阅读说明：本技术 一种含有纳米氧化锌的高性能橡胶的加工方法 (Processing method of high-performance rubber containing nano zinc oxide ) 是由 刘艺 于 2019-10-28 设计创作，主要内容包括：本发明公开了一种含有纳米氧化锌的高性能橡胶的加工方法,包括如下步骤：S1、纳米氧化锌表面处理；S2、聚乙烯醇水溶液制备；S3、混合料水溶液制备；S4、固体混合物制备；S5、活化纳米氧化锌制备；S6、成品橡胶制备。本发明提供了一种橡胶的加工方法,其整体的工艺简单,各步骤搭配合理,利于商业化推广应用,制得的橡胶力学品质好,使用稳定性高,寿命长。(The invention discloses a processing method of high-performance rubber containing nano zinc oxide, which comprises the following steps: s1, surface treatment of nano zinc oxide; s2, preparing a polyvinyl alcohol aqueous solution; s3, preparing a mixture water solution; s4, preparing a solid mixture; s5, preparing activated nano zinc oxide; s6, preparing finished rubber. The invention provides a processing method of rubber, which has the advantages of simple integral process, reasonable matching of all steps, good mechanical quality of the prepared rubber, high use stability and long service life, and is beneficial to commercial popularization and application.)

1. A processing method of high-performance rubber containing nano zinc oxide is characterized by comprising the following steps:

s1, firstly, soaking the nano zinc oxide into a coupling agent solution, continuously carrying out ultrasonic treatment for 1-2 h, filtering, washing with deionized water once, and drying for later use;

s2, mixing the polyvinyl alcohol and the deionized water together, putting the mixture into a stirring tank, and uniformly stirring at a medium speed to obtain a polyvinyl alcohol aqueous solution for later use;

s3, adding zinc nitrate hexahydrate and the nano zinc oxide treated in the step S1 into the stirring tank in the step S2, and uniformly stirring at a high speed to obtain a mixture water solution for later use;

s4, fully pre-freezing the mixture water solution prepared in the step S3, putting the mixture water solution into a vacuum freeze drying oven for freeze drying treatment, and taking out the mixture water solution to obtain a solid mixture for later use;

s5, putting the solid mixture prepared in the step S4 into a muffle furnace for calcination, and taking out the solid mixture for 4-6 hours to obtain activated nano zinc oxide for later use;

s6, mixing the activated nano zinc oxide prepared in the step S5, a rubber matrix, an accelerator, an anti-aging agent and sulfur together, putting the mixture into an open mill for mixing treatment, and taking out the mixture after the mixing treatment to obtain the finished rubber product.

2. The processing method of high-performance rubber containing nano zinc oxide according to claim 1, wherein the coupling agent solution in step S1 is a silane coupling agent aqueous solution, and the mass fraction of the silane coupling agent in the silane coupling agent aqueous solution is 12-15%; the silane coupling agent is any one of a silane coupling agent kh550, a silane coupling agent kh560 and a silane coupling agent kh 570.

3. The processing method of the high-performance rubber containing nano zinc oxide according to claim 1, wherein the ultrasonic frequency is controlled to be 600 to 700kHz during the ultrasonic treatment in the step S1; the drying temperature is 85-90 ℃, and the drying time is 3-4 h.

4. The processing method of high-performance rubber containing nano zinc oxide according to claim 1, wherein the weight ratio of the polyvinyl alcohol mixed with the deionized water in step S2 is 0.5-1: 20; and controlling the stirring speed to be 1400-1600 revolutions per minute during medium-speed stirring treatment.

5. The processing method of high-performance rubber containing nano zinc oxide according to claim 1, wherein the addition amount of zinc nitrate hexahydrate in step S3 is 3-4 times of the total mass of polyvinyl alcohol; the adding amount of the nano zinc oxide treated in the step S1 is 1-1.5 times of the total mass of the polyvinyl alcohol; and the rotating speed of stirring is controlled to be 2200-2400 rpm during high-speed stirring treatment.

6. The method for processing the high-performance rubber containing nano zinc oxide according to claim 1, wherein the temperature in the vacuum freeze drying oven is controlled to be-30 to-35 ℃ and the pressure in the vacuum freeze drying oven is controlled to be 1 to 10Pa during the freeze drying process in step S4.

7. The method for processing high-performance rubber containing nano zinc oxide according to claim 1, wherein the temperature in the muffle furnace is controlled to be 680-720 ℃ during the calcination treatment in step S5.

8. The processing method of high-performance rubber containing nano-zinc oxide according to claim 1, wherein the weight ratio of the activated nano-zinc oxide, the rubber matrix, the accelerator, the anti-aging agent and the sulfur in the step S6 is 2-3: 100-110: 2.5-3.5: 1-1.5: 3-5; and controlling the temperature in the open mill to be 55-60 ℃ during mixing treatment.

Technical Field

The invention belongs to the technical field of rubber preparation, and particularly relates to a processing method of high-performance rubber containing nano zinc oxide.

Background

Rubber is a high polymer material with excellent elasticity, is widely used for manufacturing automobile tires, waterproof sheets, adhesive tapes, rubber tubes, sealing elements and the like, has a history of nearly one hundred years, in the process of applying rubber materials, various fillers are usually added into rubber materials to improve the performance of the rubber materials and meet various performances such as strength, wear resistance, ageing resistance and the like required by modern engineering, when the structural units of the materials are as small as a nanometer level, the properties of the materials are changed greatly, the properties of the original materials are obviously improved, new properties or effects are generated, namely the special small-size effect, quantum effect and volume effect of the nanometer materials, zinc oxide is used as a traditional rubber filler, is mainly used as an active agent in the rubber and is used as a reinforcing agent and a coloring agent, and the properties of the zinc oxide influence the performance of the zinc oxide in the rubber, the service life of the hydraulic shock absorber used for the automobile is as low as 180-220 ten thousand times, the shock insulation block prepared from the rubber is matched with the hydraulic shock absorber, and the service life of the shock insulation block prepared from the rubber often cannot meet the corresponding requirement, so that the comprehensive service life of the hydraulic shock absorber is greatly influenced. When the nano zinc oxide commonly used in the prior art is used as an inorganic filler for filling, the nano zinc oxide has very high surface energy, is hydrophilic and oleophobic and has strong polarity, is easy to agglomerate in the mixing process, has small acting force with a rubber matrix and poor reinforcing effect, and causes poor adding and using effect and needs continuous improvement treatment.

Disclosure of Invention

The invention aims to provide a processing method of high-performance rubber containing nano zinc oxide aiming at the existing problems.

The invention is realized by the following technical scheme:

a processing method of high-performance rubber containing nano zinc oxide comprises the following steps:

s1, firstly, soaking the nano zinc oxide into a coupling agent solution, continuously carrying out ultrasonic treatment for 1-2 h, filtering, washing with deionized water once, and drying for later use;

s2, mixing the polyvinyl alcohol and the deionized water together, putting the mixture into a stirring tank, and uniformly stirring at a medium speed to obtain a polyvinyl alcohol aqueous solution for later use;

s3, adding zinc nitrate hexahydrate and the nano zinc oxide treated in the step S1 into the stirring tank in the step S2, and uniformly stirring at a high speed to obtain a mixture water solution for later use;

s4, fully pre-freezing the mixture water solution prepared in the step S3, putting the mixture water solution into a vacuum freeze drying oven for freeze drying treatment, and taking out the mixture water solution to obtain a solid mixture for later use;

s5, putting the solid mixture prepared in the step S4 into a muffle furnace for calcination, and taking out the solid mixture for 4-6 hours to obtain activated nano zinc oxide for later use;

s6, mixing the activated nano zinc oxide prepared in the step S5, a rubber matrix, an accelerator, an anti-aging agent and sulfur together, putting the mixture into an open mill for mixing treatment, and taking out the mixture after the mixing treatment to obtain the finished rubber product.

Further, the coupling agent solution in the step S1 is a silane coupling agent aqueous solution, and the mass fraction of the silane coupling agent in the silane coupling agent aqueous solution is 12-15%; the silane coupling agent is any one of a silane coupling agent kh550, a silane coupling agent kh560 and a silane coupling agent kh 570.

Further, the frequency of the ultrasonic wave is controlled to be 600-700 kHz during the ultrasonic treatment in the step S1; the drying temperature is 85-90 ℃, and the drying time is 3-4 h.

Further, the weight ratio of the polyvinyl alcohol and the deionized water in the step S2 is 0.5-1: 20; and controlling the stirring speed to be 1400-1600 revolutions per minute during medium-speed stirring treatment.

Further, the adding amount of the zinc nitrate hexahydrate in the step S3 is 3-4 times of the total mass of the polyvinyl alcohol; the adding amount of the nano zinc oxide treated in the step S1 is 1-1.5 times of the total mass of the polyvinyl alcohol; and the rotating speed of stirring is controlled to be 2200-2400 rpm during high-speed stirring treatment.

Further, the temperature in the vacuum freeze drying box is controlled to be-30 to-35 ℃ and the pressure is controlled to be 1 to 10Pa during the freeze drying treatment in the step S4.

Further, the temperature in the muffle furnace is controlled to be 680 to 720 ℃ during the calcination treatment in step S5.

Further, the activated nano zinc oxide, the rubber matrix, the accelerator, the anti-aging agent and the sulfur in the step S6 are mixed according to the weight ratio of 2-3: 100-110: 2.5-3.5: 1-1.5: 3-5; and controlling the temperature in the open mill to be 55-60 ℃ during mixing treatment.

The invention provides a novel processing method of rubber, wherein a nano zinc oxide component is still added, and the processing method is different from the prior art, the adding and using mode of the nano zinc oxide is optimized, in order to improve the filling and dispersing uniformity of the nano zinc oxide, the prior art generally carries out surface modification treatment on the nano zinc oxide and then carries out filling, the common modification treatment is surface modification treatment of a coupling agent, the surface modification treatment of the coupling agent is to attach a coupling agent film layer on the surface of the nano zinc oxide, although the uniform dispersion effect is achieved, the surface characteristics of the nano zinc oxide have no special influence on the initial surface structure and the morphological characteristics of the nano zinc oxide, but the vulcanization of the rubber and the crosslinking degree between the nano zinc oxide and a rubber matrix are influenced, and an activated nano zinc oxide is prepared firstly on the basis of the processing method, compared with the conventional preparation method of nano zinc oxide, the invention firstly actively adds the nano zinc oxide after surface treatment in the precursor, aims at ensuring that the nano zinc oxide after surface treatment of the coupling agent has good surface activity and good dispersion effect, when the precursor is decomposed to generate a finished product, the dispersed nano zinc oxide after surface treatment can be used as an anchor point to realize the attachment and combination of the nascent nano zinc oxide, because the interface action of the coupling agent can not influence the particle fineness of the nascent nano zinc oxide and can also endow the nascent nano zinc oxide with good surface performance, the most important point is that the nano zinc oxide after surface treatment added in advance has a guiding function, the particle uniformity of the nascent nano zinc oxide is improved, the overall appearance is in an ellipsoid shape, the surface structure appearance is in a shape, the filling and using effects are obviously improved, and finally the nano zinc oxide is added in the traditional preparation of rubber, the service performance of the rubber is obviously improved.

Compared with the prior art, the invention has the following advantages:

the invention provides a processing method of rubber, which has simple integral process and reasonable matching of all steps, is beneficial to commercial popularization and application, and the prepared rubber has good mechanical quality, high use stability, long service life, and great market competitiveness and economic benefit.

Detailed Description

The invention is further illustrated by the following examples.

A processing method of high-performance rubber containing nano zinc oxide comprises the following steps:

s1, firstly, soaking the nano zinc oxide into a coupling agent solution, continuously carrying out ultrasonic treatment for 1-2 h, filtering, washing with deionized water once, and drying for later use;

s2, mixing the polyvinyl alcohol and the deionized water together, putting the mixture into a stirring tank, and uniformly stirring at a medium speed to obtain a polyvinyl alcohol aqueous solution for later use;

s3, adding zinc nitrate hexahydrate and the nano zinc oxide treated in the step S1 into the stirring tank in the step S2, and uniformly stirring at a high speed to obtain a mixture water solution for later use;

s4, fully pre-freezing the mixture water solution prepared in the step S3, putting the mixture water solution into a vacuum freeze drying oven for freeze drying treatment, and taking out the mixture water solution to obtain a solid mixture for later use;

s5, putting the solid mixture prepared in the step S4 into a muffle furnace for calcination, and taking out the solid mixture for 4-6 hours to obtain activated nano zinc oxide for later use;

s6, mixing the activated nano zinc oxide prepared in the step S5, a rubber matrix, an accelerator, an anti-aging agent and sulfur together, putting the mixture into an open mill for mixing treatment, and taking out the mixture after the mixing treatment to obtain the finished rubber product.