CN113564761A - Pot-type treatment method for high silica fiber fixed-length yarn - Google Patents
Pot-type treatment method for high silica fiber fixed-length yarn Download PDFInfo
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- CN113564761A CN113564761A CN202110661385.6A CN202110661385A CN113564761A CN 113564761 A CN113564761 A CN 113564761A CN 202110661385 A CN202110661385 A CN 202110661385A CN 113564761 A CN113564761 A CN 113564761A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 286
- 239000000835 fiber Substances 0.000 title claims abstract description 167
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 150
- 238000000034 method Methods 0.000 title claims abstract description 66
- 238000011282 treatment Methods 0.000 title claims description 67
- 239000002253 acid Substances 0.000 claims abstract description 114
- 239000011159 matrix material Substances 0.000 claims abstract description 87
- 238000002386 leaching Methods 0.000 claims abstract description 71
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 230000008569 process Effects 0.000 claims abstract description 40
- 238000005406 washing Methods 0.000 claims abstract description 27
- 238000001035 drying Methods 0.000 claims abstract description 26
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 8
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 8
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 82
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 239000006185 dispersion Substances 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 16
- 208000005156 Dehydration Diseases 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 10
- 238000006297 dehydration reaction Methods 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000004513 sizing Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000007796 conventional method Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 230000008901 benefit Effects 0.000 abstract description 3
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- 238000012797 qualification Methods 0.000 abstract description 2
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- 239000011521 glass Substances 0.000 description 7
- 239000003365 glass fiber Substances 0.000 description 5
- 238000005507 spraying Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000004804 winding Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
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- 239000000376 reactant Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 210000005069 ears Anatomy 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
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- 239000011734 sodium Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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Classifications
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/02—Yarns or threads characterised by the material or by the materials from which they are made
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B15/00—Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B15/00—Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
- D06B15/10—Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours by use of centrifugal force
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/02—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fibres, slivers or rovings
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/01—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof
- D06M11/05—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with hydrogen, water or heavy water; with hydrides of metals or complexes thereof; with boranes, diboranes, silanes, disilanes, phosphines, diphosphines, stibines, distibines, arsines, or diarsines or complexes thereof with water, e.g. steam; with heavy water
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
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- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2101/00—Inorganic fibres
- D10B2101/02—Inorganic fibres based on oxides or oxide ceramics, e.g. silicates
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
A pot-type treating method for the fixed-length high-silica fibre includes dispersing the high-silica fibres by disperser, removing the surface impregnating agent from the high-silica fibres, acid leaching in forward and backward directions, and treating the resultant SiO2And washing the high silica matrix fiber bundle with the content of more than 96% with water until the PH value is 5-7. Dewatering and drying to obtain the high silica fiber yarn. The invention breaks through the conventional process, improves the production efficiency of the high silica matrix fiber by 20 percent, and has no pollution to the environmentThe observation qualified rate is improved by 3 to 5 percent. The retention rate of the strength of the dispersed high silica matrix fiber is not obviously different from that of the undispersed high silica matrix fiber. The method has the advantages of short process flow, high automation degree and good service performance of the high silica fiber yarn such as strength, temperature resistance and the like, the efficiency of the acid leaching and water washing process is improved by more than 20%, water is saved by more than 50% in the water washing process, the yarn strength of the obtained high silica fiber yarn is improved by more than 10%, the qualification rate is improved from 74% to more than 95%, and the method has high popularization and application values.
Description
Technical Field
The invention relates to the technical field of non-woven fabrics, in particular to a method for manufacturing high-temperature resistant fiber fixed-length yarns.
Background
The high silica fiber is used as a high-temperature resistant inorganic fiber, has excellent performance and relative price advantage, is widely used in the aspects of high-temperature metal liquid melting and filtering, high-temperature gas dust collection, aerospace heat ablation resistant materials and the like, and has wide application prospect and market potential. In recent years, the demand of high silica fiber is increasing, and companies at home and abroad make intensive research on the strength and heat resistance of the high silica fiber, so that the application of high silica fiber products is expanded, and part of the high silica fiber products is successfully applied to the filtration of high-temperature gas, liquid and corrosive media and various high-end fields.
The high silica fiber fixed-length yarn belongs to one kind of high silica fiber product, and is produced through phase separating treatment, acid leaching, water washing and stoving.
In the prior art, the high silica fiber fixed-length yarn is prepared by manufacturing high silica matrix fibers into yarn bundles through the working procedures of unwinding, cabling, shaking hanging and the like, and then performing the working procedures of acid leaching, water washing, drying, short cutting and the like to prepare a finished product. Chinese patent document CN101654833A discloses a high silica glass fiber staple yarn and its manufacturing process, which comprises preparing a yarn bobbin from glass fiber raw yarn through twisting and plying processes, winding the yarn bundle with a winding device, arranging the yarn uniformly on a special creel, placing the yarn in an acid leaching tank for processing in a suspension manner, then soaking the yarn in clear water, and washing at 40-60 ℃. And simultaneously, testing the acid-containing state of the surface of the yarn by using a pH test paper, finishing washing when the pH value is more than 5, and chopping the yarn into a certain length after drying.
The invention with the publication number of CN102839476A discloses a production process of high-strength high-silica glass fiber yarn, which comprises the steps of carrying out unwinding and stranding processes on sodium borosilicate glass fiber protofilament to prepare high-silica glass fiber raw yarn, winding the raw yarn on a yarn frame by using a winding machine to prepare yarn rolls, uniformly distributing the yarn rolls in a hanging manner, and placing the yarn rolls in an acid leaching tank for treatment. After acid discharge, hot water with the temperature of 50-65 ℃ is added into an acid tank in a spraying mode, the acid tank is circularly stirred by an acid-proof pump and cleaned for 20-30 minutes, then the water is discharged, then normal-temperature water is added into an acid leaching tank in a spraying mode after the water discharge, the acid tank is circularly stirred by the acid-proof pump and cleaned for 20-30 minutes, and then the water is discharged.
In the invention with publication number CN102643036A, a batch production process of high silica glass fiber chopped yarn is disclosed, the glass blank yarn is cut to form glass chopped yarn; placing the cut glass chopped yarns in an acid leaching tank, carrying out acid leaching treatment, selecting hydrochloric acid with the molar concentration of 1.6-3.3 mol/L, electrically heating the hydrochloric acid, controlling the temperature at 90-96 ℃, and treating for 1-2.8 hours; removing residual acid on the surface of the glass chopped yarn after the acid leaching treatment, soaking the glass chopped yarn in clear water, controlling the water temperature to be 45-58 ℃, washing under the flowing of the water liquid, and finishing the washing when the pH value is more than 5; by adopting an intermittent production process technology, the content of silicon dioxide in the high-silica fiber chopped yarns is more than 94%, and the high-temperature resistance is better.
It can be seen that the high silica fiber staple yarns made according to the two different processes described above have the following disadvantages. The first process method comprises the following steps: 1. before acid leaching, the high silica-based yarn needs to be subjected to a plurality of procedures of unwinding, cabling and shaking hanging, and the problems of raw silk bundle breakage, abrasion and oil spike quality are easily caused due to long process route and production process of each procedure. Along with the continuous improvement of labor cost, the personnel of operation, transportation, equipment maintenance of each process are too much, the manufacturing cost is increased, and the competitiveness of products in the market is reduced. 2. In the acid leaching process, the yarn roll is placed in the acid leaching tank in a hanging mode to react with acid liquor, and alkaline substances separated out through reaction are continuously accumulated at the position where the yarn roll is contacted with the rod, so that the fiber is prevented from further reacting with the acid liquor, the high-silica matrix fiber is blocked, and the product quality is influenced. In the above process, the contact part of the yarn and the rod can only be manually kneaded and turned by workers to avoid caking, and the operation is very inconvenient and the product quality is difficult to ensure because of high acid temperature and acid gas choking. 3. In the washing process, the yarn roll stands in an acid tank, and is washed by adopting the modes of spraying, soaking in clear water and overflowing from the tank body, the acid liquid and organic matters attached to the surface of the yarn roll can be taken away by the spraying through the flowing of water, and the acid liquid and alkaline matters precipitated by reaction attached to the inside of the yarn roll can only be slowly dissolved in the water and continuously migrate from inside to outside. Because the yarn roll is thick, the inside acidizing fluid, the alkaline material that the reaction is appeared are difficult to the sanitization, use the sour groove washing, need 3 ~ 4 hours just can replace the water in the groove completely once to lead to the washing time long, the water consumption is big, the inconsistent problem inside and outside the pH value. 4. Because the tank body used in the acid leaching process has larger volume, the unorganized discharge caused by the overflow of acid gas in the tank body has certain influence on the environment and the health of operators. With the increasing enhancement of environmental protection requirements, the process cannot meet the requirements of the production of the high silica fiber fixed-length yarns.
The second process method comprises the following steps: cutting the glass greige yarn to form glass chopped yarns; the cut blank yarns are stacked together and placed in an acid leaching tank, the reaction rate and degree of the inner layer and the outer layer of each blank yarn in hydrochloric acid are different, the content of silicon dioxide in the high silica fiber chopped yarns obtained by reaction is inconsistent, the content of silicon dioxide in the outer layer of each blank yarn can reach 96%, the content of silicon dioxide in the inner layer of each blank yarn can only reach 94% -95%, and the high temperature resistance of the high silica fiber chopped yarns is general due to the fact that the content of silicon dioxide is low, and the quality of products cannot be guaranteed.
The second process method comprises the following steps: chopping the high silica-based yarn to form a fixed-length yarn; the chopped high silica-based yarns are stacked together and placed in an acid leaching tank, the reaction speed and degree of the inner layer and the outer layer of the base yarns in hydrochloric acid are different, the content of silicon dioxide in the high silica fiber fixed length yarns obtained through reaction is inconsistent, the content of silicon dioxide in the outer layer can meet the technical requirement, and the content of silicon dioxide in the inner layer is lower. Meanwhile, the same problem exists in water washing, and because the content of silicon dioxide in the inner layer is low and the water washing is not thorough, the high-temperature resistance of the high-silica fiber fixed-length yarn is affected, and the quality of the product cannot be guaranteed.
Disclosure of Invention
In order to overcome the defects of excessive previous working procedures of the high silica fiber fixed-length yarn, acid leaching and blocking, difference of the content of silicon dioxide on the inner side and the outer side, incomplete water washing, poor consistency of high temperature resistance and unorganized discharge caused by acid gas overflow in the prior art, the invention provides a pot-type treatment method of the high silica fiber fixed-length yarn.
The specific process of the invention is as follows:
step 1, preparing high silica matrix fiber:
the high silica matrix fiber is prepared by a chopping machine. Specifically, high silica matrix fibers with the diameter of 3-12 mu m, the length of 500-1000 mm and the weight of 5-100 kg are cut into high silica matrix fibers with the length of 20-150 mm by a chopping machine.
Step 2, preparing high silica matrix fiber bundles:
and (3) sending the chopped 5-100 kg of high-silica matrix fibers into a dispersion machine for dispersion through a conveyer belt, wherein the running speed of the conveyer belt is 5-15 m/h, the rotating speed of the dispersion machine is 100-2120 revolutions per minute, and the dispersion amount of the dispersion machine is 20-350 kg/h. Dispersing into single-bundle high silica matrix fibers with the diameter of 1-10 mm. Obtaining the high silica matrix fiber bundle. And (5) standby.
Step 3, removing the impregnating compound on the surface of the fiber
And putting the obtained high silica matrix fiber bundle into an acid-resistant tank with the diameter of 200-1500 mm and the height of 300-1500 mm, injecting hot water through a circulating pump, and soaking the high silica matrix fiber bundle in the acid-resistant tank in the hot water to remove the impregnating compound on the surface of the fiber, thereby being beneficial to phase separation of the matrix fiber in the acid leaching process. The liquid level of the hot water is 10-100 mm higher than the upper surface of the high silica matrix fiber bundle. The hot water temperature is 35-60 ℃, and the flow rate is 5-15 m3Soaking for 0.5-1.5 h, and removing the fiber surface of the high silica matrix fiber bundleThe impregnating agent of (1).
Step 4, acid leaching treatment
And injecting a hydrochloric acid solution into the acid-resistant tank in which the high silica matrix fiber bundle subjected to the fiber surface treating compound removal is placed through a circulating pump, and performing acid leaching reactions in different directions on the fiber bundle, so that the hydrochloric acid in the acid leaching treatment can fully and uniformly react with the high silica matrix fiber bundle subjected to the fiber surface treating compound removal. The acid leaching reactions in different directions comprise an acid leaching reaction process in a reverse direction from bottom to top along the acid-resistant tank body and an acid leaching reaction process in a positive direction from top to bottom along the acid-resistant tank body. The concentration of the hydrochloric acid solution is 1.8-3.3 mol/L, and the temperature is 80-95 ℃.
In the reverse-direction acid leaching reaction, injecting a hydrochloric acid solution from the bottom of the acid-proof tank through an acid-proof pump, discharging the hydrochloric acid solution from the top of the acid-proof tank, and performing reverse-direction circulating acid leaching treatment; the flow rate of the hydrochloric acid solution is 5-15 m3The pressure of the acid-proof pump is 0.2-1.0 MP per hour, and the reaction time is 30-150 min.
And after the reverse acid leaching treatment is finished, performing forward acid leaching treatment. In the positive acid leaching treatment, a hydrochloric acid solution is injected from the top of the acid-proof tank through an acid-proof pump, and the hydrochloric acid solution is discharged from the bottom of the acid-proof tank, wherein the flow rate of the hydrochloric acid solution is 5-15 m3The pressure of the acid-proof pump is 0.2-1.0 MP, and the reaction time is 30-150 min. After the positive acid leaching treatment is finished, the first acid leaching treatment of the high silica matrix fiber bundle subjected to fiber surface treating compound removal is finished.
And repeating the forward acid leaching treatment process and the reverse acid leaching treatment process for 3-5 times to complete the acid leaching treatment of the high silica matrix fiber bundle with the fiber surface treating compound removed and drain the hydrochloric acid solution. To obtain SiO2High silica matrix fiber bundles with a content of greater than 96%.
Step 5, water washing treatment
Injecting water with the temperature of 20-35 ℃ into the acid-resistant tank by using an acid-resistant pump to ensure that the SiO in the acid-resistant tank is opposite2The high silica matrix fiber bundle with the content of more than 96 percent is cleanedAnd washing until the pH value of the fiber bundle is 5-7.
Step 6, dehydration treatment
Cleaning the SiO2The high silica fiber matrix bundles with the content of more than 96 percent are put into a cleaning and spin-drying machine for dehydration. The rotating speed of the cleaning and spin-drying machine is 10-150 r/min, and the dehydration time is 1-30 min.
Step 7, drying treatment
Dehydrating the SiO2The high silica matrix fiber bundle with the content of more than 96 percent is put into a microwave oven for drying. The drying temperature is 120-160 ℃, and the drying time is 10-120 min. And drying to obtain the high silica fiber fixed length yarn.
Experiments prove that the invention breaks through the conventional process, has scientific and reasonable process steps and provides a novel method for producing the high silica fiber fixed-length yarn. Compared with the prior art, the invention has the following beneficial effects:
1. the process does not need to be subjected to a plurality of procedures of untwisting, cabling and swinging, reduces the damage to the high silica matrix fiber caused by repeated loading and unloading of the machine, avoids the quality problems of abrasion of the matrix fiber, oily ears and other appearance unqualified products, adopts a new process, improves the production efficiency by 20 percent, and improves the appearance qualified rate by 3 to 5 percent.
2. Researches show that the reaction agglomeration of the high silica matrix fiber and hydrochloric acid is mainly caused by the fact that alkaline substances precipitated by reaction are not discharged smoothly and are accumulated around the matrix fiber, and the continuous reaction of the fiber and a hydrochloric acid solution is prevented, so that the alkaline substances are accumulated continuously. The invention disperses the high silica matrix fiber to change the fiber from compact sheet shape to loose single bundle shape, thus improving the dispersibility of the fiber, and the disperser has good dispersing effect and little damage to the fiber. The specific parameters of the dispersion machine are shown in tables 1 and 2. Tests show that the retention of strength of the dispersed high silica matrix fiber is not significantly different from that of the undispersed high silica matrix fiber. The tensile strength versus ratio of the high silica matrix fibers is shown in table 3.
TABLE 1 Effect of distance between dispersing teeth and stationary teeth on dispersing Performance
TABLE 2 statistical table of the influence of the rotational speed of the drum on the dispersion properties
TABLE 3 tensile Strength comparison of high silica matrix fibers
3. The flow of the hydrochloric acid solution among the high silica matrix fibers is introduced, so that the solution of the reactant hydrochloric acid is increased, and the concentration of the alkaline product is reduced, so that the high silica matrix fibers can fully react with the hydrochloric acid solution, the continuous accumulation of the alkaline product is avoided, and the technical problem of agglomeration of the high silica matrix fibers and the hydrochloric acid is solved. Meanwhile, the reaction speed of the inner layer and the outer layer of the dispersed high silica matrix fiber in hydrochloric acid can be kept consistent, and the high silica fiber fixed-length yarn obtained through reaction has good silica content consistency. Tests show that the content of the silicon dioxide produced by the pot-type treatment process can reach more than 96 percent. As shown in table 4.
TABLE 4 comparison of silica content values for trough and tank treatments
4. Use acid-resistant jar to wash high silica fiber length fixing yarn, water intaking on the acid-resistant jar, the lower extreme goes out water, the clear water can permeate high silica fiber length fixing yarn fast, take away remaining acidizing fluid and reactant on the yarn, use acid-resistant jar washing, 8 ~ 10 times can circulate every hour, relative motion between yarn and the water has been accelerated, can be quick wash the pH value of yarn to 5 ~ 7, the inlayer pH value uniformity that has both guaranteed the yarn is good, and the water consumption has been practiced thrift again, the water washing efficiency is improved. As shown in table 5.
TABLE 5 pH comparison of trough and tank treatments
Remarking: the pH of the tank treatment and the tank treatment described in the table were sampled inside the yarn.
5. The high silica matrix fiber is put into a completely closed acid-resistant tank for acid leaching, so that the acid gas does not overflow, and the pollution to the environment and the corrosion to production equipment are reduced.
The invention has the advantages of short process flow, high degree of automation, good use performances of strength, temperature resistance and the like of the high silica fiber fixed-length yarn, the efficiency of the whole acid leaching and water washing process is improved by more than 20%, the water washing mode saves more than 50% of water compared with the traditional process, the strength of the high silica fiber fixed-length yarn produced by the new process is improved by more than 10% compared with the yarn produced by the prior process, the qualification rate is improved to more than 95% from the original 74%, and the invention has high popularization and application values.
Drawings
FIG. 1 is a chopped fiber of the present invention;
FIG. 2 is a fiber bundle of the present invention after dispersion;
FIG. 3 is a finished fiber yarn obtained by the present invention;
FIG. 4 is a fiber in a trough process;
FIG. 5 is a view of a finished yarn of fibers from a vat treatment block;
fig. 6 is a flow chart of the present invention.
Detailed Description
The invention relates to a method for producing a high silica fiber fixed length yarn, which is described in detail by 6 specific examples.
The specific process of the pot-type treatment of the high silica fiber fixed-length yarn provided by the invention comprises the following steps:
step 1, preparing high silica matrix fiber:
high silica matrix fibers prepared by chopping. The method comprises the following steps: cutting the high silica matrix fiber with the diameter of 3-12 mu m, the length of 500-1000 mm and the weight of 5-100 kg into the high silica matrix fiber with the length of 20-150 mm by a chopping machine.
Table 6 high silica matrix fiber parameters in each example
Step 2, preparing high silica matrix fiber bundles:
and (3) sending the chopped 5-100 kg of high-silica matrix fiber bundles into a dispersion machine for dispersion through a conveyer belt, wherein the running speed of the conveyer belt is 5-15 m/h, the rotating speed of the dispersion machine is 100-2120 revolutions per minute, and the dispersion amount of the dispersion machine is 20-350 kg/h. Dispersing into single-bundle high silica matrix fibers with the diameter of 1-10 mm by a conventional method. Obtaining the high silica matrix fiber bundle. And (5) standby.
TABLE 7 high silica matrix fiber bundle parameters prepared in the examples
Step 3, removing the impregnating compound on the surface of the fiber
And putting the obtained high silica matrix fiber bundle into an acid-resistant tank with the diameter of 200-1500 mm and the height of 300-1500 mm, injecting hot water by using a circulating pump, and soaking the high silica matrix fiber bundle in the acid-resistant tank in the hot water to remove the impregnating compound on the surface of the fiber, thereby being beneficial to the item division of the matrix fiber in the acid leaching process. The liquid level of the hot water is 10-100 mm higher than the upper surface of the high silica matrix fiber bundle. The hot water temperature is 35-60 ℃, and the flow rate is 5-15 m3The soaking time is 0.5-1.5 h.
TABLE 8 high silica matrix fiber bundle parameters prepared in the examples
Step 4, acid leaching treatment
And injecting a hydrochloric acid solution into the acid-resistant tank in which the high silica matrix fiber bundle subjected to the fiber surface removing sizing agent is placed through a circulating pump, and carrying out acid leaching reactions in different directions on the high silica matrix fiber bundle subjected to the fiber surface removing sizing agent, so that the hydrochloric acid in the acid leaching treatment can fully and uniformly react with the high silica matrix fiber bundle subjected to the fiber surface removing sizing agent. The acid leaching reactions in different directions comprise an acid leaching reaction process in a reverse direction from bottom to top along the acid-resistant tank body and an acid leaching reaction process in a positive direction from top to bottom along the acid-resistant tank body. The concentration of the hydrochloric acid solution is 1.8-3.3 mol/L, and the temperature is 80-95 ℃.
In the reverse-direction acid leaching reaction, injecting a hydrochloric acid solution from the bottom of the acid-proof tank through an acid-proof pump, discharging the hydrochloric acid solution from the top of the acid-proof tank, and performing reverse-direction circulating acid leaching treatment; the flow rate of the hydrochloric acid solution is 5-15 m3The pressure of the acid-proof pump is 0.2-1.0 MP per hour, and the reaction time is 30-150 min.
And after the reverse acid leaching treatment is finished, performing forward acid leaching treatment. In the positive acid leaching treatment, a hydrochloric acid solution is injected from the top of the acid-proof tank through an acid-proof pump, and the hydrochloric acid solution is discharged from the bottom of the acid-proof tank, wherein the flow rate of the hydrochloric acid solution is 5-15 m3The pressure of the acid-proof pump is 0.2-1.0 MP, and the reaction time is 30-150 min. After the positive acid leaching treatment is finished, the first acid leaching treatment of the high silica matrix fiber bundle subjected to fiber surface treating compound removal is finished.
And repeating the forward acid leaching treatment process and the reverse acid leaching treatment process for 4 times to complete the acid leaching treatment of the high silica matrix fiber bundle with the fiber surface treating compound removed and to empty the hydrochloric acid solution. To obtain SiO2High silica matrix fiber bundles with a content of greater than 96%.
TABLE 9 Process parameters for the acid leach treatment in each example
Step 5, water washing treatment
Injecting water with the temperature of 20-35 ℃ into the acid-resistant tank by using an acid-resistant pump to ensure that the SiO in the acid-resistant tank is opposite2The high silica matrix fiber bundle with the content of more than 96% is washed until the pH value of the fiber bundle is 5-7, and then the washing is completed.
TABLE 10 Process parameters for the water washing treatment in each example
Step 6, dehydration treatment
Cleaning the SiO2The high silica fiber matrix bundles with the content of more than 96 percent are put into a cleaning and spin-drying machine for dehydration. The rotating speed of the cleaning and spin-drying machine is 10-150 r/min, and the dehydration time is 1-30 min.
TABLE 11 Process parameters for dehydration treatment in examples
And 7, drying:
dehydrating the SiO2The high silica matrix fiber bundle with the content of more than 96 percent is put into a microwave oven for drying. The drying temperature is 120-160 ℃, and the drying time is 10-120 min. And drying to obtain the high silica fiber fixed length yarn.
TABLE 12 Process parameters for drying treatment in examples
Claims (8)
1. A pot-type treatment method of high silica fiber fixed-length yarns is characterized by comprising the following specific steps:
step 1, preparing high silica matrix fiber:
preparing high silica matrix fibers by a chopping machine;
step 2, preparing high silica matrix fiber bundles:
sending the chopped 5-100 kg of high silica matrix fibers into a dispersion machine for dispersion through a conveyer belt, wherein the running speed of the conveyer belt is 5-15 m/h, the rotating speed of the dispersion machine is 100-2120 revolutions per minute, and the dispersion amount of the dispersion machine is 20-350 kg/h; dispersing into single-bundle high silica matrix fibers with the diameter of 1-10 mm by a conventional method; obtaining high silica matrix fiber bundles; standby;
step 3, removing the fiber surface sizing agent:
putting the obtained high silica matrix fiber bundle into an acid-resistant tank, injecting hot water through a circulating pump, and soaking the high silica matrix fiber bundle in the acid-resistant tank in the hot water to remove the impregnating compound on the surface of the fiber, so that phase splitting of the matrix fiber in the acid leaching process is facilitated; removing the impregnating compound on the surface of the high silica matrix fiber bundle;
step 4, acid leaching treatment:
injecting a hydrochloric acid solution into the acid-resistant tank in which the high silica matrix fiber bundle with the fiber surface treating compound removed is placed through a circulating pump, and performing acid leaching reactions in different directions on the fiber bundle, so that the hydrochloric acid in the acid leaching process can fully and uniformly react with the high silica matrix fiber bundle with the fiber surface treating compound removed; the acid leaching reactions in different directions comprise an acid leaching reaction process in a reverse direction from bottom to top along the acid-resistant tank body and an acid leaching reaction process in a positive direction from top to bottom along the acid-resistant tank body; the concentration of the hydrochloric acid solution is 1.8-3.3 mol/L, and the temperature is 80-95 ℃;
repeatedly circulating the forward direction acid leaching treatment process and the reverse direction acid leaching treatment process for 3-5 times to complete the acid leaching treatment of the high silica matrix fiber bundle with the fiber surface treating compound removed and emptying the hydrochloric acid solution; to obtain SiO2High silica matrix fiber bundles with a content of greater than 96%;
and 5, water washing treatment:
washing the obtained high silica matrix fiber bundle until the pH value of the fiber bundle is 5-7
And 6, dehydration treatment:
putting the cleaned high silica fiber matrix bundle into a cleaning and spin-drying machine for dehydration;
and 7, drying:
putting the dehydrated high silica matrix fiber bundle into a microwave oven for drying; and drying to obtain the high silica fiber fixed length yarn.
2. The pot-type treatment method for the high silica fiber staple yarn according to claim 1, wherein the high silica matrix fiber is prepared by cutting a high silica matrix fiber having a diameter of 3 to 12 μm, a length of 500 to 1000mm, and a weight of 5 to 100kg into a high silica matrix fiber having a length of 20 to 150mm by a chopper.
3. The pot-type treatment method for the high silica fiber staple yarn according to claim 1, wherein the acid-resistant pot has a diameter of 200 to 1500mm and a height of 300 to 1500 mm.
4. The pot-type treatment method for the high silica fiber fixed-length yarn according to claim 1, wherein when the fiber surface sizing agent is removed, the liquid level of the hot water is 10-100 mm higher than the upper surface of the high silica matrix fiber bundle; the hot water temperature is 35-60 ℃, and the flow rate is 5-15 m3The soaking time is 0.5-1.5 h.
5. The pot treatment method for the high silica fiber staple yarn of claim 1, wherein in the reverse acid leaching reaction, the acid leaching treatment is performed by injecting a hydrochloric acid solution from the bottom of the acid-proof pot through an acid-proof pump and discharging the hydrochloric acid solution from the top of the acid-proof pot, and the reverse circulation acid leaching treatment is performed; the flow rate of the hydrochloric acid solution is 5-15 m3The pressure of the acid-proof pump is 0.2-1.0 MP per hour, and the reaction time is 30-150 min;
when the reverse acid is presentAfter the leaching treatment is finished, carrying out forward acid leaching treatment; in the positive acid leaching treatment, a hydrochloric acid solution is injected from the top of the acid-proof tank through an acid-proof pump, and the hydrochloric acid solution is discharged from the bottom of the acid-proof tank, wherein the flow rate of the hydrochloric acid solution is 5-15 m3The pressure of the acid-proof pump is 0.2-1.0 MP, and the reaction time is 30-150 min; after the positive acid leaching treatment is finished, the first acid leaching treatment of the high silica matrix fiber bundle subjected to fiber surface treating compound removal is finished.
6. The pot-type treatment method for the high silica fiber staple yarn according to claim 1, wherein the temperature of the water washing is 20 to 35 ℃.
7. The pot-type treatment method for the high silica fiber staple yarns according to claim 1, wherein the rotation speed of the cleaning and spin-drying machine is 10-150 r/min, and the dehydration time is 1-30 min.
8. The pot-type treatment method for the high silica fiber staple yarn according to claim 1, wherein the drying temperature is 120 to 160 ℃ and the drying time is 10 to 120min during the drying treatment.
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