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Carbon fiber oiling agent for dry spray wet spinning technology and preparation method thereof

A technology of dry jet wet spinning and carbon fiber, which is applied in the fields of carbon fiber, fiber treatment, textiles and papermaking, etc., which can solve the problems of high content of polymerized monomers, increased emulsification difficulty, and poor protection of carbon fibers, etc. Good electrostatic effect and protect carbon fiber

Active Publication Date: 2017-12-22
新元化学(山东)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using amino silicone oil with medium and low viscosity and high ammonia value as the main agent, adding polyether modified silicone oil, epoxy modified silicone oil and other additives to prepare oil agent, such as Chinese patent document CN200910234655.4, the sticking phenomenon is alleviated, but heat resistance Insufficient resistance; use amino silicone oil with high viscosity and low ammonia value as the main agent, add polyether modified silicone oil, epoxy modified silicone oil and other additives to prepare oil agent, such as Chinese patent document CN201410420266.1, the sticking phenomenon is improved, and the resistance The heat is also slightly improved, but the difficulty of emulsification increases, and there is a problem of emulsion stability; in order to completely solve the problem of sticking rollers, Chinese patent document CN201210440069.7 proposes to prepare a stable silicone oil emulsion by emulsion polymerization, and mix it with amino silicone oil emulsion Oiling after mixing, but there is a complex process, and the problem of high monomer content in the emulsion after emulsion polymerization is used, which affects the quality of carbon fiber
In addition, the above methods all have the problem that the silicone oil becomes brittle at high temperature and has a poor protective effect on carbon fibers. At present, there is still no good solution

Method used

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  • Carbon fiber oiling agent for dry spray wet spinning technology and preparation method thereof
  • Carbon fiber oiling agent for dry spray wet spinning technology and preparation method thereof
  • Carbon fiber oiling agent for dry spray wet spinning technology and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1, the preparation of compound A

[0037] Add 2Kg of polyetheramine D400 (ammonia value 4.5mmol / g) and 19Kg of isopropanol to the reactor, stir, heat up to 85°C to 90°C, add 36Kg of epoxy-terminated silicone oil (molecular weight 10000) dropwise, add dropwise After reflux for 4 hours, the solvent was evaporated under reduced pressure, and finally the pressure was reduced to 133Pa, and the temperature was raised to 120°C to remove small molecules to obtain compound A-1 with a viscosity of 5600cp and an ammonia value of 0.22mmol / g.

[0038] Compound A-1 H NMR spectrum such as figure 1 As shown, the solvent is CDCl 3 . Among them, the chemical shift δ=0.093 is the proton peak of the silicon methyl group, δ=0.526 is the proton peak of the methyl group connected with silicon, δ=1.166 is the proton peak of the methyl group in the polyoxypropylene link, and δ=1.622 is the proton peak of the methyl group connected with silicon. The proton peak of the methylene gro...

Embodiment 2

[0039] Embodiment 2, the preparation of compound A

[0040] Add 3Kg polyetheramine ED600 (ammonia value 3.1mmol / g) and 15Kg isopropanol to the reactor, stir, raise the temperature to 85°C-90°C, add 27.9Kg terminal epoxy silicone oil (molecular weight 7000) dropwise, and the dropwise addition is completed After reflux for 4 hours, the solvent was evaporated under reduced pressure, and finally the pressure was reduced to 133Pa, and the temperature was raised to 120°C to remove small molecules to obtain compound A-2 with a viscosity of 13000cp and an ammonia value of 0.28mmol / g.

[0041] The specific proportioning and composition of Examples 3-5 are shown in Table 1.

[0042] The specific proportioning and composition are shown in Table 1, and the preparation steps are as follows:

[0043] After mixing the materials, stir and drip water, neutralize with acetic acid to neutral after phase inversion, and finally obtain a stable emulsion with a particle size of 0.01 μm to 0.5 μm th...

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Abstract

The invention relates to a carbon fiber oiling agent for a dry spray wet spinning technology and a preparation method thereof. The oiling agent comprises the following components in parts by weight: 65-75 parts of compound A shown as formula (I), 5-15 parts of polyether modified silicone, 1-5 parts of a polyquaternium anti-static agent, 1-5 parts of a liquid antioxidant and 5-15 parts of a surfactant. The invention solves the problems of roll banding, embrittlement under high temperature, and the like, of the oiling agent in the present dry spray wet spinning carbon fiber preparation process, meets the preparation requirement of the carbon fiber based on the dry spray wet spinning technology and increases the carbon fiber quality.

Description

technical field [0001] The invention relates to an oil agent, in particular to a carbon fiber oil agent for a dry spray wet spinning process and a preparation method thereof, belonging to the technical field of oil agents. Background technique [0002] Carbon fiber is a key material supporting strategic emerging industries. It is widely used in aerospace, national defense, wind power, sporting goods, rail transit, automobile lightweight, construction and other fields, and its demand is growing rapidly. The carbon fiber prepared by the dry jet wet spinning process has high strength and low cost, and has gradually become the mainstream development direction in the field of civilian product applications. [0003] Carbon fiber oil is an indispensable key additive in the carbon fiber manufacturing process, which can ensure the smooth progress of carbon fiber production, effectively reduce hair, and thus improve the quality of carbon fiber. At present, oils for domestic carbon fi...

Claims

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Application Information

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IPC IPC(8): D06M15/647D06M15/37D06M101/40
CPCD06M15/37D06M15/647D06M2101/40
Inventor 田志钢解乐福解承钢杜辉邵军强王爱卿赵伟洁
Owner 新元化学(山东)股份有限公司
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