CN107382372B - A kind of aluminium oxide continuous fiber twisted yarn sizing agent special and preparation method thereof - Google Patents
A kind of aluminium oxide continuous fiber twisted yarn sizing agent special and preparation method thereof Download PDFInfo
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- CN107382372B CN107382372B CN201710637728.9A CN201710637728A CN107382372B CN 107382372 B CN107382372 B CN 107382372B CN 201710637728 A CN201710637728 A CN 201710637728A CN 107382372 B CN107382372 B CN 107382372B
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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 aluminium oxide continuous fiber twisted yarn sizing agent specials and preparation method thereof, the size is consisted of the following compositions according to weight percent: 3~6% aqueous epoxy emulsions, 0.2~0.6% lubricant, 0.1~0.2% antistatic agent, 0.3~0.8% organo silane coupling agent, 0.02~0.05%pH value regulator, surplus are water.Size through the invention is modified processing to fiber surface, is directly coated on fiber surface, drying in aluminium oxide continuous fiber production drawing process.Assign the excellent flexibility of aluminium oxide continuous fiber, convergence, lubricity; and aluminium oxide continuous fiber is solved in doubling twisting technical process; since friction generates electrostatic between fibre bundle; fiber surface does not lubricate; fiber poor in flexibility itself is easy to happen the problems such as bend fracture causes fiber generation filoplume and fiber to be not easy bunchy, and aluminium oxide continuous fiber mechanical property is protected not lose.
Description
Technical field
The present invention relates to a kind of continuous fiber surface modification technologies, and in particular to a kind of aluminium oxide continuous fiber twisted yarn is special
With size and preparation method thereof, belong to inorganic ceramic fiber size field.
Background technique
Aluminium oxide continuous fiber is important high-performance inorganic nonmetallic materials, belongs to one kind of ceramic fibre, with Al2O3
For main component, while also adding Fe2O3、SiO2Deng.The aluminium oxide prepared by sol-gal process combination dry spinning is continuously fine
Dimension have diameter is small, high-intensitive, high temperature resistant, it is corrosion-resistant, can weave, is 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.
Preparing aluminium oxide continuous fiber by sol-gal process at present is that the spinnability colloidal sol that will be prepared is added to barrel
In, so that 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, water quickly volatilizees in thread, and fiber is cured, receive roll dies winding power under the action of elongation attenuate to be formed it is solidifying
Glue fiber, then gelatinous fibre is put into calcining in high temperature furnace and forms aluminium oxide continuous fiber, silk is received by twisting and obtains aluminium oxide
Continuous fiber finished product.And alumina gel fiber is in high-temperature burning process, and since fiber is shunk by thermal decomposition, fiber list
Friction is generated between silk and forms stronger electrostatic interaction, since strong electrostatic interaction influences fiber in subsequent doubling twisting technique
Bunchy, along with fiber surface does not lubricate, alumina fibre flexibility itself it is poor in twisting process by distortion power
Cause fiber that fracture of wire phenomenon occurs, influence the performance of fibre bundle, to influence the finished product production of aluminium oxide continuous fiber.It solves
It is modified that the problem present on just needs to carry out aluminium oxide continuous fiber surface, eliminates electrostatic, assigns fiber certain flexible
Property, surface lubrication, while hundreds of or even thousands of fibers monofilament being integrated a branch of, so that 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 it can improve the performances such as fiber wetness, caking property, hydrophily and to fiber using plasma modification technology
Disinfection 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 can improve fiber surface state (ginseng using oxidation modification technical treatment fiber
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 is carried out to fiber and is modified, is mentioned
The convergence of high microsteping, lubricity, the performances such as abrasion resistance (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 easy to operate, it is suitable for continuous fiber production, good to fiber surface modification effect, controllability is strong.
Aluminium oxide continuous fiber compared with the inorfils such as glass continuous fiber, basalt continuous fiber, due to chemistry at
It is grouped as difference, the technique difference of use causes fibre diameter, intensity and surface state different from property.As glass fibre be with
Glass marble or post-consumer glass are raw material through caused by the techniques systems such as high temperature melting, wire drawing, doff, woven fabric, glass diameter is generally small
In 23 μm, tensile strength is 2300~4300MPa.Basalt fibre is by silica, aluminium oxide, calcium oxide, magnesia, oxygen
Change the basalt building stones of the oxides such as iron and titanium dioxide composition after high-temperature fusion, it is single by made of bushing Defect
Silk diameter is generally less than 9 μm, and intensity is suitable with high intensity S glass fibre, and aluminium oxide continuous fiber is with Al2O3For main component,
Fe is also added simultaneously2O3、SiO2It is prepared by collosol and gel combination dry spinning technology, diameter is less than 10 μm, tensile strength
For 1500~2500MPa.Aluminium 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 component difference leads to different fibers connecing to different size ingredients
Feeler, surface tension, surface can be different different so as to cause wetting property of the different fibers to 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 aluminium oxide continuous fiber is also
To pass through high-temperature burning process, this results in aluminium oxide continuous fiber production process increasingly complex, the protection for fibre bundle
It is required that it is higher, size is required also higher.
Size described in patent document CN106587659A is suitable for the glass fiber infiltration agent of panel grider manufacture；Patent text
Size described in part CN106242320A is suitable for fiberglass weaving size；It is soaked described in patent document CN106277847A
Profit agent, which is sprayed and rubbed suitable for glass fibre high speed, uses size；Size described in patent document CN103936302A is suitable for
Basalt fibre combines non-twist coarse sand；Size described in patent document CN102898044A is suitable for basalt fibre wire-drawing operation
Use size.It can be seen that infiltration agent prescription used in glass fibre described in different patent documents and basalt fibre is all different,
Illustrate that different inorganic continuous fibers, the fiber of different purposes have special infiltration agent prescription matched, can not lead to
With.
Currently, having not been reported about aluminium oxide continuous fiber size, other fiber sizes are used to infiltrate aluminium oxide
Continuous fiber effect is poor, for this purpose, proposing the present invention.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of aluminium oxide continuous fiber twisted yarn sizing agent special and its system
Preparation Method, the size can assign aluminium oxide continuous fiber certain convergence, antistatic property, lubricity, wearability, purpose
Solving electrostatic problem, fibre bundle generation fracture and the fiber that aluminium oxide continuous fiber generates in twisting process, bunchy is not asked
Topic, improves its applicability during post-processing, while reducing aluminium oxide continuous fiber mechanical property in process
Loss.
Size of the invention uses aqueous epoxy emulsion film forming agent, lubricant, the organosilan of constant weight percentage
It is continuous to carry out aluminium oxide by coating device during heat treatment using the size for coupling agent, pH adjusting agent and water composition
Fiber surface is coating modified, and after drying twisting, aluminium oxide continuous fiber finished product can be made.
Technical scheme is as follows:
A kind of aluminium oxide continuous fiber twisted yarn sizing agent special includes following components composition according to weight percent:
It is 3~6% aqueous epoxy emulsions, 0.2~0.6% lubricant, 0.1~0.2% antistatic agent, 0.3~0.8% organic
Silane coupling agent, 0.02~0.05%pH value regulator, surplus is water.
, according to the invention it is preferred to, the 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 type water-base epoxy cream
Liquid, BH-644 type aqueous epoxy emulsion or BH-653 type aqueous epoxy emulsion.
Preferably, molecular weight of epoxy resin contained by the bisphenol A-type aqueous epoxy emulsion is 340~560/mol.This point
Son amount range in aqueous epoxy resins (low, middle-molecular-weihydroxyethyl aqueous epoxy resins) have it is highly polar, lotion drying film forming after
It can assign aluminium oxide continuous fiber precursor excellent convergence.
, according to the invention it is preferred to, the lubricant includes lubricant A and lubricant B, and including or do not include profit
Lubrication prescription C；
The lubricant A is acid amide type cationic lubricant, and the further preferred trade mark is 3760B type lubricant；
The lubricant B is aliphatic and non-ionic composite lubricant, and the further preferred trade mark is 3550 types lubrication
Agent；
The lubricant C is cationic lubricant, and the further preferred trade mark is 3512 type lubricants；
Preferably, the mass ratio of lubricant A, lubricant B and lubricant C are 1:(0.3~1): (0.3~0.8).
Lubricating action can be played, while antistatic work can be played there are two types of cationic lubricant in the lubricant
With principle is that cationic size can reduce coefficient of friction, and aluminium oxide continuous fiber is made to be difficult to generate electrostatic.
, according to the invention it is preferred to, the antistatic agent is inorganic chlorinating lithium.Principle is that inorganic chlorinating lithium has strong shape
At the trend of hydrate, become the salt with the crystallization water, there is stronger moisture absorption, moisture is absorbed on size film
It is dissociated into ion in itself simultaneously, so conductive effect is fine.
, according to the invention it is preferred to, the organo silane coupling agent is gamma-aminopropyl-triethoxy-silane or γ-(first
Base acryloyl-oxy) propyl trimethoxy silicane.The hydroxyl that organo silane coupling agent after hydrolysis contains in triol base silane with
The hydroxyl of fiber surface forms hydrogen bond.In drying course, etherification reaction occurs at high temperature for hydroxyl, sloughs a water and generates ether
Base forms firm covalent bond.
, according to the invention it is preferred to, the pH adjusting agent is glacial acetic acid.
, according to the invention it is preferred to, the aluminium oxide continuous fiber twisted yarn sizing agent special, according to weight percent
It is formed including following components:
It is 3~5% aqueous epoxy emulsions, 0.2~0.6% lubricant, 0.1~0.2% antistatic agent, 0.3~0.6% organic
Silane coupling agent, 0.02~0.05%pH value regulator, surplus is water.
According to the present invention, the preparation method of above-mentioned aluminium oxide continuous fiber twisted yarn size, comprises the following steps that
(1) pH adjusting agent is added in water, the pH value of water is adjusted to 3~4, adds quantitative organosilan coupling
Agent adds pH adjusting agent after continuing stirring to aqueous solution clarification, 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 agent is dissolved with 10~20 times of deionized water, mixing time is 1~2h；
(5) solution in step (2), (3), (4) is uniformly 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 is to get aluminium oxide continuous fiber twisted yarn sizing agent special.
All materials component in preparation method of the invention, including it is aqueous epoxy emulsion, lubricant, antistatic agent, organic
The mass percent adduction of silane coupling agent, pH adjusting agent and water is 100%.
The preparation method of aluminium oxide continuous fiber twisted yarn size of the invention, step is simple, is suitable for industrial metaplasia
It produces, it is easy to spread.
The present invention has the advantages that
1. fiber twisting process can be effectively removed using the coated aluminium oxide continuous fiber of the size in the present invention
Electrostatic between middle fiber filament and silk assigns fiber excellent bunchy and lubricity, while assigning fiber good mechanical property.
2. it is simple using size preparation method of the present invention, it is easy to operate.
3. each ingredient is all water-soluble in heretofore described aluminium oxide continuous fiber twisted yarn sizing agent special, have very
Good caking property and film forming, and can avoid a large amount of uses of volatile organic matter, there is significant environmental protection feature and using valence
Value.
Detailed description of the invention
Fig. 1 is the aluminium oxide continuous fiber photo handled in test example 1 of the present invention without size.
Fig. 2 is to pass through the processed aluminium oxide continuous fiber photo of size in test example 1 of the present invention.
Fig. 3 is the processed aluminium oxide continuous fiber photo of size in test example 2 of the present invention Jing Guo comparative example 1.
Fig. 4 is that the processed aluminium oxide of size in test example 2 of the present invention Jing Guo comparative example 2 or comparative example 3 is continuously fine
Tie up photo.
Fig. 5 is the processed aluminium oxide continuous fiber photo of size in test example 2 of the present invention Jing Guo comparative example 4.
Fig. 6 is that the processed aluminium oxide continuous fiber form of size in test example 2 of the present invention Jing Guo comparative example 5 is shone
Piece.
Fig. 7 is to pass through the processed aluminium oxide continuous fiber form photo of size in test example 1 of the present invention.
Specific 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 regular market purchase product.
Embodiment 1
A kind of aluminium oxide continuous fiber twisted yarn sizing agent special, consists of the following compositions according to weight percent:
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 agent and 0.02%pH value regulator.
In the present embodiment, the 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 type aqueous epoxy emulsion (molecular weight is 340~360/mol), is had purchased from Shanghai love Expo
Machine silicon materials Co., Ltd.
The organo silane coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane, is purchased from Chinese medicines group
Chemical reagent Co., Ltd.
The lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, is purchased from Xi'an friend based composites
Co., Ltd.
The lubricant B is the aliphatic and non-ionic composite lubricant that the trade mark is 3550, multiple purchased from Xi'an friend base
Condensation material Co., Ltd.
The lubricant C is the cationic lubricant that the trade mark is 3512, is purchased from the limited public affairs of Xi'an friend based composites
Department.
The antistatic agent is inorganic chlorinating lithium.
The pH adjusting agent is using glacial acetic acid.
The preparation method of above-mentioned aluminium oxide continuous fiber twisted yarn size is matched according to above-described size,
And including the following steps:
(1) pH adjusting agent is added in water, the pH value of water is adjusted to 3~4, adds quantitative organosilan coupling
Agent adds pH adjusting agent after continuing stirring to aqueous solution clarification, 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 agent is dissolved with 10~20 times of deionized water, mixing time is 1~2h；
(5) solution in step (2), (3), (4) is uniformly 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 is to get aluminium oxide continuous fiber twisted yarn sizing agent special.
Embodiment 2
A kind of aluminium oxide continuous fiber twisted yarn sizing agent special, consists of the following compositions according to weight percent:
3.5% aqueous epoxy resins, 0.4% organo silane coupling agent, 0.3% lubricant A, 0.3% lubricant B, 0.1%
Antistatic agent and 0.02%pH value regulator.
In the present embodiment, the 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 type aqueous epoxy emulsion (molecular weight is 340~360/mol), is had purchased from Shanghai love Expo
Machine silicon materials Co., Ltd.
The organo silane coupling agent is gamma-aminopropyl-triethoxy-silane, limited purchased from Chinese medicines group chemical reagent
Company.
The lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, is purchased from Xi'an friend based composites
Co., Ltd.
The lubricant B is the aliphatic and non-ionic composite lubricant that the trade mark is 3550, multiple purchased from Xi'an friend base
Condensation material Co., Ltd.
The antistatic agent is inorganic chlorinating lithium.
The pH adjusting agent is using glacial acetic acid.
The preparation method of above-mentioned aluminium oxide continuous fiber twisted yarn sizing agent special, matches according to above-described size
Than, and including the following steps:
(1) pH adjusting agent is added in water, the pH value of water is adjusted to 3~4, adds quantitative organosilan coupling
Agent adds pH adjusting agent after continuing stirring to aqueous solution clarification, 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 agent is dissolved with 10~20 times of deionized water, mixing time is 1~2h；
(5) solution in step (2), (3), (4) is uniformly 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 is to get aluminium oxide continuous fiber twisted yarn sizing agent special.
Embodiment 3
A kind of aluminium oxide continuous fiber twisted yarn sizing agent special, consists of the following compositions according to weight percent:
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 agent and 0.02%pH value regulator.
In the present embodiment, the 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 type aqueous epoxy emulsion (molecular weight is 340~360/mol), is had purchased from Shanghai love Expo
Machine silicon materials Co., Ltd.
The organo silane coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane, is purchased from Chinese medicines group
Chemical reagent Co., Ltd.
The lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, is purchased from Xi'an friend based composites
Co., Ltd.
The lubricant B is the aliphatic and non-ionic composite lubricant that the trade mark is 3550, multiple purchased from Xi'an friend base
Condensation material Co., Ltd.
The lubricant C is the cationic lubricant that the trade mark is 3512, is purchased from the limited public affairs of Xi'an friend based composites
Department.
The antistatic agent is inorganic chlorinating lithium.
The pH adjusting agent is using glacial acetic acid.
The preparation method of above-mentioned aluminium oxide continuous fiber twisted yarn sizing agent special, matches according to above-described size
Than, and including the following steps:
(1) pH adjusting agent is added in water, the pH value of water is adjusted to 3~4, adds quantitative organosilan coupling
Agent adds pH adjusting agent after continuing stirring to aqueous solution clarification, 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 agent is dissolved with 10~20 times of deionized water, mixing time is 1~2h；
(5) solution in step (2), (3), (4) is uniformly 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 is to get aluminium oxide continuous fiber twisted yarn sizing agent special.
Embodiment 4
Above-mentioned aluminium oxide continuous fiber twisted yarn sizing agent special, consists of the following compositions according to weight percent:
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 agent and 0.02%pH value regulator.
In the present embodiment, the 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 type aqueous epoxy emulsion (molecular weight is 360~460/mol), is purchased from the wide Tonghua work in Dongguan
Products Co., Ltd.
The organo silane coupling agent is γ-(methacryloxypropyl) propyl trimethoxy silicane, is purchased from Chinese medicines group
Chemical reagent Co., Ltd.
The lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, is purchased from Xi'an friend based composites
Co., Ltd.
The lubricant B is the aliphatic and non-ionic composite lubricant that the trade mark is 3550, multiple purchased from Xi'an friend base
Condensation material Co., Ltd.
The lubricant C is the cationic lubricant that the trade mark is 3512, is purchased from the limited public affairs of Xi'an friend based composites
Department.
The antistatic agent is inorganic chlorinating lithium.
The pH adjusting agent is using glacial acetic acid.
Embodiment 5
A kind of aluminium oxide continuous fiber twisted yarn size, is grouped as according to weight percent by following groups:
4.5% aqueous epoxy resins, 0.4% organo silane coupling agent, 0.3% lubricant A, 0.3% lubricant B, 0.1%
Antistatic agent and 0.02%pH value regulator.
In the present embodiment, the aqueous epoxy resin emulsion is the bisphenol A-type water of 180~230 grams/equivalent of epoxide equivalent
Property epoxy emulsion.BH-653 type aqueous epoxy emulsion (epoxide equivalent is 360~460 grams/equivalent), is purchased from the wide Tonghua work system in Dongguan
Product Co., Ltd.
The organo silane coupling agent is gamma-aminopropyl-triethoxy-silane, limited purchased from Chinese medicines group chemical reagent
Company.
The lubricant A is the acid amide type cationic lubricant that the trade mark is 3760B, is purchased from Xi'an friend based composites
Co., Ltd.
The lubricant B is the cationic lubricant that the trade mark is 3512, is purchased from the limited public affairs of Xi'an friend based composites
Department.
The antistatic agent is inorganic chlorinating lithium.
The pH adjusting agent is using glacial acetic acid.
The preparation method is the same as that of Example 1.
Comparative example 1
As described in Example 1, unlike: 0.6% lubricant A being used only in the lubricant.
Comparative example 2
As described in Example 1, unlike: 0.6% lubricant B being used only in the lubricant.
Comparative example 3
As described in Example 1, unlike: the profit of 0.3% lubricant B and 0.3% being used only in the lubricant
Lubrication prescription C.
Comparative example 4
It is compared using fiberglass weaving is suitable for described in patent document CN106242320A with size.
Comparative example 5
It is compared using the glass fiber infiltration agent for being suitable for panel grider manufacture described in patent document CN106587659A.
Test example 1
Using the coated aluminium oxide continuous fiber form of the size of the embodiment of the present invention 1 as shown in Fig. 2, with uncoated
The fiber precursor form of size is as shown in Figure 1, compare.
As can be seen from Figure 1 without size handle aluminium oxide continuous fiber and silk between due to there are electrostatic without at
Beam adds fiber poor in flexibility itself, and 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 influencing the use of fiber following process；The Fig. 2 that compares can be seen
For several hundred fiber filaments of fiber by size processing at a branch of, surface Glabrous plumage does not allow easy fracture yet out, be conducive to plus
It twists production and following process uses.
Test example 2
The coated aluminium 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 aluminium 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 stiffening using only the processed aluminium oxide continuous fiber of lubricant A in size
Spend bigger than normal, surface is less smooth, and such fiber is poorly suitable for existing twisting production technology, and fiber is easy in twisting process
In fracture or fracture of wire phenomenon occur.
The coated aluminium oxide continuous fiber form of the size of Comparison study example 2 or comparative example 3 is as shown in figure 4, with this
The coated aluminium oxide continuous fiber form of the size 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 handles
The aluminium oxide continuous fiber crossed is excessively soft, and can be seen that collection of filaments effect is not very well, to influence the skill of whole bundle fiber
Art performance, such fiber are poorly suitable for existing twisting production technology, and fiber is easy to slide or occur in twisting process
Fracture of wire phenomenon.
The coated aluminium oxide continuous fiber form of the size of Comparison study example 4 and comparative example 5 is as shown in Figure 5, Figure 6,
The aluminium oxide continuous fiber form coated with the size of the embodiment of the present invention 1 is compared as shown in Fig. 2, Fig. 7.
As can be seen from Figure 5, using described in patent document CN106242320A be suitable for fiberglass weaving size or
Using the glass fiber infiltration agent for being suitable for panel grider manufacture described in patent document CN106587659A, processed aluminium oxide connects
Continuous fiber coated weight is excessive or certain ingredients are not suitable for aluminium oxide continuous fiber, buckles after making fiber coating drying, Er Qieji
Beam is excessive, makes fiber that can not but resile after fibre bundle is flattened drying by coating device, and fibre bundle is adhered to one
Rise can not completely extract out monofilament (such as Fig. 6 is compared with Fig. 7, the whole beam of aluminium 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 influenced, such fiber is not available.
Test example 3
It is tested using the size coating alumina continuous fiber of 1-5 of the embodiment of the present invention and comparative example 1-5, as a result
As shown in table 1.
1. aluminium oxide continuous fiber of table applies size and is not coated with size test result
| Test item | 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 by the size of the present invention aluminium oxide continuous fiber ratio that treated not by leaching
The fiber stiffness of profit agent processing slightly improves and within the scope of the stiffness for being suitble to twisting to require, and whole bundle fiber tension failure is strong
Power improves a lot, and illustrates to play boundling protective effect to aluminium 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 and comparative example combined data are compared, it can be seen that lubricant composition only makes in size
With lubricator A, although whole bundle fiber tension failure strength increases coated rear aluminium oxide continuous fiber, but fiber is stiffening
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 rear whole bundle fiber tension failure strength of aluminium oxide continuous fiber does not significantly improve, and fiber stiffness is too small, profit
Cunning is slight over, is easy to slide when continuous fiber is twisted, is not also suitable for existing twisting process, it is necessary to be that several lubricants are multiple
With using could from stiffness, lubricity, whole bundle fiber tension failure strength etc. reach twisting process requirement well, and
Using described in patent document CN106242320A be suitable for fiberglass weaving size or use patent document
It is suitable for the glass fiber infiltration agent of panel grider manufacture described in CN106587659A, although whole bundle fiber tension failure is strong after coating
Power increases, but coated weight is excessive, will lead to the carbon ion damage that fiber is dissociated after high-temperature process when in use
Seriously, the whole service performance of fiber is influenced, and the collection of filaments is excessive, fibre bundle, which is sticked together, which can not separate monofilament, causes
Aluminium 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 aluminium oxide continuous fiber can not be produced.
Claims (8)
1. a kind of aluminium oxide continuous fiber twisted yarn sizing agent special, which is characterized in that the size is according to weight percent packet
Include following components composition:
3 ~ 6% aqueous epoxy emulsions, 0.2 ~ 0.6% lubricant, 0.1 ~ 0.2% antistatic agent, 0.3 ~ 0.8% organo silane coupling agent,
0.02 ~ 0.05% pH adjusting agent, surplus are water；
The lubricant includes lubricant A and lubricant B, and including or do not include lubricant C；
The lubricant A is acid amide type cationic lubricant；The acid amide type cationic lubricant is Xi'an friend's base
The trade mark of composite material Co., Ltd is 3760B type lubricant；
The lubricant B is aliphatic and non-ionic composite lubricant；The aliphatic and non-ionic composite lubrication
Agent is that the trade mark of Xi'an friend's based composites Co., Ltd is 3550 type lubricants；
The lubricant C is cationic lubricant；The cationic lubricant is that Xi'an friend's based composites are limited
The trade mark of company is 3512 type lubricants.
2. size according to claim 1, which is characterized in that the aqueous epoxy emulsion is the aqueous ring of bisphenol A-type
Oxygen lotion.
3. size according to claim 1, which is characterized in that the 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, which is characterized in that the matter of the lubricant A, lubricant B and lubricant C
Amount is than being 1:(0.3 ~ 1): (0.3 ~ 0.8).
5. size according to claim 1, which is characterized in that the antistatic agent is inorganic chlorinating lithium.
6. size according to claim 1, which is characterized in that the organo silane coupling agent is γ-aminopropyl three
Ethoxysilane or γ-(methacryloxypropyl) propyl trimethoxy silicane, the pH adjusting agent are glacial acetic acid.
7. size according to claim 1, which is characterized in that the dedicated infiltration of aluminium oxide continuous fiber twisted yarn
Agent includes following components composition according to weight percent:
3 ~ 5% aqueous epoxy emulsions, 0.2 ~ 0.6% lubricant, 0.1 ~ 0.2% antistatic agent, 0.3 ~ 0.6% organo silane coupling agent,
0.02 ~ 0.05%pH value regulator, surplus are water.
8. the preparation method of the described in any item aluminium oxide continuous fiber twisted yarn sizes of claim 1-7, including step
It is as follows:
(1) pH adjusting agent is added in water, the pH value of water is adjusted to 3 ~ 4, adds quantitative organo silane coupling agent, after
PH adjusting agent is added after continuous stirring to aqueous solution clarification, 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 agent is dissolved with 10 ~ 20 times of deionized water, mixing time is 1 ~ 2h；
(5) solution in step (2), (3), (4) is uniformly mixed, stirs 0.5 ~ 1h；
(6) mixed solution that step (5) obtain is added in the organo silane coupling agent hydrolyzed in step (1) and the water of surplus
In, 1 ~ 2h of uniform stirring is to get aluminium 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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| 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 |
| CN114438779B (en) * | 2022-03-15 | 2023-02-17 | 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 |
| CN106587659A (en) * | 2016-11-04 | 2017-04-26 | 巨石集团有限公司 | Glass fiber impregnating compound and application thereof |
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2017
- 2017-07-28 CN CN201710637728.9A patent/CN107382372B/en active Active
- 2017-09-29 WO PCT/CN2017/104318 patent/WO2019019366A1/en active Application Filing
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106587659A (en) * | 2016-11-04 | 2017-04-26 | 巨石集团有限公司 | Glass fiber impregnating compound and application thereof |
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| WO2019019366A1 (en) | 2019-01-31 |
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