour process of driving.Nitro-cotton enters rinse bath after driving acid, after fully mixing, is pumped into boil washes operation by cotton transport with the water adding or diluted acid.Described acid nitro-cotton refers to the nitro-cotton that nitrated operation prepares and the acid solution comprising, nitro-cotton approximately 3% left and right in acid nitro-cotton, acid solution 97% left and right, sulfuric acid concentration 50% left and right, concentration of nitric acid 20% left and right in acid solution.
Acid nitro-cotton drives after acid through driving sour machine, residual acid amount (driving the quality of contained acid and the ratio of nitro-cotton total mass in the rear nitro-cotton of acid) is generally in 20% left and right, this residual acid of 20% can be diffused in the liquid of follow-up generation, form the higher spent acid solution of concentration ratio, make to need a large amount of lime neutralizing treatment, increase wastewater treatment expense, produce a large amount of solid waste.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of nitro-cotton that improves the spent acid rate of recovery, reduce production costs and drives sour technique.
The technical solution adopted for the present invention to solve the technical problems is: nitro-cotton drives sour technique, comprises the steps:
The mixture of a, the nitro-cotton that nitrated operation is obtained and acid is sent into continuously and is driven sour machine and carry out solid-liquid separation and washing, and liquid enters acid tank;
B, enter continuously rinse bath No. 1 through the nitro-cotton of solid-liquid separation and washing, the follow-up washings returning enters rinse bath continuously No. 1, adds continuously water or diluted acid simultaneously, is uniformly mixed;
C, nitro-cotton and liquid after step b is uniformly mixed are pumped into dashpot by cotton transport continuously, and the sour machine that drives that the partially liq of dashpot turns back to described in step a continuously washs nitro-cotton; Nitro-cotton in dashpot and all the other liquid are sent into centrifugal washer and are washed, water spray or diluted acid when washing, and the washing water that obtain after washing enter No. 1 rinse bath described in step b continuously;
D, nitro-cotton after centrifugal washer washing enter into rinse bath No. 2, be pumped into boil wash operation with the water adding or diluted acid after mixing by cotton transport.
Wherein, in aforesaid method step c, water or the diluted acid of atomization when the nitro-cotton in dashpot and all the other liquid are sent into centrifugal washer and washed.
Wherein, in aforesaid method step a, acid nitro-cotton enters continuously the amount of driving sour machine and is: by 9～11 kilograms of nitro-cotton dry weight basis per minutes.
Further, in aforesaid method step b, adding continuously the amount of water or diluted acid is 450～550 ls/h; The amount that liquid in step c in dashpot turns back to the liquid that drives sour machine is continuously 600～800 ls/h; 150～250 ls/h of water spray or the amounts of diluted acid when centrifugal washer washs in step c.Wherein, in aforesaid method, in described diluted acid, the concentration of acid is less than 20g/L.
Further, in described diluted acid, the concentration of acid is less than 5g/L.
Sulfur acid and nitric acid in described diluted acid.
The inventive method specifically can be implemented in such a way: nitro-cotton drives sour technique, comprises the steps:
The mixture of a, the nitro-cotton that nitrated operation is obtained and acid is sent into continuously and is driven sour machine and carry out solid-liquid separation and washing, and liquid enters acid tank; Acid nitro-cotton enters the amount of driving sour machine continuously: by 9～11 kilograms of nitro-cotton dry weight basis per minutes;
B, enter continuously rinse bath No. 1 through the nitro-cotton of solid-liquid separation and washing, the follow-up washings returning enters rinse bath continuously No. 1, adds water or diluted acid continuously by the amount of 450～550 ls/h simultaneously, is uniformly mixed;
C, nitro-cotton and liquid after step b is uniformly mixed are pumped into dashpot by cotton transport continuously, and the sour machine that drives that the liquid of dashpot turns back to described in step a by the amount of 600～800 ls/h continuously washs nitro-cotton; Nitro-cotton in dashpot and all the other liquid are sent into centrifugal washer and are washed, and press water or the diluted acid of the amount atomization of 150～250 ls/h when washing, and the washing water that obtain after washing enter No. 1 rinse bath described in step b continuously;
D, nitro-cotton after centrifugal washer washing enter into rinse bath No. 2, be pumped into boil wash operation with the water adding or diluted acid after mixing by cotton transport;
Wherein, in described diluted acid, the concentration of acid is less than 5g/L.
The invention has the beneficial effects as follows: the process that the present invention has increased rinse bath and with centrifugal washer, nitro-cotton washed with respect to prior art, and nitro-cotton is washed as the acid solution of driving of driving sour machine from dashpot recovered acid liquid, improve the concentration of recovered acid in acid tank, thereby improve the yield of nitric acid and sulfuric acid, also just reduced the absolute consumption of nitric acid and sulfuric acid in nitro-cotton production process, reduce the acidity of waste water, also just reduce the processing cost to waste water and the pollution to environment, improved the economic benefit of producing nitro-cotton.Diluted acid of the present invention can derive from the spent acid producing in nitro-cotton production process, thereby further reduces the processing cost to spent acid and the pollution to environment.
Accompanying drawing explanation
Fig. 1 is the existing sour process flow diagram that drives;
Fig. 2 is that the present invention drives sour process flow diagram.
Embodiment
Below by embodiment, the present invention is further illustrated.
Nitro-cotton drives sour technique, comprises the steps:
The mixture of a, the nitro-cotton that nitrated operation is obtained and acid is sent into continuously and is driven sour machine and carry out solid-liquid separation and washing, and liquid enters acid tank;
B, enter continuously rinse bath No. 1 through the nitro-cotton of solid-liquid separation and washing, the follow-up washings returning enters rinse bath continuously No. 1, adds continuously water or diluted acid simultaneously, is uniformly mixed;
C, nitro-cotton and liquid after step b is uniformly mixed are pumped into dashpot by cotton transport continuously, and the sour machine that drives that the partially liq of dashpot turns back to described in step a continuously washs nitro-cotton; Nitro-cotton in dashpot and all the other liquid are sent into centrifugal washer and are washed, water spray or diluted acid when washing, and the washing water that obtain after washing enter No. 1 rinse bath described in step b continuously;
D, nitro-cotton after centrifugal washer washing enter into rinse bath No. 2, be pumped into boil wash operation with the water adding or diluted acid after mixing by cotton transport.
As shown in Figure 2, the process that the present invention has increased rinse bath and with centrifugal washer, nitro-cotton washed with respect to prior art, first sprays into water or diluted acid is washed nitro-cotton to centrifugal washer, and the washings after washing enters rinse bath No. 1; Because the water spraying into centrifugal washer or diluted acid are not enough to meet cotton transport pump to carrying the requirement of nitro-cotton, therefore need to add again water or diluted acid to wash nitro-cotton in No. 1 rinse bath, after washing by cotton transport pump delivery to dashpot, the liquid in dashpot again part is sent to and drives sour machine as driving acid solution.Therefore, washing process of the present invention is different from three conventional stage countercurrent washings, the present invention is at all according to the practical situation of equipment, adding of water or diluted acid is a little two places, mainly add from No. 1 rinse bath, adding of centrifugal washer can further be washed nitro-cotton, but can not exceed the load of centrifugal washer, produces steadily.The present invention can fully reclaim sulfuric acid contained in acid nitro-cotton and nitric acid, improves the rate of recovery of nitric acid and sulfuric acid, reduces costs.
Preferably, in aforesaid method step c, water or the diluted acid of atomization when the nitro-cotton in dashpot and all the other liquid are sent into centrifugal washer and washed.It is a little two that the present invention adds water or the adding of diluted acid of washing use, one is at No. 1 rinse bath, another is at centrifugal washer, and the mode that adds of centrifugal washer adopts water or the diluted acid of atomization, the one, in order to alleviate the working strength of centrifugal washer, make its stable operation, the 2nd, can improve the washing effect of centrifugal washer, make the present invention drive sour technique more reasonable.
Wherein, in aforesaid method step a, acid nitro-cotton enters continuously the amount of driving sour machine and is: by 9～11 kilograms of nitro-cotton dry weight basis per minutes.
Preferably, in order to make technique of the present invention more stable aborning, make technique more reasonable, further improve washing effect, the amount that adds continuously water or diluted acid in aforesaid method step b is 450～550 ls/h; The amount that liquid in step c in dashpot turns back to the liquid that drives sour machine is continuously 600～800 ls/h; 150～250 ls/h of water spray or the amounts of diluted acid when centrifugal washer washs in step c.
Preferably, in order to guarantee washing effect, in aforesaid method, in described diluted acid, the concentration of acid is less than 20g/L.Further, in diluted acid, the concentration of acid is less than 5g/L.
Below by embodiment, the specific embodiment of the present invention is further described, but therefore protection scope of the present invention is not limited among embodiment.
Embodiment mono-
A, first acid nitro-cotton is sent into continuously and driven sour machine and carry out nitro-cotton and separate and wash with spent acid, in acid nitro-cotton, contain nitro-cotton 3%, acid solution 97%, sulfuric acid concentration 50%, concentration of nitric acid 20% in acid solution, press nitro-cotton dry weight basis, control per minute and send into 10 kilograms of the amounts of the nitro-cotton that drives sour machine, the acid solution that washing adopts dashpot to return, liquid after separating and washing enters acid tank, restored acid molten sulfur acid concentration 8%, concentration of nitric acid 5% in acid tank.
B, the nitro-cotton that separates and wash with spent acid through nitro-cotton enter rinse bath continuously No. 1, press nitro-cotton dry weight basis, the nitro-cotton that control per minute is sent into No. 1 rinse bath is 10 kilograms, the follow-up washings returning enters rinse bath continuously No. 1, add continuously 500 ls/h of diluted acids simultaneously, diluted acid concentration is 10-15g/L, is uniformly mixed;
C, nitro-cotton and liquid after step b is uniformly mixed are pumped into dashpot by cotton transport, and the partially liq of dashpot washs nitro-cotton by 700 ls/h of sour machines that drive that turn back to described in step a; Nitro-cotton in dashpot and all the other liquid are sent into centrifugal washer and are washed, and when washing, by the diluted acid of 200 ls/h of atomizations, the diluted acid concentration of atomization is less than 5g/L, and the washing water that obtain after washing enter No. 1 rinse bath described in step b continuously;
D, the residual acid amount of nitro-cotton after centrifugal washer washing are less than 5%, enter into rinse bath No. 2, be pumped into boil wash operation with the diluted acid adding after mixing by cotton transport.
Washing process of the present invention can fully reclaim sulfuric acid contained in acid nitro-cotton and nitric acid, improve the rate of recovery of nitric acid and sulfuric acid, the residual acid amount of nitro-cotton after washing is controlled in the scope that is less than 5% the most at last, has reduced the processing cost to waste water and the pollution to environment.Water or adding of diluted acid that the present invention washs use are a little two, one is at No. 1 rinse bath, another is at centrifugal washer, and the mode that adds of centrifugal washer adopts water or the diluted acid of atomization, the one, in order to alleviate the working strength of centrifugal washer, the 2nd, can improve the washing effect of centrifugal washer, make its stable operation, in the control to water or diluted acid add-on in conjunction with the present invention, make the present invention drive sour technique more reasonable.
Claims (6)
1. nitro-cotton drives sour technique, it is characterized in that comprising the steps:
The mixture of a, the nitro-cotton that nitrated operation is obtained and acid is sent into continuously and is driven sour machine and carry out solid-liquid separation and washing, and liquid enters acid tank;
B, enter continuously rinse bath No. 1 through the nitro-cotton of solid-liquid separation and washing, the follow-up washings returning enters rinse bath continuously No. 1, adds continuously water or diluted acid simultaneously, is uniformly mixed;
C, nitro-cotton and liquid after step b is uniformly mixed are pumped into dashpot by cotton transport continuously, and the sour machine that drives that the partially liq of dashpot turns back to described in step a continuously washs nitro-cotton; Nitro-cotton in dashpot and all the other liquid are sent into centrifugal washer and are washed, water spray or diluted acid when washing, and the washing water that obtain after washing enter No. 1 rinse bath described in step b continuously;
D, nitro-cotton after centrifugal washer washing enter into rinse bath No. 2, be pumped into boil wash operation with the water adding or diluted acid after mixing by cotton transport.
2. nitro-cotton according to claim 1 drives sour technique, it is characterized in that: in step c, and water or the diluted acid of atomization when the nitro-cotton in dashpot and all the other liquid are sent into centrifugal washer and washed.
3. nitro-cotton according to claim 1 and 2 drives sour technique, it is characterized in that: in step a, nitro-cotton and sour mixture enter continuously the amount of driving sour machine and be: by 9～11 kilograms of nitro-cotton dry weight basis per minutes.
4. nitro-cotton according to claim 3 drives sour technique, it is characterized in that: the amount that adds continuously water or diluted acid in step b is 450～550 ls/h; The amount that liquid in step c in dashpot turns back to the liquid that drives sour machine is continuously 600～800 ls/h; 150～250 ls/h of water spray or the amounts of diluted acid when centrifugal washer washs in step c.
5. nitro-cotton according to claim 1 and 2 drives sour technique, it is characterized in that: in described diluted acid, the concentration of acid is less than 20g/L.
6. nitro-cotton according to claim 5 drives sour technique, it is characterized in that: in described diluted acid, the concentration of acid is less than 5g/L.
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| CN201210295139.4A CN102807623B (en) | 2012-08-17 | 2012-08-17 | Acid removal process for nitrocotton |
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| CN201210295139.4A CN102807623B (en) | 2012-08-17 | 2012-08-17 | Acid removal process for nitrocotton |
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| CN102807623A CN102807623A (en) | 2012-12-05 |
| CN102807623B true CN102807623B (en) | 2014-07-09 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN105484085A (en) * | 2015-09-23 | 2016-04-13 | 四川北方硝化棉股份有限公司 | Two-segment continuous squeezing washing method for refined cotton |
| 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 |
| CN106349395A (en) * | 2016-08-31 | 2017-01-25 | 四川北方硝化棉股份有限公司 | Improving method of acid dispelling device for nitrocotton production |
| CN109056402B (en) * | 2018-09-13 | 2021-05-07 | 北方化学工业股份有限公司 | Continuous multi-stage acid-displacement washing process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436793A (en) * | 2003-03-21 | 2003-08-20 | 泸州北方化学工业有限公司 | Continuous nitrocotton dewatering process and apparatus |
| 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 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB440203A (en) * | 1933-06-21 | 1935-12-23 | Du Pont | Improvements in the manufacture of nitrocellulose |
| JP2000313701A (en) * | 1999-04-28 | 2000-11-14 | Asahi Chem Ind Co Ltd | Separation and recovery of nitrocellulose |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436793A (en) * | 2003-03-21 | 2003-08-20 | 泸州北方化学工业有限公司 | Continuous nitrocotton dewatering process and apparatus |
| 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 |
Non-Patent Citations (1)
| Title |
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| GB 440,203 A,1935.12.23,全文. |
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Address after: 646003 Gaoba North Chemical Industry Co., Ltd., Longmatan District, Luzhou City, Sichuan Province Patentee after: North Chemical Industry Co., Ltd Address before: The 646003 Luzhou city of Sichuan province Sichuan District North nitrocellulose Limited by Share Ltd Patentee before: SICHUAN NITROCELLULOSE Corp. |
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