CN113718375A - Method and device for post-treatment of carbon fiber production stock solution - Google Patents
Method and device for post-treatment of carbon fiber production stock solution Download PDFInfo
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- CN113718375A CN113718375A CN202111197147.0A CN202111197147A CN113718375A CN 113718375 A CN113718375 A CN 113718375A CN 202111197147 A CN202111197147 A CN 202111197147A CN 113718375 A CN113718375 A CN 113718375A
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- 239000011550 stock solution Substances 0.000 title claims abstract description 83
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 26
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 26
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000007380 fibre production Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 131
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 20
- 239000010959 steel Substances 0.000 claims abstract description 20
- 230000003068 static effect Effects 0.000 claims abstract description 18
- 238000003860 storage Methods 0.000 claims abstract description 14
- 229910021529 ammonia Inorganic materials 0.000 claims description 28
- 239000012535 impurity Substances 0.000 claims description 7
- 238000009987 spinning Methods 0.000 claims description 7
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 6
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000011144 upstream manufacturing Methods 0.000 claims description 5
- 238000007664 blowing Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000003780 insertion Methods 0.000 claims description 3
- 230000037431 insertion Effects 0.000 claims description 3
- 238000012958 reprocessing Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 8
- 238000010924 continuous production Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 15
- 239000000203 mixture Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000004176 ammonification Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Images
Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/32—Apparatus therefor
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention provides a method and a device for post-treatment of stock solution produced by carbon fibers, which are provided with a demonomerization tower, a defoaming tower, a stock solution storage tank and an ammonia gas steel cylinder, wherein the demonomerization tower is connected with the defoaming tower through a pipeline I, the defoaming tower is connected with the stock solution storage tank through a pipeline II, the pipeline I is provided with a gear pump I and a static mixer, the static mixer is positioned at the downstream of the gear pump I, the pipeline II is provided with the gear pump II, the ammonia gas steel cylinder is provided with a pipeline III, the pipeline III is provided with an ammonia gas nozzle, the pipeline III is connected to the pipeline I through the ammonia gas nozzle, and the pipeline III is also provided with a filter and a thermal type flowmeter. The method solves the technical problems of uneven mixing, insufficient reaction, difficult quantitative control of ammoniation degree, unstable quality of stock solution, inconvenient operation and difficult realization of high-load continuous production in the post-treatment of the existing carbon fiber production stock solution during ammoniation. The invention can be widely applied to the production of carbon fiber.
Description
Technical Field
The invention relates to a method and a device for post-treating carbon fiber stock solution, in particular to a method and a device for post-treating carbon fiber production stock solution.
Background
In the production process of carbon fibers, a variety of methods for post-processing stock solution include demonomerization, defoaming, cooling, ammonification, concentration, storage and the like, and the quality of carbon fibers is affected when the processing in each step is not in place. And the post-treatment ammoniation is particularly important in the production of the carbon fiber with DMSO as a solvent. Because of DMSO uses in the air for a long time, can take place oxidation reaction, after the oxidation reaction, DMSO's aqueous solution can present the acidity, and DMSO decomposes easily under the acid condition, and spinning under the acid condition in addition, the inside hole that forms easily of precursor causes the precursor not compact, has influenced the quality of precursor, and then influences the carbon silk quality, and the ammoniation has just prevented that DMSO from decomposing under the acid condition, has avoided the precursor to appear the hole.
In the production process of carbon fiber, there are many ammoniation methods, some of which use ammonia gas as a terminator after the reaction is finished, and introduce the ammonia gas into a polymerization kettle after the reaction, and some of which use ammoniation before demonomerization, ammoniation before defoaming, ammoniation after defoaming, or ammoniation directly in a spinning coagulation bath, but because ammonia gas is a gas and a stock solution is a liquid with viscosity, the ammonia gas is mixed into the liquid with viscosity uniformly and reacts sufficiently, which is difficult, and the ammoniation methods generally have the following defects:
1. the mixing is not uniform, the reaction is not sufficient, and the uniformity and the stability are poor;
2. the ammoniation degree of the stock solution is difficult to quantitatively control;
3. the quality of stock solution is unstable, and spinning is difficult;
4. the operation is inconvenient, and the high-load continuous production is difficult to realize.
Disclosure of Invention
The invention provides a method and a device for post-treatment of a carbon fiber production stock solution, which can accurately control the ammoniation degree of the stock solution, can uniformly mix ammonia gas and the stock solution, are convenient to operate and can realize high-load continuous production, aiming at the technical problems of unstable quality of the stock solution, inconvenience in operation and difficulty in realizing high-load continuous production caused by uneven mixing, insufficient reaction and difficulty in quantitative control of the ammoniation degree in the post-treatment of the existing carbon fiber production stock solution.
The device for post-treatment of the carbon fiber production stock solution comprises a demonomerization tower, a defoaming tower, a stock solution storage tank and an ammonia gas steel cylinder, wherein the demonomerization tower is connected with the defoaming tower through a pipeline I, the defoaming tower is connected with the stock solution storage tank through a pipeline II, the pipeline I is provided with a gear pump I and a static mixer, the static mixer is positioned at the downstream of the gear pump I, the pipeline II is provided with the gear pump II, the ammonia gas steel cylinder is provided with a pipeline III, the pipeline III is provided with an ammonia gas nozzle, the pipeline III is connected to the pipeline I through the ammonia gas nozzle, the ammonia gas nozzle is arranged between the gear pump I and the demonomerization tower, and the pipeline III is also provided with a filter and a thermal type flowmeter.
Preferably, the filter is located upstream of the thermal flow meter, and a pressure reducing valve is further disposed on the pipeline III, and the pressure reducing valve is located upstream of the filter.
Preferably, the ammonia nozzle is a seamless steel pipe, one end of the seamless steel pipe is connected with the pipeline III through a flange, the other end of the seamless steel pipe is plugged by a plug screw, and the seamless steel pipe is provided with a gas orifice.
Preferably, the included angle between the ammonia gas nozzle and the pipeline I is 20-30 degrees, and the insertion direction of the ammonia gas nozzle is opposite to the flowing direction of the stock solution.
A method for post-treating carbon fiber production stock solution comprises the following specific steps:
(1) the stock solution is discharged from the demonomerization tower and enters a pipeline I under the action of a gear pump I;
(2) conveying ammonia gas from an ammonia gas cylinder into a pipeline III, filtering impurities of the ammonia gas by a filter, then uniformly blowing the ammonia gas into stock solution of the pipeline I in a bubble form by an ammonia gas nozzle after passing through a thermal flowmeter;
(3) in the pipeline I, the gear pump I stirs the stock solution, the stirred stock solution enters a static mixer, and ammonia gas and the stock solution are fully mixed in the static mixer;
(4) the stock solution mixed with the ammonia gas enters a defoaming tower, and the ammonia gas which does not react with the stock solution and exists in a bubble form is removed;
(6) and the stock solution without bubbles is conveyed to a stock solution storage tank through a pipeline II under the action of a gear pump II for spinning.
Preferably, the pressure before the feed inlet of the gear pump I is 0.01-0.03MPa, and the outlet pressure of the ammonia gas after passing through the filter is 0.2-0.3 MPa.
Preferably, the amount of the comonomer itaconic acid in the stock solution is calculated according to the opening of the gear I, and the flow of ammonia gas is adjusted according to the amount of 0.65-0.85mol ammonia gas corresponding to 1mol of the comonomer itaconic acid.
The beneficial effects of the invention are that,
(1) the filter can filter impurities in the ammonia gas, so that the ammonia gas with impurities is prevented from entering the stock solution to influence the quality of the stock solution;
(2) the thermal flowmeter can monitor the flow of ammonia in real time to ensure the reasonable proportion of the ammonia and the stock solution, and the ammonia neutralization degree can be 0.95-1.24 and the pH value of the stock solution is 8-9.6 according to the amount of 0.65-0.85mol of ammonia blown into 1mol of comonomer itaconic acid;
(3) after ammonia gas is blown into the stock solution, the mixture is stirred by a gear pump I and mixed by a static mixer, and the mixture is fully reacted and has good stability;
(4) the ammonia nozzle is provided with a gas orifice and is inserted into the pipeline I in an included angle of 20-30 degrees and in a direction opposite to the flowing direction of the stock solution, so that ammonia can enter the pipeline I in a bubbling manner and is fully mixed with the stock solution;
(5) the technical scheme is simple in structure and convenient to operate, the stability of the stock solution after sufficient ammoniation is obviously improved, and a foundation guarantee is provided for producing high-quality carbon fibers.
Drawings
FIG. 1 is a schematic diagram of the overall structure of an embodiment of the present invention;
FIG. 2 is a schematic structural view of an ammonia gas nozzle according to an embodiment of the present invention.
The symbols in the drawings illustrate that:
1. a demonomerization tower; 2. a thermal flow meter; 3. an ammonia gas nozzle; 4. a filter; 5. ammonia cylinder; 6. a gear pump I; 7. a static mixer; 8. a deaeration tower; 9. a gear pump II; 10. a stock solution storage tank; 11. a pipeline I; 12. line II; 13. line III; 14. the top is provided with a hole; 15. the bottom is provided with a hole; 16. a flange; 17. and (4) a screw plug.
Detailed Description
The present invention will be further described with reference to the following examples.
As shown in figure 1, the device for post-treatment of the carbon fiber production stock solution is provided with a demonomerization tower 1, a defoaming tower 8, a stock solution storage tank 10 and an ammonia gas steel cylinder 5, wherein the demonomerization tower 1 is connected with the defoaming tower 8 through a pipeline I11, the defoaming tower 8 is connected with the stock solution storage tank 10 through a pipeline II 12, the ammonia gas steel cylinder 5 is provided with a pipeline III 13, the pipeline III 13 is provided with an ammonia gas nozzle 3, the pipeline III 13 is connected onto a pipeline I11 through the ammonia gas nozzle 3, the included angle between the ammonia gas nozzle 3 and the pipeline I11 is 20-30 degrees, the insertion direction of the ammonia gas nozzle 3 is opposite to the flowing direction of the stock solution, and ammonia gas can enter the pipeline I11 in a bubbling mode and is fully mixed with the stock solution.
The pipeline I11 is provided with a gear pump I6 and a static mixer 7, the ammonia nozzle 3 is arranged between the gear pump I6 and the demonomerization tower 1, the pressure at the position is small and stable, and the ammonia is easy to be blown into the stock solution. Static mixer 7 is located gear pump I6's low reaches, and after the ammonia gas was blown into the stoste, through gear pump I6 stirring and static mixer 7's mixture, the abundant reaction, stability is good. Be equipped with filter 4 and thermal flowmeter 2 on pipeline III 13, filter 4 is located thermal flowmeter 2's upper reaches, and filter 4 can filter the impurity in the ammonia, avoids the ammonia that has impurity to enter into the stoste, causes the influence to the stoste quality, and thermal flowmeter 2 can the real-time supervision ammonia flow to guarantee the rational ratio of ammonia and stoste. A pressure relief valve is also provided in line III 13, upstream of the filter 4.
A method for post-treating carbon fiber production stock solution comprises the following specific steps:
(1) the stock solution is discharged from the demonomerization tower 1 and enters a pipeline I11 under the action of a gear pump I6;
(2) conveying ammonia gas from an ammonia gas cylinder 5 into a pipeline III 13, filtering impurities of the ammonia gas by a filter 4, then passing the ammonia gas through a thermal flowmeter 2, and uniformly blowing the ammonia gas into stock solution of a pipeline I11 in a bubble form by an ammonia gas nozzle 4;
(3) in a pipeline I11, a gear pump I6 is used for stirring the stock solution, the mixture enters a static mixer 7 after being stirred, and ammonia gas and the stock solution are fully mixed in the static mixer 7;
(4) the stock solution mixed with ammonia gas enters a defoaming tower 8, and the ammonia gas which does not react with the stock solution and exists in the form of bubbles is removed;
(6) the pipeline II 12 is provided with a gear pump II 9, and the stock solution without bubbles is conveyed to a stock solution storage tank 10 through the pipeline II 12 under the action of the gear pump II 9 for spinning.
As shown in figure 2, the ammonia nozzle 3 is made of a seamless steel tube with the diameter of 21.3, the length of the seamless steel tube is 500mm, the material is 304, one end of the seamless steel tube is provided with a flange 16 connected with a pipeline III 13, the other end of the seamless steel tube is blocked by a screw plug 17, the seamless steel tube is provided with a gas orifice, the aperture of the gas orifice is 2-3mm, the surface roughness is less than or equal to 0.2 mu m, the spinneret orifice comprises a top opening 14 and a bottom opening 15, 6-8 openings are respectively arranged, and the ammonia can be ensured to smoothly enter a pipeline I11 in a bubbling mode.
Example 1
The raw liquid after demonomerization is conveyed to a defoaming tower 8 through a gear pump I6, ammonia gas enters a pipeline I11 through an ammonia gas nozzle 3, the gear pump I6 is started, the opening degree of the gear pump I6 is adjusted, and the comonomer itaconic acid (hereinafter referred to as M for short) in the raw liquid is calculated2) The mole number of the obtained ammonia gas is 0.65 times M2The mole number is controlled manually, and the pressure in front of the feed inlet of the gear pump I6 is 0.01-0.03 MPa. Opening the valve of ammonia gas steel cylinder 5, introducing ammonia gas into pipeline I11 through pressure reducing valve, filter 4 and thermal flowmeter 2 on pipeline III 13, and adjusting ammonia gas flow to 0.65 times M2The mole number and the outlet pressure of the ammonia gas after passing through the filter 4 are adjusted to be 0.2-0.3MPa, and the manual state is converted into the automatic state after the ammonia gas is finished. Ammonia gas was blown into the line I11 through the ammonia gas nozzle 3, and the reaction occurred in the line I11 after stirring by the gears of the gear pump I6 and mixing by the static mixer 7. After the reaction, unreacted ammonia exists in the stock solution in the form of bubbles, the stock solution with the unreacted ammonia enters a defoaming tower 8 to be defoamed, the bubbles are removed, and the stock solution without the bubbles is conveyed to a stock solution storage tank 10 through a gear pump II 9 for spinning.
The scheme is sampled and detected, the pH value of the stock solution is 8, the ammonia neutralization degree is 0.95, and no bubbles exist.
Example 2
Unlike example 1, the opening degree of the gear pump I6 was adjusted to calculate M in the stock solution2The mole number of the obtained ammonia gas is 0.75 time M2Molar number, adjusting ammonia flow to 0.75 times M2The number of moles, sampling and detection, the pH value of the stock solution is 9.2, the ammonia neutralization degree is 1.11, and no bubbles exist.
Example 3
Unlike example 1, the opening degree of the gear pump I6 was adjusted to calculate M in the stock solution2The mole number of the obtained ammonia gas is 0.85 times M2Molar number, adjusting ammonia flow to 0.85 times M2The number of moles, sampling and detection, the pH value of the stock solution is 9.6, the ammonia neutralization degree is 1.24, and no bubbles exist.
The technical scheme is simple in structure and convenient to operate, the stability of the stock solution after sufficient ammoniation is obviously improved, and a foundation guarantee is provided for producing high-quality carbon fibers.
However, the above description is only exemplary of the present invention, and the scope of the present invention should not be limited thereby, and the replacement of the equivalent components or the equivalent changes and modifications made according to the protection scope of the present invention should be covered by the claims of the present invention.
Claims (7)
1. The utility model provides a device of carbon fiber production stoste aftertreatment, its characterized in that is equipped with demould tower, defoaming tower, stoste storage tank, ammonia cylinder, demould the tower with the defoaming tower passes through pipeline I and connects, the defoaming tower with the stoste storage tank passes through pipeline II and connects, be equipped with gear pump I and static mixer on the pipeline I, static mixer is located gear pump I's low reaches, be equipped with gear pump II on the pipeline II, be equipped with pipeline III on the ammonia cylinder, be equipped with the ammonia nozzle on the pipeline III, pipeline III passes through the ammonia nozzle is connected to on the pipeline I, the ammonia nozzle is established gear pump I with between the demould tower, still be equipped with filter and hot type flowmeter on the pipeline III.
2. The apparatus for reprocessing a carbon fiber production dope as claimed in claim 1, wherein said filter is located upstream of said thermal flow meter, and a pressure reducing valve is further provided on said line III, said pressure reducing valve being located upstream of said filter.
3. The device for post-treatment of the carbon fiber production stock solution according to claim 1, wherein the ammonia gas nozzle is a seamless steel pipe, one end of the seamless steel pipe is connected with the pipeline III through a flange, the other end of the seamless steel pipe is blocked by a plug screw, and the seamless steel pipe is provided with a gas orifice.
4. The device for post-treatment of carbon fiber production stock solution according to claim 3, wherein the included angle between the ammonia gas nozzle and the pipeline I is 20-30 degrees, and the insertion direction of the ammonia gas nozzle is opposite to the flowing direction of the stock solution.
5. A method for post-treating the carbon fiber production stock solution of any one of claims 1 to 4, which comprises the following specific steps:
(1) the stock solution is discharged from the demonomerization tower and enters a pipeline I under the action of a gear pump I;
(2) conveying ammonia gas from an ammonia gas cylinder into a pipeline III, filtering impurities of the ammonia gas by a filter, then uniformly blowing the ammonia gas into stock solution of the pipeline I in a bubble form by an ammonia gas nozzle after passing through a thermal flowmeter;
(3) in the pipeline I, the gear pump I stirs the stock solution, the stirred stock solution enters a static mixer, and ammonia gas and the stock solution are fully mixed in the static mixer;
(4) the stock solution mixed with the ammonia gas enters a defoaming tower, and the ammonia gas which does not react with the stock solution and exists in a bubble form is removed;
(6) and the stock solution without bubbles is conveyed to a stock solution storage tank through a pipeline II under the action of a gear pump II for spinning.
6. The method for post-treating carbon fiber production stock solution as recited in claim 5, wherein the pressure before the feed inlet of the gear pump I is 0.01 to 0.03MPa, and the outlet pressure of ammonia gas after passing through the filter is 0.2 to 0.3 MPa.
7. The method for post-treating the carbon fiber production stock solution according to claim 5, wherein the amount of the comonomer itaconic acid in the stock solution is calculated according to the opening degree of the gear I, and the flow of ammonia gas is adjusted according to the amount of 0.65-0.85mol ammonia gas corresponding to 1mol comonomer itaconic acid.
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| CN202111197147.0A CN113718375B (en) | 2021-10-14 | 2021-10-14 | Method and device for post-treatment of carbon fiber production stock solution |
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