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Preparation method of ultraviolet-light-resistant thiophene-structure-containing polybenzoxazole fibre

A polybenzoxazole, UV-resistant technology, applied in the direction of chemical characteristics of fibers, one-component synthetic polymer rayon, textiles and papermaking, etc. and other problems, to achieve the effects of excellent UV resistance, excellent uniformity and serious equipment corrosion

Active Publication Date: 2013-09-04
DALIAN RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] This preparation method has the following disadvantages: (1) in the reaction, 4,6-diaminoresorcinol dihydrochloride needs to be decompressed to remove HCl in polyphosphoric acid, and this process requires that HCl must be completely removed, Otherwise, the reactivity will be affected
Because 4,6-diaminoresorcinol is very easy to oxidize, must be anaerobic in order to prevent oxidation requirement system, higher to equipment requirement, and remove HCl time longer, the HCl that produces is serious to equipment corrosion; (2 ) Due to the very low solubility of terephthalic acid in polyphosphoric acid, the particle size of terephthalic acid is usually required to be less than 5 microns; (3) Due to the solubility of terephthalic acid and 2,5-thiophenedicarboxylic acid in polyphosphoric acid The difference is large, resulting in different reaction speeds between 4,6-diaminoresorcinol dihydrochloride and terephthalic acid and 2,5-thiophenedicarboxylic acid, and the obtained copolymer resin is not uniform

Method used

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  • Preparation method of ultraviolet-light-resistant thiophene-structure-containing polybenzoxazole fibre
  • Preparation method of ultraviolet-light-resistant thiophene-structure-containing polybenzoxazole fibre
  • Preparation method of ultraviolet-light-resistant thiophene-structure-containing polybenzoxazole fibre

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Preparation of 4,6-diaminoresorcinol / terephthalic acid compound salt

[0034]In a 125mL four-neck flask equipped with stirring, condenser and thermometer, add 10.66g (0.05mol) 4,6-diaminoresorcinol dihydrochloride and 100mL deionized water under the protection of nitrogen inert gas, and Dissolve 9.30g (0.05mol) of terephthalic acid in 200g of aqueous sodium hydroxide (the concentration of sodium hydroxide is 2%) to prepare an aqueous solution of disodium terephthalic acid, and add the solution dropwise to the above-mentioned solution at 80°C. In 4,6-diaminoresorcinol dihydrochloride aqueous solution, react at 80°C for 10 minutes, filter, wash, filter again and vacuum dry to obtain 4,6-diaminoresorcinol / terephthalic acid compound salt.

[0035] Preparation of 4,6-diaminoresorcinol / thiophenedicarboxylic acid compound salt

[0036] In a 125mL four-neck flask equipped with stirring, condenser and thermometer, add 10.66g (0.05mol) 4,6-diaminoresorcinol dihydrochloride ...

Embodiment 2

[0041] The preparation process of 4,6-diaminoresorcinol / terephthalic acid compound salt and 4,6-diaminoresorcinol / thiophenedicarboxylic acid compound salt is the same as in Example 1.

[0042] In a 125mL four-neck flask equipped with stirring, condenser tube, drying tube and thermometer, add 12.4g (0.04mol) 4,6-diaminoresorcinol / terephthalic acid compound salt, 3.12g (0.01mol) 4,6-diaminoresorcinol / thiophenedicarboxylic acid compound salt, 10.5g phosphorus pentoxide (content in P 2 o 5 Calculated as 84%), 119.1g polyphosphoric acid, stirred and heated to 120°C for 6h, and slowly raised the temperature to 30°C for 6h, 150°C for 12h, 180°C for 2h, and 200°C for 1h. The liquid is transferred to the spinning equipment, and the dry-jet wet spinning process is used to make fibers. The obtained fibers are further removed with 5% sodium hydroxide aqueous solution and water to remove residual phosphoric acid, and then dried in a vacuum drying oven to obtain a golden yellow thiophene-c...

Embodiment 3

[0045] The preparation process of 4,6-diaminoresorcinol / terephthalic acid compound salt and 4,6-diaminoresorcinol / thiophenedicarboxylic acid compound salt is the same as in Example 1.

[0046] In a 125mL four-neck flask equipped with stirring, condenser, drying tube and thermometer, add 14.99g (0.049mol) 4,6-diaminoresorcinol / terephthalic acid compound salt, 0.31g (0.001mol) 4,6-diaminoresorcinol / thiophenedicarboxylic acid compound salt, 12.60g phosphorus pentoxide, 91.36g polyphosphoric acid (content in P 2 o 5 Calculated as 84%), stirred and heated to 120°C for 6h, and slowly raised the temperature to 130°C for 12h, 150°C for 12h, 180°C for 2h, and 200°C for 1h. After the reaction was completed, the reaction solution was transferred to the spinning equipment In the process, dry-jet wet-spinning technology is used to make fibers, and the obtained fibers are further removed with 5% sodium hydroxide aqueous solution and water to remove residual phosphoric acid, and then dried ...

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Abstract

A method for manufacturing UV-resistant polybenzoxazole fiber containing thiophene structure is provided, which comprises the following steps : mixing 4,6-diaminoresorcinoldihydrochloride with terephthalic acid and thiophenedicarboxylic acid respectively to prepare the corresponding composite salts, and then performing condensation reaction of the two composite salts in a phosphorus pentoxide / polyphosphoric acid solvent system under the protection of a noble gas; and at the end of the reaction, transferring the reactant solution into a spinning device and spinning to obtain a fiber. The method in this invention avoids the process difficulty of the large solubility difference of terephthalic acid and 2,5-thiophenedicarboxylic acid in polyphosphoric acid, is inexpensive and environment-friendly, and produces a copolymer resin with good uniformity and a fiber with improved UV resistance.

Description

technical field [0001] The invention relates to a preparation method of high-performance polybenzoxazole fiber, more specifically, to a preparation method of polybenzoxazole fiber containing thiophene structure. Background technique [0002] High-performance poly[(1,4)-phenylene 2,6-(1,2-d:5,4-d)-benzobisoxazole] (PBO for short) fiber has excellent strength, modulus, Heat resistance and flame resistance, but its UV aging resistance is poor. Japan's Toyobo Company has tested the light stability of PBO fiber, and the results show that its modulus is only 35% of its original value after being exposed to sunlight for 6 months. Lin Lantian and others reported that PBO fiber has poor sun resistance, and the longer it is exposed to ultraviolet rays, the more its strength will decrease. Especially after 40h of sunlight, the breaking strength of PBO fiber is only 37% of the original (Lin Lantian, Zhou Jing. Discussion on the mechanical properties of PBO-AS fiber. Shanghai Textile S...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/78C08G73/22
CPCD01F6/78C08G73/22D01F6/74
Inventor 左洪亮邵玉昌张海涛蔡小川许汉
Owner DALIAN RES & DESIGN INST OF CHEM IND
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