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A kind of polyimide fiber and preparation method thereof

A technology of polyimide fiber and imidization, applied in the field of fiber or fiber fabric, can solve the problems such as severe temperature difference alternation in space, shape limitation, shedding, etc., to achieve the effect of improving elongation at break

Active Publication Date: 2018-11-27
吉林省亚安新材料有限公司
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AI Technical Summary

Problems solved by technology

According to the current literature reports, there are several ways to improve the AO resistance performance: 1. Composite method, coating a passivation layer with AO resistance performance on the surface of polyimide, the passivation layer can be metal or metal oxide substances (such as Al 2 o 3 , SiO 2 , CrO 3 , Ge, ZrO 2 、TiO 2 etc.), it can also be an inorganic or organic compound (such as fluororesin, etc.), and the Chinese patents whose publication numbers are CN1629225A, CN101724822B, CN101724823A, CN104233207A and CN104592893A all disclose this related technology, but there are certain limitations in this method. On the one hand, in order to prepare dense and uniform coatings, special equipment and processes are often required, and there are restrictions on the shape and size. layer or even shedding phenomenon; 2. Filling method, some AO-resistant metal or metal compound (such as Al 2 O3, SiO 2 , CrO 3 , Ge, ZrO 2 、TiO 2 ) into the matrix material, which can be achieved by blending, doping or ion implantation. Related technologies are reported in Chinese patents with publication numbers CN101402796B, CN103435826A, CN103214846A, CN102731809A, CN101388422A, CN101429350A and CN1865350A. The method solves the problem of the compound method, but this method has the problem of uneven filler dispersion or even agglomeration, or the problem of fine cracks in the matrix due to ion implantation. AO penetrates the surface and erodes the underlying layer)

Method used

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  • A kind of polyimide fiber and preparation method thereof
  • A kind of polyimide fiber and preparation method thereof
  • A kind of polyimide fiber and preparation method thereof

Examples

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preparation example Construction

[0054] The present invention also provides a kind of preparation method of above-mentioned polyimide fiber, comprising:

[0055] A) Polymerize the dianhydride compound and the diamine compound to obtain a polyamic acid spinning solution; the dianhydride compound and / or the diamine compound contains phosphorus; the dianhydride compound includes at least the following formula (I-1)~ One or more of the structures of formula (I-9):

[0056]

[0057] B) spinning the polyamic acid spinning solution to obtain polyamic acid fibers;

[0058] C) Imidizing the polyamic acid fibers to obtain polyimide fibers.

[0059] The present invention has no special limitation on the sources of all raw materials, which can be commercially available or self-made. The types of the diamine compound and the dianhydride compound are the same as those described above, and will not be repeated here.

[0060] The dianhydride compound and the diamine compound are polymerized, and the molar ratio of the ...

Embodiment 1

[0081] 1.1 Dissolve 192.23g (0.96mol) of 4,4'-diaminodiphenyl ether, 59.10g (0.24mol) of bis(3-aminophenyl)methylphosphine (III-11) in 4025ml of dimethyl sulfoxide , add 176.53g (0.60mol) biphenyltetralic acid dianhydride and 241.38g (0.60mol) 1,3-bis(3,4-dicarboxyphenoxy)phthalic anhydride (I-3) under stirring state, React at 50° C. for 4 hours to obtain a light yellow viscous polyamic acid spinning solution (concentration: 15 wt %), which is directly used as spinning slurry after filtering.

[0082] 1.2 The polyamic acid slurry obtained in 1.1 is spun and formed by dry-wet spinning technology. After the spinning slurry at room temperature is accurately measured by a metering pump, it is extruded from the spinneret hole and enters the dimethyl In the coagulation bath of sulfoxide and water (1:4 volume ratio). The spinneret has 200 holes, the hole diameter is Φ0.15mm, the spray ratio is 1.6 times, the spinning speed is 30m / min, and the air layer height is 10mm. The as-spun f...

Embodiment 2

[0087] The molar ratio of the diamine monomer in Example 1 was adjusted so that the phosphorus-containing monomer accounted for 40%. With other conditions unchanged, polyimide fibers were obtained.

[0088] The polyimide fiber obtained in Example 2 was analyzed, and the tensile breaking strength of the fiber was 4.41 cN / dtex, the initial modulus was 49.31 cN / dtex, and the elongation at break was 98%.

[0089] The AO irradiation test was carried out on the polyimide fiber obtained in Example 2, and the strength retention data of the fiber after irradiation is shown in Table 1.

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Abstract

The invention provides a polyimide fiber and a preparation method thereof, wherein a dianhydride compound and a diamine compound are polymerized to obtain a polyamic acid spinning solution; the dianhydride compound and / or the diamine compound contain phosphorus; The dianhydride compound at least includes one or more of the structures of the following formula (I-1) to formula (I-9): the polyamic acid spinning solution is spun to obtain a polyamic acid fiber; The polyamic acid fiber is subjected to imidization treatment to obtain polyimide fiber. Compared with the prior art, the present invention introduces phosphorus into the polyimide fiber, and when the material is exposed to space atomic oxygen (AO) environment, the material itself will form a passivation layer, thereby blocking the further action of AO on the material, Moreover, this is a self-repairing process, which makes the material more intelligent. At the same time, the present invention introduces triphenylene diether dianhydride monomer into the structure, so that the elongation at break of the prepared polyimide fiber is improved.

Description

technical field [0001] The invention belongs to the technical field of fibers or fiber fabrics, and in particular relates to a polyimide fiber and a preparation method thereof. Background technique [0002] The preparation method of polyimide fiber is divided into one-step method and two-step method. One-step method refers to directly spinning with polyimide solution, and then obtaining polyimide fiber through hot drawing. The one-step method for preparing polyimide fibers has a short technological process, but spinning fibers using this method requires that the polyimide polymer system must be soluble, and more importantly, the solvents used in the preparation process are generally highly toxic. Chinese Patent Publication No. CN1232686C, U.S. Patent No. US4370290 and US5378420 all disclose the above method. [0003] The two-step method refers to the use of polyamic acid solution spinning, and then through the imidization process to obtain polyimide fibers. Although this m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/78D01F6/74C08G73/10
Inventor 邱雪鹏赵勇董志鑫代学民刘芳芳李国民高连勋
Owner 吉林省亚安新材料有限公司
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