CN102807623A - Acid removal process for nitrocotton - Google Patents
Acid removal process for nitrocotton Download PDFInfo
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- CN102807623A CN102807623A CN2012102951394A CN201210295139A CN102807623A CN 102807623 A CN102807623 A CN 102807623A CN 2012102951394 A CN2012102951394 A CN 2012102951394A CN 201210295139 A CN201210295139 A CN 201210295139A CN 102807623 A CN102807623 A CN 102807623A
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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 the nitro-cotton production technical field, be specifically related to a kind of nitro-cotton and drive sour technology.
Background technology
At present, the mode that centrifuge washing is generally adopted in acid is driven to acid nitro-cotton by nitro-cotton manufacturer both at home and abroad, and driving sour machine is to drive imperative equipment in the sour technology.Drive sour machine and be whizzer, because it uses in the sour operation of driving of nitro-cotton production process, so this area all is referred to as the sour machine that drives.To drive sour technology following usually for nitro-cotton in the prior art: as shown in Figure 1, acid cotton (being acid nitro-cotton, the nitro-cotton that obtains for nitrated operation and the mixture of acid) joins preceding half section that drives sour machine screen frame, carries out solid-liquid separation earlier, and liquid gets into acid tank; Solid receives the thrust of material-pulling device, move to gradually screen frame second half section, carry out displacement washing with the acid solution of driving that adds, the liquid after the washing gets into acid tank equally, accomplishes the process of driving acid.Nitro-cotton gets into rinse bath through driving acid back, carry out thorough mixing with the water of adding or diluted acid after, be pumped into to boil by defeated cotton and wash operation.Said acid nitro-cotton is meant nitro-cotton that nitrated operation prepares and the acid solution that is comprised, and nitro-cotton is about about 3% in the acid nitro-cotton, acid solution about 97%, sulfuric acid concentration about 50%, concentration of nitric acid about 20% in the acid solution.
Acid nitro-cotton is after driving sour machine and driving acid; Residual acid amount (promptly driving the ratio of the acidiferous quality of institute and nitro-cotton total mass in the nitro-cotton of acid back) is generally about 20%; This residual acid of 20% can be diffused in the liquid of follow-up generation, forms the higher spent acid solution of concentration ratio, and making needs a large amount of lime neutralizing treatment; Increase the wastewater treatment expense, produce a large amount of solid waste.
Summary of the invention
Technical problem to be solved by this invention provides a kind of nitro-cotton that improves the spent acid recovery, reduces production costs and drives sour technology.
The technical solution adopted for the present invention to solve the technical problems is: nitro-cotton drives sour technology, 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 gets into acid tank;
B, get into No. 1 rinse bath continuously through the nitro-cotton of solid-liquid separation and washing, the follow-up washings that returns gets into No. 1 rinse bath continuously, adds entry or diluted acid continuously simultaneously, mixes;
C, the nitro-cotton after step b mixes and liquid are pumped into dashpot by defeated cotton continuously, and the partially liq of dashpot turns back to continuously that step a is described to be driven sour machine nitro-cotton is washed; Nitro-cotton in the dashpot is sent into centrifugal washer with all the other liquid and is washed, water spray or diluted acid during washing, and the washing water that obtain after the washing get into described No. 1 rinse bath of step b continuously;
D, the nitro-cotton after the centrifugal washer washing enter into rinse bath No. 2, mix afterwards to be pumped into to boil by defeated cotton with water that adds or diluted acid and wash operation.
Wherein, among the aforesaid method step c, the water or the diluted acid of atomization when the nitro-cotton in the dashpot and all the other liquid are sent into centrifugal washer and washed.
Wherein, among the aforesaid method step a, acid nitro-cotton gets into the amount of driving sour machine continuously and is: press 9～11 kilograms of nitro-cotton dry weight basis PMs.
Further, the amount that adds entry or diluted acid among the aforesaid method step b continuously is 450～550 liters/hour; The amount that liquid among the step c in the dashpot turns back to the liquid that drives sour machine continuously is 600～800 liters/hour; The water spray or the amount of diluted acid were 150～250 liters/hour when centrifugal washer washed among the step c.Wherein, in the aforesaid method, the concentration of acid is less than 20g/L in the said diluted acid.
Further, in the said diluted acid acid concentration less than 5g/L.
Sulfur acid and nitric acid in the said diluted acid.
The inventive method specifically can be implemented in such a way: nitro-cotton drives sour technology, 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 gets into acid tank; Acid nitro-cotton gets into the amount of driving sour machine continuously: press 9～11 kilograms of nitro-cotton dry weight basis PMs;
B, get into No. 1 rinse bath continuously through the nitro-cotton of solid-liquid separation and washing, the follow-up washings that returns gets into No. 1 rinse bath continuously, adds entry or diluted acid by 450～550 liters/hour amount continuously simultaneously, mixes;
C, the nitro-cotton after step b mixes and liquid are pumped into dashpot by defeated cotton continuously, and the liquid of dashpot turns back to by 600～800 liters/hour amount continuously that step a is described to be driven sour machine nitro-cotton is washed; Nitro-cotton in the dashpot is sent into centrifugal washer with all the other liquid and is washed, and presses the water or the diluted acid of 150～250 liters/hour amount atomization during washing, and the washing water that obtain after the washing get into described No. 1 rinse bath of step b continuously;
D, the nitro-cotton after the centrifugal washer washing enter into rinse bath No. 2, mix afterwards to be pumped into to boil by defeated cotton with water that adds or diluted acid and wash operation;
Wherein, in the said diluted acid acid concentration 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 as the acid solution of driving of driving sour machine nitro-cotton is washed from dashpot recovered acid liquid; Improved the concentration of recovered acid in the acid tank; Thereby improved nitric acid and vitriolic yield, just reduced also that nitric acid and vitriolic definitely consume in the nitro-cotton production process, reduced the acidity of waste water; Also just reduced to the processing cost of waste water with to the pollution of environment, improved the economic benefit of producing nitro-cotton.Diluted acid of the present invention can derive from the spent acid that produces in the nitro-cotton production process, thereby further reduces to the processing cost of spent acid with to the pollution of environment.
Description of drawings
Fig. 1 drives sour process flow diagram for having now;
Fig. 2 is sour process flow diagram for the present invention drives.
Embodiment
Through embodiment the present invention is further described below.
Nitro-cotton drives sour technology, 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 gets into acid tank;
B, get into No. 1 rinse bath continuously through the nitro-cotton of solid-liquid separation and washing, the follow-up washings that returns gets into No. 1 rinse bath continuously, adds entry or diluted acid continuously simultaneously, mixes;
C, the nitro-cotton after step b mixes and liquid are pumped into dashpot by defeated cotton continuously, and the partially liq of dashpot turns back to continuously that step a is described to be driven sour machine nitro-cotton is washed; Nitro-cotton in the dashpot is sent into centrifugal washer with all the other liquid and is washed, water spray or diluted acid during washing, and the washing water that obtain after the washing get into described No. 1 rinse bath of step b continuously;
D, the nitro-cotton after the centrifugal washer washing enter into rinse bath No. 2, mix afterwards to be pumped into to boil by defeated cotton with water that adds or diluted acid and wash operation.
Process as shown in Figure 2, that the present invention has increased rinse bath and with centrifugal washer nitro-cotton washed with respect to prior art at first sprays into water or diluted acid is washed nitro-cotton to centrifugal washer, and the washings after the washing gets into No. 1 rinse bath; Because the water or the diluted acid that spray into to centrifugal washer are not enough to satisfy defeated cotton pump to carrying the requirement of nitro-cotton; Therefore need in No. 1 rinse bath, add entry again or diluted acid is washed nitro-cotton; To dashpot, the liquid in the dashpot partly is sent to and drives sour machine as driving acid solution by defeated cotton pump delivery in the washing back.Therefore; Washing process of the present invention is different from conventional three stage countercurrents washing, and according to the practical situation of equipment, the adding point of water or diluted acid is two places at all in the present invention; Mainly add from No. 1 rinse bath; The adding of centrifugal washer can further be washed nitro-cotton, but can not surpass the load of centrifugal washer, produces steadily.The present invention can fully reclaim sulfuric acid contained in the acid nitro-cotton and nitric acid, improves the nitric acid and the vitriolic recovery, reduces cost.
Preferably, among the aforesaid method step c, the water or the diluted acid of atomization when the nitro-cotton in the dashpot and all the other liquid are sent into centrifugal washer and washed.The present invention adds the water of washing use or the adding point of diluted acid is two; One is that another is at centrifugal washer at No. 1 rinse bath, and the adding mode of centrifugal washer adopts the 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, it is more reasonable to make the present invention drive sour technology.
Wherein, among the aforesaid method step a, acid nitro-cotton gets into the amount of driving sour machine continuously and is: press 9～11 kilograms of nitro-cotton dry weight basis PMs.
Preferably, more stable aborning in order to make technology of the present invention, make technology more reasonable, further improve washing effect, the amount that adds entry or diluted acid among the aforesaid method step b continuously is 450～550 liters/hour; The amount that liquid among the step c in the dashpot turns back to the liquid that drives sour machine continuously is 600～800 liters/hour; The water spray or the amount of diluted acid were 150～250 liters/hour when centrifugal washer washed among the step c.
Preferably, in order to guarantee washing effect, in the aforesaid method, the concentration of acid is less than 20g/L in the said diluted acid.Further, in the diluted acid acid concentration less than 5g/L.
Be further described through the embodiment specific embodiments of the invention below, but therefore protection scope of the present invention be not limited among the embodiment.
Embodiment one
A, at first acid nitro-cotton is sent into continuously driven sour machine and carry out nitro-cotton and separate with spent acid and wash, contain nitro-cotton 3% in the acid nitro-cotton, acid solution 97%; Sulfuric acid concentration 50%, concentration of nitric acid 20% in the acid solution; Press the nitro-cotton dry weight basis, the control PM is sent 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 separation and the washing gets into acid tank, restored acid molten sulfur acid concentration 8%, concentration of nitric acid 5% in the acid tank.
B, separate with spent acid and the nitro-cotton that washs gets into No. 1 rinse bath continuously through nitro-cotton; Press the nitro-cotton dry weight basis; The nitro-cotton that the control PM is sent into No. 1 rinse bath is 10 kilograms, and the follow-up washings that returns gets into No. 1 rinse bath continuously, adds 500 liters/hour of diluted acids simultaneously continuously; Diluted acid concentration is 10-15g/L, mixes;
C, the nitro-cotton after step b mixes and liquid are pumped into dashpot by defeated cotton, and the partially liq of dashpot turns back to by 700 liters/hour that step a is described to be driven sour machine nitro-cotton is washed; Nitro-cotton in the dashpot is sent into centrifugal washer with all the other liquid and is washed, and by the diluted acid of 200 liters of/hour atomizations, the diluted acid concentration of atomizing is less than 5g/L during washing, and the washing water that obtain after the washing get into described No. 1 rinse bath of step b continuously;
D, the residual acid amount of the nitro-cotton after centrifugal washer washing enter into rinse bath No. 2 less than 5%, wash operation with being pumped into to boil by defeated cotton after the diluted acid that adds is mixed.
Washing process of the present invention can fully reclaim sulfuric acid contained in the acid nitro-cotton and nitric acid; Improve the nitric acid and the vitriolic recovery; The residual acid amount of nitro-cotton after the washing is controlled at less than in 5% the scope the most at last, has reduced to the processing cost of waste water with to the pollution of environment.The present invention washs the water of use or the adding point of diluted acid is two, and one is that another is at centrifugal washer at No. 1 rinse bath; And the adding mode of centrifugal washer adopts the 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 that combines the present invention to water or diluted acid add-on, it is more reasonable to make the present invention drive sour technology.
Claims (6)
1. nitro-cotton drives sour technology, 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 gets into acid tank;
B, get into No. 1 rinse bath continuously through the nitro-cotton of solid-liquid separation and washing, the follow-up washings that returns gets into No. 1 rinse bath continuously, adds entry or diluted acid continuously simultaneously, mixes;
C, the nitro-cotton after step b mixes and liquid are pumped into dashpot by defeated cotton continuously, and the partially liq of dashpot turns back to continuously that step a is described to be driven sour machine nitro-cotton is washed; Nitro-cotton in the dashpot is sent into centrifugal washer with all the other liquid and is washed, water spray or diluted acid during washing, and the washing water that obtain after the washing get into described No. 1 rinse bath of step b continuously;
D, the nitro-cotton after the centrifugal washer washing enter into rinse bath No. 2, mix afterwards to be pumped into to boil by defeated cotton with water that adds or diluted acid and wash operation.
2. nitro-cotton according to claim 1 drives sour technology, it is characterized in that: among the step c, and the water or the diluted acid of atomization when the nitro-cotton in the dashpot and all the other liquid are sent into centrifugal washer and washed.
3. nitro-cotton according to claim 1 and 2 drives sour technology, it is characterized in that: among the step a, acid nitro-cotton gets into the amount of driving sour machine continuously and is: press 9～11 kilograms of nitro-cotton dry weight basis PMs.
4. nitro-cotton according to claim 3 drives sour technology, it is characterized in that: the amount that adds entry or diluted acid among the step b continuously is 450～550 liters/hour; The amount that liquid among the step c in the dashpot turns back to the liquid that drives sour machine continuously is 600～800 liters/hour; The water spray or the amount of diluted acid were 150～250 liters/hour when centrifugal washer washed among the step c.
5. nitro-cotton according to claim 1 and 2 drives sour technology, it is characterized in that: the concentration of acid is less than 20g/L in the said diluted acid.
6. nitro-cotton according to claim 5 drives sour technology, it is characterized in that: the concentration of acid is less than 5g/L in the said diluted acid.
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| Application Number | Priority Date | Filing Date | Title |
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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 true CN102807623A (en) | 2012-12-05 |
| CN102807623B CN102807623B (en) | 2014-07-09 |
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Cited By (5)
| 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 |
| 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 |
| CN109056402A (en) * | 2018-09-13 | 2018-12-21 | 四川北方硝化棉股份有限公司 | Continuous multi-stage drives sour displacement washing process |
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2012
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Cited By (7)
| 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 |
| 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 |
| CN109056402A (en) * | 2018-09-13 | 2018-12-21 | 四川北方硝化棉股份有限公司 | Continuous multi-stage drives sour displacement washing process |
| 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 |
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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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