CN1793822A - Fracture end protective agent used for brittle fiber mechanics measurement, its proparation and use - Google Patents
Fracture end protective agent used for brittle fiber mechanics measurement, its proparation and use Download PDFInfo
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Abstract
A method for preparing protectant of brittle fiber breaking end in mechanical test includes using white oil, water, wetting agent and emulsifier as main composition then carrying out water phase preparation, oil phase preparation and two phase mixed emulsification on water-in-oil latex for obtaining protectant of breaking end.
Description
Technical field:
The present invention is the complete reservation technology of fibre breakage end when being used for the fragile fibre mechanical meaurement, is a kind of fracture end protective agent, preparation and purposes that is used for the fragile fibre mechanical meaurement furtherly.
Background technology:
The mechanical meaurement of flexible fiber comprises stretching, bending, shears, reverses, and it destroys first and is difficult for generation, because the deformation wear energy; Even second rupture failure, what its fracture end can be intact remains, and is convenient to people and understands or be familiar with its fracture mechanism.Therefore, the problem that does not exist the fracture end to keep.And fragile fibre, as carbon fiber, glass fibre, ceramic fiber, mineral fibres, its stretching, bending, shear, reverse then and not only can under small deformation, rupture failure take place, and because impact shock also can cause rupture failure for the second time, especially (Hayes Gary J. in the stretching experiment of routine, Analysis of the singlefilament recoil test, Clemson University, 1993 Ph.D.Dissertation).Therefore, analyze, study the mechanism of fracture of this fibrid, keeping its original broken end becomes vital condition.
In the existing fragile fibre mechanical meaurement, generally only survey mechanical strength, elongation and the modulus value of fiber, these eigenwerts are subjected to fibre morphology, especially the influence of fracture location form.But because the restriction of various measuring conditions and fibre morphology in site measurement, characteristic quantity takes the mode of mean value to express, this measurement can't correctly characterize the discrete essential characteristic of fibrous mechanical property at all, more can't disclose the feature of the weak joint of fiber and produce reason (Yu Weidong. the weak joint of fiber with mechanical characteristics and judgement, Donghua University's journal, 2003,29 (2): 29-33).And the weak joint of fiber is unique, the direct influence factor of fibre property, and promptly the mechanical property of fiber does not depend on the integral body or the average properties of fiber, and depends on its weak joint.Facts have proved, the sign of the weak joint of fiber has only the analysis by the fibre breakage end could obtain (YU Weidong, Ron Postle, YANHaojing, The Weak-Link Morphology and Tensile Behaviour of Wool and High-Modulus Polyethylene Terephthalate Fibres in Situ, Proceedings of The Institute 83rdWorld Conference (83rdTIWC), May 23-27,2004, Shanghai, China, 163～168).So, in practicality is measured, keep the original broken end of fiber, evade the pseudomorphism that its secondary breakdown causes, be the gordian technique in the fragile fibre mechanical meaurement.
The fiber fractograph analysis is meant fiber is intactly remained because of stressed two fracture ends that fracture takes place, and this fracture end is used for microscopy observation, especially scanning electron microscopy (SEM) is observed, by the morphology analysis fibre breakage generation initial configuration and the reaction of this structure under stress of fiber section.Stretching research (the Yao Jiangwei of existing carbon fiber, Yu Weidong. the carbon fiber monofilament is stretched the influence factor of experiment by force, the Materials Science and Engineering journal, 2005,23 (5): 1-4) existing fragile fibre tension failure moment two the fibre breakage ends that prove can take place by the high speed resilience (recoil) of rupture surface to the bite direction because of the abrupt release of elastic potential energy, finally cause the fibre breakage end in replying at a high speed, to be damaged and can't completely keep, thus the situation that causes fragile fibre stretching fractograph analysis to carry out.The guard method of Chan Shenging also has report (S.C.Bennett.D.J.Johnson.Strength-structure relationships in PAN-based carbonfibers.Journal of materials science for this reason, 1983,18:3337-3347; B.J.Jnice; B.B.John; S.Roberte.Analysis of flaws in high-strength carbon fibers from mesophase pitch.Journal of materials science; 1980; 15:2455-2465); but the quantitative values of the retention rate whether can with a hook at the end really effect and protective agent produce lacks the data support, and does not have patent report.
Therefore; all be necessary to research and develop a kind of protective agent of fragile fibre in practicality and the theoretical research; the fracture end that can keep fragile fibre truely and completely is to the fragile fibre fractograph analysis, understands the weak joint structure of fragile fibre and producing and the usability of processing link raising fragile fibre all has extremely profound significance.
Summary of the invention:
The purpose of this invention is to provide the fracture end protective agent that is used for the fragile fibre mechanical meaurement.A kind of water-in-oil latex is proposed as the true at high proportion protective agent that keeps of fracture end in the fragile fibre mechanical meaurement; to reduce fragile fibre fracture end when the mechanical function; the moment fracture suffers to destroy once more because of the high speed resilience, and significantly improves the retention rate that fragile fibre truly ruptures and holds.
Another object of the present invention provides this protectant preparation and purposes.
Of the present invention to be used for the protective agent that the fragile fibre mechanical property measures be a kind of water-in-oil latex, is made up of the water that accounts for combination substance weight 60%～70.2%, the water-in-oil emulsifier that accounts for the oil phase of combination substance weight 28%～39% and account for combination substance weight 0.8%～2%.
Water is made up of 55%～60% the water that accounts for the composition gross weight, 5%～9.5% the wetting agent that accounts for the composition gross weight and micro-waterborne-type preservation and antioxidant are formed.Wherein, water is distilled water or pure water; Wetting agent can be selected from following material: a kind or their 2～3 kinds of potpourris in glycerine, sorbierite, polyglycol, propylene glycol, corn syrup, monosodium glutamate, natural honey, sodium lactate and the derivant thereof; Antiseptic accounts for 0.01%～0.3% of water-in-oil latex substance weight, can be selected from following material: methyl dibromo glutaronitrile, Phenoxyethanol, imidazolidinyl urea, the interior uride of dihydroxymethyl dimethyl, parachlorometaxylenol, two imidazolidinyl ureas, two imidazolidinyl ureas, iodine propinyl butyl carbamate, the two urides of acetaldehyde, sodium hydroxy methyl glycinate, 1,3-dihydroxymethyl-5, the 5-dimethyl hydantion, 2-methyl-4-isothiazoline-3-ketone, 5-chloro-2-2 methyl-4-isothiazoline-3-ketone, the interior uride of dimethyl dihydroxy first, 2,4,4-three chloro-2-dihydroxy diphenyl ethers, methyl p-hydroxybenzoate, 1 kind or their 2～3 kinds of potpourris in propylparaben and the hexamethylene tetramine derivant; Antioxidant accounts for 0.01%～0.4% of water-in-oil latex substance weight, can be selected from following material: a kind or their 2～3 kinds of potpourris in tocopherol, tertiary butyl hydroxyl fennel seeds brain, tertiary butyl hydroxy-methylbenzene, the gallic acid third lipoprotein.
Oil phase is made up of White Mineral Oil that accounts for composition gross weight 20%～25% and 8%～14% the vegetable oil that accounts for the composition gross weight.Wherein, White Mineral Oil is the White Mineral Oil of general commercially available 7#～60#; Vegetable oil can be selected from following material: a kind or their 2～3 kinds of potpourris in soybean oil, peanut oil, rapeseed oil, sunflower oil, camellia seed oil, rice bran oil, cottonseed oil, corn oil, apricot kernel oil, the wheat germ oil.
Water-in-oil emulsifier can be selected from following material: polyglycol-2 sesquistearate, C
16-18Alkyl glucoside, C
16-18Pure tristerin, methyl glucoside, polyglycol-20 ether sesquistearate, C
16-18Alcohol/polyglycol-20, C
16-18Alcohol ether, lauryl glucoside polyglycereol-2 dimerization hydroxy stearic acid ester/glycerine, cetearyl ether-20, cetearyl alcohol alcohol ether-21, fatty alcohol ether-6, stearyl alcohol, polyglyceryl-2 dimerization hydroxy stearic acid ester, polyglyceryl-3 diisopstearate, polyoxyethylene ether phosphotriester in a kind or their 2～3 kinds of potpourris.
Main preparation methods of the present invention can be divided into for 3 steps: the preparation of water; The preparation of oil phase; Water mixes with oil phase.
The compound method of water is to get an amount of distilled water or pure water, under the state of high-speed stirred, in liquid, add wetting agent, add the waterborne-type preservation and the antioxidant of trace then, continue to stir and heating, make mixed solution limpid evenly, and reach 70 ℃ of water temperatures.The component of described water, wetting agent and weight ratio are as previously mentioned.
The compound method of oil phase is to get an amount of White Mineral Oil and an amount of vegetable oil, stirs, and add the water-in-oil emulsifier of described amount under the state that stirs in fluid, continues to stir and oil phase is heated 70 ℃.The component of described White Mineral Oil, vegetable oil and emulsifying agent and weight ratio are as previously mentioned.
The high-speed stirred oil phase also slowly adds oil phase with water, notes vented exhaust, continues to stir after 30 minutes the latex that obtains was got final product with the homogenizer homogeneous in 15～30 minutes.The weight ratio of described water and oil phase as previously mentioned.
Protective agent of the present invention is not only easy to prepare, with low cost, but also has three tangible advantages: one, can improve greatly and break fibre breakage end retention rate.This mixed water-in-oil latex is coated in the fragile fibre surface equably, the vibration damping protective seam in the time of can forming the fragile fibre mechanical meaurement.Stretching experiment with carbon fiber is an example, use this protective agent after, tension failure end retention rate is by significantly rising to more than 60% below 10%.
Its two, the present invention can keep the fracture end in the fragile fibre mechanical failure truely and completely not influencing under the prerequisite of fibrous mechanical property test.Protective agent is relevant with protective agent viscosity to the influence of fragile fibre Mechanics Performance Testing.Stretching experiment with carbon fiber is an example, and the viscosity of water-in-oil latex is about 100 ± 10 pools, in the actual measurement, closes with protective agent and not to add protectant result and contrast discovery, and generally the former is a little more than the latter, but recruitment is less than 5 * 10
-2CN (li ox), the average 13cN of tensile strength value (li ox) of this relative carbon fiber itself only is the error of ppt, can ignore fully.
Its three, the present invention is applicable to carbon fiber, glass fibre, the mechanical meaurement of fragile fibres such as ceramic fiber and other mineral fibres.Need not the mechanical meaurement experimental apparatus is reequiped, have easy to operate, do not pollute fragile fibre fracture end, do not influence experimental result, advantage such as effect is obvious.
Embodiment:
To help to understand the present invention by embodiment, but not limit content of the present invention.
The present invention is heated to 70 ℃ after the waterborne-type preservation of an amount of water, an amount of wetting agent and trace and antioxidant are stirred, again an amount of White Mineral Oil and an amount of vegetable oil are stirred, under the state that stirs, in liquid, add an amount of water-in-oil emulsifier, oil phase is heated to 70 ℃.The high-speed stirred oil phase also slowly adds oil phase with water, continues to stir 30 minutes, and homogeneous can use in 15～30 minutes again.Concrete component is seen embodiment.Using method of the present invention is the outside surface that protective agent is spread upon equably tested fragile fibre, and the clamping fragile fibre carries out mechanical meaurement then.After measure finishing, fiber head end and the protective agent that is attached on the fiber head end surfaces be placed in alcohol or the ether clean, be cleaned, obtain clean fragile fibre fracture end until protective agent.
Embodiment 1:
Composition Weight% (percentage by weight)
White Mineral Oil 23.5%
Soybean oil 14%
Glycerine 5%
Water 55%
Polyglyceryl-2 dimerization hydroxy stearic acid ester 2%
Methyl p-hydroxybenzoate 0.2%
Tocopherol 0.3%
For detecting the influence of protective agent, carry out one group of contrast experiment to fiber section retention rate.Experimental result proves, because fiber is broken the resilience rapidly of moment, unshielded fragile fibre almost can't keep the true stretching section of fiber when stretching, but after applying protective agent, the reservation situation of tensile fiber section be improved significantly.The detection method of following examples is identical.
Table 1 carbon fiber is broken the efficiency analysis of residual segment of fiber
| Experiment condition | Number of fiber | Section keeps radical | Section retention rate/% | Average brute force/cN |
| Unprotect agent protective agent | 321 40 | 30 29 | 9.4 72.5 | 12.96 13.00 |
Embodiment 2:
Composition Weight% (percentage by weight)
White Mineral Oil 20%
Peanut oil 9.3%
Sorbierite (70% solution) 9.5%
Water 60%
Polyglycol-2 sesquistearate 1%
Propylparaben 0.1%
Tertiary butyl hydroxy-methylbenzene 0.1%
Table 2 carbon fiber is broken the efficiency analysis of residual segment of fiber
| Experiment condition | Number of fiber | Section keeps radical | Section retention rate/% | Average brute force/cN |
| Unprotect agent protective agent | 321 67 | 30 43 | 9.4 64.2 | 12.96 12.99 |
Embodiment 3:
Composition Weight% (percentage by weight)
White Mineral Oil 25%
Wheat germ oil 14%
Glycerine 5%
Water 55%
Polyoxyethylene ether phosphotriester 0.8%
Phenoxyethanol 0.1%
Tocopherol 0.1%
Table 3 pottery is broken the efficiency analysis of residual segment of fiber
| Experiment condition | Number of fiber | Section keeps radical | Section retention rate/% | Average brute force/cN |
| Unprotect agent protective agent | 230 76 | 21 61 | 9.1 80.3 | 38.52 38.56 |
Embodiment 4:
Composition Weight% (percentage by weight)
White Mineral Oil 20%
Apricot kernel oil 8.5%
Polyglycol 9.5%
Water 65%
Polyglyceryl-3 isostearate 1.8%
The interior uride 0.1% of dihydroxymethyl dimethyl
Gallic acid third lipoprotein 0.1%
Table 4 glass is broken the efficiency analysis of residual segment of fiber
| Experiment condition | Number of fiber | Section keeps radical | Section retention rate/% | Average brute force/cN |
| Unprotect agent protective agent | 205 64 | 15 44 | 7.3 68.8 | 62.47 62.51 |
Embodiment 5:
Composition Weight% (percentage by weight)
White Mineral Oil 20%
Corn oil 8%
Apricot kernel oil 4%
Glycerine 5%
Sorbierite (70% solution) 3%
Water 58%
Polyglyceryl-2 gathers hydroxy stearic acid ester 1.5%
Propylparaben 0.3%
Tertiary butyl hydroxy-methylbenzene 0.2%
Table 5 carbon fiber is broken the efficiency analysis of residual segment of fiber
| Experiment condition | Number of fiber | Section keeps radical | Section retention rate/% | Average brute force/cN |
| Unprotect agent protective agent | 321 55 | 30 41 | 9.4 75 | 12.96 12.99 |
Embodiment 6:
Composition Weight% (percentage by weight)
White Mineral Oil 20%
Soybean oil 4.6%
Corn oil 3%
Wheat germ oil 2%
Natural sweet 5%
Glycerine 6%
Water 57%
Polyoxyethylene ether phosphotriester 2%
The interior uride 0.2% of dihydroxymethyl dimethyl
Gallic acid third lipoprotein 0.2%
Table 6 glass is broken the efficiency analysis of residual segment of fiber
| Experiment condition | Number of fiber | Section keeps radical | Section retention rate/% | Average brute force/cN |
| Unprotect agent protective agent | 205 77 | 15 54 | 7.3 72 | 62.47 62.50 |
Embodiment 7:
Composition Weight% (percentage by weight)
White Mineral Oil 23%
Soybean oil 13%
Glycerine 5.5%
Water 56%
Polyglyceryl-2 dimerization hydroxy stearic acid ester 2%
Methyl p-hydroxybenzoate 0.1%
Propylparaben 0.1%
Phenoxyethanol 0.1%
Tocopherol 0.2%
Table 7 pottery is broken the efficiency analysis of residual segment of fiber
| Experiment condition | Number of fiber | Section keeps radical | Section retention rate/% | Average brute force/cN |
| Unprotect agent protective agent | 230 72 | 21 52 | 9.1 72.2 | 38.52 38.57 |
Embodiment 8:
Composition Weight% (percentage by weight)
White Mineral Oil 20%
Peanut oil 14%
Glycerine 7.5%
Water 56%
Polyglyceryl-2 dimerization hydroxy stearic acid ester 2%
Phenoxyethanol 0.2%
The interior uride 0.1% of dihydroxymethyl dimethyl
Tertiary butyl hydroxy-methylbenzene 0.1%
Gallic acid third lipoprotein 0.1%
Table 8 carbon fiber is broken the efficiency analysis of residual segment of fiber
。
| Experiment condition | Number of fiber | Section keeps radical | Section retention rate/% | Average brute force/cN |
| Unprotect agent protective agent | 321 80 | 30 54 | 9.4 67.5 | 12.96 13.00 |
Claims (10)
1, a kind of fragile fibre mechanical property fracture end protective agent that is used for is characterized in that the water-in-oil latex be made up of water and oil phase, and water accounts for 60%～70.2% of protective agent weight; Oil phase accounts for 28%～39% of protective agent weight; Water-in-oil emulsifier accounts for 0.8%～2% of protective agent weight; Described water is made up of the antiseptic and the antioxidant of the water that accounts for protective agent gross weight 55%～60%, the wetting agent that accounts for protective agent gross weight 5%～9.5% and trace (0.02%～0.7%); Described oil phase is made up of White Mineral Oil that accounts for protective agent gross weight 20%～25% and the vegetable oil that accounts for protective agent gross weight 8%～14%.
2,, it is characterized in that described emulsifying agent can be selected from following material: polyglycol-2 sesquistearate, C according to the described protective agent of claim 1
16-18Alkyl glucoside, C
16-18Pure tristerin, methyl glucoside, polyglycol-20 ether sesquistearate, C
16-18Alcohol/polyglycol-20, C
16-18Alcohol ether, lauryl glucoside polyglycereol-2 dimerization hydroxy stearic acid ester/glycerine, cetearyl ether-20, cetearyl alcohol alcohol ether-21, fatty alcohol ether-6 and stearyl alcohol, polyglyceryl-2 dimerization hydroxy stearic acid ester, polyglyceryl-3 diisopstearate, a kind or 2～3 kinds potpourri in the polyoxyethylene ether phosphotriester.
3,, it is characterized in that the White Mineral Oil of described White Mineral Oil for general commercially available 7#～60# according to the described protective agent of claim 1.
4, according to the described protective agent of claim 1, it is characterized in that described wetting agent can be selected from following material: a kind or 2～3 kinds of potpourris in glycerine, sorbierite, polyglycol, propylene glycol, corn syrup, monosodium glutamate, natural honey, sodium lactate and the derivant thereof.
5, according to the described protective agent of claim 1, it is characterized in that described vegetable oil can be selected from following material: a kind or their 2～3 kinds of potpourris in soybean oil, peanut oil, rapeseed oil, sunflower oil, camellia seed oil, rice bran oil, cottonseed oil, corn oil, apricot kernel oil, the wheat germ oil.
6; according to the described protective agent of claim 1; it is characterized in that described aqueous phase; antiseptic is 0.01%～0.3% of a protective agent weight; can be selected from following material: methyl dibromo glutaronitrile; Phenoxyethanol; imidazolidinyl urea; dihydroxymethyl dimethyl hydantoin; parachlorometaxylenol; two imidazolidinyl ureas; two imidazolidinyl ureas; iodine propinyl butyl carbamate; the two urides of acetaldehyde; sodium hydroxy methyl glycinate; 1; 3-dihydroxymethyl-5; the 5-dimethyl hydantion; 2-methyl-4-isothiazoline-3-ketone; 5-chloro-2-2 methyl-4-isothiazoline-3-ketone; dimethyl dihydroxy first hydantoin; 2; 4,4-three chloro-2-dihydroxy diphenyl ethers; methyl p-hydroxybenzoate; 1 kind or their 2～3 kinds of potpourris in propylparaben and the hexamethylene tetramine derivant.
7, according to the described protective agent of claim 1; it is characterized in that described aqueous phase; antioxidant is 0.01%～0.4% of a protective agent weight, can be selected from following material: a kind or their 2～3 kinds of potpourris in tocopherol, tertiary butyl hydroxyl fennel seeds brain, tertiary butyl hydroxy-methylbenzene, the gallic acid third lipoprotein.
8, according to the described protective agent of claim 1, it is characterized in that described aqueous phase, described water is distilled water or pure water.
9, according to the described protectant preparation method of claim 1, it is characterized in that under agitation wetting agent joins distilled water or pure water, the waterborne-type preservation and the antioxidant that add trace then, continue to stir and heating, make mixed solution limpid evenly, and reach 70 ℃ of water temperatures, be mixed with the water of water-in-oil latex; Get White Mineral Oil and an amount of vegetable oil, and under the state that stirs, add emulsifying agent again, continue to stir and oil phase is heated to 70 ℃, be mixed with oil phase; Under the effect of high-speed stirred and water-in-oil emulsifier, water and oil phase two-phase are mixed into water-in-oil latex; Above-mentioned compound and weight ratio thereof are according to claim 1; Wherein emulsifying agent, White Mineral Oil, wetting agent, vegetable oil, antiseptic and antioxidant are successively as described in the claim 2,3,4,5,6 and 7.
10, according to the described protectant purposes of claim 1, it is characterized in that being used for the protective seam of fragile fibre, described fragile fibre is selected from carbon fiber, glass fibre, ceramic fiber or other mineral fibres.
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| CN100580415C CN100580415C (en) | 2010-01-13 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636414A (en) * | 2012-05-02 | 2012-08-15 | 北京北矿亿博科技有限责任公司 | Method for evaluating emulsifying capacity of emulsifier for emulsion explosive |
| CN104122202A (en) * | 2014-07-29 | 2014-10-29 | 厦门大学 | Method for testing interfacial bonding strength of ceramic fiber-reinforced resin matrix composite material |
| US9034833B1 (en) | 2013-12-20 | 2015-05-19 | L'oreal | Anti-aging composition containing high levels of a jasmonic acid derivative |
| CN104625481A (en) * | 2014-12-31 | 2015-05-20 | 芜湖协诚金属制品有限公司 | Protective agent for welding spot in metal welding |
| US9237998B2 (en) | 2013-12-20 | 2016-01-19 | L'oreal | Carrier system for water-soluble active ingredients |
| US9539198B2 (en) | 2013-12-20 | 2017-01-10 | L'oreal | Photoprotection composition containing high levels of water-soluble UV filters |
| US9545373B2 (en) | 2013-12-20 | 2017-01-17 | L'oreal | Translucent cosmetic composition in the form of a water-in-oil emulsion |
| US9943477B2 (en) | 2013-12-20 | 2018-04-17 | L'oreal | Emulsion compositions containing a novel preservative system |
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2005
- 2005-12-02 CN CN200510111088A patent/CN100580415C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102636414A (en) * | 2012-05-02 | 2012-08-15 | 北京北矿亿博科技有限责任公司 | Method for evaluating emulsifying capacity of emulsifier for emulsion explosive |
| US9034833B1 (en) | 2013-12-20 | 2015-05-19 | L'oreal | Anti-aging composition containing high levels of a jasmonic acid derivative |
| US9237998B2 (en) | 2013-12-20 | 2016-01-19 | L'oreal | Carrier system for water-soluble active ingredients |
| US9539198B2 (en) | 2013-12-20 | 2017-01-10 | L'oreal | Photoprotection composition containing high levels of water-soluble UV filters |
| US9545373B2 (en) | 2013-12-20 | 2017-01-17 | L'oreal | Translucent cosmetic composition in the form of a water-in-oil emulsion |
| US9943477B2 (en) | 2013-12-20 | 2018-04-17 | L'oreal | Emulsion compositions containing a novel preservative system |
| CN104122202A (en) * | 2014-07-29 | 2014-10-29 | 厦门大学 | Method for testing interfacial bonding strength of ceramic fiber-reinforced resin matrix composite material |
| CN104625481A (en) * | 2014-12-31 | 2015-05-20 | 芜湖协诚金属制品有限公司 | Protective agent for welding spot in metal welding |
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| CN100580415C (en) | 2010-01-13 |
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