CN109455953A - A kind of reinforced polypropylene glass fiber infiltration agent and its preparation method and application - Google Patents
A kind of reinforced polypropylene glass fiber infiltration agent and its preparation method and application Download PDFInfo
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- CN109455953A CN109455953A CN201811465888.0A CN201811465888A CN109455953A CN 109455953 A CN109455953 A CN 109455953A CN 201811465888 A CN201811465888 A CN 201811465888A CN 109455953 A CN109455953 A CN 109455953A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/40—Organo-silicon compounds
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/26—Macromolecular compounds or prepolymers
- C03C25/28—Macromolecular compounds or prepolymers obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C03C25/30—Polyolefins
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Abstract
The invention discloses a kind of reinforced polypropylene glass fiber infiltration agents, include coupling agent, film forming agent, lubricant and water, and the solid masses of size accounts for the 2%~3% of size gross mass；Dosage of each component is expressed as follows in size with the percentage that its solid masses accounts for size solid masses: coupling agent 10~25%, lubricant 5~20%, film forming agent 55~85%；Wherein, film forming agent is modified polypropene wax emulsion；Lubricant is the composition of PE wax emulsion and silicone oil demoulding lubricant.The product produced by the size can complete excellent dipping effect under the working condition of ultrahigh speed LFT；It is surface-treated by size, product has extraordinary dispersibility, and superior with the interfacial bonding property of resin, can quickly be combined with acrylic resin under ultrahigh speed.
Description
Technical field
The present invention relates to size technical fields, and in particular to a kind of reinforced polypropylene glass fiber infiltration agent and its system
Preparation Method and application.
Background technique
LFT (Long Fiber reinforced Thermoplastics) technology is Long Fiber Reinforced Thermoplastics
With composite material, it is widely used in building template, sports equipment, communications and transportation, military equipment etc..In recent years, LFT technique quilt
It is widely used in processing of auto parts and components, including front-end module, automobile tail gate, automotive trim panel, instrument board etc..Use LFT work
The glass fibre reinforced composite material of skill production, it is longer that glass retains length, and the glass fiber content of product is so controllable that quite high (to have
Up to 80%), so that product has good intensity and rigidity, alternative metal material, for automobile, ship, building and special
With tool etc..It is at present PP using most matrix resins, followed by PA, furthermore it is the resins such as PBT, PPS, SAN；For difference
Resin need just to can achieve preferable effect using different fibers.
LFT technique is divided into melting cladding process technique, direct method (LFT~D) technique and material grain method (LFT~G) technique.Wherein
Melting cladding process is traditional LFT processing technology, and advantage is high production efficiency, at low cost, the disadvantage is that needing further shearing point
It dissipates；LFT~D technique is straight forming technique, and the component of various sizes does not need post-processing complex component, but its equipment investment
Greatly, process and process are complex；LFT~G is material grain method technique, and advantage is that glass disperses more uniform, product properties
Height, but production efficiency is more slow, seldom producer can extensive, mass production.
In terms of LFT production equipment, traditional LFT processing technology is formed using common injection molding machine, but performance is difficult to be filled
The performance divided；Later equipment is by improving, using the molding of dedicated injection molding machine (as Nippon Steel Works is researched and developed).Since screw rod is made
Biggish improvement, length homogeneity of the fiber in finished product is good, and corresponding performance is also much better, but traditional drawback is still
It not can solve, for example production efficiency still can not improve, glass by screw rod retains length not enough etc..By nearly 10 years hairs
Exhibition, LFT contour machining equipment also obtains breakthrough progress, wherein using Krauss Maffei and Dieffenbacher as generation
Table is directly molded and is molded directly into the skills such as type in LFT respectively after the technical problem for solving screw-rod structure and quick press
Breakthrough is achieved in terms of art, production efficiency is further promoted.
For the demand for catering to automotive light weight technology, LFT capacity requirements are further promoted.Currently, producer improves one after another both at home and abroad
Speed of production is increased to 70 meters per minute or more, belongs to superfast production line by starting up speed, some typical producers of industry；
And general LFT production line, even if speed is promoted, generally also at 30~50 meters per minute or so, few enterprises can accomplish every point
60 meters of clock or more.In order to adapting to use under superfast working condition, not only to solve the problems, such as glass using technique,
More to solve the problems, such as glass polymolecularity.Therefore, it is necessary to develop a kind of novel reinforced polypropylene resins to be infiltrated with glass fibre
Agent enables glass normal use under superfast LFT technique, and has good service performance.
Summary of the invention
Present invention seek to address that problem as described above.The object of the present invention is to provide a kind of reinforced polypropylene glass fibers
Size is tieed up, the product produced by the size can be in the production of ultrahigh speed (speed of production i.e. per minute is greater than 70 meters) LFT
Under the conditions of complete excellent dipping effect；It is surface-treated by size, product is made to have extraordinary dispersibility, and and resin
Interfacial bonding property it is superior, can be with acrylic resin Flashmelt under ultrahigh speed.
According to an aspect of the present invention, the present invention provides a kind of reinforced polypropylene glass fiber infiltration agent, include
Coupling agent, film forming agent, lubricant and water, the solid masses of the size account for the 2%~3% of the size gross mass；
Dosage of each component is expressed as follows in the size with the percentage that its solid masses accounts for size solid masses:
Coupling agent 10~25%
Lubricant 5~20%
Film forming agent 55~85%；
Wherein, the film forming agent is modified polypropene wax emulsion；The lubricant is PE wax emulsion and silicone oil demoulding profit
The composition of lubrication prescription.
Wherein, the film forming agent be maleic acid bar grafting modified polypropene wax emulsion, molecular weight be 10000~
70000, emulsion particle diameter is 0.1~4um.
Wherein, the molecular weight of the modified polypropene wax emulsion is 30000~50000.
Wherein, the mass ratio of the PE wax emulsion and the silicone oil demoulding lubricant is 1~3:1.
Wherein, the mass ratio of the PE wax emulsion and the silicone oil demoulding lubricant is 1.2~1.8:1.
Wherein, dosage of each component is indicated such as in the size with the percentage that its solid masses accounts for size solid masses
Under:
Coupling agent 13~22%
Lubricant 7~18%
Film forming agent 60~80%.
Wherein, dosage of each component is indicated in the size with the percentage that its solid masses occupies size solid masses
It is as follows:
Coupling agent 15~20%
Lubricant 10~17%
Film forming agent 63~78%.
Reinforced polypropylene of the invention can be selected with the coupling agent that glass fiber infiltration agent uses for amino silicane coupling agent
The trade mark be A1100, A1120 etc..Reactive group after coupling agent hydrolysis can rise for the combination of glass and acrylic resin
It is acted on to " bridge joint ", can preferably improve film forming agent and resin compatible, substantially improve the service performance of glass product.Cause
This, the use of coupling agent is an important factor for influencing glass rapid impregnation, to play key using the dipping effect of technique to the later period
Effect；Suitable coupling agent selection, can be such that the LFT reinforced polypropylene alkali-free glass fibre produced has more superior
Dipping effect.If coupling agent ratio is excessively high, its own can generate polymerization reaction, the shape that the group branch after polymerization keeps product final
State generates variation, is easy to keep yarn beam brittle, filoplume is caused to increase；And the too low free radical group that will lead to free state of coupling agent ratio
It is point very few, it is unfavorable for the interface cohesion with resin, influences the final mechanical performance of product.Therefore, in the present invention, design silane is even
Joining agent content is 10%~25%, to guarantee product final performance and state；It preferably, is 13%~22%；It is further excellent
Choosing, be 15~20%, much further preferably from 16~18%.
In the present invention, water-soluble organic compound, preferably PE wax emulsion and silicone oil demoulding profit can be used in lubricant
The composition of lubrication prescription.The use of lubricating system can play a good protective effect to glass, protection glass make its production and
It is not damaged in use process, therefore is major influence factors of the product in terms of craftsmanship, usability.The total content control of lubricant
5~20% are made as, the excessive use of lubricant will affect subsequent product dipping effect；And lubricant content is too low, it also can be right
Later product performance causes adverse effect.Therefore needing to control suitable ratio, it is preferred that the total content of lubricant is 7~
18%, further preferably 10~17%, it is still more preferably 12~15%.
The use smoothness for being advantageously selected for improving LFT reinforced polypropylene yarn of reasonable lubricant system, improves glass
Fine production efficiency in use.The study found that by two kinds of lubricant compoundings of PE wax emulsion and silicone oil demoulding lubricant
It can achieve the above production requirement.Wherein, PE wax emulsion lubricant can make the film of PP wax more continuous in PP wax emulsion, thus
So that wearability is reinforced；Have a better role to the butt of glass lubrication, but viscosity wax-like simultaneously increase glass it
Between interlayer adhesion.And silicone oil demoulding lubricant can be free in rapidly film surface in film forming procedure, and form surface painting
Layer, can make interfacial separation, to function similarly to demoulding effect；Yarn can be made to move back in solution preocess quickly, reduce interlayer adhesion, make
It is more smoothly that solution must be moved back, advantageously reduce the interlayer adhesion of glass.Therefore, the collocation by the two by a certain percentage, can be in reality
While existing excellent lubrication, realize that good yarn beam moves back solution.In the present invention, the quality of PE wax emulsion and silicone oil demoulding lubricant
Than for 1~3:1, it is preferred that the two mass ratio is 1.2~1.8:1, and the above ratio is the best proportion after overtesting authenticates.
The film forming agent that the present invention uses is modified polypropene wax emulsion, belongs to high molecular weight polypropylene wax emulsion.Film forming agent
It is the key that influence glass service performance as the chief component of sizing system；Primarily serve protection tow at band
Property, reaction carriers are provided for glass, the effect of excellent dipping effect and mechanical performance is provided.Therefore film forming agent selection and match
It is main to consider and the compatibility of target resin (polypropylene) in R&D process than the emphasis that ratio is size of the present invention, i.e., with
Resin reaction, compatible speed.In the present invention, film forming agent uses maleic anhydride grafted PP wax emulsion, in alkali neutralization
Under the conditions of obtain modified polypropene wax emulsion.The molecular weight of modified polypropene wax emulsion is 10000~70000, preferably 30000
~50000；Emulsion particle diameter is 0.1~4um, preferably 2~3um.
The percentage control that the solid masses of film forming agent accounts for size solid masses is 55~85%, preferably 60~80%,
Further preferred ratio is 63~78%, still more preferably 67~75%.Film forming agent ratio is more than 85%, the convergence of glass
It is good, and leads to glass in use, is unfavorable for scattering, and the combination of influence and resin leads to final mechanical performance
It reduces；And too low film forming agent ratio, the then protectiveness that will lead to glass are inadequate, and filoplume in use process is caused to increase.
Water used in the present invention is deionized water.
The ratio of glass fiber infiltration agent of the invention, coupling agent component and film former component is arranged in pairs or groups to final product
Key effect can be played.Realize impregnation state excellent under ultrahigh speed, it is necessary to select suitable film forming agent ratio, simultaneously
Coupling agent ratio is also required to corresponding, in order to both realize good reaction in film forming procedure, and reduces as far as possible
The component of coupling agent auto polymerization, in order to the performance state being optimal.
According to the second aspect of the invention, a kind of preparation side of aforementioned reinforced polypropylene glass fiber infiltration agent is provided
Method, comprising the following steps:
1S: being added the water of size total amount 30%~40% in a reservoir, and coupling agent is then added, and stirs 20~30 points
Clock；
2S: 2~5 times of its quality of water of lubricant is diluted, is then added to the container；Wherein, water temperature is 50~60 DEG C.
3S: 3~5 times of its quality of water of film forming agent is diluted, is then added to the container；The water of surplus is supplied, stirring is equal
It is even, solid content is detected to get to reinforced polypropylene glass fiber infiltration agent.
According to the third aspect of the present invention, aforementioned size is provided in ultrahigh speed LFT glass fibre reinforced composite material product
In application.
Compared with prior art, sizing system of the present invention, by limit size in film forming agent content, with
And the ratio of corresponding coupling agent, lower combustible content can be obtained, to be more advantageous to the dispersion of glass, is also beneficial to
Interface cohesion is more quickly completed in resin.Film forming agent is as the main component in sizing system, the selection and ratio control of type
It makes most important；Whether suitable film forming agent type and lower film former content, not only influencing glass can be quickly in resin
Middle dispersion, also will affect whether glass and acrylic resin have better interface compatibility, pass through optimization coupling agent and film forming agent
Ratio so that infiltration system has a more preferable reactivity in ultrahigh speed LFT technical process, impregnating speed faster, to make
It is more preferable to obtain its using effect；In LFT production technology, suitable for the dipping under quick working condition, it is raw that LFT can be improved rapidly
Produce efficiency.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with of the invention specific
Technical solution of the present invention is clearly and completely described in embodiment, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.It should be noted that
In the case where not conflicting, the features in the embodiments and the embodiments of the present application can mutual any combination.
Reinforced polypropylene glass fiber infiltration agent of the invention, size include coupling agent, film forming agent, lubricant and
Water, the solid masses of size account for the 2%~3% of the size gross mass；
Wherein, dosage of each component accounts for the percentage of size solid masses with its solid masses in size are as follows: coupling agent
10~25%, lubricant 5~20%, film forming agent 55~85%；
Preferably, coupling agent 13~22%, lubricant 7~18%, film forming agent 60~80%；
It is further preferred that coupling agent 15~20%, lubricant 10~17%, film forming agent 63~78%.
Still more preferably, coupling agent 16~18%, lubricant 12%~15%, film forming agent 67~75%.
Wherein,
Film forming agent is the modified polypropene wax emulsion of maleic acid bar grafting；Molecular weight is 10000~70000, preferably
30000~50000；Emulsion particle diameter is 0.1~4um, preferably 2~3um.
Lubricant is the composition of PE wax emulsion and silicone oil demoulding lubricant；PE wax emulsion and silicone oil demoulding profit
The mass ratio of lubrication prescription is 1~3:1, it is preferred that is 1.2~1.8:1.
Coupling agent is amino silicane coupling agent；
Water is deionized water.
The preparation method of the reinforced polypropylene glass fiber infiltration agent, includes the following steps:
1S: being added the water of size total amount 30%~40% in a reservoir, and coupling agent is then added, and stirs 20~30 points
Clock；
2S: 2~5 times of its quality of water of lubricant is diluted, container is then added；Wherein, water temperature is 50~60 DEG C.
3S: 3~5 times of its quality of water of film forming agent is diluted, container is then added；The water for supplying surplus, stirs evenly,
Solid content is detected to get to reinforced polypropylene glass fiber infiltration agent.
The some embodiments of the application reinforced polypropylene glass fiber infiltration agent are listed below.
Embodiment
Table 1 shows the specific embodiment of each component content in partial wetting agent, and the corresponding numerical value of each component is quality hundred
Divide ratio/%.The solid content Theoretical Design of size is 2~3%, remaining is deionized water, and following component ratio is each component
Effective solid content accounts for the ratio of the effective component (i.e. solid masses) in size.
Wherein, coupling agent selects amino silicane coupling agent, Dow corning company Z~6020.
Lubricant selects the composition of PE wax emulsion and silicone oil demoulding lubricant, the respectively D313 of DIC company, Japan
With the Dow290 of Dow corning company.
Film forming agent selects MODIFIED PP wax emulsion, Jushi Group Co., Ltd., TX170B.
1 size specific embodiment list of table
Test case
In order to further embody beneficial effects of the present invention, using different formulations combination size as a comparison case, and
Test is compared to the product properties of embodiment and comparative example.
Comparative example 1 is formulated:
Coupling agent: amino silicane coupling agent, the A1120 of U.S.'s figure advanced in years, 15%；
Lubricant: modified dormant oil class, section triumphant 7607,15%；
Film forming agent: macromolecule PP wax emulsion, Mai Kemen company, the U.S. 91735,70%；
Comparative example 2 is formulated:
Coupling agent: amino silane coupling, Dow corning company A1100,20%；
Lubricant: PEG series lubricant agent, the triumphant 2658A of section, 18%.
Film forming agent: MODIFIED PP wax emulsion, molecular weight are 1~20,000, Mai Kemen company, the U.S. 28640,62%；
Table 2 shows the concrete component formula of comparative example 3~6.
The comparative example example of 2 different content of table proportion
Table 3 shows the performance test results of each embodiment and comparative example product.Wherein, dipping effect is 70 meters/min speed
The lower dipping effect using LFT~G technique of degree, the test of tensile strength use ISO527 standard.
3 product properties contrast test result of table
From the comparison of the above formula test case, selection and different ratio ratio including the variety classes raw material trade mark, I
It can be seen that application variation influence to service performance of the formula of the present invention on LFT enhancing PP roving product,
By the appropriate promotion of lubricant ratio, filoplume is substantially reduced, and dispersibility is also improved；In the melting process with resin,
Glass can be quickly dispersed, but lubricant ratio is too high, has a certain impact to performance, by matching between two kinds of lubricants
Than optimization, facilitate dispersion and the dipping effect of equilibrium product.In addition, the ratio of coupling agent also has a fixing to the dipping of product
It rings, the mechanical performance that the coupling agent of proper proportion can also improve rapidly product adapts to ultrahigh speed that is, in LFT technique
Manufacturing process under (70m/min), effectively improves production efficiency, the too low combination for being unfavorable for glass and resin of coupling agent ratio,
Mechanical performance significantly reduces, and coupling agent ratio is excessively high, causes moiety agent autohemagglutination, easily causes glass embrittlement, and filoplume is significant
Increase, and mechanical performance also reduces obviously.Wherein, the indices of embodiment 5 meet the requirement of our designs, and filoplume is lower than
50mg/kg, immersion good using LFT technique under 70 meters of speed, comprehensive mechanical performance highest.
The present invention is according to the technical characterstic of LFT technique, by the selection of raw material, the optimization of recipe ingredient ratio, using conjunction
Mature glass fibre production technology is fitted, the direct yarn product of alkali-free glass fibre for meeting high-end customer demand is produced.Pass through
The product of size production can be completed excellent under the working condition of ultrahigh speed (speed of production i.e. per minute is greater than 70 meters)
Dipping effect；It is surface-treated by size, so that product is had extraordinary dispersibility, and excellent with the interfacial bonding property of resin
It more, can be with acrylic resin Flashmelt under ultrahigh speed.
Descriptions above can combine implementation individually or in various ways, and these variants all exist
Within protection scope of the present invention.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations.Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of reinforced polypropylene glass fiber infiltration agent, which is characterized in that the size include coupling agent, film forming agent,
Lubricant and water, the solid masses of the size account for the 2%~3% of the size gross mass；
Dosage of each component is expressed as follows in the size with the percentage that its solid masses accounts for size solid masses:
Coupling agent 10~25%
Lubricant 5~20%
Film forming agent 55~85%；
Wherein, the film forming agent is modified polypropene wax emulsion；The lubricant is PE wax emulsion and silicone oil demoulding lubricant
Composition.
2. reinforced polypropylene glass fiber infiltration agent as described in claim 1, which is characterized in that the film forming agent is Malaysia
The modified polypropene wax emulsion of sour bar grafting, molecular weight are 10000~70000, and emulsion particle diameter is 0.1~4um.
3. reinforced polypropylene glass fiber infiltration agent as claimed in claim 1 or 2, which is characterized in that the modification poly- third
The molecular weight of alkene wax emulsion is 30000~50000.
4. reinforced polypropylene glass fiber infiltration agent as described in claim 1, which is characterized in that the PE wax emulsion and institute
The mass ratio for stating silicone oil demoulding lubricant is 1~3:1.
5. reinforced polypropylene glass fiber infiltration agent as claimed in claim 4, which is characterized in that the PE wax emulsion and institute
The mass ratio for stating silicone oil demoulding lubricant is 1.2~1.8:1.
6. reinforced polypropylene glass fiber infiltration agent as described in claim 1, which is characterized in that each group in the size
Point dosage is expressed as follows with the percentage that its solid masses accounts for size solid masses:
Coupling agent 13~22%
Lubricant 7~18%
Film forming agent 60~80%.
7. reinforced polypropylene glass fiber infiltration agent as claimed in claim 6, which is characterized in that each group in the size
Point dosage is expressed as follows with the percentage that its solid masses occupies size solid masses:
Coupling agent 15~20%
Lubricant 10~17%
Film forming agent 63~78%.
8. reinforced polypropylene glass fiber infiltration agent as described in claim 1, which is characterized in that the coupling agent is amino
Silane coupling agent.
9. a kind of preparation method of reinforced polypropylene glass fiber infiltration agent as described in any one of claims 1 to 8, special
Sign is, includes the following steps:
1S: being added the water of size total amount 30%~40% in a reservoir, and coupling agent is then added, and stirs 20~30 minutes；
2S: 2~5 times of its quality of water of lubricant is diluted, the container is then added；
3S: 3~5 times of its quality of water of film forming agent is diluted, the container is then added；The water for supplying surplus, stirs evenly,
Solid content is detected to get to the reinforced polypropylene glass fiber infiltration agent.
10. a kind of reinforced polypropylene glass fiber infiltration agent as described in any one of claims 1 to 8 is in ultrahigh speed LFT glass
Application in fibre reinforced composite material product.
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| CN111533467A (en) * | 2020-06-09 | 2020-08-14 | 巨石集团有限公司 | Impregnating compound for glass fiber direct roving and preparation method, product and application thereof |
| CN112573840A (en) * | 2020-12-25 | 2021-03-30 | 巨石集团有限公司 | Glass fiber impregnating compound and preparation method and application thereof |
| CN112723759A (en) * | 2021-01-06 | 2021-04-30 | 泰山玻璃纤维有限公司 | Low-odor glass fiber impregnating compound and preparation method and application thereof |
| CN114014560A (en) * | 2021-10-22 | 2022-02-08 | 巨石集团有限公司 | Glass fiber impregnating compound and application thereof |
| CN114507400A (en) * | 2020-10-27 | 2022-05-17 | 合肥杰事杰新材料股份有限公司 | Modified glass fiber reinforced polypropylene composition and preparation method thereof |
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| CN112573840A (en) * | 2020-12-25 | 2021-03-30 | 巨石集团有限公司 | Glass fiber impregnating compound and preparation method and application thereof |
| CN112723759A (en) * | 2021-01-06 | 2021-04-30 | 泰山玻璃纤维有限公司 | Low-odor glass fiber impregnating compound and preparation method and application thereof |
| CN114014560A (en) * | 2021-10-22 | 2022-02-08 | 巨石集团有限公司 | Glass fiber impregnating compound and application thereof |
| CN114014560B (en) * | 2021-10-22 | 2023-02-03 | 巨石集团有限公司 | Glass fiber impregnating compound and application thereof |
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