CN113564761B - 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 PDF

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CN113564761B
CN113564761B CN202110661385.6A CN202110661385A CN113564761B CN 113564761 B CN113564761 B CN 113564761B CN 202110661385 A CN202110661385 A CN 202110661385A CN 113564761 B CN113564761 B CN 113564761B
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high silica
fiber
acid
silica matrix
acid leaching
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CN113564761A (en
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蔡博
王福
吴新全
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Shaanxi Huatek New Materials Co ltd
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    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02Yarns or threads characterised by the material or by the materials from which they are made
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B15/00Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B15/00Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours
    • D06B15/10Removing liquids, gases or vapours from textile materials in association with treatment of the materials by liquids, gases or vapours by use of centrifugal force
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B3/00Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
    • D06B3/02Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fibres, slivers or rovings
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/01Treating 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
    • D06M11/05Treating 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/07Treating 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
    • D06M11/11Treating 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
    • D06M11/13Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2101/00Inorganic fibres
    • D10B2101/02Inorganic fibres based on oxides or oxide ceramics, e.g. silicates

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  • 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 SiO 2 And 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 improves the appearance qualification rate 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

Pot-type treatment method for high silica fiber fixed-length yarn
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 been widely used in the aspects of high-temperature metal liquid melting and filtering, high-temperature gas dust collection, aerospace heat ablation prevention materials and the like due to excellent performance and relative price advantage, 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 researches 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 fixed length yarn and a manufacturing process thereof, a glass fiber raw yarn is adopted to be prepared into a yarn bobbin through twisting and plying processes, winding equipment is used for winding the yarn bobbin into yarn bundles, the yarns are uniformly arranged on a special creel, the yarns are placed in an acid leaching tank in a hanging mode for treatment, then the yarns are soaked in clear water and washed at the temperature of 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 precursor 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, and uniformly distributing the yarn rolls in a hanging manner and placing the yarn rolls in an acid leaching tank for processing. After the acid is discharged, hot water with the temperature of 50-65 ℃ is added into the 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 the acid leaching tank in a spraying mode after the water is discharged, the acid tank is circularly stirred by the acid-proof pump and cleaned for 20-30 minutes, and then the water is discharged.
The invention with the publication number of CN102643036A discloses an intermittent production process of high silica glass fiber chopped yarns, which cuts glass blank yarns to form glass chopped yarns; placing the cut glass chopped yarns in an acid leaching tank for 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 yarns subjected to acid leaching treatment, soaking the glass chopped yarns in clear water, controlling the water temperature to be 45-58 ℃, washing under the flowing of water liquid, and finishing 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 thickness of the yarn roll is thick, the internal acid liquid and the alkaline substances separated out by reaction are difficult to clean, and the water in the tank can be completely replaced once by using the acid tank for washing, so that the problems of long washing time, high water consumption and inconsistent pH value are caused. 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 gob yarns 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 inner layer and the outer layer of each base yarn have different reaction speeds and degrees in hydrochloric acid, 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 requirements, and the content of silicon dioxide in the inner layer is relatively low. 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
The invention provides a pot-type treatment method for high silica fiber fixed-length yarns, which aims to overcome the defects of excessive previous working procedures of the high silica fiber fixed-length yarns, acid leaching agglomeration, difference of the content of silicon dioxide inside and outside, incomplete water washing, poor consistency of high temperature resistance and unorganized discharge caused by acid gas overflow in the prior art.
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 fiber with diameter of 3-12 μm, length of 500-1000 mm and weight of 5-100 kg is cut into high silica matrix fiber with length of 20-150 mm by a chopping machine.
Step 2, preparing high silica matrix fiber bundles:
and (2) 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 fiber 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 m 3 And/h, soaking for 0.5-1.5 h, and removing the impregnating compound on the fiber surface of the high silica matrix fiber bundle.
Step 4, acid leach 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 m 3 The 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. The acid leaching treatment in the positive direction injects a hydrochloric acid solution from the top of the acid-proof tank through an acid-proof pump, and discharges the hydrochloric acid solution from the bottom of the acid-proof tank, wherein the flow rate of the hydrochloric acid solution is 5-15 m 3 The 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 to exhaust the hydrochloric acid solution. To obtain SiO 2 A high silica matrix fiber bundle having 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, and then, oppositely arranging SiO in the acid-resistant tank 2 The high silica matrix fiber bundle with the content of more than 96 percent is washed until the pH value of the fiber bundle is 5-7, and the water washing is completed.
Step 6, dehydration treatment
Cleaning the SiO 2 The 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 SiO 2 The 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 the 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
Figure BDA0003115496080000051
TABLE 2 influence of drum speed on dispersion property
Figure BDA0003115496080000052
TABLE 3 tensile Strength comparison of high silica matrix fibers
Figure BDA0003115496080000053
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
Figure BDA0003115496080000054
Figure BDA0003115496080000061
4. Use acid-resistant jar to wash high silica fibre length fixing yarn, water intaking on the acid-resistant jar, the lower extreme goes out water, the clear water can permeate too high silica fibre length fixing yarn fast, take away remaining acidizing fluid and reactant on the yarn, use acid-resistant jar washing, can circulate 8 ~ 10 times per hour, relative motion between yarn and the water has been accelerated, can be quick wash the PH value of yarn to 5 ~ 7, the ectonexine PH value uniformity that has both guaranteed the yarn is good, the water consumption has been practiced thrift again, the washing efficiency is improved. As shown in table 5.
TABLE 5 PH value comparison of tank and tank treatments
Figure BDA0003115496080000062
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 dispersed fiber bundle of the present invention;
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 is a method for producing a high silica fiber staple 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
Figure BDA0003115496080000071
Step 2, preparing high silica matrix fiber bundles:
and (2) 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 fiber 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
Figure BDA0003115496080000072
Step 3, removing the impregnating compound on the surface of the fiber
And (3) 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 adopting a circulating pump, and soaking the high silica matrix fiber bundle in the acid-resistant tank in the hot water to remove the wetting agent 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 m 3 The soaking time is 0.5 to 1.5 hours.
TABLE 8 high silica matrix fiber bundle parameters prepared in the examples
Figure BDA0003115496080000081
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 acid leaching reaction, the hydrochloric acid solution is injected from the bottom of the acid-proof tank through the acid-proof pump, and the hydrochloric acid solution is discharged from the top of the acid-proof tankCarrying out reverse direction circulating acid leaching treatment; the flow rate of the hydrochloric acid solution is 5-15 m 3 The 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. The acid leaching treatment in the positive direction injects a hydrochloric acid solution from the top of the acid-proof tank through an acid-proof pump, and discharges the hydrochloric acid solution from the bottom of the acid-proof tank, wherein the flow rate of the hydrochloric acid solution is 5-15 m 3 The pressure of the acid-proof pump is 0.2-1.0 MP, and the reaction time is 30-150 min. And after the forward acid leaching treatment is finished, finishing the first acid leaching treatment of the high silica matrix fiber bundle subjected to fiber surface sizing agent removal.
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 sizing removed and drain the hydrochloric acid solution. To obtain SiO 2 High silica matrix fiber bundles with a content of greater than 96%.
TABLE 9 Process parameters for the acid leach treatment in each example
Figure BDA0003115496080000091
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 opposite 2 The high silica matrix fiber bundle with the content of more than 96 percent is washed until the PH value of the fiber bundle is 5 to 7, and the water washing is finished.
TABLE 10 Process parameters for the water washing treatment in each example
Figure BDA0003115496080000092
Step 6, dehydration treatment
Cleaning the SiO 2 The high silica fiber matrix bundles with the content of more than 96 percent are put into a cleaning and spin-drying machine for dehydration. Rotating speed of cleaning and spin-drying machine is 10 ℃150r/min, and the dehydration time is 1-30 min.
TABLE 11 Process parameters for dehydration treatment in examples
Figure BDA0003115496080000101
And 7, drying:
dehydrating the SiO 2 The 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
Figure BDA0003115496080000102

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 fiber 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 fiber with the diameter of 1-10 mm; 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 with the temperature of 35-60 ℃ through a circulating pump, and soaking the high silica matrix fiber bundle in the acid-resistant tank to remove the impregnating compound on the surface of the fiber, thereby being beneficial to phase splitting of the matrix fiber in the acid leaching process; 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 an acid-resistant tank of the high silica matrix fiber bundle provided with the fiber surface treating compound removing agent through a circulating pump, and performing acid leaching reactions in different directions on the fiber bundle, so that hydrochloric acid in the acid leaching treatment can fully and uniformly react with the high silica matrix fiber bundle with the fiber surface treating compound removing 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 ℃;
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 to empty the hydrochloric acid solution; to obtain SiO 2 High silica matrix fiber bundles with a content of greater than 96%;
and 5, water washing treatment:
the obtained high silica matrix fiber bundle is washed until the pH value of the fiber bundle is 5-7, and the water washing step is completed
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 treatment method of the high silica fiber fixed length yarn according to claim 1, wherein the high silica matrix fiber is prepared by cutting the 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 the high silica matrix fiber having a length of 20 to 150mm by a chopper.
3. The pot treatment method of high silica fiber staple yarn of claim 1, wherein the acid-resistant pot has a diameter of 200 to 1500 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 the liquid level of the hot water at 35-60 ℃ is 10-100 mm higher than the upper surface of the high silica matrix fiber bundle when the sizing agent on the fiber surface is removed; the hot water flow is 5-15 m 3 The 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 m 3 The pressure of the acid-proof pump is 0.2-1.0 MP per hour, and the reaction time is 30-150 min;
after the reverse direction acid leaching treatment is finished, carrying out forward direction acid leaching treatment; the acid leaching treatment in the positive direction injects a hydrochloric acid solution from the top of the acid-proof tank through an acid-proof pump, and discharges the hydrochloric acid solution from the bottom of the acid-proof tank, wherein the flow rate of the hydrochloric acid solution is 5-15 m 3 H, the 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 treatment method of the high silica fiber staple yarn according to claim 1, wherein the temperature of the water washing is 20 to 35 ℃.
7. The pot treatment method of the high silica fiber staple yarn of claim 1, wherein the rotation speed of the washing and spin-drying machine is 10 to 150r/min, and the dehydration time is 1 to 30min.
8. The pot-type treatment method of 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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