CN103469367A - Preparation technology of high-strength and high modulus carbon fibers - Google Patents

Abstract

The invention discloses a preparation technology of high-strength and high modulus carbon fibers. The preparation technology comprises following steps: in presence of inert atmosphere, 5% of perylene-3, 4, 9, 10-tetracarboxylic dianhydride, 5% of 2, 6-naphthalic acid and 5% of alkyl phenyl polysiloxane are added into matrix asphalt, and the mixture is subjected to heat processing at a temperature controlled at 350 to 430 DEG C so as to obtain mesophase pitch, wherein the weight of the ingredients is based on the weight of matrix asphalt; mesophase pitch is subjected to spinning so as to obtain asphalt wires; the asphalt wires are subjected to heat processing for 30min, at a temperature controlled at 340 DEG C, in the presence of inert atmosphere, and in an oxidizing medium so as to obtain mesophase pitch fibers; and at last, the mesophase pitch fibers are subjected to carbonization treatment for 45min at a temperature of 1100 DEG C in the presence of inert atmosphere, and then is subjected to graphitization treatment for 15min at a temperature of 2400 DEG C so as to obtain the high-strength and high modulus carbon fibers. The high-strength and high modulus carbon fibers prepared by the preparation technology are capable of meeting high-strength and high modulus carbon fiber standards, and the preparation technology is simple, and is easy for operation.

Description

A kind of high-strength and high-modulus type carbon fiber preparation technology

Technical field:

The present invention relates to the Carbon Fiber Technology field, relate in particular to a kind of high-strength and high-modulus type carbon fiber preparation technology.

Background technology:

Asphalt base carbon fiber is that a kind of to take asphalt or coal tar pitch be raw material, the special fibre that the phosphorus content made through refining, spinning, pre-oxidation, carbonization or graphitization is greater than 92%, belong to novel reinforcing material, it not only has the inherent feature of material with carbon element, and have flexibility and the processability of textile fabric concurrently, be widely used in the fields such as military affairs, aviation, sports goods, racing car.The raw material for preparing carbon fiber has multiple, as methane, ethane, benzene vapor, high molecular polymer (artificial fibre, polyacrylonitrile, polyvinyl chloride, phenolic resins) and pitch etc.But the synthetic of commercial carbon fiber can only be from three kinds of materials: polyacrylonitrile, pitch and organic fiber (nylon yarn, acrylics filament etc.).Although carbon fiber is because its superior performance is widely used, but manufacturing cost is too high, the defects such as the lower and technology of middle phase productive rate is too complicated are restricting the development of carbon fiber industry, yet the low cost of asphalt base carbon fiber and high-carbon content have determined competitiveness that it is remarkable and optimistic development prospect.

Summary of the invention:

The purpose of this invention is to provide a kind of high-strength and high-modulus type carbon fiber preparation technology, take matrix pitch as basic material process series of process process, obtain high-strength and high-modulus type carbon fiber, technical process is simple, easy to operate.

Purpose of the present invention is achieved through the following technical solutions:

A kind of high-strength and high-modulus type carbon fiber preparation technology comprises the following steps:

(1): under inert atmosphere, in matrix pitch, take matrix pitch weight as benchmark add 5% 3,4,9,10-perylene tetracarboxylic acid dianhydride, 5% 2,6-naphthalenedicarboxylic acid and 5% alkyl phenyl polysiloxanes, control temperature and heat-treat at 350～430 ℃, makes mesophase pitch;

(2): mesophase pitch is obtained to the pitch silk through spinning technique;

(3): under inert atmosphere by the pitch silk that obtains in oxide isolation, control temperature and be 340 ℃ and heat-treat and within 30 minutes, obtain the Mesophase pitch fiber;

(4): last, the Mesophase pitch fiber first carries out carbonization treatment 45 minutes under inert atmosphere under 1100 ℃, then under 2400 ℃, carries out graphitization processing and within 15 minutes, obtains described high-strength and high-modulus type carbon fiber.

As technique scheme preferably, a kind of in the aqueous solution that the oxide isolation in step (3) is hydrogen peroxide, sulfuric acid, nitric acid.

Beneficial effect of the present invention is: basic material is matrix pitch, with low cost, and technical process is simple, easily applies.

The accompanying drawing explanation:

Below in conjunction with accompanying drawing, the present invention is described further:

Fig. 1 is pitch spinning technique procedure chart;

Fig. 2 is the asphalt base carbon fiber process chart.

The specific embodiment:

In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment only, for explaining the present invention, does not form limiting the scope of the present invention.

Under inert atmosphere, in matrix pitch, take matrix pitch weight as benchmark add 5% 3,4,9,10-perylene tetracarboxylic acid dianhydride, 5% NDA and 5% alkyl phenyl polysiloxanes, control temperature and heat-treat at 400 ℃, makes mesophase pitch; Mesophase pitch is obtained to the pitch silk through spinning technique (shown in accompanying drawing 1); Under inert atmosphere by the pitch silk that obtains in the oxide isolation hydrogen peroxide, control temperature and be 340 ℃ and heat-treat and within 30 minutes, obtain the Mesophase pitch fiber; Finally, the Mesophase pitch fiber first carries out carbonization treatment 45 minutes under inert atmosphere under 1100 ℃, then under 2400 ℃, carries out graphitization processing and within 15 minutes, obtains described high-strength and high-modulus type carbon fiber, and the concrete technology flow process as shown in Figure 2.

The mechanical property of the asphalt base carbon fiber made by above-mentioned technique is as shown in the table:

?	Diameter/μ m	Tensile strength/MPa	Tensile modulus/GPa	Extension at break/%
					The present invention	13.1	3240	4500	0.6
High-strength	7	2500～4500	2000～2400	1.4～1.8
					Universal	10～15	420～1000	3800～4000	2.1～2.5
High model	5～8	2000～2800	3500～7000	0.4～0.8
					The high-strength and high-modulus type	9～18	3000～5000	4000～8000	0.4～0.8

The data of upper table show that the asphalt base carbon fiber that according to the present invention prepared by technique meets high-strength and high-modulus type carbon fiber standard.

Claims (2)

1. a high-strength and high-modulus type carbon fiber preparation technology, it is characterized in that: described preparation technology comprises the following steps:

(1): under inert atmosphere, in matrix pitch, take matrix pitch weight as benchmark add 5% 3,4,9,10-perylene tetracarboxylic acid dianhydride, 5% 2,6-naphthalenedicarboxylic acid and 5% alkyl phenyl polysiloxanes, control temperature and heat-treat at 350～430 ℃, makes mesophase pitch;

(2): mesophase pitch is obtained to the pitch silk through spinning technique;

(3): under inert atmosphere by the pitch silk that obtains in oxide isolation, control temperature and be 340 ℃ and heat-treat and within 30 minutes, obtain the Mesophase pitch fiber;

(4): last, the Mesophase pitch fiber first carries out carbonization treatment 45 minutes under inert atmosphere under 1100 ℃, then under 2400 ℃, carries out graphitization processing and within 15 minutes, obtains described high-strength and high-modulus type carbon fiber.

2. high-strength and high-modulus type carbon fiber preparation technology according to claim 1 is characterized in that: a kind of in the aqueous solution that the oxide isolation in step (3) is hydrogen peroxide, sulfuric acid, nitric acid.

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