阅读说明：本技术 一种用于改善氧化铝连续纤维耐老化性能的浸润剂及其制备方法和应用 (Impregnating compound for improving aging resistance of alumina continuous fibers and preparation method and application thereof ) 是由 王安琪 贾玉娜 陈代荣 焦秀玲 于 2020-07-21 设计创作，主要内容包括：本发明公开了一种用于改善氧化铝连续纤维耐老化性能的浸润剂及其制备方法和应用,其中,浸润剂中按照重量百分比包括0.5～2％的聚乙烯醇缩丁醛树脂、0.5～2％的润滑剂、0.05～0.2％的抗静电剂,余量为有机溶剂。所用成膜剂为醇溶性高分子,其溶液为稳定透明的均匀溶液。用于氧化铝连续纤维后,一方面,能够避免纤维免受外部环境老化的影响,保持纤维本身的性能。另一方面,浸润剂自身成膜后具有耐老化的作用,而且,能够使纤维具有较好的力学性能,可提高纤维耐磨性,在满足其涂覆率要求的基础上,纤维较为柔软,长时间保持外观亮白及力学性能稳定,能够满足后序纺织加工的要求。(The invention discloses an impregnating compound for improving aging resistance of alumina continuous fibers, and a preparation method and application thereof, wherein the impregnating compound comprises 0.5-2% of polyvinyl butyral resin, 0.5-2% of a lubricant, 0.05-0.2% of an antistatic agent and the balance of an organic solvent in percentage by weight. The film forming agent is alcohol soluble polymer, and the solution is stable and transparent uniform solution. After the composite material is used for the alumina continuous fiber, on one hand, the fiber can be prevented from being influenced by the aging of the external environment, and the performance of the fiber is kept. On the other hand, the sizing agent has an anti-aging effect after being formed into a film, can enable the fiber to have better mechanical property, can improve the wear resistance of the fiber, is softer on the basis of meeting the requirement of the coating rate, keeps bright and white appearance and stable mechanical property for a long time, and can meet the requirement of subsequent textile processing.)

1. The impregnating compound for improving the aging resistance of the alumina continuous fibers is characterized by comprising the following components in percentage by weight:

0.5-2% of polyvinyl butyral resin, 0.5-2% of lubricant, 0.05-0.2% of antistatic agent and the balance of organic solvent.

2. An impregnating compound according to claim 1, wherein: the lubricant is a non-ionic compound lubricant, and the non-ionic compound lubricant comprises one or more of triethylene glycol diisocaprylate, polyethylene glycol, Tween 80, glycerol and span 80.

3. An impregnating compound according to claim 2, wherein: the lubricant comprises triethylene glycol diisooctanoate.

4. A sizing composition according to claim 3, wherein: the lubricant is a mixture of triethylene glycol diisocaprylate and Tween-80, and the mass ratio of the triethylene glycol diisocaprylate to the Tween-80 is 2: (2.5-3.5).

5. An impregnating compound according to claim 1, wherein: the antistatic agent is a quaternary ammonium salt antistatic agent, and the quaternary ammonium salt antistatic agent is hexadecyl trimethyl ammonium chloride.

6. An impregnating compound according to claim 1, wherein: the organic solvent comprises one or more of methanol, isopropanol, n-propanol, ethanol, butanol, isobutanol and acetone.

7. An impregnating compound according to claim 6, wherein: the organic solvent is a mixed solvent of acetone and ethanol, and the mass ratio of the acetone to the ethanol is 1: 9.

8. An impregnating compound according to claim 1, wherein: the polyvinyl butyral resin has a butyral content of 45-50 wt% and a viscosity of 15-18 mPa^.s, molecular weight of 280-310.

9. A method for preparing an impregnating compound according to any one of claims 1 to 8, comprising:

s1: diluting polyvinyl butyral resin with 15-25 times of organic solvent, and stirring for 0.5-2 h;

s2: diluting the lubricant with 15-25 times of organic solvent, and stirring for 0.5-2 h;

s3: dissolving an antistatic agent in 15-25 times of an organic solvent, and stirring for 0.5-2 hours;

s4: and sequentially adding the solutions in the steps S1, S2 and S3 into the rest of the organic solvent, uniformly mixing, and stirring for 1-2 hours to obtain the impregnating compound for improving the aging resistance of the alumina continuous fibers.

10. An impregnating agent according to any one of claims 1 to 8, wherein: and (3) uniformly coating the impregnating compound on the surface of the alumina continuous fiber, and drying to obtain an alumina continuous fiber finished product, wherein the coating rate of the impregnating compound is 1.4-1.9 wt%.

Technical Field

The application belongs to the technical field of inorganic ceramic fiber surface modification, and particularly relates to a wetting agent for improving aging resistance of alumina continuous fibers, and a preparation method and application thereof.

Background

The alumina continuous fiber belongs to one of novel high-performance ceramic fibers, has excellent properties of high temperature resistance, corrosion resistance, high strength, high modulus and the like, and has strategic significance in the fields of war industry, aerospace and the like. At the same time, however, the alumina continuous fibers belong toBrittle materials, with low bending strength. The alumina continuous fiber is easy to generate surface cracks and defects in a series of forming processes of spinning, sintering, drawing and the like, and the size, the number and the distribution of the defects and the cracks influence the properties of the fiber, so that perfect fiber cannot be obtained in the process, and the actual performance of the fiber is usually far lower than the theoretical performance value of a perfect structure. In addition, alumina ceramic fibers are susceptible to environmental degradation, which can result in deterioration of the physical and chemical properties of the fibers, loss of tensile strength of the fibers, and discoloration of the surface of the fibers when exposed to sunlight, atmospheric radiation. The reason may be that on the one hand the organic polymers in the alumina ceramic fibers undergo a certain degree of photodegradation under ultraviolet radiation, resulting in a loss of mechanical strength of the fibers and the occurrence of surface discoloration phenomena. On the other hand TiO in the fibre₂、SiO₂And the small amount of additive components can generate discolored oxides after high-temperature oxidation, and the doped ions are oxidized to generate a color change phenomenon. These factors all contribute significantly to the performance and application of the fiber. Therefore, it is needed to coat a sizing agent for improving the aging resistance of alumina continuous fibers on the surfaces of the alumina fibers to improve the surface state of the fibers. On one hand, the crack defect on the surface of the fiber is repaired, the fiber bundling property and the antistatic property are increased, and the surface of the fiber is enhanced to be free from external force damage; on the other hand, a protective film is formed on the surface of the fiber to protect the fiber from the corrosion of the aging environment.

The alumina continuous fiber has larger difference with glass fiber, quartz fiber and the like in components, and different preparation methods lead to difference in fiber surface charge, surface defect, diameter and the like, so the used impregnating compounds are different and can not be used universally, and a special impregnating compound suitable for the alumina continuous fiber needs to be developed.

At present, in the later-stage use process of the alumina continuous fiber, the problems of surface impregnating compound aging, fiber bundle strength reduction and the like easily occur to the fiber, and the use performance of the alumina continuous fiber is influenced. Meanwhile, the sizing agent also meets various requirements of subsequent use on the basis of solving the problems of poor bundling property and poor wear resistance in the spinning process. Therefore, with the increase of the subsequent use performance requirements of the fibers, the development of the impregnating compound for improving the aging resistance of the alumina continuous fibers is needed.

In patent document CN107382372A, a special impregnating compound for twisted yarn of alumina continuous fiber and a preparation method thereof are disclosed, wherein a film-forming agent is epoxy emulsion, and the prepared impregnating compound is milky liquid, and after the impregnating compound is coated on the surface of the fiber, the fiber gloss is poor; because the epoxy emulsion is easy to oxidize, the surface of the aluminum oxide fiber is yellow after the fiber coated with the impregnating compound is used for 5-7 months, and the strength is slightly reduced.

In general, the water-soluble resin is easy to age due to thermal oxidation after a high molecular polymer is completely dissolved in water to form a film, so that the service performance of the fiber is influenced; patent document CN105924966A discloses an anti-aging and water-resistant polyimide film and a preparation method thereof, wherein polyvinyl butyral is used as a raw material to be used as a water-resistant modifier to prepare the polyimide film, so that the water resistance of the polyimide film is improved, and the anti-aging effect is not achieved; patent document CN109616625A discloses a one-dimensional porous carbon fiber containing sulfide nanoparticles, and preparation and application thereof, wherein polyvinyl butyral is used as spinning precursor slurry to prepare the one-dimensional porous carbon fiber containing sulfide, which has good cycle performance and can greatly improve the electrochemical performance as a negative electrode material of a potassium ion battery; patent document CN109903886A discloses a front fine grid paste applied to a non-mesh-junction screen printing plate, and polyvinyl butyral is used as an organic carrier of resin for making the paste, so as to have good compatibility between the selected resin and a solvent, and the fine grid paste made by the method can improve the printing performance on the non-mesh-junction screen printing plate, thereby improving the photoelectric conversion effect of a solar cell; patent document CN101349145B discloses a basalt fiber for grafting and coating plasma-treated basalt fiber, which can replace polyvinyl butyral in a basalt cable of a steel sucker rod as a resin, wherein the polyvinyl butyral is prepared into a solution with a concentration of 2-15% by using gasoline, absolute ethyl alcohol and acetone solvents during work. The basalt fiber is subjected to plasma treatment firstly, and then is coated with a layer of high-density polyethylene resin, so that the prepared basalt cable has the advantages of light weight, good flexibility, high strength and chemical corrosion resistance, and can be used for replacing a sucker rod in the aspect of oil exploitation; in patent document CN1374355A, a peelable protective coating of polyvinyl butyral and a process for producing the same are disclosed, wherein polyvinyl butyral is modified and sprayed onto articles such as automobiles, furniture, and electrical appliances as a protective layer, so that the peelability of the polyvinyl butyral film is improved, and the peeled film can be recycled without being washed with water or solvent, thus having great environmental value.

Although the prior art discloses the polyvinyl butyral as a component, the prior art does not disclose how to apply the polyvinyl butyral to the alumina continuous fiber, and the formula disclosed in the patent document is directly applied to the surface of the alumina continuous fiber, and has the following defects: 1. the anti-aging effect is not obvious, the service cycle of the fiber and the improvement effect of subsequent processing and use are not ideal, and 2, the fiber cannot be bunched, the abrasion resistance of the fiber cannot be increased, and the mechanical property of the fiber cannot be improved.

Disclosure of Invention

In order to solve the problems, the application provides a sizing agent for improving the aging resistance of alumina continuous fibers, and a preparation method and application thereof.

On one hand, the application discloses a sizing agent for improving the aging resistance of alumina continuous fibers, which comprises the following components in percentage by weight: 0.5-2% of polyvinyl butyral resin, 0.5-2% of lubricant, 0.05-0.2% of antistatic agent and the balance of organic solvent.

The polyvinyl butyral resin is used as a film forming agent in the impregnating compound, PVB is short, the PVB resin is cationic resin and is easy to combine with anions on the surface of fibers, and the PVB contains hydroxyl, acetyl and aldehyde groups, so that the adhesive has good adhesive property, light stability and moisture resistance. The PVB molecule contains longer branched chain, so that the PVB has excellent flexibility, higher tensile strength and impact strength, and excellent film-forming property. In addition, PVB has high transparency and good ultraviolet resistance, and can absorb more than 99% of ultraviolet rays, thereby protecting internal fibers from aging.

Preferably, the polyvinyl butyral resin has a butyral content of 45 to 50 wt% and a viscosity of 15 to 18mPa^.s, molecular weight of 280-310.

Preferably, the lubricant is a non-ionic compound lubricant, and the non-ionic compound lubricant comprises one or more of triethylene glycol diisocaprylate, polyethylene glycol, tween 80, glycerol and span 80.

The lubricant in the application uses a non-ionic lubricant, has emulsification and antistatic effects, and has excellent functions of diffusion and fiber protection.

Preferably, the lubricant is triethylene glycol diisooctanoate.

Preferably, the lubricant is a mixture of triethylene glycol diisocaprylate and tween-80, and the mass ratio of the triethylene glycol diisocaprylate to the tween-80 is 2: (2.5-3.5).

Preferably, the mass ratio of the triethylene glycol diisocaprylate to the Tween-80 is 2: 3.

preferably, the antistatic agent is a quaternary ammonium salt antistatic agent, and the quaternary ammonium salt antistatic agent is hexadecyltrimethylammonium chloride. The wet-type antistatic impregnating compound film has strong moisture absorption, and can be dissociated into cations to neutralize anions on the surface of fibers when absorbing moisture, so that the repulsive force between the fibers is weakened, and a good antistatic effect is achieved.

Preferably, the organic solvent comprises one or more of methanol, isopropanol, n-propanol, ethanol, butanol, isobutanol, acetone.

Preferably, the organic solvent is a mixed solvent of acetone and ethanol, and the mass ratio of the acetone to the ethanol is 1: 9.

On the other hand, the application discloses a preparation method of the impregnating compound, which comprises the following steps:

s1: diluting a certain amount of polyvinyl butyral resin with 15-25 times of organic solvent, and stirring for 0.5-2 hours;

s2: diluting a certain amount of lubricant with 15-25 times of organic solvent, and stirring for 0.5-2 hours;

s3: dissolving a certain amount of antistatic agent by using 15-25 times of organic solvent, and stirring for 0.5-2 hours;

s4: and (5) sequentially adding the solutions obtained in the steps S1, S2 and S3 into the rest of the organic solvent, uniformly mixing, and stirring for 1-2 hours to obtain the impregnating compound for improving the aging resistance of the alumina continuous fibers.

On the other hand, the application discloses the application of the impregnating compound, the impregnating compound is uniformly coated on the surface of the alumina continuous fiber, and the alumina continuous fiber finished product is obtained after drying, wherein the coating rate of the impregnating compound is 1.4-1.9 wt%.

It can be understood that the coating rate of the sizing agent is (mass of the finished fiber-mass of the fiber strand)/mass of the fiber strand

This application can bring following beneficial effect:

1. the impregnating compound for improving the aging resistance of the alumina continuous fibers is coated on the surfaces of the fibers, so that the fibers can be protected from being corroded by environmental aging, the fibers can have a longer quality guarantee period, the fibers coated with the impregnating compound are subjected to high-temperature ultraviolet light irradiation for accelerated aging, the fibers cannot be damaged, the strand strength of the fibers can be improved, and the mechanical properties of the fibers can be improved.

2. The impregnating compound for improving the aging resistance of the alumina continuous fibers is colorless and transparent in appearance, stable and uniform, long in quality guarantee period and aging resistant, can be easily formed into films and attached to the alumina fibers, and enables the fibers to be glossier on the basis of keeping the appearance of the fibers.

3. The alumina continuous fiber coated by the impregnating compound can effectively meet the requirements of textile equipment, has small static electricity among tows and good friction resistance, so that the fiber has good bundling property and lubricity, and simultaneously has good mechanical property and processability.

Detailed Description