CN113718375B - 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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- CN113718375B CN113718375B CN202111197147.0A CN202111197147A CN113718375B CN 113718375 B CN113718375 B CN 113718375B CN 202111197147 A CN202111197147 A CN 202111197147A CN 113718375 B CN113718375 B CN 113718375B
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- 239000011550 stock solution Substances 0.000 title claims abstract description 85
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 21
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 21
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000007380 fibre production Methods 0.000 title claims abstract description 16
- 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 147
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 23
- 239000010959 steel Substances 0.000 claims abstract description 23
- 230000003068 static effect Effects 0.000 claims abstract description 18
- 238000003860 storage Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 47
- 238000003756 stirring Methods 0.000 claims description 8
- 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
- 239000012535 impurity Substances 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
- 238000009987 spinning Methods 0.000 claims description 6
- 238000011144 upstream manufacturing Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000003780 insertion Methods 0.000 claims 1
- 230000037431 insertion Effects 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000010924 continuous production Methods 0.000 abstract description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 15
- 230000002378 acidificating effect Effects 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 230000005587 bubbling Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 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
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 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
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
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- 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 in carbon fiber production, wherein the method is provided with a single removal tower, a defoaming tower, a stock solution storage tank and an ammonia gas steel bottle, the single removal 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, a gear pump I and a static mixer are arranged on the pipeline I, the static mixer is positioned at the downstream of the gear pump I, a gear pump II is arranged on the pipeline II, a pipeline III is arranged on the ammonia gas steel bottle, an ammonia gas nozzle is arranged on the pipeline III, the pipeline III is connected to the pipeline I through the ammonia gas nozzle, and a filter and a thermal flowmeter are also arranged on the pipeline III. The method solves the technical problems that the quality of the stock solution is unstable, the operation is inconvenient and the high-load continuous production is difficult to realize due to uneven mixing, insufficient reaction and difficult quantitative control of the ammoniation degree in the existing carbon fiber production stock solution post-treatment. The invention can be widely applied to carbon fiber production.
Description
Technical Field
The invention relates to a method and a device for post-treatment of carbon fiber stock solution, in particular to a method and a device for post-treatment of carbon fiber production stock solution.
Background
In the production process of carbon fibers, various post-treatment methods of stock solutions are available, including single removal, defoaming, cooling, ammoniation, concentration, storage and the like, and the quality of carbon filaments can be affected when the treatment is not in place in each step. And the carbon fiber production with DMSO as a solvent is particularly important for post-treatment ammoniation. Because DMSO is used in the air for a long time, oxidation reaction can occur, after the oxidation reaction, the water solution of DMSO can be acidic, DMSO is easy to decompose under the acidic condition, and holes are easy to form in the precursor fiber under the acidic condition, so that the precursor fiber is not compact, the quality of the precursor fiber is influenced, the quality of carbon fiber is further influenced, and the decomposition of DMSO under the acidic condition is prevented by ammoniation, so that the occurrence of holes in the precursor fiber is avoided.
In the carbon fiber production process, many ammoniation methods are adopted, ammonia is used as a terminator after the reaction is finished, ammonia is directly introduced into a polymerization kettle after the reaction, and the ammonia is also ammoniated before the removal of monomers, before the defoaming, after the defoaming or directly in a spinning coagulation bath, but because ammonia is gas and stock solution is liquid with viscosity, the gas is required to be uniformly mixed into the liquid with viscosity and fully reacted, and the following defects are difficult to be caused in the ammoniation method generally:
1. uneven mixing, insufficient reaction, poor uniformity and stability;
2. the degree of the liquefied ammonia is difficult to quantitatively control;
3. the quality of the stock solution is unstable, and the spinning is difficult;
4. inconvenient operation and difficult continuous production with high load.
Disclosure of Invention
Aiming at the technical problems that the quality of the stock solution is unstable, the operation is inconvenient and the high-load continuous production is difficult to realize due to uneven mixing, insufficient reaction and difficult quantitative control of the ammoniation degree in the prior carbon fiber production stock solution post-treatment, the invention provides the method and the device for the carbon fiber production stock solution post-treatment, which can accurately control the ammoniation degree of the stock solution, ensure that the ammonia gas and the stock solution can be uniformly mixed, are convenient to operate and can realize the high-load continuous production.
Therefore, the technical scheme of the invention is that the device for post-treatment of the stock solution in carbon fiber production is provided with a single removal tower, a defoaming tower, a stock solution storage tank and an ammonia steel bottle, wherein the single removal 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, a gear pump I and a static mixer are arranged on the pipeline I, the static mixer is positioned at the downstream of the gear pump I, a gear pump II is arranged on the pipeline II, a pipeline III is arranged on the ammonia steel bottle, an ammonia nozzle is arranged on the pipeline III, the pipeline III is connected to the pipeline I through the ammonia nozzle, the ammonia nozzle is arranged between the gear pump I and the single removal tower, and a filter and a thermal flowmeter are also arranged on the pipeline III.
Preferably, the filter is located upstream of the thermal flowmeter, and a pressure reducing valve is further arranged on the pipeline III, and the pressure reducing valve is located upstream of the filter.
Preferably, the ammonia gas nozzle adopts 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 screw plug, and a gas injection hole is formed in the seamless steel pipe.
Preferably, the included angle between the ammonia gas nozzle and the pipeline I is 20-30 degrees, and the inserting direction of the ammonia gas nozzle is opposite to the flowing direction of the stock solution.
A method for post-treatment of carbon fiber production stock solution comprises the following specific steps:
(1) The stock solution comes out of the single removal tower and enters a pipeline I under the action of a gear pump I;
(2) Ammonia gas is conveyed from an ammonia gas steel bottle and enters the pipeline III, and after impurities are filtered by a filter, the ammonia gas passes through a thermal flowmeter and uniformly blasted into the stock solution of the pipeline I in a bubble form through an ammonia gas nozzle;
(3) In the pipeline I, the gear pump I stirs the stock solution, and the stock solution enters a static mixer after stirring, and ammonia gas and the stock solution are fully mixed in the static mixer;
(4) The stock solution after mixing ammonia enters a defoaming tower, and ammonia which does not react with the stock solution and exists in the form of bubbles is removed;
(6) The stock solution with bubbles removed 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 in front of 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 0.2-0.3MPa.
Preferably, 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 rate of the ammonia gas is adjusted according to the amount of the 1mol of comonomer itaconic acid corresponding to 0.65-0.85mol of ammonia gas.
The invention has the advantages that,
(1) The arrangement of the filter can filter out impurities in the ammonia gas, so that the ammonia gas with the impurities is prevented from entering the stock solution, and the quality of the stock solution is prevented from being influenced;
(2) The thermal flowmeter can monitor the flow of the ammonia in real time to ensure reasonable proportion of the ammonia and the stock solution, and the neutralization degree of the ammonia can be 0.95-1.24 according to the amount of blowing 0.65-0.85mol of ammonia into 1mol of comonomer itaconic acid, and the PH of the stock solution is 8-9.6;
(3) After ammonia gas is blown into the stock solution, stirring by a gear pump I and mixing by a static mixer are carried out, so that the reaction is fully carried out, and the stability is good;
(4) The ammonia gas nozzle is provided with an air jet hole, and is inserted into the pipeline I in an included angle of 20-30 degrees in a direction opposite to the flow direction of the raw liquid, so that ammonia gas can enter the pipeline I in a bubbling mode and is fully mixed with the raw liquid;
(5) The technical scheme of the application is simple in structure and convenient to operate, the stability of the stock solution after full ammoniation is obviously improved, and basic guarantee is provided for production of high-quality carbon fibers.
Drawings
FIG. 1 is a schematic overall structure of an embodiment of the present invention;
FIG. 2 is a schematic view of the structure of an ammonia gas nozzle according to an embodiment of the present invention.
The symbols in the drawings illustrate:
1. removing a single tower; 2. a thermal flowmeter; 3. an ammonia gas nozzle; 4. a filter; 5. ammonia gas steel cylinder; 6. a gear pump I; 7. a static mixer; 8. a defoaming tower; 9. a gear pump II; 10. a stock solution storage tank; 11. a pipeline I; 12. a pipeline II; 13. line III; 14. a top opening; 15. a bottom is provided with a hole; 16. a flange; 17. and (5) a screw plug.
Detailed Description
The invention is further described below with reference to examples.
As shown in figure 1, a device for post-treatment of stock solution in carbon fiber production is provided with a single removal tower 1, a defoaming tower 8, a stock solution storage tank 10 and an ammonia steel bottle 5, wherein the single removal 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, a pipeline III 13 is arranged on the ammonia steel bottle 5, an ammonia nozzle 3 is arranged on the pipeline III 13, the pipeline III 13 is connected to a pipeline I11 through the ammonia nozzle 3, the included angle between the ammonia nozzle 3 and the pipeline I11 is 20-30 degrees, the inserting direction of the ammonia nozzle 3 is opposite to the flowing direction of the stock solution, and ammonia can enter the pipeline I11 in a bubbling mode and be fully mixed with the stock solution.
Be equipped with gear pump I6 and static mixer 7 on the pipeline I11, ammonia nozzle 3 establishes between gear pump I6 and take off single tower 1, and this place pressure is less and stable, easily ammonia gas blast stock solution. The static mixer 7 is positioned at the downstream of the gear pump I6, and after ammonia gas is blown into the stock solution, the stock solution is stirred by the gear pump I6 and mixed by the static mixer 7, so that the reaction is fully carried out, and the stability is good. Be equipped with filter 4 and thermal flowmeter 2 on the pipeline III 13, filter 4 is located thermal flowmeter 2's the upper reaches, and filter 4 can filter the impurity in the ammonia, avoids having the ammonia of impurity to enter into the stoste, causes the influence to the stoste quality, and thermal flowmeter 2 can real-time supervision ammonia flow to guarantee the reasonable ratio of ammonia and stoste. The line III 13 is also provided with a pressure relief valve, which is located upstream of the filter 4.
A method for post-treatment of carbon fiber production stock solution comprises the following specific steps:
(1) The stock solution comes out of the single removal tower 1 and enters a pipeline I11 under the action of a gear pump I6;
(2) Ammonia gas is conveyed from an ammonia gas steel bottle 5 to enter a pipeline III 13, filtered by a filter 4, filtered by a thermal flowmeter 2, and uniformly blown into a stock solution of a pipeline I11 in a bubble form through an ammonia gas nozzle 4;
(3) In the pipeline I11, the gear pump I6 stirs the stock solution, the stock solution enters the static mixer 7 after stirring, and ammonia gas and the stock solution are fully mixed in the static mixer 7;
(4) The stock solution after mixing ammonia enters a defoaming tower 8, and ammonia which does not react with the stock solution and exists in the form of bubbles is removed;
(6) The gear pump II 9 is arranged on the pipeline II 12, and the stock solution with bubbles removed is conveyed to the stock solution storage tank 10 through the pipeline II 12 under the action of the gear pump II 9 for spinning.
As shown in FIG. 2, the ammonia gas nozzle 3 is a seamless steel pipe with the diameter of 21.3, the length of 500mm and the material of 304, one end of the seamless steel pipe is provided with a flange 16 which is connected with the pipeline III 13, the other end of the seamless steel pipe is blocked by a screw plug 17, the seamless steel pipe is provided with gas injection holes with the aperture of 2-3mm, the surface roughness is less than or equal to 0.2 mu m, and the number of the gas injection holes comprises a top opening 14 and a bottom opening 15, and 6-8 gas injection holes are respectively arranged, so that ammonia gas can be ensured to smoothly enter the pipeline I11 in a bubbling mode.
Example 1
The stock solution after the removal of the monomer is conveyed to a deaeration 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 of the gear pump I6 is adjusted, and a comonomer itaconic acid (hereinafter referred to as M) in the stock solution is calculated 2 ) Mole number, obtaining M0.65 times of ammonia 2 The number of moles is controlled manually, and the pressure before the feed inlet of the gear pump I6 is 0.01-0.03MPa. Opening the valve of the ammonia steel bottle 5, enabling ammonia to enter the pipeline I11 through the pressure reducing valve, the filter 4 and the thermal flowmeter 2 on the pipeline III 13, and adjusting the flow of the ammonia to be 0.65 times M 2 The number of moles of the catalyst is calculated,the outlet pressure of the ammonia gas after passing through the filter 4 is regulated to be 0.2-0.3MPa, and after the completion, the manual state is converted into the automatic state. Ammonia gas is blown into the line I11 through the ammonia gas nozzle 3, and the reaction occurs after the stirring by the gear of the gear pump I6 and the mixing by the static mixer 7 in the line I11. 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 remove the bubbles, and the stock solution with the bubbles removed is conveyed to a stock solution storage tank 10 through a gear pump II 9 for spinning.
The scheme is used for sampling and detecting, the pH value of the stock solution is 8, the neutralization degree of ammonia 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 solution 2 Mole number, obtaining M0.75 times of ammonia 2 Molar number, regulating ammonia flow to 0.75 times M 2 The molar number, sampling and detection are carried out, the PH value of the stock solution is 9.2, the neutralization degree of ammonia is 1.11, and no bubbles are generated.
Example 3
Unlike example 1, the opening degree of the gear pump I6 was adjusted to calculate M in the stock solution 2 Mole number, obtaining M0.85 times of ammonia 2 Molar number, regulating ammonia flow to 0.85 times M 2 The molar number, sampling and detection are carried out, the PH value of the stock solution is 9.6, the neutralization degree of ammonia is 1.24, and no bubbles are generated.
The technical scheme of the application is simple in structure and convenient to operate, the stability of the stock solution after full ammoniation is obviously improved, and basic guarantee is provided for production of high-quality carbon fibers.
However, the foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, so that the substitution of equivalent elements or equivalent variations and modifications within the scope of the invention are intended to fall within the scope of the claims.
Claims (2)
1. The device for post-treatment of the stock solution in carbon fiber production is characterized by comprising a descaler, a defoaming tower, a stock solution storage tank and an ammonia gas cylinder, wherein the descaler 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, a gear pump I and a static mixer are arranged on the pipeline I, the static mixer is positioned at the downstream of the gear pump I, a gear pump II is arranged on the pipeline II, a pipeline III is arranged on the ammonia gas cylinder, an ammonia gas nozzle is arranged on the pipeline III, 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 descaler, the ammonia gas nozzle adopts 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 screw plug, the seamless steel pipe is provided with gas holes, the gas holes comprise a top opening and a bottom opening, 6-8 gas nozzles are respectively arranged, and the included angle between the ammonia gas nozzle and the pipeline I is 20-30 degrees, and the flow direction of the ammonia gas nozzle is opposite to the flow direction of the stock solution; a filter and a thermal flowmeter are further arranged on the pipeline III; a pressure reducing valve is further arranged on the pipeline III; the filter is located upstream of the thermal flow meter and the pressure relief valve is located upstream of the filter.
2. A method of using the apparatus for post-treatment of carbon fiber production stock solution of claim 1, comprising the specific steps of:
(1) The stock solution comes out of the single removal tower and enters a pipeline I under the action of a gear pump I;
(2) Ammonia gas is conveyed from an ammonia gas steel bottle and enters the pipeline III, the ammonia gas is filtered by a filter to remove impurities, and then the filtered ammonia gas passes through a thermal flowmeter and uniformly blasted into the stock solution of the pipeline I in a bubble form through an ammonia gas nozzle, wherein the insertion direction of the ammonia gas nozzle is opposite to the flowing direction of the stock solution;
(3) In the pipeline I, the gear pump I stirs the stock solution, and the stock solution enters a static mixer after stirring, and ammonia gas and the stock solution are fully mixed in the static mixer;
(4) The stock solution after mixing ammonia enters a defoaming tower, and ammonia which does not react with the stock solution and exists in the form of bubbles is removed;
(5) The stock solution with bubbles removed is conveyed to a stock solution storage tank through a pipeline II under the action of a gear pump II for spinning;
the pressure in front of the feed inlet of the gear pump I is 0.01-0.03MPa, and the outlet pressure of ammonia gas after passing through the filter is 0.2-0.3MPa; and calculating the quantity of the comonomer itaconic acid in the stock solution according to the opening degree of the gear pump I, and regulating the flow of ammonia according to the quantity of the 1mol of comonomer itaconic acid corresponding to 0.65-0.85mol of ammonia.
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| US20050206032A1 (en) * | 2004-03-22 | 2005-09-22 | Fuji Photo Film Co., Ltd. | Preparation method of polymer solution |
| CN102336865B (en) * | 2011-06-29 | 2013-08-28 | 浙江泰先新材料股份有限公司 | Ammonification method of polyacrylonitrile polymerization liquid and device for realizing same |
| CN105088422B (en) * | 2015-08-21 | 2017-10-24 | 威海拓展纤维有限公司 | Polyacryl-nitrile spinning fluid fills ammonia method in preparing |
| DE102015114766B4 (en) * | 2015-09-03 | 2019-04-25 | Sartorius Stedim Biotech Gmbh | Apparatus and method for preparing a solution |
| CN106422771A (en) * | 2016-11-04 | 2017-02-22 | 中冶焦耐(大连)工程技术有限公司 | Ammonia spraying structural body |
| CN106799173A (en) * | 2016-12-16 | 2017-06-06 | 芜湖万向新元环保科技有限公司 | A kind of gas mixing static mixer |
| CN107504367B (en) * | 2017-06-27 | 2020-06-16 | 中国第一汽车股份有限公司 | Ammonia gas circulating charging system and ammonia gas circulating charging method thereof |
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