CN108996923B - High-impregnation alkali-free glass fiber impregnating compound for LFT (Long fiber reinforced thermoplastic) reinforced polypropylene and application thereof - Google Patents
High-impregnation alkali-free glass fiber impregnating compound for LFT (Long fiber reinforced thermoplastic) reinforced polypropylene and application thereof Download PDFInfo
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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
- C03C25/42—Coatings containing inorganic materials
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- Surface Treatment Of Glass Fibres Or Filaments (AREA)
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Abstract
The impregnating compound comprises a pH value regulator, a silane coupling agent, a film forming agent A, a film forming agent B, a lubricant, a surfactant, an antioxidant and deionized water, wherein the film forming agent A is a maleic anhydride graft modified polypropylene wax emulsion, the film forming agent B is a maleic anhydride graft modified polyethylene emulsion, the lubricant is a combination of a PEG lubricant and a mineral oil lubricant, the surfactant is a combination of a microcrystalline wax emulsion and a cationic polyacrylamide emulsion, and the antioxidant is hypophosphite. The invention also provides the application of the impregnating compound in the production of alkali-free glass fiber for LFT reinforced polypropylene, the glass fiber produced by the impregnating compound has good interface binding property, can be quickly compatible with polypropylene resin at high temperature, has high impregnation speed, good manufacturability, good wear resistance, less hairiness and high impregnation property, thereby improving the production efficiency and reducing the production cost.
Description
(I) technical field
The invention relates to a sizing agent, in particular to development and application of a novel glass fiber sizing agent for long fiber reinforced polypropylene with high impregnation property.
(II) background of the invention
With the continuous deepening of the environmental protection concept, the proportion of thermoplastic materials in composite materials is gradually improved, particularly, the novel reinforced materials mainly comprising long fiber reinforced thermoplastic resin have the advantages of rapid development speed and wide application field, and are widely applied to the automobile industry, the aerospace industry, the building material industry and the like by virtue of light weight, low price, corrosion resistance, easy recycling, excellent mechanical properties and the like. Long fiber reinforced thermoplastics (LFTs), which have a long fiber retention length compared to conventional fiber reinforced thermoplastics, are now processed to maintain fiber lengths in LFTs above 5 mm. By using the LFT process, the adopted matrix resin comprises PP, PA, PBT, PPS, SAN and other resins, and different fibers are needed to be used for different resins to achieve a better effect.
The LFT reinforced material processing technology needs to fuse continuous glass fiber with polypropylene resin through a die, impregnating at high temperature, cutting into granules, and performing later injection molding and compression molding, wherein, the impregnation effect of the LFT material particles not only affects the mechanical property of the final product, but also has important influence on the manufacturability and smoothness of the subsequent production, therefore, the development of the yarn for the LFT reinforced polypropylene with high impregnation property has certain market potential, but the glass fiber is surface treated and has certain banding property, when the resin is combined, great tension needs to be added, and the full impregnation is difficult to achieve in an extremely short time, so that a plurality of manufacturers on the market have to sacrifice the production speed to ensure the impregnation effect for completing the impregnation, this causes low efficiency in actual production and puts high demands on the technological service performance of the product.
In order to solve the problem of the impregnation speed of the glass fibers and the resin and improve the production efficiency, a novel glass fiber impregnating compound for reinforcing the polypropylene resin needs to be developed, so that the glass fibers and the polypropylene resin have good compatibility, and the effect of interface combination is improved to meet the requirements of good impregnation effect and high-efficiency production.
Disclosure of the invention
The invention aims to solve the technical problem of providing a novel impregnating compound and application thereof in producing alkali-free glass fibers for LFT reinforced polypropylene, wherein a glass fiber product produced by the impregnating compound has good interface binding property, can be quickly compatible with polypropylene resin at high temperature, has high impregnation speed, good manufacturability, good wear resistance, less hairiness, wide production process range and high impregnation property, and is convenient for reaching higher glass fiber content, so that the production efficiency of customers can be improved, the production cost is reduced, and the maximum economic benefit is created for the customers.
In order to solve the technical problems and achieve an ideal production effect, the invention adopts the following technical scheme:
the impregnating compound comprises a pH value regulator, a coupling agent, a film forming agent A, a film forming agent B, a lubricant, a surfactant, an antioxidant and deionized water, wherein the solid mass of the impregnating compound accounts for 3% -8% of the total mass of the impregnating compound, the coupling agent is a silane coupling agent, the film forming agent A is a maleic anhydride graft modified polypropylene wax emulsion, the film forming agent B is a maleic anhydride graft modified polyethylene emulsion, the lubricant is the combination of a PEG lubricant and a mineral oil lubricant, the surfactant is the combination of a microcrystalline wax emulsion and a cationic polyacrylamide emulsion, the antioxidant is a hypophosphite, and the pH value regulator is an acid; the content of each component in the impregnating compound is represented as follows by the mass amount of the component occupying the solid mass of the impregnating compound, wherein the mass amounts of the film forming agent A, the film forming agent B, the surfactant and the lubricant are calculated by the solid mass of the components:
the impregnating compound is preferably prepared from a pH value regulator, a coupling agent, a film forming agent A, a film forming agent B, a lubricant, a surfactant, an antioxidant and deionized water.
The coupling agent of the present invention generally adopts silane coupling agents with vinyl or amino groups, and the silane coupling agents suitable for the present invention can be selected from A1100, A1120, A-174, etc. The use of the coupling agent and the hydrolyzed reactive group can play a role in bridging the combination of the glass fibers and the polypropylene resin, can better improve the compatibility of the film forming agent and the resin, and greatly improve the use performance of glass fiber products, so that the use of the coupling agent is an important factor influencing the rapid impregnation of the glass fibers, and plays a key role in the impregnation effect of the later use process. The content of the silane coupling agent in the invention is 13-27%, preferably 14-25%, more preferably 15-22%, and still more preferably 17-20%.
The lubricant used by the invention can use water-soluble organic compounds, and the use of a lubricating system can play a good role in protecting glass fibers and protect the glass fibers from being damaged in the production and use processes, so the lubricant is a main influence factor of the product in the aspects of manufacturability and usability, and the reasonable selection of the lubricating system is beneficial to improving the use smoothness of the LFT reinforced polypropylene yarn and improving the production efficiency of the glass fibers in the use process, but the excessive use of the lubricant influences the subsequent product impregnation effect, so the proper proportion needs to be controlled. The lubricating system is formed by compounding two lubricants, namely PEG and mineral oil, the total content of the lubricants is preferably 2-15%, preferably 2-14%, more preferably 5-12%, and even more preferably 7-10%, and the mass ratio of the PEG lubricant to the mineral oil lubricant is controlled to be 3-1: 1 in terms of the mass ratio of respective solids.
The surfactant used in the present invention is a combination of a microcrystalline wax emulsion and a cationic polyacrylamide emulsion. The content of the surfactant adopted by the invention is 1-5%, preferably 1.5-4.5%, more preferably 2-4%, and still more preferably 2-3%. Wherein the mass ratio of the microcrystalline wax emulsion to the cationic polyacrylamide emulsion is controlled to be 10-1: 1 in terms of the mass ratio of respective solids.
The film forming agent used by the invention consists of a film forming agent A and a film forming agent B, and the film forming agent is used as a main component of an impregnating compound system, is a key for influencing the service performance of glass fibers, mainly plays a role in protecting the banding property of tows, providing a reaction carrier for the glass fibers and providing excellent impregnation effect and mechanical performance, so that the selection and proportion of the film forming agent are the key points of the impregnating compound, and the compatibility with target resin (polypropylene) and the reaction and compatibility speed with the resin are mainly considered. The film forming agent A is modified polypropylene wax emulsion obtained by grafting maleic anhydride and under the alkali neutralization condition, the selected molecular weight of the modified polypropylene wax emulsion is 3-10 ten thousand, preferably 5-7 ten thousand, and the particle size of emulsion particles is 5-20 um; the content of the film forming agent A in the impregnating compound is 30-80%, preferably 40-75%, more preferably 50-70%, and still more preferably 55-60%. The film forming agent B is a maleic anhydride graft modified polyethylene emulsion, the molecular weight is 1-5 ten thousand, preferably 2-3 ten thousand, and the particle size of emulsion particles is 1-10 um; the emulsifier is anionic or nonionic, and the content of the film-forming agent B in the impregnating compound is 1-30%, preferably 5-30%, more preferably 6-25%, and still more preferably 8-15%. Meanwhile, the mass ratio of the film forming agent A to the film forming agent B in the impregnating compound is controlled to be 4-1: 1 by the mass ratio of the respective solid. The modified polypropylene wax emulsion can provide a good reaction carrier for glass fibers; the modified polyethylene can provide a certain crosslinking effect for the glass fibers and better bundling property on the one hand, and can accelerate the reaction activity of the polypropylene wax on the other hand, so that the modified polypropylene wax emulsion and the modified polyethylene emulsion are matched for use, the yarn has good dispersibility and manufacturability, and the glass fibers can be applied under high-speed production conditions.
The pH value regulator of the invention adopts acid, which can be acetic acid, formic acid, citric acid and the like, and acetic acid is preferably adopted. The pH value regulator is mainly used for assisting the dispersion of the coupling agent and regulating the pH value of the prepared impregnating compound, and the pH value of the impregnating compound is controlled to be 4-9, preferably 5-8.
The antioxidant used in the invention is hypophosphite, and the use of the antioxidant can avoid the oxidative modification of the polypropylene modified wax emulsion under the high-temperature baking condition, thereby improving the problem of yellowing caused by over-baking oxidation. The antioxidant used in the present invention is preferably sodium hypophosphite. The content of the antioxidant in the invention is 1-5%, preferably 1-4%, more preferably 1-3%, and still more preferably 1-2%.
Preferably, the content ratio of each component of the impregnating compound is as follows:
pH value regulator: 1.5 to 4.5 percent
Coupling agent: 14 to 25 percent
Lubricant: 2 to 14 percent
Film-forming agent A: 40 to 75 percent
Film-forming agent B: 5 to 30 percent
Surfactant (b): 1.5 to 4.5 percent
Antioxidant: 1 to 4 percent.
Further preferably, the content ratio of each component of the impregnating compound is as follows:
pH value regulator: 1.5 to 4 percent
Coupling agent: 15 to 22 percent
Lubricant: 5 to 12 percent
Film-forming agent A: 50 to 70 percent
Film-forming agent B: 6 to 25 percent
Surfactant (b): 2 to 4 percent
Antioxidant: 1 to 3 percent.
More preferably, the content ratio of each component of the impregnating compound is as follows:
pH value regulator: 2 to 3 percent of
Coupling agent: 17 to 20 percent
Lubricant: 7 to 10 percent
Film-forming agent A: 55 to 60 percent
Film-forming agent B: 8 to 15 percent
Surfactant (b): 2 to 3 percent of
Antioxidant: 1 to 2 percent.
The preparation method of the impregnating compound comprises the following steps: adding deionized water accounting for 30-40% of the total weight of the impregnating compound into a clean container, then adding a pH value regulator in the impregnating compound, fully stirring for 3-5 minutes, then slowly adding a silane coupling agent in the impregnating compound, and continuously stirring for 30 minutes; fully stirring and diluting a lubricant and a surfactant in the components of the impregnating compound in warm deionized water (40-50 ℃) with the mass of 3-5 times of that of the impregnating compound, and adding the mixture into a container; diluting a film forming agent in the components of the impregnating compound by using deionized water with the mass 2-3 times that of the film forming agent, and adding the diluted film forming agent into a container; uniformly stirring an antioxidant in the impregnating compound in hot deionized water (70-90%) which is 5-7 times of the weight of the antioxidant, cooling to room temperature, and adding the antioxidant into a container; and then detecting the pH value, if the pH value cannot reach the optimal range, supplementing a proper amount of pH regulator for adjustment, uniformly stirring, and retesting until the pH value is in the optimal range.
The invention also provides application of the impregnating compound in producing alkali-free glass fibers for LFT reinforced polypropylene.
The combustible content (LOI) of the glass fiber is generally controlled to be 0.2-0.7, preferably 0.3-0.5, and the preferred scheme is a theoretical reference value designed for achieving satisfactory mechanical strength from the aspects of physical and mechanical properties required by products.
Compared with the prior art, the impregnating compound system disclosed by the invention has better interface compatibility with polypropylene resin, better reaction activity, higher impregnation speed and better effect, is suitable for production conditions at a higher speed in an LFT production process, and can be used for rapidly improving the LFT production efficiency.
(IV) detailed description of the preferred embodiments
The following are descriptions of specific formulations and experimental methods, but the present disclosure is not limited to the following examples.
The impregnating compound used in the embodiment of the invention comprises the following components:
the coupling agent is amino silane coupling agent, and the product is A1100 of the Meiji chart.
The lubricant selects PEG400 and modified mineral oil, the compounding ratio is 2:1 in terms of solid mass ratio, and the product brands are Kekei 2640 and STANTEX G7607.
The film forming agent A is maleic anhydride modified PP wax emulsion, and the product brand is American michelma NM 91735. S-OP.
The film forming agent B is maleic anhydride modified polyethylene, and the product brand is Emulsion 29730.
The selected surfactants are microcrystalline wax emulsion and polyacrylamide emulsion, the compounding ratio is 5:1 in terms of solid mass ratio, and Bayer ML723 and 6760L are selected.
The selected antioxidant and pH value regulator are sodium hypophosphite and acetic acid, which are common raw materials in the market.
The glass fiber preparation process is the production of an alkali-free glass fiber porcelain kiln wire drawing production line, the single-bottom bushing plate adopts 4000H cluster wire drawing, and the linear density of the glass fiber is 2400 tex. The applied composite material preparation process is an LFT-G process, the content of used glass fiber is 50%, the production speed is 60m/min, the used reinforced resin is polypropylene resin, the manufacturer is Korea SK, the brand is BX3900, the component of the compatilizer is 4%, the manufacturer of the compatilizer is Polyram, and the model is BONDYRAM 1001.
Referring to table 1, in order to achieve high impregnation performance and meet better process performance in these examples, different film-forming agent ratios and lubrication ratios are selected as experimental objects for adjustment, the solid content of the impregnating compound is theoretically designed to be 4-6%, and the balance is deionized water, wherein the following component ratios account for the effective solid content (i.e., solid mass) of the effective components in the impregnating compound.
Watch 1
From the comparison of the formula test examples, we can see that, through comparison of the comparative ratio, the formula disclosed by the invention can be applied to an LFT reinforced PP twistless roving product, the bundling state of yarn bundles can be effectively protected, hairiness is reduced, and in an LFT process, the formula can adapt to a manufacturing process of using LFT-G at a high speed (60m/min), and the production efficiency is effectively improved. Wherein, the indexes of the examples 2-4 meet the design requirements, the hairiness is lower than 30mg/kg, the impregnation property is good when the LFT-G is used at the speed of 60 meters, but the proportion still has a further optimization space through the design of the components and the component content.
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 mature glass fiber production process.
Claims (11)
1. The impregnating compound comprises a pH value regulator, a coupling agent, a film forming agent A, a film forming agent B, a lubricant, a surfactant, an antioxidant and deionized water, wherein the solid mass of the impregnating compound accounts for 3-8% of the total mass of the impregnating compound, the coupling agent is a silane coupling agent, the film forming agent A is a maleic anhydride graft modified polypropylene wax emulsion, the film forming agent B is a maleic anhydride graft modified polyethylene emulsion, the lubricant is a combination of a PEG lubricant and a mineral oil lubricant, the surfactant is a combination of a microcrystalline wax emulsion and a cationic polyacrylamide emulsion, the antioxidant is a hypophosphite, and the pH value regulator is an acid; the content of each component in the impregnating compound is represented as follows by the mass amount accounting for the solid mass of the impregnating compound, wherein the mass amounts of the film forming agent, the surfactant and the lubricant are calculated by the solid mass:
pH value regulator: 1 to 5 percent
Coupling agent: 17 to 27 percent
Lubricant: 2 to 15 percent
Film-forming agent A: 30 to 80 percent
Film-forming agent B: 1 to 30 percent
Surfactant (b): 1 to 5 percent
Antioxidant: 1 to 5 percent.
2. An impregnating compound as defined in claim 1, wherein: the impregnating compound is prepared from a pH value regulator, a coupling agent, a film forming agent A, a film forming agent B, a lubricating agent, a surfactant, an antioxidant and deionized water.
3. An impregnating compound as defined in claim 1, wherein: the impregnating compound comprises the following components in percentage by weight:
pH value regulator: 1.5 to 4.5 percent
Coupling agent: 17 to 25 percent
Lubricant: 2 to 14 percent
Film-forming agent A: 40 to 75 percent
Film-forming agent B: 5 to 30 percent
Surfactant (b): 1.5 to 4.5 percent
Antioxidant: 1 to 4 percent.
4. An impregnating compound as defined in claim 3, wherein: the impregnating compound comprises the following components in percentage by weight:
pH value regulator: 1.5 to 4 percent
Coupling agent: 17 to 22 percent
Lubricant: 5 to 12 percent
Film-forming agent A: 50 to 70 percent
Film-forming agent B: 6 to 25 percent
Surfactant (b): 2 to 4 percent
Antioxidant: 1 to 3 percent.
5. An impregnating compound as defined in claim 4, wherein: the impregnating compound comprises the following components in percentage by weight:
pH value regulator: 2 to 3 percent of
Coupling agent: 17 to 20 percent
Lubricant: 7 to 10 percent
Film-forming agent A: 55 to 60 percent
Film-forming agent B: 8 to 15 percent
Surfactant (b): 2 to 3 percent of
Antioxidant: 1 to 2 percent.
6. An impregnating agent according to any one of claims 1 to 5, wherein: the coupling agent adopts silane coupling agent with vinyl or amino.
7. An impregnating agent according to any one of claims 1 to 5, wherein: in the lubricant, the mass ratio of the PEG lubricant to the mineral oil lubricant is controlled to be 3-1: 1 in terms of the mass ratio of the respective solids.
8. An impregnating agent according to any one of claims 1 to 5, wherein: in the surfactant, the mass ratio of the microcrystalline wax emulsion to the cationic polyacrylamide emulsion is controlled to be 10-1: 1 in terms of the mass ratio of respective solids.
9. An impregnating agent according to any one of claims 1 to 5, wherein: the molecular weight of the maleic acid rod graft modified polypropylene wax emulsion is 3-10 ten thousand; the molecular weight of the maleic anhydride grafted and modified polyethylene emulsion is 1-5 ten thousand; the mass ratio of the film forming agent A to the film forming agent B in the impregnating compound is controlled to be 4-1: 1 by the solid mass ratio of the film forming agent A to the film forming agent B.
10. An impregnating compound as defined in claim 9, wherein: the coupling agent adopts silane coupling agent with vinyl or amino; in the lubricant, the mass ratio of the PEG lubricant to the mineral oil lubricant is controlled to be 3-1: 1 in terms of the mass ratio of respective solids; in the surfactant, the mass ratio of the microcrystalline wax emulsion to the cationic polyacrylamide emulsion is controlled to be 10-1: 1 in terms of the mass ratio of respective solids.
11. The use of the sizing of claim 1 in the production of alkali-free glass fibers for LFT-reinforced polypropylene.
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| CN201710421902.6A CN108996923B (en) | 2017-06-07 | 2017-06-07 | High-impregnation alkali-free glass fiber impregnating compound for LFT (Long fiber reinforced thermoplastic) reinforced polypropylene and application thereof |
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| CN111018366A (en) * | 2019-12-20 | 2020-04-17 | 内江华原电子材料有限公司 | Impregnating compound for glass fiber direct roving for LFT (Long fiber reinforced thermoplastic) process and preparation method thereof |
| CN112126123A (en) * | 2020-08-18 | 2020-12-25 | 北京协同创新研究院 | Continuous basalt fiber surface treating agent and preparation method thereof |
| CN112358688B (en) * | 2020-11-23 | 2023-03-14 | 上海金发科技发展有限公司 | Hydrophobic glass fiber reinforced polypropylene compound 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 |
| CN113246426B (en) * | 2021-05-11 | 2022-09-02 | 山东玻纤集团股份有限公司 | Production system and method of glass fiber reinforced composite material |
| CN115849734A (en) * | 2022-12-07 | 2023-03-28 | 巨石集团有限公司 | Glass fiber film forming agent and preparation method and application thereof |
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| CN105401422A (en) * | 2015-11-04 | 2016-03-16 | 巨石集团有限公司 | Impregnating compound and application thereof in production of non-alkali bulked glass fiber yarn |
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| CN105401422A (en) * | 2015-11-04 | 2016-03-16 | 巨石集团有限公司 | Impregnating compound and application thereof in production of non-alkali bulked glass fiber yarn |
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