CN112500500B - Device and method for recovering residual acid of nitrocellulose - Google Patents
Device and method for recovering residual acid of nitrocellulose Download PDFInfo
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- CN112500500B CN112500500B CN202011337909.8A CN202011337909A CN112500500B CN 112500500 B CN112500500 B CN 112500500B CN 202011337909 A CN202011337909 A CN 202011337909A CN 112500500 B CN112500500 B CN 112500500B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B5/00—Preparation of cellulose esters of inorganic acids, e.g. phosphates
- C08B5/02—Cellulose nitrate, i.e. nitrocellulose
- C08B5/04—Post-esterification treatments, e.g. densification of powders, including purification
Abstract
The invention discloses a device and a method for recovering residual acid of nitrocellulose, which comprises a centrifugal machine and a vacuum washing filter, wherein a screen frame of the centrifugal machine comprises a high-concentration waste acid separation section and a displacement washing section, an outlet of the high-concentration waste acid separation section is connected with an acid first-stage collecting tank, the centrifugal machine is internally provided with three displacement washing sections, meanwhile, the vacuum washing filter is internally provided with four displacement washing sections, and the centrifugal machine and the vacuum washing filter are used for realizing two-time acid-cotton separation, so that the content of the residual acid in nitrocellulose can be reduced to 5%.
Description
Technical Field
The invention belongs to the technical field of acid cotton separation equipment, relates to a device for recovering residual acid of nitrocellulose, and further relates to a method for recovering residual acid of nitrocellulose by using the device.
Background
Nitrocellulose is mainly produced by reacting nitric-sulfuric mixed acid with cellulose, acid-cotton separation is carried out on the nitrocellulose after reaction, if cotton contains a large amount of residual acid, the part of acid is directly discharged after washing, the cost of wastewater is increased, and the total nitrogen of the wastewater is increased, the total nitrogen of the wastewater in part of provinces and cities in China is required to be below 15mg/L, and the problem that the acidity in the cotton is too large exists in the following aspects: firstly, the cost of treating the residual acid in the wastewater in the post-procedure is increased, and the cost of treating the nitro-nitrogen in the wastewater is greatly increased. ② the acidity greatly increases the operation steps of the staff. And thirdly, a small amount of acid smoke exists in the field environment. The residual acidity of acid cotton after acid removal by the existing method is about 10 percent.
Disclosure of Invention
The invention aims to provide a device for recovering residual acid of nitrocellulose, which solves the problem of high residual acid degree of acid cotton in the prior art.
The technical scheme adopted by the invention is that the device for recovering the residual nitrocellulose acid comprises a centrifugal machine and a vacuum washing filter, wherein a screen frame of the centrifugal machine comprises a high-concentration waste acid separation section and a displacement washing section, an outlet of the high-concentration waste acid separation section is connected with an acid first-stage collecting tank, and the displacement washing section is sequentially set into an acid fourth section, an acid third section and an acid second section from the tail end of the screen frame to the front. The outlets of the acid four-section, the acid three-section and the acid two-section are correspondingly connected with an acid four-section collecting tank, an acid three-section collecting tank and an acid two-section collecting tank, and the acid four-section collecting tank and the acid three-section collecting tank are respectively communicated with the acid three-section and the acid two-section through a first spray pipe and a second spray pipe;
the material outlet of the centrifuge is sequentially connected with a washing machine and a distributing device, and the distributing device is positioned above the vacuum washing filter; the vacuum washing filter comprises a mother liquor collecting section and a displacement leaching section, wherein a mother liquor water collecting tank is connected to an outlet of the mother liquor collecting section and is communicated with the washing machine; the displacement leaching section comprises four countercurrent displacement washing sections, collecting tanks are correspondingly connected below each countercurrent displacement washing section, each collecting tank is communicated with the countercurrent displacement washing section through a spraying washing pipe, and each collecting tank is communicated with the next collecting tank; the collecting tank close to the mother liquor collecting section is communicated with the acid four sections through a spray washing pipe, and the spray washing pipe close to the outlet end of the vacuum washing filter is connected with a fresh washing liquor pipeline.
The invention is also characterized in that:
the displacement leaching section comprises an acid eight section, an acid seven section, an acid six section and an acid five section, the collecting tanks are respectively and correspondingly connected with acid eight section, acid seven section, acid six section and acid five section outlets, the outlet of the acid eight section collecting tank is communicated with the acid eight section through a third spraying pipe, the outlet of the acid eight section collecting tank is also communicated with the acid seven section collecting tank, the outlet of the acid seven section collecting tank is communicated with the acid seven section through a fourth spraying pipe, the outlet of the acid seven section collecting tank is also communicated with the acid six section collecting tank, the outlet of the acid six section collecting tank is communicated with the acid six section through a fifth spraying pipe, the outlet of the acid six section collecting tank is also communicated with the acid five section, and the outlet of the acid five section collecting tank is respectively communicated with the acid five section and the acid four section through a sixth spraying pipe and a seventh spraying pipe; the inlet of the third spray pipe is connected with a fresh washing liquid pipeline.
The outlet of the acid eight-section collecting tank is also communicated with the acid seven-section collecting tank, the outlet of the acid seven-section collecting tank is also communicated with the acid six-section collecting tank, and the outlet of the acid six-section collecting tank is also communicated with the acid five-section collecting tank.
The upper parts of the acid eight-section collecting tank, the acid seven-section collecting tank, the acid six-section collecting tank and the acid five-section collecting tank are respectively provided with an overflow port, and the overflow ports are communicated with the mother liquor water collecting tank through pipelines.
The acid eight-section collecting tank, the acid seven-section collecting tank, the acid six-section collecting tank, the acid five-section collecting tank and the vacuum washing filter are correspondingly connected with a liquid discharge tank respectively, a collecting tank is connected between the mother liquor collecting tank and the vacuum washing filter, the exhaust pump is further included, and exhaust ports of the liquid discharge tank and the collecting tank are communicated with the exhaust pump respectively.
The invention also aims to provide a method for recovering residual acid of nitrocellulose, which solves the problem of higher residual acid degree of acid cotton in the prior art.
The invention adopts another technical scheme that the method for recovering the residual acid of the nitrocellulose adopts the device and comprises the following steps:
The displacement flow of the acid second section and the acid third section is 1-1.5m 3 The displacement flow of the acid four stages is 0.9-1.5m 3 /h。
The spray washing amount of the acid eight section, the acid seven section, the acid six section and the acid five section is 6m 3 H, the flow rate of fresh washing liquid supplemented into the third spray pipe is 2.5m 3 /h。
The invention has the beneficial effects that:
according to the device for recovering the residual acid of the nitrocellulose, three sections of displacement washing sections are arranged in a centrifugal machine, five sections of displacement washing sections are arranged in a vacuum washing filter, and the separation of the acid cotton twice is realized through the centrifugal machine and the vacuum washing filter, so that the content of the residual acid in the nitrocellulose can be reduced; the acidic liquid discharged from each displacement washing section is used for washing the displacement washing section, the acidic liquid discharged from the acid five section is used for spraying and washing the acid four section, the washing liquid is recycled, and the water consumption is reduced; the operation is simple, the safety is high, and the output is stable. Compared with the prior art, the method for recovering the residual acid of the nitrocellulose can reduce the content of the residual acid in the nitrocellulose to be less than 5%.
Drawings
FIG. 1 is a schematic structural diagram of a device for recovering residual nitrocellulose acid according to the present invention.
In the figure, 1, a centrifuge, 2, a vacuum washing filter, 3, an acid first-stage collecting tank, 4, an acid fourth-stage collecting tank, 5, an acid third-stage collecting tank, 6, an acid second-stage collecting tank, 7, a first spray pipe, 8, a second spray pipe, 9, a washing machine, 10, a distributor, 11, an acid eight-stage collecting tank, 12, an acid seventh-stage collecting tank, 13, an acid sixth-stage collecting tank, 14, an acid fifth-stage collecting tank, 15, a third spray pipe, 16, a fourth spray pipe, 17, a fifth spray pipe, 18, a sixth spray pipe, 19, a seventh spray pipe, 20, a mother liquor collecting tank, 21, a liquid discharge tank, 22, a collecting tank and 23, an exhaust pump.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
A device for recovering nitrocellulose residual acid is shown in figure 1 and comprises a centrifugal machine 1 and a vacuum washing filter 2, wherein a screen frame of the centrifugal machine 1 comprises a high-concentration waste acid separation section and a displacement washing section, an outlet of the high-concentration waste acid separation section is connected with an acid first-section collecting tank 3, the displacement washing section is sequentially set into an acid fourth section, an acid third section and an acid second section from the tail end of the screen frame to the front, outlets of the acid fourth section, the acid third section and the acid second section are correspondingly connected with an acid fourth-section collecting tank 4, an acid third-section collecting tank 5 and an acid second-section collecting tank 6, the acid fourth-section collecting tank 4 and the acid third-section collecting tank 5 are respectively communicated with the acid third section and the acid second section through a first spray pipe 7 and a second spray pipe 8, and spray displacement is carried out on the acid third section and the acid second section. A material outlet of the centrifuge 1 is sequentially connected with a washing machine 9 and a distributing device 10, the washing machine 9 is also connected with a fresh water source and is used for washing nitrocotton discharged from the material outlet of the centrifuge 1, and the distributing device 10 is positioned above the vacuum washing filter 2; the vacuum washing filter 2 comprises a mother liquor collecting section and a displacement leaching section, the outlet of the mother liquor collecting section is connected with a mother liquor water collecting tank 20, the mother liquor water collecting tank 20 is communicated with the washing machine 9, and the washing machine 9, the distributing device 10, the vacuum washing filter 2 and the mother liquor water collecting tank 20 form a circulation loop, so that the water consumption can be reduced; the displacement leaching section is sequentially set into an acid eight section, an acid seven section, an acid six section and an acid five section from the tail end to the front, the outlets of the acid eight section, the acid seven section, the acid six section and the acid five section are correspondingly connected with an acid eight section collecting tank 11, an acid seven section collecting tank 12, an acid six section collecting tank 13 and an acid five section collecting tank 14, the outlet of the acid eight section collecting tank 11 is communicated with the acid eight section through a third spraying pipe 15 for displacement spraying of the acid eight section, a flowmeter is arranged in the third spraying pipe 15, the outlet of the acid eight section collecting tank 11 is also communicated with the acid seven section collecting tank 12, washing liquid is injected into the acid seven section collecting tank 12, a vacuum pump is arranged on an outlet pipeline of the acid eight section 11, valves are respectively arranged between the vacuum pump and the third spraying pipe 15 and the acid seven section collecting tank 12, and the flow rates of acidic liquid entering the third spraying pipe 15 and the acid seven section collecting tank 12 are controlled; the inlet of the third spray pipe 15 is connected with a fresh washing liquid pipeline and is used for supplementing spray liquid to the acid eight section. An outlet of the seven-acid-section collecting tank 12 is communicated with the seven-acid-section through a fourth spraying pipe 16, the seven-acid-section is subjected to displacement spraying, a flow meter is arranged in the fourth spraying pipe 16, an outlet of the seven-acid-section collecting tank 12 is further communicated with the six-acid-section collecting tank 13, washing liquid is injected into the six-acid-section collecting tank 13, a vacuum pump is arranged on an outlet pipeline of the seven-acid-section collecting tank 12, valves are respectively arranged between the vacuum pump and the fourth spraying pipe 16 and between the vacuum pump and the six-acid-section collecting tank 13, and the flow of acidic liquid entering the fourth spraying pipe 16 and the six-acid-section collecting tank 13 is controlled. An outlet of the acid six-section collecting tank 13 is communicated with the acid six section through a fifth spraying pipe 17, the acid six section is subjected to displacement spraying, a flowmeter is arranged in the fifth spraying pipe 17, an outlet of the acid six-section collecting tank 13 is also communicated with the acid five-section collecting tank 14, washing liquid is injected into the acid five-section collecting tank 14, a vacuum pump is arranged on an outlet pipeline of the acid six-section collecting tank 13, valves are respectively arranged between the vacuum pump and the fifth spraying pipe 17 as well as between the vacuum pump and the acid five-section collecting tank 14, and the flow of acidic liquid entering the fifth spraying pipe 17 and the acid five-section collecting tank 14 is controlled. The outlets of the acid five-section collecting tank 14 are respectively communicated with the acid five section and the acid four section through a sixth spraying pipe 18 and a seventh spraying pipe 19, one part of liquid in the acid five-section collecting tank 14 is used for replacing and spraying the acid five section, the other part of liquid is used for replacing and spraying the acid four section, a flow meter is arranged in the sixth spraying pipe 18, and a vacuum pump is arranged on an outlet pipeline of the acid five-section collecting tank 14.
In this embodiment, the vacuum washing filter 2 has a mesh size of 200 meshes, a size of 1m × 15m, and is made of rubber. The spray pipes all comprise pipelines, and spray heads are arranged at the tail ends of the pipelines.
The upper parts of the acid eight-section collecting tank 11, the acid seven-section collecting tank 12, the acid six-section collecting tank 13 and the acid five-section collecting tank 14 are respectively provided with overflow ports, and the overflow ports are communicated with a mother liquor water collecting tank 20 through pipelines.
The acid eight-section collecting tank 11, the acid seven-section collecting tank 12, the acid six-section collecting tank 13, the acid five-section collecting tank 14 and the vacuum washing filter 2 are correspondingly connected with a liquid discharge tank 21 respectively, the mother liquor collecting tank 20 and the vacuum washing filter 2 are connected with a collecting tank 22 respectively, the vacuum washing filter further comprises an exhaust pump 23, and exhaust ports of the liquid discharge tank 21 and the collecting tank 22 are communicated with the exhaust pump 23 respectively.
A method for recovering residual acid of nitrocellulose specifically comprises the following steps:
The replacement flow of the acid second section and the acid third section is 1-1.5m 3 The displacement flow of the acid four stages is 0.9-1.5m 3 H is used as the reference value. The spray washing amount of the acid eight section, the acid seven section, the acid six section and the acid five section is 6m 3 H, the flow rate of fresh washing liquid supplemented into the third spraying pipe 15 is 2.5m 3 /h。
Through the mode, the device for recovering the residual acid of the nitrocellulose is characterized in that the three-section displacement washing section is arranged in the centrifuge, the four-section displacement washing section is arranged in the vacuum washing filter, and the separation of the acid cotton twice is realized through the centrifuge and the vacuum washing filter, so that the residual acid content in the nitrocellulose can be reduced; the acidic liquid discharged from each displacement washing section is used for washing the displacement washing section, the acidic liquid discharged from the acid five section is used for spraying and washing the acid four section, the washing liquid is recycled, and the water consumption is reduced; the operation is simple, the safety is high, and the output is stable. Compared with the prior art, the method for recovering the residual acid of the nitrocellulose can reduce the content of the residual acid in the nitrocellulose to below 5%.
Claims (4)
1. A device for recovering residual nitrocellulose acid is characterized by comprising a centrifuge (1) and a vacuum washing filter (2), wherein a screen frame of the centrifuge (1) comprises a high-concentration waste acid separation section and a displacement washing section, an outlet of the high-concentration waste acid separation section is connected with a first-acid section collection tank (3), the displacement washing section is sequentially set into a fourth-acid section, a third-acid section and a second-acid section from the tail end of the screen frame to the front, outlets of the fourth-acid section, the third-acid section and the second-acid section are correspondingly connected with a fourth-acid section collection tank (4), a third-acid section collection tank (5) and a second-acid section collection tank (6), and the fourth-acid section collection tank (4) and the third-acid section collection tank (5) are respectively communicated with the third-acid section and the second-acid section through a first spray pipe (7) and a second spray pipe (8);
the material outlet of the centrifuge (1) is sequentially connected with a washing machine (9) and a distributing device (10), and the distributing device (10) is positioned above the vacuum washing filter (2); the vacuum washing filter (2) comprises a mother liquor collecting section and a displacement leaching section, an outlet of the mother liquor collecting section is connected with a mother liquor water collecting tank (20), and the mother liquor water collecting tank (20) is communicated with the washing machine (9); the displacement leaching section comprises four countercurrent displacement washing sections, collecting tanks are correspondingly connected below each countercurrent displacement washing section, each collecting tank is communicated with the countercurrent displacement washing section through a spray washing pipe, and each collecting tank is communicated with the next collecting tank; the collecting tank close to the mother liquor collecting section is communicated with the acid four section through a spray washing pipe, and the spray washing pipe close to the outlet end of the vacuum washing filter (2) is connected with a fresh washing liquid pipeline;
the displacement leaching section comprises an acid eight section, an acid seven section, an acid six section and an acid five section, the acid eight section collecting tank (11), the acid seven section collecting tank (12), the acid six section collecting tank (13) and the acid five section collecting tank (14) are respectively correspondingly connected with outlets of the acid eight section, the acid seven section, the acid six section and the acid five section, an outlet of the acid eight section collecting tank (11) is communicated with the acid eight section through a third spraying pipe (15), an outlet of the acid eight section collecting tank (11) is also communicated with the acid seven section collecting tank (12), an outlet of the acid seven section collecting tank (12) is communicated with the acid seven section collecting tank through a fourth spraying pipe (16), an outlet of the acid seven section collecting tank (12) is also communicated with the acid six section collecting tank (13), an outlet of the acid six section (13) is communicated with the acid six section through a fifth spraying pipe (17), and an outlet of the acid six section collecting tank (13) is also communicated with the acid five section collecting tank (14), the outlet of the acid five-section collecting tank (14) is respectively communicated with the acid five section and the acid four section through a sixth spray pipe (18) and a seventh spray pipe (19); the inlet of the third spray pipe (15) is connected with a fresh washing liquid pipeline;
the upper parts of the acid eight-section collecting tank (11), the acid seven-section collecting tank (12), the acid six-section collecting tank (13) and the acid five-section collecting tank (14) are respectively provided with an overflow port, and the overflow ports are communicated with a mother liquor water collecting tank (20) through pipelines;
the acid cleaning device is characterized in that a liquid discharge tank (21) is respectively and correspondingly connected between the acid eight-section collecting tank (11), the acid seven-section collecting tank (12), the acid six-section collecting tank (13), the acid five-section collecting tank (14) and the vacuum washing filter (2), a collecting tank (22) is connected between the mother liquor collecting tank (20) and the vacuum washing filter (2), the acid cleaning device further comprises an exhaust pump (23), and exhaust ports of the liquid discharge tank (21) and the collecting tank (22) are respectively communicated with the exhaust pump (23).
2. A method for recovering residual nitrocellulose acid, comprising the steps of, using the apparatus of claim 1:
step 1, placing acidic nitrocotton in a centrifuge (1) for centrifugal separation, enabling acidic liquid to enter an acid first-stage collecting tank (3), enabling the nitrocotton to sequentially pass through an acid second stage, an acid third stage and an acid fourth stage, enabling the acidic liquid in the acid third-stage collecting tank (5) to serve as washing liquid of the acid second stage, and enabling the acidic liquid in the acid fourth-stage collecting tank (4) to serve as washing liquid of the acid third stage;
step 2, the nitrocotton after replacement by the centrifuge (1) is sent to a washing machine (9) to be mixed with water, and then the nitrocotton sequentially enters the distributing device (10) and the vacuum washing filter (2), in the vacuum washing filter (2), liquid enters a mother liquor water collecting tank (20) through the mother liquor collecting section, so that the liquid circulates in the washing machine (9), the distributing device (10), the vacuum washing filter (2) and the mother liquor water collecting tank (20), the nitrocotton is distributed on filter cloth of the vacuum washing filter (2) and sequentially passes through an acid eight section, an acid seven section, an acid six section and an acid five section, a fresh washing liquid pipeline injects washing liquid into a third spraying pipe (15), the washing liquid after replacement enters an acid eight section collecting tank (11), a part of the washing liquid in the acid eight section collecting tank (11) enters the third spraying pipe (15), the other part of the washing liquid enters the acid seven-section collecting tank (12) to be used as washing liquid of the acid seven section, one part of the washing liquid in the acid seven-section collecting tank (12) enters a fourth spraying pipe (16), the other part of the washing liquid enters the acid six-section collecting tank (13), one part of the washing liquid in the acid six-section collecting tank (13) enters a fifth spraying pipe (17), the other part of the washing liquid enters the acid five-section collecting tank (14), one part of the washing liquid in the acid five-section collecting tank (14) enters a sixth spraying pipe (18), and the other part of the washing liquid enters the acid four section through a seventh spraying pipe (19).
3. The method for recycling residual nitrocellulose acid as claimed in claim 2, wherein the displacement flow rate of the second acid stage and the third acid stage is from 1 to 1.5m for cultivation/h, and the displacement flow rate of the fourth acid stage is from 0.9 to 1.5m for cultivation/h.
4. The method for recovering residual nitrocellulose acid according to claim 2, wherein the spraying and washing amounts of the eight, seven, six and five stages are all 6m for each year, and the flow rate for replenishing fresh washing liquid into the third spraying pipe (15) is 2.5m for each year.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011337909.8A CN112500500B (en) | 2020-11-25 | 2020-11-25 | Device and method for recovering residual acid of nitrocellulose |
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| CN202011337909.8A CN112500500B (en) | 2020-11-25 | 2020-11-25 | Device and method for recovering residual acid of nitrocellulose |
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| CN112500500B true CN112500500B (en) | 2022-08-05 |
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| CN113426391A (en) * | 2021-06-29 | 2021-09-24 | 山东尚舜化工有限公司 | Equipment and method for continuously producing diphenylthiourea |
| CN113387858A (en) * | 2021-06-29 | 2021-09-14 | 山东尚舜化工有限公司 | Equipment and method for continuously producing accelerant TMTD |
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| GB781534A (en) * | 1955-09-20 | 1957-08-21 | Hercules Powder Co Ltd | Improvements in or relating to nitric acid esters of cellulose and process of preparing same |
| US4046621A (en) * | 1974-12-17 | 1977-09-06 | The Ontario Paper Company Limited | Process for treating a slurry of cellulosic material |
| US4184891A (en) * | 1976-06-16 | 1980-01-22 | Societe Nationale Des Poudres Et Explosifs | Process for washing a solid substance impregnated with a liquid substance |
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| KR101967310B1 (en) * | 2017-12-12 | 2019-08-19 | 주식회사 한화 | Manufacturing apparatus of nitrocellulose and manufacturing method of nitrocellulose using the same |
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