CN116285330A - A kind of carbon fiber reinforced PA6T/10T flame retardant material and its preparation method - Google Patents

Abstract

The invention provides a carbon fiber reinforced PA6T/10T flame retardant material, which comprises the following components in percentage by mass: 60% -80% of PA6T/10T resin; 10% -30% of modified carbon fiber; 1 to 10 percent of modified hydrotalcite. The carbon fiber reinforced PA6T/10T flame retardant material has excellent mechanical property and flame retardant property.

Description

A kind of carbon fiber reinforced PA6T/10T flame retardant material and its preparation method

technical field

The invention belongs to the technical field of polymer materials, and in particular relates to a carbon fiber reinforced PA6T/10T flame-retardant material and a preparation method thereof.

Background technique

Nylon 6T/10T (PA6T/10T) is semi-aromatic nylon, which has excellent high temperature rigidity, excellent welding resistance, excellent chemical resistance, low water absorption, excellent dimensional stability, and is not easy to fluff during molding. performance. However, the polymer material PA6T/10T is flammable, which limits its processing and application. At present, there are few research reports on the flame retardancy and mechanical properties of PA6T/10T.

Therefore, how to improve the flame retardancy and mechanical properties of PA6T/10T and expand the application field of PA6T/10T is a technical problem urgently needed to be solved by those skilled in the art.

Contents of the invention

In order to solve the above problems, the first aspect of the present invention provides a carbon fiber reinforced PA6T/10T flame retardant material, the composition of the carbon fiber reinforced PA6T/10T flame retardant material includes: PA6T/10T resin 60%-80 %; Modified carbon fiber 10%-30%; Modified hydrotalcite 1%-10%.

In the first aspect, the modified carbon fiber is a modified carbon fiber surface-modified by a silane coupling agent.

In the first aspect, the modified hydrotalcite is obtained as follows: add hydrotalcite powder to deionized water, stir to obtain a dispersion, add an ester-containing quaternary ammonium salt surfactant to the dispersion, and heat up to 70 Stir at -85°C, condense and reflux for 2-4 hours to obtain a suspension; ultrasonically disperse the suspension evenly, then centrifuge to remove the supernatant to obtain a precipitate, wash, dry, and grind the obtained precipitate to obtain modified water talc.

In the first aspect, the concentration of the dispersion liquid is 30-50 g/L.

In the second aspect, the application provides a method for preparing a carbon fiber reinforced PA6T/10T flame retardant material, the preparation method comprising the following steps: preparing modified carbon fiber; preparing modified hydrotalcite; weighing PA6T/10T according to the material formula 10T resin, carbon fiber and modified hydrotalcite; dry the PA6T/10T resin in a vacuum oven at 120°C for 4 hours, and mix the modified hydrotalcite with the dried PA6T/10T resin to obtain a premix; the premix and Modified carbon fiber is extruded and granulated to obtain carbon fiber reinforced PA6T/10T flame retardant material.

In the second aspect, the material formula includes the following components in mass percentage: 60%-80% of PA6T/10T resin, 10%-30% of modified carbon fiber and 1%-10% of modified hydrotalcite.

In the second aspect, the modified carbon fiber is a modified carbon fiber surface-modified by a silane coupling agent.

In the second aspect, the preparation of the modified hydrotalcite includes: adding hydrotalcite powder to deionized water, stirring to obtain a dispersion liquid, adding an ester group-containing quaternary ammonium salt surfactant to the dispersion liquid, and raising the temperature to 70-85 °C, stirring and reflux for 2-4 hours to obtain a suspension; ultrasonically disperse the suspension evenly, and then centrifuge to remove the supernatant to obtain a precipitate, which is washed, dried, and ground to obtain modified hydrotalcite.

In the second aspect, the concentration of the dispersion is 30-50 g/L.

Beneficial effects: the present invention proposes a carbon fiber reinforced PA6T/10T flame retardant material. The components of the carbon fiber reinforced PA6T/10T flame retardant material include: PA6T/10T resin 60%-80%; modified carbon fiber 10%- 30%; modified hydrotalcite 1%-10%. The modified carbon fiber selected by the present invention can be uniformly dispersed in the PA6T/10T resin, and has good interface compatibility with the resin, so that the mechanical properties of the PA6T/10T composite material are greatly improved; the modified water Talc has good dispersion in PA6T/10T resin, organic hydrotalcite carbon layer migrates to the surface of polyamide PA6T/10T carbon layer, and the combination of the two forms a denser carbon layer, which is more conducive to blocking the heat conduction between the polymer and the heat source At the same time, the modified hydrotalcite makes the hydrotalcite sheet structure form a good labyrinth effect, which can effectively prevent the diffusion of external oxygen to the surface of the uncracked polymer, and effectively improve the flame retardancy of carbon fiber reinforced PA6T/10T composites.

Description of drawings

In order to more clearly illustrate the embodiments of this specification or the technical solutions in the prior art, the following will briefly introduce the accompanying drawings required in the embodiments. Obviously, the accompanying drawings in the following description are only some of the present invention. Embodiments, for those of ordinary skill in the art, other drawings can also be obtained based on these drawings without any creative effort.

Fig. 1 is the flow chart of the preparation method of carbon fiber reinforced PA6T/10T flame retardant material in the embodiment of the present invention;

Detailed ways

The technical solutions in the present invention will be clearly and completely described below in conjunction with the accompanying drawings. Apparently, the described embodiments are only some, not all, embodiments of the present invention. All other embodiments obtained by persons of ordinary skill in the art based on the embodiments of the present invention belong to the protection scope of the present invention.

Meanwhile, throughout the specification, unless otherwise specifically stated, terms used herein should be understood as meanings generally used in the art. Therefore, unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, this specification shall take precedence.

Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods.

Example 1

Obtain carbon fiber reinforced PA6T/10T flame retardant material as follows:

(1) prepare modified carbon fiber; prepare modified hydrotalcite;

The modified carbon fiber is a modified carbon fiber modified on the surface of a silane coupling agent; the preparation of the modified hydrotalcite includes: adding hydrotalcite powder to deionized water, and stirring to obtain a dispersed concentration of 30-50g/L Liquid, add ester-containing quaternary ammonium salt surfactant to the dispersion, heat up to 70-85°C, fully stir and condense and reflux for 2-4 hours to obtain a uniform suspension; ultrasonically disperse the suspension evenly, and then centrifuge The supernatant liquid is removed to obtain a precipitate, which is washed, dried and ground to obtain a modified hydrotalcite.

(2) According to the material formula, it includes the following components in mass percentage: 72.5% of PA6T/10T resin, 20% of modified carbon fiber and 7.5% of modified hydrotalcite; accurately weigh each component;

(3) Dry the PA6T/10T resin in a vacuum oven at 120°C for 4 hours, and mix the modified hydrotalcite with the dried PA6T/10T resin to obtain a premix;

(4) Extrude and granulate the premixed material and the modified carbon fiber to obtain a carbon fiber reinforced PA6T/10T flame retardant material.

Example 2

Obtain carbon fiber reinforced PA6T/10T flame retardant material as follows:

(1) prepare modified carbon fiber; prepare modified hydrotalcite;

The modified carbon fiber is a modified carbon fiber modified on the surface of a silane coupling agent; the preparation of the modified hydrotalcite includes: adding hydrotalcite powder to deionized water, and stirring to obtain a dispersed concentration of 30-50g/L Liquid, add ester-containing quaternary ammonium salt surfactant to the dispersion, heat up to 70-85°C, fully stir and condense and reflux for 2-4 hours to obtain a uniform suspension; ultrasonically disperse the suspension evenly, and then centrifuge The supernatant liquid is removed to obtain a precipitate, which is washed, dried and ground to obtain a modified hydrotalcite.

(2) According to the material formula, it includes the following components in mass percentage: 65% of PA6T/10T resin, 30% of modified carbon fiber and 5% of modified hydrotalcite; accurately weigh each component;

(3) Dry the PA6T/10T resin in a vacuum oven at 120°C for 4 hours, and mix the modified hydrotalcite with the dried PA6T/10T resin to obtain a premix;

(4) Extrude and granulate the premixed material and the modified carbon fiber to obtain a carbon fiber reinforced PA6T/10T flame retardant material.

Example 3

Obtain carbon fiber reinforced PA6T/10T flame retardant material as follows:

(1) prepare modified carbon fiber; prepare modified hydrotalcite;

The modified carbon fiber is a modified carbon fiber modified on the surface of a silane coupling agent; the preparation of the modified hydrotalcite includes: adding hydrotalcite powder to deionized water, and stirring to obtain a dispersed concentration of 30-50g/L Liquid, add ester-containing quaternary ammonium salt surfactant to the dispersion, heat up to 70-85°C, fully stir and condense and reflux for 2-4 hours to obtain a uniform suspension; ultrasonically disperse the suspension evenly, and then centrifuge The supernatant liquid is removed to obtain a precipitate, which is washed, dried and ground to obtain a modified hydrotalcite.

(2) According to the material formula, it includes the following components by mass percentage: 62.5% of PA6T/10T resin, 30% of modified carbon fiber and 7.5% of modified hydrotalcite; accurately weigh each component;

(3) Dry the PA6T/10T resin in a vacuum oven at 120°C for 4 hours, and mix the modified hydrotalcite with the dried PA6T/10T resin to obtain a premix;

(4) Extrude and granulate the premixed material and the modified carbon fiber to obtain a carbon fiber reinforced PA6T/10T flame retardant material.

Comparative example 1

Obtain PA6T/10T material as follows:

(1) According to the material formula, it includes the following components by mass percentage: PA6T/10T resin 100%; accurately weigh PA6T/10T resin;

(2) Dry the PA6T/10T resin in a vacuum oven at 120°C for 4 hours;

(3) Extrude and granulate the dried PA6T/10T resin to obtain PA6T/10T material.

Comparative example 2

Obtain PA6T/10T material as follows:

(1) prepare modified carbon fiber;

The modified carbon fiber is a modified carbon fiber surface-modified by a silane coupling agent;

(2) According to the material formula, it includes the following components in mass percentage: 70% of PA6T/10T resin and 30% of modified carbon fiber; accurately weigh each component;

(3) Dry the PA6T/10T resin in a vacuum oven at 120°C for 4 hours;

(4) Extrude and granulate PA6T/10T resin and modified carbon fiber to obtain PA6T/10T material.

Comparative example 3

Obtain PA6T/10T material as follows:

(1) prepare modified hydrotalcite;

The preparation of the modified hydrotalcite includes: adding hydrotalcite powder to deionized water, stirring fully to obtain a dispersion with a concentration of 30-50 g/L, adding an ester-group-containing quaternary ammonium salt surfactant to the dispersion, and raising the temperature to 70-85°C, fully stir and reflux for 2-4 hours to obtain a uniform suspension; ultrasonically disperse the suspension evenly, then centrifuge to remove the supernatant to obtain a precipitate, which is washed, dried, and ground A modified hydrotalcite is obtained.

(2) According to the material formula, it includes the following components in mass percentage: 90% of PA6T/10T resin and 10% of modified hydrotalcite; accurately weigh each component;

(3) Dry the PA6T/10T resin in a vacuum oven at 120°C for 4 hours, and mix the modified hydrotalcite with the dried PA6T/10T resin to obtain a premix;

(4) Extrude and granulate the premix to obtain PA6T/10T material.

Effect Example

The properties of the materials prepared in Examples 1-3 and Comparative Examples 1-3 were tested, and the test results are shown in Table 1.

The material performance testing result of table 1 embodiment 1-3 and comparative example 1-3

It can be seen from Table 1 that the carbon fiber reinforced PA6T/10T flame retardant material developed by compounding PA6T/10T resin, modified carbon fiber and modified hydrotalcite in Examples 1-3 of the present invention has excellent flame retardancy and mechanical properties. The present invention adopts carbon fiber with high specific strength, high specific modulus and high temperature resistance as reinforcing material. After surface modification by silane coupling agent, the modified carbon fiber can be uniformly dispersed in PA6T/10T resin, and has a good relationship with resin. The interfacial compatibility effectively improves the mechanical properties of PA6T/10T composite materials; the organically modified hydrotalcite also has good dispersion in PA6T/10T resin, and at the same time, the organic hydrotalcite with sheet structure can effectively Prevent external oxygen from diffusing to the surface of the uncracked polymer and increase the carbon formation rate; in addition, the organic hydrotalcite carbon layer migrates to the surface of the polyamide PA6T/10T carbon layer, forming a uniform and dense carbon layer with the resin, which can effectively block the polymer and The heat conduction between heat sources significantly improves the flame retardancy of carbon fiber reinforced PA6T/10T composites.

Finally, it should also be noted that the term "comprises", "comprises" or any other variation thereof is intended to cover a non-exclusive inclusion such that a process, method, article or apparatus comprising a set of elements includes not only those elements, but also Other elements not expressly listed, or inherent to the process, method, article, or apparatus are also included.

While preferred embodiments of the invention have been described, additional changes and modifications to these embodiments can be made by those skilled in the art once the basic inventive concept is appreciated. Therefore, it is intended that the appended claims be construed to cover the preferred embodiment as well as all changes and modifications which fall within the scope of the invention.

Obviously, those skilled in the art can make various changes and modifications to the present invention without departing from the spirit and scope of the present invention. Thus, if these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalent technologies, the present invention also intends to include these modifications and variations.

Claims (9)

1. The carbon fiber reinforced PA6T/10T flame retardant material is characterized by comprising the following components in percentage by mass:

60% -80% of PA6T/10T resin; 10% -30% of modified carbon fiber; 1 to 10 percent of modified hydrotalcite.

2. The PA6T/10T flame retardant material of claim 1, wherein the modified carbon fiber is a modified carbon fiber surface-modified with a silane coupling agent.

3. The carbon fiber reinforced PA6T/10T flame retardant material according to claim 2, characterized in that the modified hydrotalcite is obtained by: adding hydrotalcite powder into deionized water, stirring to obtain a dispersion liquid, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, stirring, condensing and refluxing for 2-4 hours to obtain a suspension liquid; and (3) uniformly dispersing the suspension by ultrasonic, centrifuging to remove supernatant to obtain a precipitate, and washing, drying and grinding the obtained precipitate to obtain the modified hydrotalcite.

4. A carbon fiber reinforced PA6T/10T flame retardant material according to claim 3, characterized in that the concentration of the dispersion is 30-50g/L.

5. The preparation method of the carbon fiber reinforced PA6T/10T flame retardant material is characterized by comprising the following steps:

preparing modified carbon fibers; preparing modified hydrotalcite;

weighing PA6T/10T resin, modified carbon fiber and modified hydrotalcite according to a material formula;

drying the PA6T/10T resin in a vacuum oven at 120 ℃ for 4 hours, and mixing the modified hydrotalcite and the dried PA6T/10T resin to obtain a premix;

and extruding and granulating the premix and the modified carbon fiber to obtain the carbon fiber reinforced PA6T/10T flame-retardant material.

6. The preparation method of the carbon fiber reinforced PA6T/10T flame retardant material according to claim 5, wherein the material formula comprises the following components in percentage by mass: 60% -80% of PA6T/10T resin, 10% -30% of carbon fiber and 1% -10% of modified hydrotalcite.

7. The method for preparing a carbon fiber reinforced PA6T/10T flame retardant material according to claim 6, wherein the modified carbon fiber is a modified carbon fiber surface-modified with a silane coupling agent.

8. The method for preparing a carbon fiber reinforced PA6T/10T flame retardant material according to claim 7, wherein the preparing modified hydrotalcite comprises: adding hydrotalcite powder into deionized water, stirring to obtain a dispersion liquid, adding an ester group-containing quaternary ammonium salt surfactant into the dispersion liquid, heating to 70-85 ℃, stirring, condensing and refluxing for 2-4 hours to obtain a suspension liquid; and (3) uniformly dispersing the suspension by ultrasonic, centrifuging to remove supernatant to obtain a precipitate, and washing, drying and grinding the obtained precipitate to obtain the modified hydrotalcite.

9. The method for producing a carbon fiber-reinforced PA6T/10T flame retardant material according to claim 8, wherein the concentration of the dispersion is 30-50g/L.

Images