CN109455953B - Glass fiber impregnating compound for reinforced polypropylene and preparation method and application thereof - Google Patents
Glass fiber impregnating compound for reinforced polypropylene and preparation method and application thereof Download PDFInfo
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- CN109455953B CN109455953B CN201811465888.0A CN201811465888A CN109455953B CN 109455953 B CN109455953 B CN 109455953B CN 201811465888 A CN201811465888 A CN 201811465888A CN 109455953 B CN109455953 B CN 109455953B
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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 glass fiber impregnating compound for reinforcing polypropylene, which comprises a coupling agent, a film-forming agent, a lubricant and water, wherein the solid mass of the impregnating compound accounts for 2-3% of the total mass of the impregnating compound; the dosage of each component in the impregnating compound is expressed by the percentage of the solid mass of the impregnating compound to the solid mass of the impregnating compound as follows: 10-25% of a coupling agent, 5-20% of a lubricant and 55-85% of a film forming agent; wherein the film forming agent is modified polypropylene wax emulsion; the lubricant is a combination of a PE wax emulsion and a silicone oil type release lubricant. The product produced by the impregnating compound can achieve excellent impregnation effect under the production condition of ultra-high speed LFT; through the surface treatment of the impregnating compound, the product has very good dispersibility, has excellent interface bonding property with resin, and can be quickly bonded with polypropylene resin at a super high speed.
Description
Technical Field
The invention relates to the technical field of impregnating compounds, in particular to a glass fiber impregnating compound for reinforcing polypropylene and a preparation method and application thereof.
Background
LFT (Long Fiber reinforced thermoplastics) technology is a composite material for long glass Fiber reinforced thermoplastics, and is widely used for building templates, sports equipment, transportation, military equipment and the like. In recent years, LFT processes have been widely used in the processing of automobile parts, including front end modules, automobile tail doors, automobile interior panels, instrument panels, and the like. The glass fiber reinforced composite material produced by the LFT process has longer glass fiber retention length, and the glass fiber content of the product can be controlled to be quite high (up to 80 percent in some cases), so that the product has good strength and rigidity, can replace metal materials, and can be used for automobiles, ships, buildings, special tools and the like. At present, the most adopted matrix resin is PP, PA, PBT, PPS, SAN and other resins; different fibers are needed to be used according to different resins, so that a better effect can be achieved.
The LFT process is classified into a melt coating process, a direct process (LFT-D) process, and a pellet process (LFT-G) process. The melting coating method is a traditional LFT processing technology, and has the advantages of high production efficiency and low cost, and the defect of further shearing dispersion; the LFT-D process is a direct forming process, parts of various sizes do not need to be subjected to post-processing on complex parts, but equipment investment is large, and the processing process and working procedures are complex; LFT-G is a material particle method process, and has the advantages that glass fibers are uniformly dispersed, the product performance is high, but the production efficiency is slow, and few manufacturers can produce the glass fibers in large scale and in batch.
In the LFT production equipment aspect, the traditional LFT processing technology adopts a common injection molding machine for molding, but the performance is difficult to give full play; later the equipment was modified to shape using a dedicated injection molding machine (as developed by japan steel works). Due to the great improvement of the screw, the length uniformity of the fiber in a finished product is good, the corresponding performance is better, but the traditional defects are not solved, such as the production efficiency cannot be improved, the length of the glass fiber after passing through the screw is not enough, and the like. Through the development of the last 10 years, LFT forming and processing equipment is also developed in a breakthrough way, wherein Krauss Maffei and Dieffenbacher are taken as representatives, and after the technical problems of a screw structure and a rapid press are solved, the LFT forming and processing equipment is developed in a breakthrough way in the aspects of LFT direct injection molding, direct compression molding and other technologies, and the production efficiency is further improved.
In order to meet the requirement of light weight of the automobile, the LFT capacity requirement is further improved. At present, manufacturers at home and abroad increase the starting speed, and manufacturers typical in some industries increase the production speed to more than 70 meters per minute, so that the production line belongs to an ultra-high-speed production line; even if the speed of a common LFT production line is increased, the speed is generally about 30-50 meters per minute, and few enterprises can achieve more than 60 meters per minute. In order to be suitable for being used under the condition of ultra-high-speed production, the problem of the glass fiber using process and the problem of high dispersibility of the glass fiber are solved. Therefore, it is necessary to develop a novel glass fiber impregnating compound for reinforced polypropylene resin, so that the glass fiber can be normally used in the LFT process at the ultra-high speed and has good service performance.
Disclosure of Invention
The present invention is directed to solving the problems described above. The invention aims to provide a glass fiber impregnating compound for reinforced polypropylene, and a product produced by the impregnating compound can complete excellent impregnation effect under the production condition of ultra-high speed (namely the production speed per minute is more than 70 meters) LFT; the product has good dispersibility and excellent interface bonding property with resin by surface treatment of the impregnating compound, and can be rapidly melted with polypropylene resin at ultrahigh speed.
According to one aspect of the invention, the invention provides a glass fiber impregnating compound for reinforcing polypropylene, which comprises a coupling agent, a film forming agent, a lubricant and water, wherein the solid mass of the impregnating compound accounts for 2-3% of the total mass of the impregnating compound;
the amount of each component in the impregnating compound is represented by the following solid mass percentage of the impregnating compound:
10 to 25 percent of coupling agent
5 to 20 percent of lubricant
55-85% of a film forming agent;
wherein the film forming agent is modified polypropylene wax emulsion; the lubricant is a composition of PE wax emulsion and silicone oil type demoulding lubricant.
The film forming agent is maleic acid rod grafted modified polypropylene wax emulsion, the molecular weight of the emulsion is 10000-70000, and the particle size of emulsion particles is 0.1-4 um.
Wherein the molecular weight of the modified polypropylene wax emulsion is 30000-50000.
The mass ratio of the PE wax emulsion to the silicone oil demoulding lubricant is 1-3: 1.
The mass ratio of the PE wax emulsion to the silicone oil demoulding lubricant is 1.2-1.8: 1.
the amount of each component in the impregnating compound is represented by the following solid mass percentage of the impregnating compound:
13 to 22 percent of coupling agent
7 to 18 percent of lubricant
60-80% of film forming agent.
The amount of each component in the impregnating compound is represented by the following percentage of the solid mass of the impregnating compound:
15-20% of coupling agent
10 to 17 percent of lubricant
63-78% of a film forming agent.
The glass fiber impregnating compound for reinforcing polypropylene adopts aminosilane coupling agent, and the available marks are A1100, A1120 and the like. The hydrolyzed reactive group of the coupling agent can play a role of bridging for the combination of the glass fiber and the polypropylene resin, can better improve the compatibility of the film-forming agent and the resin, and greatly improve the service performance of glass fiber products. Therefore, the use of the coupling agent is an important factor influencing the rapid impregnation of the glass fiber, and plays a key role in the impregnation effect of the later use process; the proper selection of the coupling agent can ensure that the produced alkali-free glass fiber for LFT reinforced polypropylene has more excellent impregnation effect. If the proportion of the coupling agent is too high, the coupling agent can generate polymerization reaction, and the polymerized components can change the final state of the product, so that yarn bundles are easy to embrittle, and the hairiness is increased; and too low proportion of the coupling agent can result in too few free radical components in a free state, which is not beneficial to interface combination with resin and influences the final mechanical properties of products. Therefore, in the invention, the content of the silane coupling agent is designed to be 10-25% so as to ensure the final performance and state of the product; preferably, 13 to 22 percent; more preferably, it is 15 to 20%, and still more preferably 16 to 18%.
In the present invention, a water-soluble organic compound, preferably a combination of a PE wax emulsion and a silicone-type release lubricant, may be used as the lubricant. The lubricating system can play a good role in protecting the glass fiber, and the glass fiber is protected from being damaged in the production and use processes, so that the lubricating system is a main influence factor of the product in the aspects of manufacturability and usability. The total content of the lubricant is controlled to be 5-20%, and the subsequent product impregnation effect is influenced by excessive use of the lubricant; and the low content of the lubricant can also cause adverse effect on the performance of the later product. Therefore, the proportion needs to be controlled properly, and preferably, the total content of the lubricant is 7 to 18%, more preferably 10 to 17%, and still more preferably 12 to 15%.
The reasonable selection of the lubricant system is beneficial to improving the use smoothness of the LFT reinforced polypropylene yarn and improving the production efficiency of the glass fiber in the use process. Researches find that the production requirements can be met by compounding the PE wax emulsion and the silicone oil demoulding lubricant. Wherein, the PE wax emulsion lubricant is in the PP wax emulsion, which can make the film of the PP wax more continuous, thereby enhancing the wear resistance; the wax-like glass fiber adhesive has a good improvement effect on dry-base lubrication of glass fibers, but the viscosity of wax-like glass increases interlayer adhesion between the glass fibers. The silicone oil demoulding lubricant can be quickly dissociated on the surface of the film in the film forming process, and forms a surface coating which can separate the interface, thereby playing a role similar to demoulding; the yarn can be rapidly removed, the interlayer adhesion is reduced, the removal is smoother, and the reduction of the interlayer adhesion of glass fibers is facilitated. Therefore, the two components are matched according to a certain proportion, so that excellent lubrication can be realized, and good yarn bundle unwinding can be realized. According to the invention, the mass ratio of the PE wax emulsion to the silicone oil demoulding lubricant is 1-3: 1, preferably, the mass ratio of the two is 1.2-1.8: 1, the proportion is the optimal proportion after experimental certification.
The film forming agent used in the invention is modified polypropylene wax emulsion, belonging to high molecular weight polypropylene wax emulsion. The film forming agent is used as a main component of the impregnating compound system and is the key for influencing the service performance of the glass fiber; the fiber is mainly used for protecting the banding property of the fiber bundles, providing a reaction carrier for glass fibers and providing excellent impregnation effect and mechanical property. Therefore, the selection and proportion of the film forming agent are the key points of the sizing agent, and the compatibility with the target resin (polypropylene), namely the reaction and compatibility speed with the resin, is mainly considered in the research and development process. In the invention, the film forming agent adopts maleic anhydride graft modified polypropylene wax emulsion, and the modified polypropylene wax emulsion is obtained under the alkali neutralization condition. The molecular weight of the modified polypropylene wax emulsion is 10000-70000, preferably 30000-50000; the particle size of the emulsion particles is 0.1-4 um, preferably 2-3 um.
The solid mass of the film forming agent accounts for 55-85% of the solid mass of the impregnating compound, preferably 60-80%, more preferably 63-78%, and even more preferably 67-75%. The proportion of the film forming agent is over 85 percent, the bundling property of the glass fiber is too good, so that the glass fiber is not easy to disperse in the using process, the combination with resin is influenced, and the final mechanical property is reduced; and too low proportion of the film forming agent can lead to insufficient protection of the glass fiber and increase hairiness in the using process.
The water used in the present invention is deionized water.
The proportion of the coupling agent component and the film forming agent component of the glass fiber sizing agent plays a key role in the final product performance. To achieve a good impregnation state at ultra high speeds, a suitable film former ratio must be selected, and a coupling agent ratio must be matched therewith, so as to achieve a good reaction between the film former and the coupling agent during film formation, and to minimize self-polymerization components of the coupling agent, so as to achieve an optimal performance state.
According to a second aspect of the present invention, there is provided a method for preparing the glass fiber sizing agent for reinforced polypropylene, comprising the following steps:
1S: adding water accounting for 30-40% of the total amount of the impregnating compound into a container, then adding a coupling agent, and stirring for 20-30 minutes;
2S: diluting the lubricant with water 2-5 times of the mass of the lubricant, and adding the diluted lubricant into a container; wherein the water temperature is 50-60 ℃.
3S: diluting the film forming agent by using water with the mass being 3-5 times that of the film forming agent, and then adding the diluted film forming agent into a container; and (3) complementing the balance of water, uniformly stirring, and detecting the solid content to obtain the glass fiber impregnating compound for reinforcing the polypropylene.
According to a third aspect of the present invention, there is provided the use of the sizing as described above in a very high speed LFT fiberglass reinforced composite article.
Compared with the prior art, the impregnating compound system disclosed by the invention can obtain lower combustible content by limiting the content of the film forming agent in the impregnating compound and the proportion of the corresponding coupling agent, so that the dispersion of glass fibers is facilitated, and the interface combination in resin is facilitated to be completed more quickly. The film forming agent is used as a main component in an impregnating compound system, and the selection of the type and the proportion control are crucial; the proper type of the film forming agent and the lower content of the film forming agent not only influence whether the glass fiber can be rapidly dispersed in the resin, but also influence whether the glass fiber and the polypropylene resin have better interface compatibility, and the infiltration system has better reaction activity and higher impregnation speed in the process of the ultra-high-speed LFT process by optimizing the proportion of the coupling agent and the film forming agent, so that the use effect of the infiltration system is better; in the LFT production process, the method is suitable for impregnation under rapid production conditions, and can rapidly improve the LFT production efficiency.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments of the present invention, and it is obvious that the described embodiments are some but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. It should be noted that the embodiments and features of the embodiments in the present application may be arbitrarily combined with each other without conflict.
The glass fiber impregnating compound for reinforcing polypropylene comprises a coupling agent, a film-forming agent, a lubricant and water, wherein the solid mass of the impregnating compound accounts for 2-3% of the total mass of the impregnating compound;
the impregnating compound comprises the following components in percentage by mass of solid mass to solid mass of the impregnating compound: 10-25% of a coupling agent, 5-20% of a lubricant and 55-85% of a film forming agent;
preferably, 13-22% of coupling agent, 7-18% of lubricant and 60-80% of film forming agent;
further preferably, the coupling agent is 15-20%, the lubricant is 10-17%, and the film forming agent is 63-78%.
Further preferably, the coupling agent is 16-18%, the lubricant is 12-15%, and the film forming agent is 67-75%.
Wherein the content of the first and second substances,
the film forming agent is modified polypropylene wax emulsion grafted by maleic acid rods; the molecular weight is 10000-70000, preferably 30000-50000; the particle size of the emulsion particles is 0.1-4 um, preferably 2-3 um.
The lubricant is a composition of PE wax emulsion and silicone oil type demoulding lubricant; the mass ratio of the PE wax emulsion to the silicone oil demoulding lubricant is 1-3: 1, preferably 1.2-1.8: 1.
the coupling agent is an aminosilane coupling agent;
the water is deionized water.
The preparation method of the glass fiber impregnating compound for the reinforced polypropylene comprises the following steps:
1S: adding water accounting for 30-40% of the total amount of the impregnating compound into a container, then adding a coupling agent, and stirring for 20-30 minutes;
2S: diluting the lubricant with water 2-5 times of the mass of the lubricant, and adding the diluted lubricant into a container; wherein the water temperature is 50-60 ℃.
3S: diluting the film forming agent by using water with the mass being 3-5 times that of the film forming agent, and then adding the diluted film forming agent into a container; and (3) complementing the balance of water, uniformly stirring, and detecting the solid content to obtain the glass fiber impregnating compound for reinforcing the polypropylene.
Some specific examples of the glass fiber sizing for polypropylene reinforcement of the present application are listed below.
Examples
Table 1 shows specific examples of the content of each component in a part of the impregnating agent, and the corresponding value of each component is mass percent/%. The solid content of the impregnating compound is theoretically designed to be 2-3%, the balance is deionized water, and the proportion of the components is the proportion of the effective solid content of each component in the impregnating compound (namely the mass of the solid).
Wherein, the coupling agent is aminosilane coupling agent, and the American Dow Corning company Z-6020.
The lubricant is selected from the group consisting of PE wax emulsion and silicone oil type release lubricant, D313 from DIC of Japan and Dow290 from Dow Corning of America.
The film forming agent is selected from modified PP wax emulsion, Jushi group ltd, TX 170B.
TABLE 1 wetting agent example List
Test example
In order to further embody the beneficial effects of the invention, the impregnating compound with different formula combinations is adopted as a comparative example, and the performance of the products of the example and the comparative example is compared and tested.
Comparative example 1 formulation:
coupling agent: aminosilane coupling agent, a1120, 15% of the american meyer diagram;
lubricant: modified mineral oils, kekai 7607, 15%;
film-forming agent: high molecular weight PP wax emulsion, Meketham 91735, 70%;
comparative example 2 formulation:
coupling agent: aminosilane coupling, dow corning a1100, 20%;
lubricant: PEG lubricant, Kekai 2658A, 18%.
Film-forming agent: the molecular weight of the modified PP wax emulsion is 1-2 ten thousand, 28640 and 62 percent of Meeketon company in America;
table 2 shows the specific component formulations of comparative examples 3-6.
Table 2 comparative examples with different content ratios
Table 3 shows the results of the performance tests for each of the examples and comparative examples. Wherein the dipping effect is the dipping effect of using the LFT-G process at the speed of 70m/min, and the test of the tensile strength adopts the ISO527 standard.
Table 3 comparative test results for article properties
From the comparison of the formula test examples, including the selection of different types of raw material grades and different proportion ratios, we can see that the application change of the formula on the LFT reinforced PP twistless roving product has influence on the service performance, and through the proper improvement of the lubricant ratio, the hairiness is obviously reduced, and the dispersibility is also improved; during the melting process of the glass fiber and resin, the glass fiber can be rapidly dispersed, but the proportion of the lubricant is too high, so that the performance is influenced to a certain extent, and the proportion optimization of the two lubricants is helpful for balancing the dispersion and impregnation effects of the product. In addition, the proportion of the coupling agent also has certain influence on the impregnation of the product, the coupling agent with proper proportion can also rapidly improve the mechanical property of the product, namely, the LFT process can adapt to a manufacturing process at ultra-high speed (70m/min), the production efficiency is effectively improved, the combination of glass fibers and resin is not facilitated due to too low proportion of the coupling agent, the mechanical property is obviously reduced, the self-aggregation of part of the coupling agent is caused due to too high proportion of the coupling agent, the glass fibers are easy to embrittle, the hairiness is obviously increased, and the mechanical property is obviously reduced. Wherein, each index of the embodiment 5 meets the design requirement, the hairiness is lower than 50mg/kg, the impregnation property is good by using the LFT process under the speed of 70 meters, and the comprehensive mechanical property is highest.
According to the technical characteristics of the LFT process, the alkali-free glass fiber direct yarn product meeting the requirements of high-end customers is produced by selecting raw materials, optimizing the proportion of formula components and adopting a proper and mature glass fiber production process. The products produced by the impregnating compound can complete excellent impregnation effect under the production condition of ultra high speed (namely the production speed per minute is more than 70 meters); the product has good dispersibility and excellent interface bonding property with resin by surface treatment of the impregnating compound, and can be rapidly melted with polypropylene resin at ultrahigh speed.
The above-described aspects may be implemented individually or in various combinations, and such variations are within the scope of the present invention.
Finally, it should be noted that: the above examples are only for illustrating the technical solutions of the present invention, and are not limited thereto. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. The glass fiber impregnating compound for reinforcing polypropylene is characterized by comprising a coupling agent, a film forming agent, a lubricant and water, wherein the solid mass of the impregnating compound accounts for 2-3% of the total mass of the impregnating compound;
the amount of each component in the impregnating compound is represented by the following solid mass percentage of the impregnating compound:
10 to 25 percent of coupling agent
5 to 20 percent of lubricant
55-85% of a film forming agent;
wherein the film forming agent is modified polypropylene wax emulsion; the lubricant is a composition of PE wax emulsion and silicone oil type demoulding lubricant; the mass ratio of the PE wax emulsion to the silicone oil demoulding lubricant is 1-3: 1;
the film forming agent is maleic acid rod grafted modified polypropylene wax emulsion, the molecular weight of the emulsion is 10000-70000, and the particle size of emulsion particles is 0.1-4 um;
the coupling agent is an aminosilane coupling agent.
2. The glass fiber sizing agent for reinforced polypropylene according to claim 1, wherein the molecular weight of the modified polypropylene wax emulsion is 30000 to 50000.
3. The glass fiber sizing agent for reinforced polypropylene according to claim 1, wherein the mass ratio of the PE wax emulsion to the silicone oil type release lubricant is 1.2-1.8: 1.
4. the glass fiber sizing agent for reinforced polypropylene according to claim 1, wherein the amounts of the components in the sizing agent are expressed as the following percentages of the solid mass of the components in the sizing agent:
13 to 22 percent of coupling agent
7 to 18 percent of lubricant
60-80% of film forming agent.
5. The glass fiber sizing for reinforced polypropylene according to claim 4, wherein the amounts of the components in the sizing are expressed as the following percentages of the solid mass of the sizing to the solid mass of the sizing:
15-20% of coupling agent
10 to 17 percent of lubricant
63-78% of a film forming agent.
6. A method for preparing the glass fiber impregnating compound for the reinforced polypropylene according to any one of claims 1 to 5, characterized by comprising the following steps:
1S: adding water accounting for 30-40% of the total amount of the impregnating compound into a container, then adding a coupling agent, and stirring for 20-30 minutes;
2S: diluting the lubricant with water 2-5 times of the mass of the lubricant, and adding the diluted lubricant into the container;
3S: diluting the film forming agent by using water with the mass of 3-5 times of that of the film forming agent, and then adding the diluted film forming agent into the container; and (3) complementing the balance of water, uniformly stirring, and detecting the solid content to obtain the glass fiber impregnating compound for the reinforced polypropylene.
7. Use of the glass fiber sizing for reinforced polypropylene according to any one of claims 1 to 5 in ultra high speed LFT glass fiber reinforced composite articles.
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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 |
| CN114507400B (en) * | 2020-10-27 | 2023-12-08 | 合肥杰事杰新材料股份有限公司 | Modified glass fiber reinforced polypropylene composition and preparation method 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 |
| 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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