CN101736593B - Preparation method of water-base epoxy resin sizing agent for carbon fiber - Google Patents
Preparation method of water-base epoxy resin sizing agent for carbon fiber Download PDFInfo
- Publication number
- CN101736593B CN101736593B CN2010103001313A CN201010300131A CN101736593B CN 101736593 B CN101736593 B CN 101736593B CN 2010103001313 A CN2010103001313 A CN 2010103001313A CN 201010300131 A CN201010300131 A CN 201010300131A CN 101736593 B CN101736593 B CN 101736593B
- Authority
- CN
- China
- Prior art keywords
- water
- epoxy resin
- carbon fiber
- hit
- base epoxy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method of water-base epoxy resin sizing agent for carbon fiber, relating to a sizing agent preparation. The invention solves the problems that the cost of existing foreign latex sizing agent and that the performance of domestically researched emulsion sizing agent is not good. The method comprises: 1. preparing water-base epoxy resin; 2. preparing water-base epoxy resin curing agent; 3. diluting water-base epoxy resin with de-ionized water, and dispersing to obtain water-base epoxy resin emulsion; 4. mixing the water-base epoxy resin emulsion with the water-base epoxy resin curing agent to obtain a water-base epoxy resin emulsion system; and 5. mixing the water-base epoxy resin emulsion system with aid to obtain water-base epoxy resin sizing agent for carbon fiber. The water-base epoxy resin sizing agent for carbon fiber in the invention has good performance, good strengthening function to carbon fiber, better clustering property, smoothness and flexibility, and low cost, and the performance indexes such as overall loose degree of filaments of the fiber, fiber opening property and cross-linking degree among signal fibers.
Description
Technical field
The present invention relates to a kind of preparation method of sizing agent.
Background technology
Carbon fiber is a fragile material, in production and process, be easy to generate phenomenons such as lousiness and single wire fracture through mechanical friction, the intensity of carbon fiber is reduced, and because the existence of lousiness, make the matrix resin can not abundant wetting carbon fiber, make it in the composite of preparation, to be easy to generate hole, thereby influence the mechanical property of composite, and lousiness can exert an influence also to working environment.Therefore; must carry out starching to carbon fiber; the effect of starching is to form diaphragm at carbon fiber surface; in follow-up process, not only can protect carbon fiber surface like this; reduce lousiness and single wire fracture phenomenon, make the easy and boundling of carbon fiber, but also can play a transition zone; improve the compatibility of carbon fiber and matrix resin, thereby improved the interface bonding of composite.
At present, carbon fiber sizing agent can be divided into two kinds, a kind of is solution-type, be dissolved in the acetone and other organic solvent organic resin such as polyvinyl alcohol, vinyl acetate polymer, polymerizing acrylic acid thing, polyurethane, epoxy resin etc. formulated, but the solution-type sizing agent needs a large amount of inflammable organic solvents, can bring the problem of aspects such as economy, safety, health.Another kind is an emulsion-type, based on a kind of resin, be equipped with quantitative emulsifying agent and also contain little amount of crosslinking agent sometimes, decide on resin properties, and the emulsion made of the auxiliary agent that improves interfacial adhesion, it generally is difficult for residual resin down on deflector roll, solvent-free again contaminated environment, and owing to contain the wetted property that surfactant has improved fiber surface in the emulsion, simultaneously again can be by auxiliary agent, coupling agent, reach the purpose of raising, thereby external extensively employing emulsion-type sizing agent, but the cost height of emulsion-type sizing agent limits it and promotes suitable; At present, the emulsion-type sizing agent performance of domestic research is not very desirable, can not guarantee simultaneously that carbon fiber has convergence, smoothness, flexibility, pliability etc. preferably, and can not satisfy the whole loosening degree of strand between fiber simultaneously, open the performance indications such as crosslinking degree between fibre, single fiber, can not satisfy the demand of present production and the needs in market.
Summary of the invention
The present invention is in order to solve existing external emulsion-type sizing agent cost height; The emulsion-type sizing agent performance of domestic research is bad, to the problem of the humidification difference of carbon fiber, and provides a kind of preparation method of water-base epoxy resin sizing agent for carbon fiber.
The preparation method of water-base epoxy resin sizing agent for carbon fiber realizes according to the following steps: one, press mass ratio and add epoxy resin and water-base epoxy emulsifying agent at 80: 20 in 70 ℃ water-bath, place high-shearing dispersion emulsifying machine then, rotating speed with 1500～16000r/min stirs, and drip deionized water to mixed system generation phase transfer, dripping deionized water to the solid content of mixed system behind 20～90min again is 40%～50%, continue to stir 30min, get aqueous epoxy resins HIT-WE; Two, in 70 ℃ water-bath, press mass ratio and add epoxy curing agent and water-base epoxy emulsifying agent at 80: 20, place high-shearing dispersion emulsifying machine then, rotating speed with 1500～8000r/min stirs and drips deionized water, dripping deionized water to the solid content of mixed system behind 3～5h again is 40%～50%, water-soluble epoxy resin curing agent HIT-GY; Three, with deionized water aqueous epoxy resins HIT-WE being diluted to solid content is 0.5%～5%, and being dispersed to particle diameter then is 100～500nm, gets aqueous epoxy resin emulsion HIT-Y; Four, press mass ratio and 100: 0.01～0.25 aqueous epoxy resin emulsion HIT-Y mixed with water-soluble epoxy resin curing agent HIT-GY, aqueous epoxy resin emulsion system HIT-S; Five, by mass percentage the auxiliary agent of 90%～98% aqueous epoxy resin emulsion system HIT-S and 2%～10% is mixed, promptly get water-base epoxy resin sizing agent for carbon fiber; Wherein epoxy curing agent is triethylene tetramine, p-phenylenediamine (PPD), aliphatic amine or aromatic diamines in the step 2; Disperse in the step 3 is to adopt high-shearing dispersion emulsifying machine to disperse with the rotating speed of 3000～8000r/min or adopt ultrasonic dispersion 10～30min; Auxiliary agent is aliphatic acid SR-GWS and aliphatic amide SR-508 in the step 5.
Water-base epoxy resin sizing agent for carbon fiber of the present invention; has good compatibility with resin matrix commonly used; can reach simultaneously protection carbon fiber surface and enhanced carbon fiber and with the purpose of the adhesion strength of resin matrix; the excellent properties of carbon fiber can be given full play to, the sufficient convergence of carbon fiber, the mechanical property of excellence and lower saturated water absorption (＜0.6%) can be given.Water-base epoxy resin sizing agent for carbon fiber of the present invention has good permeability, can bond infiltrated fiber inside; Well water-soluble, be convenient to gluing; Adhesion strength is preferably arranged, give carbon fiber, to bear tension force and friction with good processing properties; The glue that do not fall is not taken glue, and is wide to temperature and humidity accommodation.The performance of water-base epoxy resin sizing agent for carbon fiber of the present invention is good, humidification to carbon fiber is good, can guarantee simultaneously that carbon fiber has convergence, smoothness, flexibility, pliability preferably, and can satisfy between fiber the whole loosening degree of strand simultaneously, open the crosslinking degree performance indications between fibre, single fiber.Preparation method of the present invention is simple, and cost is low, satisfies the demand of production at present and the needs in market.
Description of drawings
Fig. 1 is the sem photograph that the carbon fiber after the starching of employing water-base epoxy resin sizing agent for carbon fiber is prepared into the section of composite in the specific embodiment 11; Fig. 2 is the sem photograph that the carbon fiber after the existing sizing agent starching of employing is prepared into the section of composite in the specific embodiment 11.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: the preparation method of present embodiment water-base epoxy resin sizing agent for carbon fiber realizes according to the following steps: one, press mass ratio and add epoxy resin and water-base epoxy emulsifying agent at 80: 20 in 70 ℃ water-bath, place high-shearing dispersion emulsifying machine then, rotating speed with 1500～16000r/min stirs, and drip deionized water to mixed system generation phase transfer, dripping deionized water to the solid content of mixed system behind 20～90min again is 40%～50%, continue to stir 30min, get aqueous epoxy resins HIT-WE; Two, in 70 ℃ water-bath, press mass ratio and add epoxy curing agent and water-base epoxy emulsifying agent at 80: 20, place high-shearing dispersion emulsifying machine then, rotating speed with 1500～8000r/min stirs and drips deionized water, dripping deionized water to the solid content of mixed system behind 3～5h again is 40%～50%, water-soluble epoxy resin curing agent HIT-GY; Three, with deionized water aqueous epoxy resins HIT-WE being diluted to solid content is 0.5%～5%, and being dispersed to particle diameter then is 100～500nm, gets aqueous epoxy resin emulsion HIT-Y; Four, press mass ratio and 100: 0.01～0.25 aqueous epoxy resin emulsion HITY mixed with water-soluble epoxy resin curing agent HIT-GY, aqueous epoxy resin emulsion system HIT-S; Five, by mass percentage the auxiliary agent of 90%～98% aqueous epoxy resin emulsion system HIT-S and 2%～10% is mixed, promptly get water-base epoxy resin sizing agent for carbon fiber; Wherein epoxy curing agent is triethylene tetramine, p-phenylenediamine (PPD), aliphatic amine or aromatic diamines in the step 2; Disperse in the step 3 is to adopt high-shearing dispersion emulsifying machine to disperse with the rotating speed of 3000～8000r/min or adopt ultrasonic dispersion 10～30min; Auxiliary agent is aliphatic acid SR-GWS and aliphatic amide SR-508 in the step 5.
The model of high-shearing dispersion emulsifying machine is FA25 in the present embodiment step 1, is that Shanghai Fu Luke mechanical ﹠ electronic equipment corporation, Ltd produces.
Mixed system generation phase transfer in the present embodiment step 1 is exactly the instantaneous decline of viscosity of system, and electrical conductivity begins to descend suddenly.
Aqueous epoxy resin emulsion HIT-Y in the present embodiment step 3, particle diameter is 100～500nm, and particle diameter can be controlled, distribution of particles narrower (100～300nm), good stability (＞6 months), temperature tolerance be better, saturated water absorption low (＜0.1%), and environment friendly and pollution-free.
Aliphatic acid SR-GWS and aliphatic amide SR-508 are direct purchase and obtain in the present embodiment step 5.
The specific embodiment two: what present embodiment and the specific embodiment one were different is the preparation of water-base epoxy emulsifying agent in the step 1: the four-hole bottle that the 250ml of agitator, reflux condensing tube and thermometer will be housed places 80 ℃ of water-baths, added bisphenol A type epoxy resin and polyethylene glycol in 1: 1 in molar ratio then, and be stirred to molten condition with the speed of 200～500r/min; Be warming up to 100 ℃, add the triphenyl phosphorus that accounts for bisphenol A type epoxy resin and polyethylene glycol gross mass 0.15%, and stir 6h, then product is poured in the surface plate, promptly get the water-base epoxy emulsifying agent with the speed of 200-500r/min; Putting into drier preserves.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: what present embodiment and the specific embodiment one were different is that the rotating speed with 2000～10000r/min stirs in the step 1.Other step and parameter are identical with the specific embodiment one.
The specific embodiment four: what present embodiment and the specific embodiment one were different is that the rotating speed with 8000r/min stirs in the step 1.Other step and parameter are identical with the specific embodiment one.
The specific embodiment five: present embodiment and the specific embodiment four are different is that to drip deionized water to the solid content of mixed system in the step 1 behind the 60min again be 50%.Other step and parameter are identical with the specific embodiment four.
The specific embodiment six: present embodiment and the specific embodiment five are different is that with deionized water aqueous epoxy resins HIT-WE to be diluted to solid content in the step 3 be 3%～4%, and being dispersed to particle diameter then is 200～400nm.Other step and parameter are identical with the specific embodiment five.
The specific embodiment seven: present embodiment and the specific embodiment five are different is that with deionized water aqueous epoxy resins HIT-WE to be diluted to solid content in the step 3 be 3.5%, and being dispersed to particle diameter then is 300nm.Other step and parameter are identical with the specific embodiment five.
The specific embodiment eight: present embodiment is different with the specific embodiment six or seven is by mass ratio 100: 0.011 aqueous epoxy resin emulsion HIT-Y to be mixed with water-soluble epoxy resin curing agent HIT-GY in the step 4 in the step 4, aqueous epoxy resin emulsion system HIT-S.Other step and parameter are identical with the specific embodiment six or seven.
The specific embodiment nine: present embodiment and the specific embodiment eight are different is by mass percentage 92%～96% aqueous epoxy resin emulsion system HIT-S and 4%～8% auxiliary agent to be mixed in the step 5.Other step and parameter are identical with the specific embodiment eight.
The specific embodiment ten: present embodiment and the specific embodiment eight are different is by mass percentage 98% aqueous epoxy resin emulsion system HIT-S and 2% auxiliary agent to be mixed in the step 5.Other step and parameter are identical with the specific embodiment eight.
The specific embodiment 11: the preparation method of present embodiment water-base epoxy resin sizing agent for carbon fiber realizes according to the following steps: one, press mass ratio and add epoxy resin and water-base epoxy emulsifying agent at 80: 20 in 70 ℃ water-bath, place high-shearing dispersion emulsifying machine then, rotating speed with 8000r/min stirs, and drip deionized water to mixed system generation phase transfer, dripping deionized water to the solid content of mixed system behind the 60min again is 50%, continue to stir 30min, get water-base epoxy tree HIT-WE; Two, in 70 ℃ water-bath, press mass ratio and add epoxy curing agent and water-base epoxy emulsifying agent at 80: 20, place high-shearing dispersion emulsifying machine then, rotating speed with 4000r/min stirs and drips deionized water, dripping deionized water to the solid content of mixed system behind the 4h again is 50%, water-soluble epoxy resin curing agent HIT-GY; Three, with deionized water aqueous epoxy resins HIT-WE being diluted to solid content is 3%, and being dispersed to particle diameter then is 200nm, gets aqueous epoxy resin emulsion HIT-Y; Four, press mass ratio 100: 0.011 aqueous epoxy resin emulsion HIT-Y mixed with water-soluble epoxy resin curing agent HIT-GY, aqueous epoxy resin emulsion system HIT-S; Five, by mass percentage the auxiliary agent of 98% aqueous epoxy resin emulsion system HIT-S and 2% is mixed, promptly get water-base epoxy resin sizing agent for carbon fiber; Wherein epoxy curing agent is a triethylene tetramine in the step 2; Disperse in the step 3 is to adopt high-shearing dispersion emulsifying machine to disperse with the rotating speed of 5000r/min; Auxiliary agent is aliphatic acid SR-GWS and aliphatic amide SR-508 in the step 5.
Water-base epoxy resin sizing agent for carbon fiber in the present embodiment is used on the carbon fiber production line carbon fiber being carried out starching and handles, and 120～150 ℃ of oven dry down, receives silk more then.
Carbon fiber after the starching is carried out the test of performance and saturated water absorption, and the result is as shown in table 1, and present embodiment sizing agent performance is good, can make carbon fiber have excellent mechanical property and lower saturated water absorption.TENSILE STRENGTH before the carbon fiber starching is 3.30, and crisp, more easy to break.
Table 1
| TENSILE STRENGTH Gpa | Intensity cv value % | Elongation at break % | Elongation at break cv value % | Gel content % | Saturated water absorption % |
| ?3.36 | 4.7 | 2.07 | 6.21 | 1.32 | 0.05 |
Carbon fiber in the employing present embodiment after the water-base epoxy resin sizing agent for carbon fiber starching is prepared into composite, as shown in Figure 1, the port of composite is very neat, does not extract phenomenon, illustrate that the direct adhesion of fiber and resin is fine, the compatibility of the two is better.And the composite that adopts the carbon fiber after the existing sizing agent starching to be prepared into, as shown in Figure 2, the port of composite has fiber to extract, and the interface is in conjunction with relatively poor.
Water-base epoxy resin sizing agent for carbon fiber and the Japanese 4# sizing agent that produces in the present embodiment, simultaneously to after a kind of carbon fiber starching, test its interlayer shear power, be respectively 87.06331 and 85.58375, as seen adopt sizing agent performance in the present embodiment to be better than the 4# sizing agent that Japan produces.
Water-base epoxy resin sizing agent for carbon fiber and the Japanese 4# sizing agent that produces in the present embodiment, simultaneously to after a kind of carbon fiber starching, carry out the analysis of sizing agent temperature tolerance, the result is as shown in table 2, the good heat resistance of water-base epoxy resin sizing agent for carbon fiber in the present embodiment can avoid the structure of carbon fiber and performance at high temperature to be damaged.
Table 2
| Sample | Initial decomposition temperature/℃ | Maximum decomposition temperature/℃ | Starching amount/% |
| Water-base epoxy resin sizing agent for carbon fiber | 197 | 346 | 1.3 |
| Japan 4# sizing agent | 178 | 319 | 0.9 |
The specific embodiment 12: the preparation method of present embodiment water-base epoxy resin sizing agent for carbon fiber realizes according to the following steps: one, press mass ratio and add epoxy resin and water-base epoxy emulsifying agent at 80: 20 in 70 ℃ water-bath, place high-shearing dispersion emulsifying machine then, rotating speed with 10000r/min stirs, and drip deionized water to mixed system generation phase transfer, dripping deionized water to the solid content of mixed system behind the 50min again is 40%, continue to stir 30min, get aqueous epoxy resins HIT-WE; Two, in 70 ℃ water-bath, press mass ratio and add epoxy curing agent and water-base epoxy emulsifying agent at 80: 20, place high-shearing dispersion emulsifying machine then, rotating speed with 6000r/min stirs and drips deionized water, dripping deionized water to the solid content of mixed system behind the 5h again is 40%, water-soluble epoxy resin curing agent HIT-GY; Three, with deionized water aqueous epoxy resins HIT-WE being diluted to solid content is 4%, and being dispersed to particle diameter then is 100nm, gets aqueous epoxy resin emulsion HIT-Y; Four, press mass ratio 100: 0.012 aqueous epoxy resin emulsion HIT-Y mixed with water-soluble epoxy resin curing agent HIT-GY, aqueous epoxy resin emulsion system HIT-S; Five, by mass percentage the auxiliary agent of 92% aqueous epoxy resin emulsion system HIT-S and 8% is mixed, promptly get water-base epoxy resin sizing agent for carbon fiber; Wherein epoxy curing agent is a p-phenylenediamine (PPD) in the step 2; Disperse in the step 3 is to adopt ultrasonic dispersion 30min; Auxiliary agent is aliphatic acid SR-GWS and aliphatic amide SR-508 in the step 5.
Water-base epoxy resin sizing agent for carbon fiber in the present embodiment is used on the carbon fiber production line carbon fiber being carried out starching and handles, and 120～150 ℃ of oven dry down, receives silk more then.
Carbon fiber after the starching is carried out the test of performance and saturated water absorption, and the result is as shown in table 3, and present embodiment sizing agent performance is good, can make carbon fiber have excellent mechanical property and lower saturated water absorption.
Table 3
| TENSILE STRENGTH Gpa | Intensity cv value % | Elongation at break % | Elongation at break cv value % | Gel content % | Saturated water absorption % |
| ?3.45 | 4.71 | 1.98 | 5.16 | 1.28 | 0.05 |
The specific embodiment 13: the preparation method of present embodiment water-base epoxy resin sizing agent for carbon fiber realizes according to the following steps: one, press mass ratio and add epoxy resin and water-base epoxy emulsifying agent at 80: 20 in 70 ℃ water-bath, place high-shearing dispersion emulsifying machine then, rotating speed with 12000r/min stirs, and drip deionized water to mixed system generation phase transfer, dripping deionized water to the solid content of mixed system behind the 80min again is 45%, continue to stir 30min, get aqueous epoxy resins HIT-WE; Two, in 70 ℃ water-bath, press mass ratio and add epoxy curing agent and water-base epoxy emulsifying agent at 80: 20, place high-shearing dispersion emulsifying machine then, rotating speed with 7000r/min stirs and drips deionized water, dripping deionized water to the solid content of mixed system behind the 3h again is 45%, water-soluble epoxy resin curing agent HIT-GY; Three, with deionized water aqueous epoxy resins HIT-WE being diluted to solid content is 2%, and being dispersed to particle diameter then is 300nm, gets aqueous epoxy resin emulsion HIT-Y; Four, press mass ratio 100: 0.013 aqueous epoxy resin emulsion HIT-Y mixed with water-soluble epoxy resin curing agent HIT-GY, aqueous epoxy resin emulsion system HIT-S; Five, by mass percentage the auxiliary agent of 97% aqueous epoxy resin emulsion system HIT-S and 3% is mixed, promptly get water-base epoxy resin sizing agent for carbon fiber; Wherein epoxy curing agent is an aliphatic amine in the step 2; Disperse in the step 3 is to adopt ultrasonic dispersion 25min; Auxiliary agent is aliphatic acid SR-GWS and aliphatic amide SR-508 in the step 5.
Water-base epoxy resin sizing agent for carbon fiber in the present embodiment is used on the carbon fiber production line carbon fiber being carried out starching and handles, and 120～150 ℃ of oven dry down, receives silk more then.
Carbon fiber after the starching is carried out the test of performance and saturated water absorption, and the result is as shown in table 4, and present embodiment sizing agent performance is good, can make carbon fiber have excellent mechanical property and lower saturated water absorption.
Table 4
| TENSILE STRENGTH Gpa | Intensity cv value % | Elongation at break % | Elongation at break cv value % | Gel content % | Saturated water absorption % |
| 3.35 | 5.72 | 1.83 | 7.18 | 1.40 | 0.06 |
Claims (10)
1. the preparation method of a water-base epoxy resin sizing agent for carbon fiber, the preparation method who it is characterized in that water-base epoxy resin sizing agent for carbon fiber realizes according to the following steps: one, in 70 ℃ water-bath, press mass ratio 80:20 and add epoxy resin and water-base epoxy emulsifying agent, place high-shearing dispersion emulsifying machine then, rotating speed with 1500～16000r/min stirs, and drip deionized water to mixed system generation phase transfer, dripping deionized water to the solid content of mixed system behind 20～90min again is 40%～50%, continue to stir 30min, get aqueous epoxy resins HIT-WE; Two, in 70 ℃ water-bath, press mass ratio 80:20 and add epoxy curing agent and water-base epoxy emulsifying agent, place high-shearing dispersion emulsifying machine then, rotating speed with 1500～8000r/min stirs and drips deionized water, dripping deionized water to the solid content of mixed system behind 3～5h again is 40%～50%, water-soluble epoxy resin curing agent HIT-GY; Three, with deionized water aqueous epoxy resins HIT-WE being diluted to solid content is 0.5%～5%, and being dispersed to particle diameter then is 100～500nm, gets aqueous epoxy resin emulsion HIT-Y; Four, press mass ratio 100:0.01～0.25 aqueous epoxy resin emulsion HIT-Y is mixed with water-soluble epoxy resin curing agent HIT-GY, get aqueous epoxy resin emulsion system HIT-S; Five, by mass percentage the auxiliary agent of 90%～98% aqueous epoxy resin emulsion system HIT-S and 2%～10% is mixed, promptly get water-base epoxy resin sizing agent for carbon fiber; Wherein epoxy curing agent is triethylene tetramine or p-phenylenediamine (PPD) in the step 2; Disperse in the step 3 is to adopt high-shearing dispersion emulsifying machine to disperse with the rotating speed of 3000～8000r/min or adopt ultrasonic dispersion 10～30min; Auxiliary agent is aliphatic acid SR-GWS and aliphatic amide SR-508 in the step 5.
2. the preparation method of a kind of water-base epoxy resin sizing agent for carbon fiber according to claim 1, it is characterized in that the preparation of water-base epoxy emulsifying agent in the step 1: the four-hole bottle that the 250ml of agitator, reflux condensing tube and thermometer will be housed places 80 ℃ of water-baths, 1:1 adds bisphenol A type epoxy resin and polyethylene glycol in molar ratio then, and is stirred to molten condition with the speed of 200～500r/min; Be warming up to 100 ℃, add the triphenyl phosphorus that accounts for bisphenol A type epoxy resin and polyethylene glycol gross mass 0.15%, and stir 6h, then product is poured in the surface plate, promptly get the water-base epoxy emulsifying agent with the speed of 200-500r/min.
3. the preparation method of a kind of water-base epoxy resin sizing agent for carbon fiber according to claim 1 is characterized in that the rotating speed with 2000～10000r/min stirs in the step 1.
4. the preparation method of a kind of water-base epoxy resin sizing agent for carbon fiber according to claim 1 is characterized in that the rotating speed with 8000r/min stirs in the step 1.
5. the preparation method of a kind of water-base epoxy resin sizing agent for carbon fiber according to claim 4, it is characterized in that dripping behind the 60min in the step 1 deionized water to the solid content of mixed system is 50% again.
6. the preparation method of a kind of water-base epoxy resin sizing agent for carbon fiber according to claim 5 is characterized in that with deionized water aqueous epoxy resins HIT-WE being diluted to solid content in the step 3 is 3%～4%, and being dispersed to particle diameter then is 200～400nm.
7. the preparation method of a kind of water-base epoxy resin sizing agent for carbon fiber according to claim 5 is characterized in that with deionized water aqueous epoxy resins HIT-WE being diluted to solid content in the step 3 is 3.5%, and being dispersed to particle diameter then is 300nm.
8. according to the preparation method of claim 6 or 7 described a kind of water-base epoxy resin sizing agent for carbon fiber, it is characterized in that by mass ratio 100:0.011 aqueous epoxy resin emulsion HIT-Y being mixed with water-soluble epoxy resin curing agent HIT-GY in the step 4, get aqueous epoxy resin emulsion system HIT-S.
9. the preparation method of a kind of water-base epoxy resin sizing agent for carbon fiber according to claim 8 is characterized in that in the step 5 by mass percentage 92%～96% aqueous epoxy resin emulsion system HIT-S and 4%～8% auxiliary agent are mixed.
10. the preparation method of a kind of water-base epoxy resin sizing agent for carbon fiber according to claim 8 is characterized in that in the step 5 by mass percentage 98% aqueous epoxy resin emulsion system HIT-S and 2% auxiliary agent are mixed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010103001313A CN101736593B (en) | 2010-01-08 | 2010-01-08 | Preparation method of water-base epoxy resin sizing agent for carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010103001313A CN101736593B (en) | 2010-01-08 | 2010-01-08 | Preparation method of water-base epoxy resin sizing agent for carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101736593A CN101736593A (en) | 2010-06-16 |
| CN101736593B true CN101736593B (en) | 2011-11-30 |
Family
ID=42460581
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010103001313A Active CN101736593B (en) | 2010-01-08 | 2010-01-08 | Preparation method of water-base epoxy resin sizing agent for carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101736593B (en) |
Families Citing this family (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101886336B (en) * | 2010-06-23 | 2011-12-21 | 北京航空航天大学 | Polyalcohol modified epoxy resin carbon fiber emulsion sizing agent component and preparation method thereof |
| CN101982602B (en) * | 2010-10-22 | 2011-11-30 | 北京化工大学 | Sizing agent for carbon fiber |
| KR101557568B1 (en) * | 2011-08-22 | 2015-10-05 | 미쯔비시 레이온 가부시끼가이샤 | Carbon fiber sizing agent, aqueous dispersion thereof, carbon fiber bundle having adsorbed sizing agent, sheet-shaped article, and carbon fiber reinforced composite material |
| CN102735571A (en) * | 2012-06-27 | 2012-10-17 | 中国科学院宁波材料技术与工程研究所 | Method for determining carbon fiber sizing agent content |
| CN102912641A (en) * | 2012-11-20 | 2013-02-06 | 哈尔滨工业大学 | Preparation method of aqueous sizing agent for carbon fibers |
| CN103046347B (en) * | 2012-12-24 | 2014-09-10 | 金发科技股份有限公司 | Sizing agent for emulsion type carbon fiber, preparation method and application thereof |
| CN103103775B (en) * | 2013-02-01 | 2014-09-10 | 金发科技股份有限公司 | Sizing agent for emulsion type carbon filter and preparation method and application thereof |
| CN104420204B (en) * | 2013-09-10 | 2016-08-10 | 济南大学 | A kind of carbon fiber water soluble epoxy sizing agent |
| JP5802877B2 (en) | 2013-10-18 | 2015-11-04 | 国立大学法人岐阜大学 | Mixed yarn and its manufacturing method, braid, woven fabric, knitted fabric and non-woven fabric |
| CN104131459B (en) * | 2014-07-31 | 2016-03-16 | 哈尔滨工业大学 | A kind of vinyl ester carbon fiber sizing agent containing CNTs and preparation method thereof |
| CN104389176B (en) * | 2014-11-03 | 2017-01-11 | 哈尔滨工业大学 | Emulsion type carbon fiber sizing agent containing graphene oxide and preparation method thereof |
| CN104878603A (en) * | 2015-06-05 | 2015-09-02 | 中国科学院山西煤炭化学研究所 | Carbon nanotube modified carbon fiber emulsion sizing agent and preparation method |
| CN105908511B (en) * | 2016-04-26 | 2018-03-30 | 北京化工大学 | A kind of preparation method of self-emulsification aqueous epoxy resin carbon fiber sizing agent |
| CN107573526B (en) * | 2017-09-06 | 2020-08-11 | 中车青岛四方机车车辆股份有限公司 | Carbon fiber composite material, preparation method thereof and carbon fiber composite material plate |
| CN107447522A (en) * | 2017-09-11 | 2017-12-08 | 哈尔滨工业大学 | A kind of preparation method of high-temperature-resistant epoxy resin emulsion type carbon fiber sizing agent |
| CN108731992A (en) * | 2018-03-26 | 2018-11-02 | 北京化工大学 | A kind of preparation method of carbon fiber bundle filament test batten |
| CN114481618B (en) * | 2022-03-21 | 2023-10-24 | 江苏恒神股份有限公司 | Carbon fiber sizing agent for water-based treatment, and preparation method and application thereof |
| CN115710824A (en) * | 2022-06-20 | 2023-02-24 | 四川大学 | Water-soluble epoxy resin emulsion for carbon fiber surface treatment and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1537188A (en) * | 2001-07-31 | 2004-10-13 | ������������ʽ���� | Sizing agent for carbon fiber, method for sizing carbon fiber by said sizing agent, sized carbon fiber and knitted or woven fabric using said carbon fiber |
| CN1701148A (en) * | 2001-05-25 | 2005-11-23 | 三菱丽阳株式会社 | Sizing agent for carbon fiber, aqueous dispersion thereof, carbon fiber treated by sizing, sheet-form object comprising the carbon fiber, and carbon fiber-reinforced composite material |
| JP2007023454A (en) * | 2005-07-21 | 2007-02-01 | Jsr Corp | Copolymer for fiber-sizing agent, fiber-sizing agent, fiber bundle, and fiber-reinforced resin |
| CN100999867A (en) * | 2006-12-20 | 2007-07-18 | 中国科学院山西煤炭化学研究所 | Temp, resisting type carbon fibre emulsion sizing agent and its preparation process and application |
| JP2009144303A (en) * | 2007-12-18 | 2009-07-02 | Mitsubishi Rayon Co Ltd | Sizing agent and sized carbon fiber bundle |
-
2010
- 2010-01-08 CN CN2010103001313A patent/CN101736593B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1701148A (en) * | 2001-05-25 | 2005-11-23 | 三菱丽阳株式会社 | Sizing agent for carbon fiber, aqueous dispersion thereof, carbon fiber treated by sizing, sheet-form object comprising the carbon fiber, and carbon fiber-reinforced composite material |
| CN1537188A (en) * | 2001-07-31 | 2004-10-13 | ������������ʽ���� | Sizing agent for carbon fiber, method for sizing carbon fiber by said sizing agent, sized carbon fiber and knitted or woven fabric using said carbon fiber |
| JP2007023454A (en) * | 2005-07-21 | 2007-02-01 | Jsr Corp | Copolymer for fiber-sizing agent, fiber-sizing agent, fiber bundle, and fiber-reinforced resin |
| CN100999867A (en) * | 2006-12-20 | 2007-07-18 | 中国科学院山西煤炭化学研究所 | Temp, resisting type carbon fibre emulsion sizing agent and its preparation process and application |
| JP2009144303A (en) * | 2007-12-18 | 2009-07-02 | Mitsubishi Rayon Co Ltd | Sizing agent and sized carbon fiber bundle |
Non-Patent Citations (1)
| Title |
|---|
| 关蓉波.炭纤维乳液上浆剂.《新型炭纤维》.2002,第17卷(第3期),第49－51、55. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101736593A (en) | 2010-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101736593B (en) | Preparation method of water-base epoxy resin sizing agent for carbon fiber | |
| CN108589319B (en) | Packaging material for photovoltaic module | |
| CN101550325B (en) | Wind-power class bi-component epoxy adhesive and preparation method thereof | |
| CN103287032B (en) | The application of laminated material and preparation method thereof and hollow glass micro-ball | |
| CN106753134B (en) | Epoxy structural adhesive for die assembly and bonding of salt mist-resistant and damp-heat-resistant wind power generation blade and preparation method thereof | |
| CN106750553B (en) | Biodegradable composite material and preparation method and application | |
| CN107385918B (en) | A kind of carbon fiber Wesy emulsion-type thermoplasticity sizing agent and preparation method thereof | |
| CN111484706B (en) | Preparation method of carbon fiber composite material for IV-type gas cylinder | |
| CN103030921A (en) | Clutch facing without rubber winding and preparation method thereof | |
| CN112680156A (en) | High-toughness bi-component epoxy structural adhesive and preparation method thereof | |
| CN102977730A (en) | Metal antirust paint treating modified attapulgite as filler, and its preparation method | |
| CN102392392A (en) | Emulsified phenolic resin composition for automobile engine oil filter paper and preparation method for composition | |
| CN102898621A (en) | Water-based latent curing agent for epoxy resin and application of water-based latent curing agent | |
| CN105778574A (en) | Preparation method of urea-formaldehyde resin coated nanometer rare earth oxide | |
| CN104711705A (en) | Modified PET (polyethylene terephthalate) fiber and production method thereof | |
| CN115109385A (en) | Epoxy resin composition for prepreg and preparation method thereof | |
| CN105254188A (en) | Film forming agent specially used for glass fibers for wind turbine blades, and preparation method thereof | |
| CN103172977A (en) | Anti-flaming, high-temperature-resistant, high-property and hybrid glass-fiber prepreg and preparation method thereof | |
| CN102603979A (en) | Multi-monomer melt-grafted polypropylene-grafted masterbatch compatibilizer | |
| CN107337892A (en) | A kind of shock resistance lead-acid accumulator plastic housing material | |
| CN106675001A (en) | Gear made from high polymer material | |
| CN104072726A (en) | Epoxy resin curing agent and modification method thereof | |
| CN104387992B (en) | A kind of wood-based plate Environment-friendlyadhesive adhesive and preparation method thereof | |
| CN105968871B (en) | Fiberglass boiling-bed drying for drying haloflex | |
| CN105199152B (en) | A kind of conductive clip |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |