CN107382372A - A kind of aluminum oxide continuous fiber twisted yarn sizing agent special and preparation method thereof - Google Patents
A kind of aluminum oxide continuous fiber twisted yarn sizing agent special and preparation method thereof Download PDFInfo
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- CN107382372A CN107382372A CN201710637728.9A CN201710637728A CN107382372A CN 107382372 A CN107382372 A CN 107382372A CN 201710637728 A CN201710637728 A CN 201710637728A CN 107382372 A CN107382372 A CN 107382372A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/4584—Coating or impregnating of particulate or fibrous ceramic material
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Abstract
The present invention relates to a kind of aluminum oxide continuous fiber twisted yarn sizing agent special and preparation method thereof, the size consists of the following composition according to percentage by weight：3~6% aqueous epoxy emulsions, 0.2~0.6% lubricant, 0.1~0.2% antistatic additive, 0.3~0.8% organo silane coupling agent, 0.02~0.05%pH value conditioning agents, surplus is water.Processing is modified to fiber surface by the size of the present invention, fiber surface, drying are directly coated in aluminum oxide continuous fiber produces drawing process.Assign the excellent pliability of aluminum oxide continuous fiber, convergence, lubricity; and solves aluminum oxide continuous fiber in doubling twisting technical process; because friction produces electrostatic between fibre bundle; fiber surface does not lubricate; the fracture that easily bends of fiber poor in flexibility itself causes fiber to produce the problems such as filoplume and fiber are not easy bunchy, protects aluminum oxide continuous fiber mechanical property not lose.
Description
Technical field
The present invention relates to a kind of continuous fiber process for modifying surface, and in particular to a kind of aluminum oxide continuous fiber twisted yarn is special
With size and preparation method thereof, belong to inorganic ceramic fiber size field.
Background technology
Aluminum oxide continuous fiber is important high-performance inorganic nonmetallic materials, belongs to one kind of ceramic fibre, with Al2O3
For main component, while also add Fe2O3、SiO2Deng.The aluminum oxide prepared by sol-gal process combination dry spinning is continuously fine
Dimension have diameter is small, high intensity, high temperature resistant, it is corrosion-resistant, can weave, be in light weight, the series of advantages such as any surface finish, height can be done
Warm high efficiency heat insulation material, high-performance composite materials and catalyst carrier etc., apply high temperature industrial furnace, new material, chemical industry and
The fields such as military project, nuclear industry, space flight and aviation.
It is that the spinnability colloidal sol that will be prepared is added to barrel to prepare aluminum oxide continuous fiber by sol-gal process at present
In, spinnability colloidal sol is extruded into spinning shaft from spinneret orifice by the extruding of certain pressure and form thread, in path heat
Under air effect, thread reclaimed water is quickly volatilized, and fiber solidifies, receive roll dies winding power in the presence of elongation attenuate to be formed it is solidifying
Glue fiber, then gelatinous fibre is put into calcining in high temperature furnace and forms aluminum oxide continuous fiber, obtain aluminum oxide by twisting receipts silk
Continuous fiber finished product.And alumina gel fiber is in high-temperature burning process, because fiber is shunk by thermal decomposition, fiber list
Friction is produced between silk and forms stronger electrostatic interaction, because strong electrostatic interaction influences fiber in follow-up doubling twisting technique
Bunchy, along with fiber surface does not lubricate, alumina fibre pliability itself it is poor in twisting process by distortion power
Cause fiber that fracture of wire phenomenon occurs, influence the performance of fibre bundle, so as to influence the production of the finished product of aluminum oxide continuous fiber.Solve
The problem present on just needs to carry out surface modification to aluminum oxide continuous fiber, eliminates electrostatic, assigns fiber certain flexible
Property, surface lubrication, while hundreds of or even thousands of fibers monofilament are integrated a branch of, fiber is smoothly completed doubling twisting work
Skill.
Fiber surface modification technology is substantially segmented into three classes：Plasma modification, oxidation modification technology and coating modified
Technology.Wherein the performances such as fiber wetness, caking property, hydrophily can be improved and to fiber using plasma modification technology
Sterilization cleaning etc. (referring to：Bi Songmei etc., fabrics for industrial use 2013,6,32-35)；Oxidation modification technology is divided into electrochemistry again
Oxidation, vapour phase oxidation process and liquid phase oxidation, using oxidation modification technical finesse fiber, fiber surface state (ginseng can be improved
See：Zhang Meiyun, the 13rd Annual Conference collection of thesis of China Paper Industry Technical Association (under), 2008)；Coating modified technology generally by
Fiber sizing agent special is prepared, using coupling agent in fiber surface grafting polymer film forming agent, surface modification is carried out to fiber, carried
The performances such as the convergence of high microsteping, lubricity, rub (referring to：Jiang Xue, basalt continuous fiber sizing agent special are ground
Study carefully, Harbin Institute of Technology's Master's thesis, 2009).Three of the above method is compared, coating modified technology is easy to use,
It is simple to operate, it is suitable for continuous fiber production, good to fiber surface modification effect, controllability is strong.
Aluminum oxide continuous fiber compared with the inorfils such as glass continuous fiber, basalt continuous fiber, due to chemistry into
Difference is grouped into, the technique difference of use causes fibre diameter, intensity and surface state different from property.As glass fibre be with
Glass marble or discarded glass are raw material to be manufactured into through high temperature melting, wire drawing, doff, the technique such as weave cotton cloth, and glass diameter is typically small
In 23 μm, tensile strength is 2300~4300MPa.Basalt fibre is by silica, aluminum oxide, calcium oxide, magnesia, oxygen
Change the basalt building stones of the oxide such as iron and titanium dioxide composition after high-temperature fusion, formed by bushing Defect, it is single
Silk diameter is generally less than 9 μm, and intensity is suitable with high intensity S glass fibres, and aluminum oxide continuous fiber is with Al2O3For main component,
Also add Fe simultaneously2O3、SiO2It is prepared by collosol and gel combination dry spinning technology, diameter is less than 10 μm, tensile strength
For 1500~2500MPa.Aluminum oxide continuous fiber fibre diameter compared with glass continuous fiber and basalt continuous fiber is different
Cause the specific surface area of different fiber surfaces different；Chemical composition difference causes different fibers connecing to different size compositions
Feeler, surface tension, surface energy difference is so as to causing different fibers different to the wetting property of heterogeneity size；Glass connects
Continuous fiber and basalt continuous fiber are all to make process drawing using melt-spinning to form, the difference is that aluminum oxide continuous fiber is also
To pass through high-temperature burning process, it is increasingly complex that this results in aluminum oxide continuous fiber production process, the protection for fibre bundle
It is required that it is higher, also higher is required to size.
Size described in patent document CN106587659A is applied to the glass fiber infiltration agent of panel grider manufacture；Patent text
Size described in part CN106242320A is applied to fiberglass weaving size；Leaching described in patent document CN106277847A
Profit agent, which is sprayed and kneaded at a high speed suitable for glass fibre, uses size；Size described in patent document CN103936302A is applied to
The non-twist coarse sand of basalt fibre plying；Size described in patent document CN102898044A is applied to basalt fibre wire-drawing operation
Use size.It can be seen that the infiltration agent prescription used in glass fibre and basalt fibre described in different patent documents is all different,
Illustrate different inorganic continuous fibers, the fiber of different purposes has special infiltration agent prescription matched, can not led to
With.
At present, report is had no on aluminum oxide continuous fiber size, other fiber sizes is used to infiltrate aluminum oxide
Continuous fiber effect is poor, therefore, proposing the present invention.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of aluminum oxide continuous fiber twisted yarn sizing agent special and its system
Preparation Method, the size can assign aluminum oxide continuous fiber certain convergence, antistatic behaviour, lubricity, wearability, purpose
Solving aluminum oxide continuous fiber, bunchy is not asked for caused electrostatic problem, fibre bundle generation fracture and fiber in twisting process
Topic, improves its applicability during post-processing, while reduces aluminum oxide continuous fiber mechanical property in process
Loss.
The size of the present invention uses aqueous epoxy emulsion film forming agent, lubricant, the organosilan of constant weight percentage
Coupling agent, pH value regulator and water composition, using the size in heat treatment process by coating device carry out aluminum oxide it is continuous
Fiber surface is coating modified, and after drying is twisted, aluminum oxide continuous fiber finished product can be made.
Technical scheme is as follows：
A kind of aluminum oxide continuous fiber twisted yarn sizing agent special, formed according to percentage by weight including following components：
It is 3~6% aqueous epoxy emulsions, 0.2~0.6% lubricant, 0.1~0.2% antistatic additive, 0.3~0.8% organic
Silane coupler, 0.02~0.05%pH value conditioning agents, surplus is water.
, according to the invention it is preferred to, described aqueous epoxy emulsion is bisphenol A-type aqueous epoxy emulsion, further preferably
For epoxide equivalent 160~280 grams/equivalent bisphenol A-type aqueous epoxy emulsion；More preferably EX-305 types water-base epoxy breast
Liquid, BH-644 types aqueous epoxy emulsion or BH-653 type aqueous epoxy emulsions.
Preferably, molecular weight of epoxy resin contained by described bisphenol A-type aqueous epoxy emulsion is 340~560/mol.This point
Son amount in the range of aqueous epoxy resins (low, middle-molecular-weihydroxyethyl aqueous epoxy resins) have it is highly polar, its emulsion drying film forming after
It can assign aluminum oxide continuous fiber precursor excellent convergence.
, according to the invention it is preferred to, described lubricant includes lubricant A and lubricant B, and including or do not include profit
Lubrication prescription C；
Described lubricant A is acid amide type cationic lubricant, and the further preferred trade mark is 3760B type lubricants；
Described lubricant B is aliphatic and non-ionic composite lubricant, and the further preferred trade mark lubricates for 3550 types
Agent；
Described lubricant C is cationic lubricant, and the further preferred trade mark is 3512 type lubricants；
Preferably, lubricant A, lubricant B and lubricant C mass ratio are 1：(0.3~1)：(0.3~0.8).
There can be two kinds of cationic lubricants in described lubricant, play lubrication, while antistatic work can be played
With principle is that cationic size can reduce coefficient of friction, makes aluminum oxide continuous fiber be difficult to produce electrostatic.
, according to the invention it is preferred to, described antistatic additive is inorganic chlorinating lithium.Principle is that inorganic chlorinating lithium has strong shape
Into the trend of hydrate, turn into the salt with the crystallization water, there is stronger moisture absorption, moisture is absorbed on size film
Ion is dissociated into itself simultaneously, so conductive effect is fine.
, according to the invention it is preferred to, described organo silane coupling agent is gamma-aminopropyl-triethoxy-silane or γ-(first
Base acryloyl-oxy) propyl trimethoxy silicane.Hydroxyl in the triol base silane that organo silane coupling agent after hydrolysis contains with
The hydroxyl of fiber surface forms hydrogen bond.In drying course, etherification reaction occurs at high temperature for hydroxyl, sloughs a water generation ether
Base, form firm covalent bond.
, according to the invention it is preferred to, described pH value regulator is glacial acetic acid.
, according to the invention it is preferred to, described aluminum oxide continuous fiber twisted yarn sizing agent special, according to percentage by weight
Formed including following components：
It is 3~5% aqueous epoxy emulsions, 0.2~0.6% lubricant, 0.1~0.2% antistatic additive, 0.3~0.6% organic
Silane coupler, 0.02~0.05%pH value conditioning agents, surplus is water.
According to the present invention, the preparation method of above-mentioned aluminum oxide continuous fiber twisted yarn size, including step are as follows：
(1) pH value regulator is added in water, the pH value of water is adjusted to 3~4, adds quantitative organosilan coupling
Agent, continue to add pH value regulator after stirring is clarified to the aqueous solution, the pH value of solution is adjusted to 4~5；
(2) quantitative aqueous epoxy emulsion is diluted with 10~15 times of deionized water, mixing time be 0.5~
1h；
(3) quantitative lubricant is diluted with 10~20 times of deionized water, mixing time is 0.5~1h；
(4) quantitative antistatic additive is dissolved with 10~20 times of deionized water, mixing time is 1~2h；
(5) solution in step (2), (3), (4) is well mixed, stirs 0.5~1h；
(6) mixing obtained the organo silane coupling agent hydrolyzed in step (1) and the water of surplus addition step (5) is molten
In liquid, 1~2h of uniform stirring, aluminum oxide continuous fiber twisted yarn sizing agent special is produced.
All materials component in the preparation method of the present invention, including it is aqueous epoxy emulsion, lubricant, antistatic additive, organic
The mass percent of silane coupler, pH value regulator and water adds and is 100%.
The preparation method of the aluminum oxide continuous fiber twisted yarn size of the present invention, step is simple, suitable for industrial metaplasia
Production, it is easy to spread.
The advantage of the invention is that：
1. fiber twisting process can effectively be removed using the coated aluminum oxide continuous fiber of the size in the present invention
Electrostatic between middle filament and silk, the excellent bunchy of fiber and lubricity are assigned, while assign fiber good mechanical property.
2., easily operation simple using size preparation method of the present invention.
3. each composition is all water miscible in heretofore described aluminum oxide continuous fiber twisted yarn sizing agent special, have very
Good caking property and film forming, and a large amount of uses of volatile organic matter can be avoided, there is significant environmental protection feature and using valency
Value.
Brief description of the drawings
Fig. 1 is the aluminum oxide continuous fiber photo handled in test example 1 of the present invention without size.
Fig. 2 is the aluminum oxide continuous fiber photo treated in test example 1 of the present invention by size.
Fig. 3 is the treated aluminum oxide continuous fiber photo of the size in test example 2 of the present invention Jing Guo comparative example 1.
Fig. 4 is continuously fine by the treated aluminum oxide of the size of comparative example 2 or comparative example 3 in test example 2 of the present invention
Tie up photo.
Fig. 5 is the treated aluminum oxide continuous fiber photo of the size in test example 2 of the present invention Jing Guo comparative example 4.
Fig. 6 is that the treated aluminum oxide continuous fiber form of the size in test example 2 of the present invention Jing Guo comparative example 5 is shone
Piece.
Fig. 7 is the aluminum oxide continuous fiber form photo treated in test example 1 of the present invention by size.
Embodiment
Below by specific embodiment, the invention will be further described, but not limited to this.
In embodiment it is raw materials used unless otherwise specified, be conventional commercial products.
Embodiment 1
A kind of aluminum oxide continuous fiber twisted yarn sizing agent special, is consisted of the following composition according to percentage by weight：
3.0% aqueous epoxy resins, 0.4% organo silane coupling agent, 0.3% lubricant A, 0.2% lubricant B, 0.1%
Lubricant C, 0.1% antistatic additive and 0.02%pH value conditioning agents.
In the present embodiment, described aqueous epoxy resin emulsion is the bisphenol A-type water of 160~180 grams/equivalent of epoxide equivalent
Property epoxy emulsion.The trade mark is EX-305 types aqueous epoxy emulsion (molecular weight is 340~360/mol), is had purchased from Shanghai love Expo
Machine silicon materials Co., Ltd.
Described organo silane coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane, purchased from Chinese medicines group
Chemical reagent Co., Ltd.
Described lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, purchased from Xi'an friend's based composites
Co., Ltd.
Described lubricant B is the aliphatic and non-ionic composite lubricant that the trade mark is 3550, is answered purchased from Xi'an friend's base
Condensation material Co., Ltd.
Described lubricant C is the cationic lubricant that the trade mark is 3512, purchased from the limited public affairs of Xi'an friend's based composites
Department.
Described antistatic additive is inorganic chlorinating lithium.
Described pH value regulator is using glacial acetic acid.
The preparation method of above-mentioned aluminum oxide continuous fiber twisted yarn size, size proportioning in accordance with the above,
And including following steps：
(1) pH value regulator is added in water, the pH value of water is adjusted to 3~4, adds quantitative organosilan coupling
Agent, continue to add pH value regulator after stirring is clarified to the aqueous solution, the pH value of solution is adjusted to 4~5；
(2) quantitative aqueous epoxy emulsion is diluted with 10~15 times of deionized water, mixing time be 0.5~
1h；
(3) quantitative lubricant is diluted with 10~20 times of deionized water, mixing time is 0.5~1h；
(4) quantitative antistatic additive is dissolved with 10~20 times of deionized water, mixing time is 1~2h；
(5) solution in step (2), (3), (4) is well mixed, stirs 0.5~1h；
(6) mixing obtained the organo silane coupling agent hydrolyzed in step (1) and the water of surplus addition step (5) is molten
In liquid, 1~2h of uniform stirring, aluminum oxide continuous fiber twisted yarn sizing agent special is produced.
Embodiment 2
A kind of aluminum oxide continuous fiber twisted yarn sizing agent special, is consisted of the following composition according to percentage by weight：
3.5% aqueous epoxy resins, 0.4% organo silane coupling agent, 0.3% lubricant A, 0.3% lubricant B, 0.1%
Antistatic additive and 0.02%pH value conditioning agents.
In the present embodiment, described aqueous epoxy resin emulsion is the bisphenol A-type water of 160~180 grams/equivalent of epoxide equivalent
Property epoxy emulsion.The trade mark is EX-305 types aqueous epoxy emulsion (molecular weight is 340~360/mol), is had purchased from Shanghai love Expo
Machine silicon materials Co., Ltd.
Described organo silane coupling agent is gamma-aminopropyl-triethoxy-silane, limited purchased from Chinese medicines group chemical reagent
Company.
Described lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, purchased from Xi'an friend's based composites
Co., Ltd.
Described lubricant B is the aliphatic and non-ionic composite lubricant that the trade mark is 3550, is answered purchased from Xi'an friend's base
Condensation material Co., Ltd.
Described antistatic additive is inorganic chlorinating lithium.
Described pH value regulator is using glacial acetic acid.
The preparation method of above-mentioned aluminum oxide continuous fiber twisted yarn sizing agent special, size in accordance with the above are matched somebody with somebody
Than, and including following steps：
(1) pH value regulator is added in water, the pH value of water is adjusted to 3~4, adds quantitative organosilan coupling
Agent, continue to add pH value regulator after stirring is clarified to the aqueous solution, the pH value of solution is adjusted to 4~5；
(2) quantitative aqueous epoxy emulsion is diluted with 10~15 times of deionized water, mixing time be 0.5~
1h；
(3) quantitative lubricant is diluted with 10~20 times of deionized water, mixing time is 0.5~1h；
(4) quantitative antistatic additive is dissolved with 10~20 times of deionized water, mixing time is 1~2h；
(5) solution in step (2), (3), (4) is well mixed, stirs 0.5~1h；
(6) mixing obtained the organo silane coupling agent hydrolyzed in step (1) and the water of surplus addition step (5) is molten
In liquid, 1~2h of uniform stirring, aluminum oxide continuous fiber twisted yarn sizing agent special is produced.
Embodiment 3
A kind of aluminum oxide continuous fiber twisted yarn sizing agent special, is consisted of the following composition according to percentage by weight：
4.5% aqueous epoxy resins, 0.4% organo silane coupling agent, 0.3% lubricant A, 0.25% lubricant B,
0.1% lubricant C, 0.1% antistatic additive and 0.02%pH value conditioning agents.
In the present embodiment, described aqueous epoxy resin emulsion is the bisphenol A-type water of 160~180 grams/equivalent of epoxide equivalent
Property epoxy emulsion.The trade mark is EX-305 types aqueous epoxy emulsion (molecular weight is 340~360/mol), is had purchased from Shanghai love Expo
Machine silicon materials Co., Ltd.
Described organo silane coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane, purchased from Chinese medicines group
Chemical reagent Co., Ltd.
Described lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, purchased from Xi'an friend's based composites
Co., Ltd.
Described lubricant B is the aliphatic and non-ionic composite lubricant that the trade mark is 3550, is answered purchased from Xi'an friend's base
Condensation material Co., Ltd.
Described lubricant C is the cationic lubricant that the trade mark is 3512, purchased from the limited public affairs of Xi'an friend's based composites
Department.
Described antistatic additive is inorganic chlorinating lithium.
Described pH value regulator is using glacial acetic acid.
The preparation method of above-mentioned aluminum oxide continuous fiber twisted yarn sizing agent special, size in accordance with the above are matched somebody with somebody
Than, and including following steps：
(1) pH value regulator is added in water, the pH value of water is adjusted to 3~4, adds quantitative organosilan coupling
Agent, continue to add pH value regulator after stirring is clarified to the aqueous solution, the pH value of solution is adjusted to 4~5；
(2) quantitative aqueous epoxy emulsion is diluted with 10~15 times of deionized water, mixing time be 0.5~
1h；
(3) quantitative lubricant is diluted with 10~20 times of deionized water, mixing time is 0.5~1h；
(4) quantitative antistatic additive is dissolved with 10~20 times of deionized water, mixing time is 1~2h；
(5) solution in step (2), (3), (4) is well mixed, stirs 0.5~1h；
(6) mixing obtained the organo silane coupling agent hydrolyzed in step (1) and the water of surplus addition step (5) is molten
In liquid, 1~2h of uniform stirring, aluminum oxide continuous fiber twisted yarn sizing agent special is produced.
Embodiment 4
Above-mentioned aluminum oxide continuous fiber twisted yarn sizing agent special, is consisted of the following composition according to percentage by weight：
4.0% aqueous epoxy resins, 0.4% organo silane coupling agent, 0.3% lubricant A, 0.2% lubricant B, 0.1%
Lubricant C, 0.1% antistatic additive and 0.02%pH value conditioning agents.
In the present embodiment, described aqueous epoxy resin emulsion is the bisphenol A-type water of 180~230 grams/equivalent of epoxide equivalent
Property epoxy emulsion.The trade mark is BH-653 types aqueous epoxy emulsion (molecular weight is 360~460/mol), purchased from the wide Tonghua work in Dongguan
Products Co., Ltd.
Described organo silane coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane, purchased from Chinese medicines group
Chemical reagent Co., Ltd.
Described lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, purchased from Xi'an friend's based composites
Co., Ltd.
Described lubricant B is the aliphatic and non-ionic composite lubricant that the trade mark is 3550, is answered purchased from Xi'an friend's base
Condensation material Co., Ltd.
Described lubricant C is the cationic lubricant that the trade mark is 3512, purchased from the limited public affairs of Xi'an friend's based composites
Department.
Described antistatic additive is inorganic chlorinating lithium.
Described pH value regulator is using glacial acetic acid.
Embodiment 5
A kind of aluminum oxide continuous fiber twisted yarn size, according to percentage by weight by following groups be grouped into：
4.5% aqueous epoxy resins, 0.4% organo silane coupling agent, 0.3% lubricant A, 0.3% lubricant B, 0.1%
Antistatic additive and 0.02%pH value conditioning agents.
In the present embodiment, described aqueous epoxy resin emulsion is the bisphenol A-type water of 180~230 grams/equivalent of epoxide equivalent
Property epoxy emulsion.BH-653 types aqueous epoxy emulsion (epoxide equivalent is 360~460 grams/equivalent), purchased from the wide Tonghua work system in Dongguan
Product Co., Ltd.
Described organo silane coupling agent is gamma-aminopropyl-triethoxy-silane, limited purchased from Chinese medicines group chemical reagent
Company.
Described lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, purchased from Xi'an friend's based composites
Co., Ltd.
Described lubricant B is the cationic lubricant that the trade mark is 3512, purchased from the limited public affairs of Xi'an friend's based composites
Department.
Described antistatic additive is inorganic chlorinating lithium.
Described pH value regulator is using glacial acetic acid.
Preparation method is the same as embodiment 1.
Comparative example 1
As described in Example 1, unlike：0.6% lubricant A is used only in described lubricant.
Comparative example 2
As described in Example 1, unlike：0.6% lubricant B is used only in described lubricant.
Comparative example 3
As described in Example 1, unlike：0.3% lubricant B and 0.3% profit is used only in described lubricant
Lubrication prescription C.
Comparative example 4
Compared using described in patent document CN106242320A suitable for fiberglass weaving with size.
Comparative example 5
Compared using the glass fiber infiltration agent for being applied to panel grider manufacture described in patent document CN106587659A.
Test example 1
Using the coated aluminum oxide continuous fiber form of the size of the embodiment of the present invention 1 as shown in Fig. 2 with it is uncoated
The fiber precursor form of size is as shown in figure 1, compare.
As can be seen from Figure 1 without size handle aluminum oxide continuous fiber and silk between due to exist electrostatic without into
Beam, along with fiber poor in flexibility itself, surface does not lubricate, and fiber is not well protected and causes fibrous fracture and production
Setation plumage, such fiber are can not to carry out twisting production, while influence the use of fiber following process；The Fig. 2 that compares can be seen
Go out hundreds of filaments of fiber handled by size into a branch of, surface Glabrous plumage, also do not allow easy fracture, be advantageous to plus
Twist with the fingers production and following process uses.
Test example 2
The coated aluminum oxide continuous fiber form of the size of Comparison study example 1 is as shown in figure 3, and the embodiment of the present invention
The coated aluminum oxide continuous fiber form of 1 size is as shown in Fig. 2 compare.
From figure 3, it can be seen that lubricant composition is endured with all one's will using only the lubricant A aluminum oxide continuous fibers treated in size
Spend bigger than normal, surface is less smooth, and such fiber is poorly suitable for existing twisting production technology, and fiber is easily in twisting process
In fracture or fracture of wire phenomenon occur.
The coated aluminum oxide continuous fiber form of the size of Comparison study example 2 or comparative example 3 as shown in figure 4, with this
The coated aluminum oxide continuous fiber form of the sizes of inventive embodiments 1 is as shown in Fig. 2 compare.
As can be seen from Figure 4, lubricant B is used only in lubricant composition in size or lubricant B, C are used in mixed way, and is handled
The aluminum oxide continuous fiber crossed is excessively soft, and can be seen that collection of filaments effect is not fine, influences the skill of whole bundle fiber
Art performance, such fiber are poorly suitable for existing twisting production technology, and fiber easily slides or occurred in twisting process
Fracture of wire phenomenon.
The coated aluminum oxide continuous fiber form of the size of Comparison study example 4 and comparative example 5 as shown in Figure 5, Figure 6,
The aluminum oxide continuous fiber form coated with the size of the embodiment of the present invention 1 compares as shown in Fig. 2, Fig. 7.
As can be seen from Figure 5, using described in patent document CN106242320A be applied to fiberglass weaving size or
The glass fiber infiltration agent manufactured using panel grider is applied to described in patent document CN106587659A, treated aluminum oxide connect
Continuous fiber coated weight is excessive or some compositions are not suitable for aluminum oxide continuous fiber, is buckled after making fiber coating drying, Er Qieji
Beam is excessive, fiber can not be but resiled after fibre bundle is flattened drying by coating device, and fibre bundle is adhered into one
Rise can not completely extract out monofilament (such as Fig. 6 compares with Fig. 7, the whole beam of aluminum oxide continuous fiber shown in Fig. 7 can integrate it is a branch of,
Monofilament can be separated, and the whole constriction beam of fiber shown in Fig. 6 is excessive, can not separate monofilament), and fiber stiffness is excessive, a folding is just
It is disconnected, the technical performance of whole bundle fiber is influenceed, such fiber can not use.
Test example 3
Tested using 1-5 of the embodiment of the present invention and comparative example 1-5 size coating alumina continuous fiber, as a result
As shown in table 1.
The aluminum oxide continuous fiber of table 1. applies size and is not coated with size test result
| Test event | Coating rate (%) | Stiffness (cm) | Whole bundle fiber tension failure strength (N/tex) | Twist effect |
| Fiber precursor | 0.00 | 1.7 | 0.371 | |
| Embodiment 1 | 1.18 | 2.0 | 0.386 | It is excellent |
| Embodiment 2 | 1.54 | 2.0 | 0.415 | It is excellent |
| Embodiment 3 | 1.71 | 2.05 | 0.402 | It is excellent |
| Embodiment 4 | 1.85 | 2.1 | 0.426 | It is excellent |
| Embodiment 5 | 1.79 | 2.2 | 0.425 | It is excellent |
| Comparative example 1 | 1.20 | 2.5 | 0.389 | It is good |
| Comparative example 2 | 1.19 | 1.8 | 0.375 | It is good |
| Comparative example 3 | 1.23 | 1.85 | 0.373 | It is good |
| Comparative example 4 | 2.69 | 4.6 | 0.392 | Difference |
| Comparative example 5 | 2.56 | 5.2 | 0.395 | Difference |
From table 1 it follows that the aluminum oxide continuous fiber ratio after size of the present invention processing is not by leaching
The fiber stiffness of profit agent processing slightly improves and in the range of the stiffness for being adapted to twisting to require, whole bundle fiber tension failure is strong
Power improves a lot, and illustrates to play boundling protective effect to aluminum oxide continuous fiber by size processing, from stiffness, lubrication
Property, whole bundle fiber tension failure strength etc. all meets fiber twisting process, and twists excellent.
The embodiment of the present invention is contrasted with comparative example combination data, it can be seen that lubricant composition only makes in size
With lubricator A, although whole bundle fiber tension failure strength increases coated rear oxidation aluminium continuous fiber, but fiber is endured with all one's will
Spend slightly larger, and lubricant effect is bad, is not suitable for existing twisting process, makes using only lubricant B or lubricant B, C mixing
With the coated whole bundle fiber tension failure strength of rear oxidation aluminium continuous fiber does not significantly improve, and fiber stiffness is too small, profit
Cunning is slight over, and continuous fiber easily slides when twisting, and is not also suitable for existing twisting process, it is necessary to be that several lubricants are answered
With using could from stiffness, lubricity, whole bundle fiber tension failure strength etc. reach twisting process requirement well, and
Using being applied to fiberglass weaving size described in patent document CN106242320A or use patent document
It is applied to the glass fiber infiltration agent of panel grider manufacture described in CN106587659A, although whole bundle fiber tension failure is strong after coating
Power is increased, but coated weight is excessive, and fiber can be caused to be damaged when in use after high-temperature process by free carbon ion
Seriously, the overall performance of fiber is influenceed, and the collection of filaments is excessive, fibre bundle, which is sticked together, which can not separate monofilament, causes
Aluminum oxide continuous fiber can not normal use, and coat after fiber stiffness cross the less folding of ambassador's fiber, lubricant effect is bad,
It is not suitable for existing twisting process and qualified aluminum oxide continuous fiber can not be produced.
Claims (10)
1. a kind of aluminum oxide continuous fiber twisted yarn sizing agent special, it is characterised in that the size is according to percentage by weight bag
Include following components composition：
3~6% aqueous epoxy emulsions, 0.2~0.6% lubricant, 0.1~0.2% antistatic additive, 0.3~0.8% organosilan
Coupling agent, 0.02~0.05%pH value conditioning agents, surplus is water.
2. size according to claim 1, it is characterised in that described aqueous epoxy emulsion is the water-based ring of bisphenol A-type
Oxygen emulsion.
3. size according to claim 1, it is characterised in that described bisphenol A-type aqueous epoxy emulsion is worked as epoxy
Measure the bisphenol A-type aqueous epoxy emulsion in 160~280 grams/equivalent.
4. size according to claim 1, it is characterised in that described lubricant includes lubricant A and lubricant B,
And including or do not include lubricant C；
Described lubricant A is acid amide type cationic lubricant；
Described lubricant B is aliphatic and non-ionic composite lubricant；
Described lubricant C is cationic lubricant.
5. size according to claim 4, it is characterised in that described lubricant A, lubricant B and lubricant C matter
Amount is than being 1：(0.3~1)：(0.3~0.8).
6. size according to claim 4, it is characterised in that described acid amide type cationic lubricant is Xi'an friend
The trade mark of based composites Co., Ltd is 3760B type lubricants；
Described aliphatic and non-ionic composite lubricant is that the trade mark of Xi'an friend's based composites Co., Ltd is 3550 types
Lubricant；
Described cationic lubricant is that the trade mark of Xi'an friend's based composites Co., Ltd is 3512 type lubricants.
7. size according to claim 1, it is characterised in that described antistatic additive is inorganic chlorinating lithium.
8. size according to claim 1, it is characterised in that described organo silane coupling agent is γ-aminopropyl three
Ethoxysilane or γ-(methacryloxypropyl) propyl trimethoxy silicane, described pH value regulator are glacial acetic acid.
9. size according to claim 1, it is characterised in that the described special infiltration of aluminum oxide continuous fiber twisted yarn
Agent, formed according to percentage by weight including following components：
3~5% aqueous epoxy emulsions, 0.2~0.6% lubricant, 0.1~0.2% antistatic additive, 0.3~0.6% organosilan
Coupling agent, 0.02~0.05%pH value conditioning agents, surplus is water.
10. the preparation method of the aluminum oxide continuous fiber twisted yarn size described in claim any one of 1-9, including step
It is as follows：
(1) pH value regulator is added in water, the pH value of water is adjusted to 3~4, adds quantitative organo silane coupling agent,
Continue to add pH value regulator after stirring is clarified to the aqueous solution, the pH value of solution is adjusted to 4~5；
(2) quantitative aqueous epoxy emulsion is diluted with 10~15 times of deionized water, mixing time is 0.5~1h；
(3) quantitative lubricant is diluted with 10~20 times of deionized water, mixing time is 0.5~1h；
(4) quantitative antistatic additive is dissolved with 10~20 times of deionized water, mixing time is 1~2h；
(5) solution in step (2), (3), (4) is well mixed, stirs 0.5~1h；
(6) mixed solution for obtaining the organo silane coupling agent hydrolyzed in step (1) and the water of surplus addition step (5)
In, 1~2h of uniform stirring, produce aluminum oxide continuous fiber twisted yarn sizing agent special.
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| CN201710637728.9A CN107382372B (en) | 2017-07-28 | 2017-07-28 | A kind of aluminium oxide continuous fiber twisted yarn sizing agent special and preparation method thereof |
| PCT/CN2017/104318 WO2019019366A1 (en) | 2017-07-28 | 2017-09-29 | Special impregnating agent for alumina continuous fiber twisted yarn and preparation method therefor |
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| CN201710637728.9A CN107382372B (en) | 2017-07-28 | 2017-07-28 | A kind of aluminium oxide continuous fiber twisted yarn sizing agent special and preparation method thereof |
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Cited By (3)
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|---|---|---|---|---|
| CN111807870A (en) * | 2020-07-21 | 2020-10-23 | 山东大学 | Impregnating compound for improving aging resistance of alumina continuous fibers and preparation method and application thereof |
| CN113666627A (en) * | 2021-07-09 | 2021-11-19 | 山东玻纤集团股份有限公司 | Preparation method of low-expansion-coefficient direct twistless roving |
| CN114438779A (en) * | 2022-03-15 | 2022-05-06 | 中南大学 | Oil agent for preparing continuous alumina fiber and preparation and application thereof |
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| CN101633567A (en) * | 2009-08-17 | 2010-01-27 | 巨石集团有限公司 | Glass fiber impregnating agent for transparent plate |
| CN103466963A (en) * | 2013-09-10 | 2013-12-25 | 西安友基复合材料有限公司 | Alkali-resistant chopped glass fiber soakage agent |
| CN105174751A (en) * | 2015-09-02 | 2015-12-23 | 巨石集团有限公司 | Impregnating agent for twisted yarns for epoxy pipeline short cutting |
| CN106380629A (en) * | 2016-08-29 | 2017-02-08 | 山东玻纤集团股份有限公司 | Glass fiber impregnating compound for dough-molding compound and preparation method thereof |
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- 2017-07-28 CN CN201710637728.9A patent/CN107382372B/en active Active
- 2017-09-29 WO PCT/CN2017/104318 patent/WO2019019366A1/en active Application Filing
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| CN101633567A (en) * | 2009-08-17 | 2010-01-27 | 巨石集团有限公司 | Glass fiber impregnating agent for transparent plate |
| CN103466963A (en) * | 2013-09-10 | 2013-12-25 | 西安友基复合材料有限公司 | Alkali-resistant chopped glass fiber soakage agent |
| CN105174751A (en) * | 2015-09-02 | 2015-12-23 | 巨石集团有限公司 | Impregnating agent for twisted yarns for epoxy pipeline short cutting |
| CN106380629A (en) * | 2016-08-29 | 2017-02-08 | 山东玻纤集团股份有限公司 | Glass fiber impregnating compound for dough-molding compound and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111807870A (en) * | 2020-07-21 | 2020-10-23 | 山东大学 | Impregnating compound for improving aging resistance of alumina continuous fibers and preparation method and application thereof |
| CN113666627A (en) * | 2021-07-09 | 2021-11-19 | 山东玻纤集团股份有限公司 | Preparation method of low-expansion-coefficient direct twistless roving |
| CN113666627B (en) * | 2021-07-09 | 2022-11-15 | 山东玻纤集团股份有限公司 | Preparation method of low-expansion-coefficient direct twistless roving |
| CN114438779A (en) * | 2022-03-15 | 2022-05-06 | 中南大学 | Oil agent for preparing continuous alumina fiber and preparation and application thereof |
| CN114438779B (en) * | 2022-03-15 | 2023-02-17 | 中南大学 | Oil agent for preparing continuous alumina fiber and preparation and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107382372B (en) | 2019-08-27 |
| WO2019019366A1 (en) | 2019-01-31 |
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