阅读说明：本技术 一种超细短切玻璃纤维增强聚丙烯共混融纺复合纤维材料及其制备方法 (Superfine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material and preparation method thereof ) 是由 刘津 谢泽金 汪庆卫 施王明 罗理达 于 2021-11-11 设计创作，主要内容包括：本发明公开了一种超细短切玻璃纤维增强聚丙烯共混融纺复合纤维材料,其特征在于,其制成原料包括：超细短切玻璃纤维、聚丙烯、相容剂；及其制备方法,其特征在于,在制备方法中包括熔融纺丝步骤。采用本发明的配方原料和优选制备工艺,可以有效增强复合纤维材料的性能。(The invention discloses an ultrafine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material, which is characterized by comprising the following raw materials: superfine chopped glass fiber, polypropylene and compatilizer; and a preparation method thereof, characterized in that the preparation method comprises a melt spinning step. By adopting the formula raw materials and the optimized preparation process, the performance of the composite fiber material can be effectively enhanced.)

1. The superfine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material is characterized by comprising the following raw materials in parts by weight: 0-5% of superfine chopped glass fiber, 92.5-100% of polypropylene and 0-2.5% of compatilizer.

2. The ultrafine chopped glass fiber reinforced polypropylene blended and melt-spun composite fiber material as claimed in claim 1, wherein the weight ratio of the raw materials is as follows: 1% of superfine chopped glass fiber, 98.5% of polypropylene and 0.5% of compatilizer; or 2% of superfine chopped glass fiber, 97% of polypropylene and 1% of compatilizer; or 3% of superfine chopped glass fiber, 95.5% of polypropylene and 1.5% of compatilizer.

3. The ultrafine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material as claimed in claim 1 or 2, wherein the diameter of the ultrafine chopped glass fiber is below 6 μm, and the length-diameter ratio is 5:1 to 20: 1.

4. The ultrafine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material as claimed in claim 1 or 2, wherein the ultrafine chopped glass fiber is a raw material after being soaked in a silane coupling agent.

5. The ultra fine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material as claimed in claim 1 or 2, wherein the compatibilizer is maleic anhydride grafted polypropylene.

6. The ultrafine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material as claimed in claim 4, wherein the silane coupling agent is KH550 solution.

7. The method for preparing the ultrafine chopped glass fiber reinforced polypropylene blended and melt-spun composite fiber material as claimed in claim 1, wherein the preparation method comprises a melt spinning step.

8. The method for preparing the ultrafine chopped glass fiber reinforced polypropylene blended and melt-spun composite fiber material as claimed in claim 7, wherein the working environment of the melt spinning step is as follows: the pressure of the assembly is 4-9MPa, and the winding speed is 600-1800 m/min.

9. The method for preparing the superfine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material as claimed in claim 7, wherein in the working environment of the melt spinning step, the assembly pressure is 8-9MPa, and the winding speed is 1200 m/min.

10. The method for preparing the ultrafine chopped glass fiber reinforced polypropylene blended and melt-spun composite fiber material as claimed in claim 7, wherein the raw materials required in the melt spinning step are prepared by the following steps: s1, uniformly mixing superfine chopped glass fibers, polypropylene and a compatilizer, and preparing blended particles by an extruder; s2, uniformly mixing the blended particles with polypropylene, and drying to remove surface moisture to obtain the required raw material.

Technical Field

The invention belongs to the field of preparation of high polymer materials, particularly relates to a glass fiber and polypropylene composite material and a preparation method thereof, and particularly relates to an ultrafine chopped glass fiber reinforced polypropylene blended melt spinning composite fiber material and a preparation method thereof.

Background

The chopped glass fiber precursor has good bundling property, low flock content, excellent dry-state fluidity, favorable uniform distribution of glass fibers in products, excellent wet-state dispersibility fluidity, easy resin impregnation and is mainly used for reinforcing thermoplastic plastics. Because of its good cost performance, it is especially suitable for compounding with resin to be used as the reinforcing material of automobile, train and ship shells, and for high-temperature resistant needled felt, automobile sound absorbing sheet, hot-rolled steel material, etc. The product is widely applied to the fields of automobiles, buildings, aviation daily necessities and the like, and typical products comprise automobile accessories, electronic and electric products, mechanical products and the like.

Polypropylene is thermoplastic synthetic resin with excellent performance, has chemical resistance, electrical insulation, high-strength mechanical performance, good high-wear-resistance processing performance and the like, and is widely developed and applied in various fields of machinery, automobiles, electronic appliances, buildings, textiles, packaging, agriculture, forestry, fishery, food industry and the like. Because of their plasticity, composites of polypropylene and other materials are being developed and used in an increasing number of industries.

The traditional preparation method of the glass fiber and polypropylene composite material is generally used for injection molding materials after continuous long glass fiber composite polypropylene is extruded and granulated.

Disclosure of Invention

The invention aims to provide an ultrafine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material and a preparation method thereof.

The invention adopts the following technical scheme:

the superfine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material is characterized by comprising the following raw materials in parts by weight: 0-5% of superfine chopped glass fiber, 92.5-100% of polypropylene and 0-2.5% of compatilizer.

Preferably, the weight ratio of the raw materials is as follows: 1% of superfine chopped glass fiber, 98.5% of polypropylene and 0.5% of compatilizer; or 2% of superfine chopped glass fiber, 97% of polypropylene and 1% of compatilizer; or 3% of superfine chopped glass fiber, 95.5% of polypropylene and 1.5% of compatilizer.

Preferably, the diameter of the superfine chopped glass fiber is less than 6 μm, and the length-diameter ratio is 5:1 to 20: 1.

Preferably, the ultrafine chopped glass fibers are raw materials after being soaked in a silane coupling agent.

Preferably, the compatilizer is maleic anhydride grafted polypropylene.

Preferably, the silane coupling agent is KH550 solution.

The preparation method of the superfine chopped glass fiber reinforced polypropylene blended melt-spun composite fiber material is characterized by comprising a melt spinning step.

Preferably, the working environment of the melt spinning step is as follows: the pressure of the assembly is 4-9MPa, and the winding speed is 600-1800 m/min.

Preferably, in the working environment of the melt spinning step, the pressure of the assembly is 8-9MPa, and the winding speed is 1200 m/min.

Preferably, the preparation method of the raw materials required by the melt spinning step comprises the following steps: s1, uniformly mixing superfine chopped glass fibers, polypropylene and a compatilizer, and preparing blended particles by an extruder; s2, uniformly mixing the blended particles with polypropylene, and drying to remove surface moisture to obtain the required raw material.

By adopting the technical scheme, the invention has the following advantages:

1. the blended particles are prepared first and then mixed with polypropylene to prepare the mixture required by melt spinning, so that the distribution of the superfine chopped glass fibers in the composite fiber material is more uniform.

2. The compatilizer is added in the invention, so that the interfacial compatibility of the superfine chopped glass fiber and the polypropylene in the composite fiber material can be effectively enhanced.

3. The invention adopts the superfine chopped glass fiber, and can effectively enhance the tensile property of the composite fiber material.

4. The superfine chopped glass fiber is soaked by the silane coupling agent, so that the interface compatibility of the superfine chopped glass fiber and polypropylene in the composite fiber material can be effectively enhanced.

5. The fiber composite material is prepared by adopting the melt spinning step, so that the tensile property of the fiber composite material, the internal orientation of the superfine chopped glass fiber in the composite fiber and the interface compatibility can be effectively enhanced.

Drawings

FIG. 1 is a micrograph of an ultra fine chopped glass fiber reinforced polypropylene blended melt spun composite fiber material of example 3.

FIG. 2 is a micrograph of an ultra fine chopped glass fiber reinforced polypropylene blended melt spun composite fiber material of example 8.

FIG. 3 is a micrograph (1.5 k magnification) of an ultra fine chopped glass fiber reinforced polypropylene blended melt spun composite fiber material of example 13.

FIG. 4 is a micrograph (10.0 k magnification) of an ultra fine chopped glass fiber reinforced polypropylene blended melt spun composite fiber material of example 13.

Detailed Description

In order that those skilled in the art will better understand the concepts of the present invention, the invention is further illustrated by the following specific examples.

The method for testing the tensile strength is based on a GB/T14344-2008 chemical fiber filament tensile property test method.

Example 1

Drying continuous glass fibers with the diameter of less than 6 mu m for 2 hours, removing surface moisture, grinding by using a planetary ball mill, and sieving to obtain the aspect ratio of 5:1 to 20: 1.

Weighing 10 wt% of superfine chopped glass fiber, 85 wt% of polypropylene and 5 wt% of maleic anhydride grafted polypropylene, uniformly mixing, drying, and preparing blended particles at 200 ℃ by a double-screw extruder to obtain blended master batch with the weight ratio of the superfine chopped glass fiber of 10%, which is hereinafter referred to as No. 1 blended master batch.

According to the weight percentage, 10% of No. 1 blending master batch and 90% of polypropylene are uniformly mixed to prepare a mixture containing 1% of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture, and then the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material is prepared through a melt spinning machine under the conditions that the melting temperature is 240 ℃, the pressure of a spinneret plate (assembly) is 4.5MPa, the winding speed is 600m/min and the winding time is 10 min.

Example 2

According to the weight percentage, 20% of No. 1 blending master batch and 80% of polypropylene are uniformly mixed to prepare a mixture containing 2% of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture, and then the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material is prepared through a melt spinning machine under the conditions that the melting temperature is 240 ℃, the pressure of a spinneret plate (assembly) is 4.5MPa, the winding speed is 600m/min and the winding time is 10 min.

Example 3

According to the weight percentage, 30% of No. 1 blending master batch and 70% of polypropylene are uniformly mixed to prepare a mixture containing 3% of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture, and then the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material is prepared by a melt spinning machine under the conditions of the melting temperature of 240 ℃, the pressure of a spinneret plate (assembly) of 4.5MPa, the winding speed of 600m/min and the winding time of 10 min.

Example 4

According to the weight percentage, 40% of No. 1 blending master batch and 60% of polypropylene are uniformly mixed to prepare a mixture containing 4% of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture, and then the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material is prepared through a melt spinning machine under the conditions that the melting temperature is 240 ℃, the pressure of a spinneret plate (assembly) is 4.5MPa, the winding speed is 600m/min and the winding time is 10 min.

Example 5

According to the weight percentage, 50% of No. 1 blending master batch and 50% of polypropylene are uniformly mixed to prepare a mixture containing 5% of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture, and then the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material is prepared through a melt spinning machine under the conditions that the melting temperature is 240 ℃, the pressure of a spinneret plate (assembly) is 4.5MPa, the winding speed is 600m/min and the winding time is 10 min.

Comparative example 1

Drying continuous glass fibers with the diameter of below 6 mu m for 2 hours, removing surface moisture, milling for a certain time by using a planetary ball mill, and sieving to obtain a product with the length-diameter ratio of 5:1 to 20: 1.

Weighing 10 wt% of superfine chopped glass fiber and 90 wt% of polypropylene, uniformly mixing, drying, and preparing blended particles at 200 ℃ by a double-screw extruder to obtain No. 2 blended master batch with 10 wt% of superfine chopped glass fiber.

According to the weight percentage, 10 percent of No. 2 blending master batch and 90 percent of polypropylene are uniformly mixed to prepare a mixture containing 1 percent of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture, and then the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material is prepared by a melt spinning machine under the conditions of the melting temperature of 240 ℃, the pressure of a spinneret plate (component) of 4.5MPa, the winding speed of 600m/min and the winding time of 10 min.

Comparative example 2

Pure polypropylene is subjected to conventional melt spinning parameters: the melting temperature of the melt spinning machine is 130 ℃, the pressure of a spinneret plate (component) is 4.5MPa, the winding speed is 600m/min, and the winding time is 10min, so that the pure polypropylene fiber is prepared by spinning.

The fiber material formulations, preparation process parameters, preparation process defects (yarn breakage) and tensile strength property test results obtained in examples 1 to 5 and comparative examples 1 to 2 are shown in Table 1 below:

TABLE 1

	Example 1	Example 2	Example 3	Example 4	Example 5	Comparative example 1	Comparative example 2
								Wt% of polypropylene	98.5	97	95.5	94	92.5	99	100
Ultra-fine chopped glass fiber wt%	1	2	3	4	5	1	0
								Maleic anhydride grafted Polypropylene wt%	0.5	1	1.5	2	2.5	0	0
Pressure of assembly MPa	4.5	4.5	4.5	4.5	4.5	4.5	4.5
								Winding speed m/min	600	600	600	600	600	600	600
Number of times of filament breakage	0	1	0	2	11	5	0
								Tensile strength cn/dtex	2.47	2.61	2.63	2.24	1.77	1.84	2.20
Tensile strength MPa	220.40	235.57	240.08	206.79	165.22	164.99	194.04

Analysis of the performance test results of the examples shows that when the content of the ultrafine chopped glass fibers is 3%, the tensile strength of the prepared composite fiber reaches an extreme value, and then an orthogonal experiment is used for observing whether the composite fiber has better tensile strength by changing two process parameters of the pressure and the winding speed of the spinneret plate (assembly) in the examples 6 to 10.

Example 6

According to the weight percentage, 30 percent of No. 1 blending master batch and 70 percent of polypropylene are uniformly mixed to prepare a mixture containing 3 percent of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture and then is passed through a melt spinning machine to prepare the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material under the conditions of the melting temperature of 240 ℃, the pressure of a spinneret plate (component) of 6.5MPa, the winding speed of 600m/min and the winding time of 10 min.

Example 7

According to the weight percentage, 30 percent of No. 1 blending master batch and 70 percent of polypropylene are uniformly mixed to prepare a mixture containing 3 percent of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture and then is passed through a melt spinning machine to prepare the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material under the conditions of the melting temperature of 240 ℃, the pressure of a spinneret plate (component) of 8.5MPa, the winding speed of 600m/min and the winding time of 10 min.

Example 8

According to the weight percentage, 30 percent of No. 1 blending master batch and 70 percent of polypropylene are uniformly mixed to prepare a mixture containing 3 percent of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture and then is passed through a melt spinning machine to prepare the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material under the conditions of the melting temperature of 240 ℃, the pressure of a spinneret plate (component) of 8.5MPa, the winding speed of 1200m/min and the winding time of 10 min.

Example 9

According to the weight percentage, 30 percent of No. 1 blending master batch and 70 percent of polypropylene are uniformly mixed to prepare a mixture containing 3 percent of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture and then is passed through a melt spinning machine to prepare the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material under the conditions of the melting temperature of 240 ℃, the pressure of a spinneret plate (component) of 8.5MPa, the winding speed of 1800m/min and the winding time of 10 min.

Example 10

According to the weight percentage, 50% of No. 1 blending master batch and 50% of polypropylene are uniformly mixed to prepare a mixture containing 5% of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture and then is passed through a melt spinning machine to prepare the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material under the conditions of melting temperature of 240 ℃, spinneret plate (component) pressure of 8.5MPa, winding speed of 1200m/min and winding time of 10 min.

The fiber material formulations, preparation process parameters, preparation process defects (filament breakage times) and tensile strength property test results obtained in examples 6 to 10 are shown in Table 2 below:

TABLE 2

	Example 6	Example 7	Example 8	Example 9	Example 10
						The polypropylene content wt%	95.5	95.5	95.5	95.5	92.5
Content wt% of superfine chopped glass fiber	3	3	3	3	5
						Maleic anhydride grafted Polypropylene content wt%	1.5	1.5	1.5	1.5	2.5
Pressure of assembly MPa	6.5	8.5	8.5	8.5	8.5
						Winding speed m/min	600	600	1200	1800	1200
Number of times of filament breakage	0	2	0	3	1
						Tensile strength cn/dtex	2.69	2.94	3.15	2.57	2.36
Tensile strength MPa	245.56	268.38	287.55	234.60	220.29

The data comparison of the examples shows that the tensile property is optimal when the pressure of the assembly is 8.5Mpa, and the tensile property is optimal when the winding speed is 1200m/min, and meanwhile, the data comparison of fig. 1 and fig. 2 shows that the microscopic pictures of the fiber composite materials of the examples 3 and 8 respectively show that after the melt spinning process, the distribution orientation and the interface compatibility of the superfine chopped glass fiber in the composite fiber are improved. Next, it was examined whether or not the examples 11 to 13 were improved in tensile strength by the addition of the silane coupling agent KH550 in the orthogonal test.

Example 11

Drying continuous glass fibers with the diameter of below 6 mu m for 2 hours, removing surface moisture, milling for a certain time by using a planetary ball mill, and sieving to obtain a product with the length-diameter ratio of 5: 1-20: 1, soaking the superfine chopped glass fiber in a silane coupling agent KH550 with the mass fraction of 2% (namely the mass ratio of the superfine chopped glass fiber to the KH550 is 98: 2) for 2 hours, and then drying for 3 hours.

Weighing 10 wt% of superfine chopped glass fiber, 85 wt% of polypropylene and 5 wt% of maleic anhydride grafted polypropylene, uniformly mixing, drying, and preparing blended particles at 200 ℃ by a double-screw extruder to obtain No. 3 blended master batch with 10 wt% of superfine chopped glass fiber.

According to the weight percentage, 10 percent of No. 3 blending master batch and 90 percent of polypropylene are uniformly mixed to prepare a mixture containing 1 percent of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture and then is passed through a melt spinning machine to prepare the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material under the conditions of the melting temperature of 240 ℃, the pressure of a spinneret plate (component) of 8.5MPa, the winding speed of 1200m/min and the winding time of 10 min.

Example 12

According to the weight percentage, 20 percent of No. 3 blending master batch and 80 percent of polypropylene are uniformly mixed to prepare a mixture containing 2 percent of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture and then is passed through a melt spinning machine to prepare the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material under the conditions of the melting temperature of 240 ℃, the pressure of a spinneret plate (component) of 8.5MPa, the winding speed of 1200m/min and the winding time of 10 min.

Example 13

According to the weight percentage, 30 percent of No. 3 blending master batch and 70 percent of polypropylene are uniformly mixed to prepare a mixture containing 3 percent of superfine chopped glass fiber, and then the mixture is dried to remove surface moisture and then is passed through a melt spinning machine to prepare the superfine chopped glass fiber reinforced polypropylene blending melt spinning composite fiber material under the conditions of the melting temperature of 240 ℃, the pressure of a spinneret plate (component) of 8.5MPa, the winding speed of 1200m/min and the winding time of 10 min.

TABLE 3

	Example 8	Example 11	Example 12	Example 13
					The polypropylene content wt%	95.5	98.5	97	95.5
Content wt% of superfine chopped glass fiber	3	1	2	3
					Maleic anhydride grafted Polypropylene content wt%	1.5	0.5	1	1.5
Whether to soak in KH550 or not	Whether or not	Is that	Is that	Is that
					Pressure of assembly MPa	8.5	8.5	8.5	8.5
Winding speed m/min	1200	1200	1200	1200
					Number of times of filament breakage	0	1	0	2
Tensile strength cn/dtex	3.15	3.23	3.58	3.71
					Tensile strength MPa	287.55	288.20	323.12	338.67

Comparing example 8 with examples 11-13, it can be seen that the tensile strength of the composite fiber is improved significantly after the superfine chopped glass fiber is soaked in the KH550, and comparing fig. 1-4, it can be seen that the distribution orientation and the interface compatibility of the superfine chopped glass fiber of example 13 in the composite fiber are further improved.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject of the invention in all its modifications, substitutions and alterations all within the spirit and scope of the appended claims.