CN111793180A - 一种粉体酚醛树脂及其制备方法 - Google Patents
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- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
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Abstract
本发明公开了一种粉体酚醛树脂，其由固体树脂和六次甲基四胺按照质量比160～180∶20～30的比例粉碎制备而成，所述固体树脂由如下质量百分比的组份混合制备得到：苯酚55～65％、甲醛30～40％、酸性催化剂1.0％～1.5％、水3～5％、疏水剂0.1～0.5％。本发明的酚醛树脂具有价格低、无毒害、无污染，不易吸潮、分散性好，储存期长的特点。本发明通过在粉体酚醛树脂加入疏水剂改性物，起到阻碍水汽和臭氧侵入砂轮内部、提高树脂与无机磨料之间的粘结性的作用，从而有效改善树脂性能衰退并提高砂轮产品的使用性能。
Description
技术领域
本发明属于工业技术领域，涉及磨具技术领域，特别涉及一种抗衰退切割砂轮用粉体酚醛树脂及其制备方法。
背景技术
切割砂轮是固结磨具中最主要的一类磨具，是磨具中用量最大、使用面最广的一种。砂轮在使用时高速旋转，可对金属或非金属材料进行开槽和切断等。砂轮的特性主要是由磨料的种类和粒度、结合剂、填料、组织、形状和尺寸等因素决定。磨料是制造砂轮的主要原料，它担负着切削工作。因此，磨料必须锋利，并具备高的硬度、良好的耐热性和一定的韧性。
用传统酚醛树脂制作的切割砂轮产品，在运输和储存过程中由于水汽、光照和臭氧等外界因素的作用，会普遍存在砂轮产品的切割性能随储存时间而下降等问题。砂轮的切割性能下降又称为砂轮衰退性，一般切割砂轮从生产到客户使用的时间跨度有几周到几个月的时间，一些出口砂轮这一周期甚至达半年到一年以上，由于运输和储存过程中环境温度、湿度及光线的影响，切割砂轮在生产后一个月切割性能就下降30-40％，三个月下降50％左右，对生产商和客户都造成较大损失。目前，市场上已经普遍采用真空塑封包装并在阴暗处保存的方式，减轻了砂轮的衰退速度，但是这样的方法没有彻底地解决问题。
发明内容
为了解决上述的问题，本发明的目的是提供一种抗衰退切割砂轮用粉体酚醛树脂及其制备方法。
为了实现上述发明目的，本发明提供以下技术方案：粉体酚醛树脂，其由固体树脂和六次甲基四胺按照质量比160～180∶20～30的比例，优选为173∶27粉碎制备而成，所述固体树脂由如下质量百分比的组份混合制备得到：苯酚55～65％、甲醛30～40％、酸性催化剂1.0％～1.5％、水3～5％、疏水剂0.1～0.5％。
粉体酚醛树脂，其由固体树脂和六次甲基四胺按照质量比173∶27的比例进行粉碎制作而成，所述固体树脂由如下质量百分比的组份混合制备得到：苯酚55～65％、甲醛30～40％、酸性催化剂1.0％～1.5％、水3～5％、消泡剂0.05～0.2％、疏水剂0.1～0.5％。
所述酸性催化剂为有机催化剂，优选为草酸或柠檬酸。
所述疏水剂选自含氟硅油、反应型疏水界面改性剂等的一种或几种混合；所述消泡剂选自有机硅类、聚醚类消泡剂。
本发明还提供了一种粉体酚醛树脂的制备方法，包括如下步骤：
(1)将一定量的苯酚、酸性催化剂和甲醛溶液投入反应容器中，在100～102℃温度下回流反应一定时间，
(2)然后常压脱水至温度达到145～155℃，再进行真空脱水至温度达到165～175℃，保温真空一段时间，直至取样检测游离酚和流动度的指标达到要求，
(3)加入疏水剂搅拌均匀后，放料制片即可获得热塑性酚醛树脂，再加入六次甲基四胺一起进行打粉，最终得到砂轮用粉体酚醛树脂；
所述步骤(1)中，在100～102℃下回流反应1.5～2.5小时；在90～95℃条件下加入甲醛。
所述步骤(2)中，在165～175℃保温1.5～2.5小时，检测游离酚达到≤1.5％、流动度达到25～35mm时，符合要求。
在所述步骤(2)的真空脱水至温度达到165～175℃后，加入适量消泡剂，继续保温真空一段时间。
本发明还提供了一种抗衰退切割砂轮，其由如下重量份的组份制备而成：46#煅烧棕刚玉90～110、60#煅烧棕刚玉90～110、冰晶石粉15～20、硫化铁8～12、炭黑0.5-1、粉体酚醛树脂40～50、液体酚醛树脂10～15。
所述体酚醛树脂，由如下质量百分比的组份混合制备得到：苯酚40～50％、甲醛45～57％、碱性催化剂0.5％～1.0％、糠醇1.0～3.0％、尿素0.5～2.0％，硅烷偶联剂0.01～0.5％。碱性催化剂为无机催化剂，优选为NaOH、KOH或氨水；所述硅烷偶联剂选自A151(乙烯基三乙氧基硅烷)、A171(乙烯基三甲氧基硅烷)、A172(乙烯基三(β-甲氧乙氧基)硅烷)等中的一种或几种混合。
液体酚醛树脂的制备方法，包括如下步骤：
(1)用一定量苯酚、甲醛和碱性催化剂投入反应容器，在85±1℃温度下恒温进行加成缩合聚合反应，当水溶性比值达到80％～100％时降温，降温到50℃以下；优选为40～50℃，否则游离酚和固含量会出现过高或者过低；
(2)加入酸或碱调节pH值，再加入尿素进行缩聚反应20～30分钟，然后真空负压脱水至粘度＝1200～1600cps，
(3)加入糠醇改性，调节粘度范围不变，最后加入硅烷偶联剂，搅拌均匀降温放料保存即可得到液体酚醛树脂。
本发明的优点：
本发明中的粉体酚醛树脂与液体酚醛树脂、磨料和填料经混料、成型、固化制成切割砂轮，由于粉体酚醛树脂含有疏水性能优良的疏水剂，在运输、储存过程中能够防止空气中的水汽侵入磨料与树脂结合剂的缝隙中，减轻树脂的降解速度和界面剥离速度，使砂轮的抗衰退性能大大提高。本发明中粉体酚醛树脂添加的疏水剂，是一种反应型表面处理剂。
具体实施方式
以下结合具体实施例对上述方案做进一步说明。应理解，这些实施例是用于说明本发明而不限于限制本发明的范围。实施例中采用的实施条件可以根据具体厂家的条件做进一步调整，未注明的实施条件通常为常规实验中的条件。
实施例：
称取1000g苯酚和80g草酸与水(草酸∶水＝20∶60)的混合液加入反应瓶中，再加入673g的37％甲醛溶液，100～102℃下回流反应2个小时后常压脱水至150℃，再转换为负压真空脱水至170℃，维持170℃一个小时后取样检测游离酚和流动度，测得游离酚＝1.28％、流动度＝33mm(游离酚≤1.5％、流动度达到25～35mm)时，加入树脂质量1.5‰～2.5‰的疏水剂，搅拌均匀后放料制片，再按照固体树脂∶六次甲基四胺＝173∶27的比例进行打粉制作粉体酚醛树脂；
对照例：
称取1000g苯酚和80g草酸与水(草酸∶水＝20∶60)的混合液加入反应瓶中，再加入673g的37％甲醛溶液，100～102℃下回流反应2个小时后常压脱水至150℃，再转换为负压真空脱水至170℃，维持170℃一个小时后取样检测游离酚和流动度，测得游离酚＝1.39％、流动度＝32mm(游离酚≤1.5％、流动度达到25～35mm)时，放料制片，再按照固体树脂∶六次甲基四胺＝173∶27的比例进行粉碎制成粉体酚醛树脂。
比较：将实施例的树脂和对照例按表1进行混料、困料、成型和高温固化制备切割砂轮，具体方法和现有技术相同，在此不再赘述；制得规格为125x1.2x22的超薄切割砂轮成品后，测试两种砂轮初始和50天后切割Φ16钢棒的切割性能。
表1，切割砂轮配方表
| 原料 | 重量(公斤) |
| 46#煅烧棕刚玉 | 50 |
| 60#煅烧棕刚玉 | 50 |
| 冰晶石粉 | 8 |
| 硫化铁 | 5 |
| 炭黑 | 0.5 |
| 粉体酚醛树脂 | 21 |
| 液体酚醛树脂 | 6 |
表2，砂轮切割性能对比
| 实施例 | 初始切割次数 | 50天后切割次数 | 保留值 |
| 对照例 | 124 | 87 | 70％ |
| 实施例 | 128 | 116 | 90.6％ |
注：保留值＝50天后切割次数/初始切割次数*100％
由上表数据对比可以得出结论：
由表2对比可知，本发明实施例中粉体酚醛树脂由于添加了疏水剂，能够阻止水汽侵入砂轮内部，能够有效的提高砂轮的抗衰退性能。
综上所述，本发明中通过添加了疏水剂进行改性，明显地改善了砂轮用酚醛树脂性能衰退的不足。本发明通过在粉体酚醛树脂加入疏水剂改性物，起到阻碍水汽和臭氧侵入砂轮内部、提高树脂与无机磨料之间的粘结性的作用，从而有效改善树脂性能衰退并提高砂轮产品的使用性能。
上述实例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所做的等效变换或修饰，都应涵盖在本发明的保护范围之内。
Claims (9)
1.一种粉体酚醛树脂，其特征在于，其由固体树脂和六次甲基四胺按照质量比160～180∶20～30的比例粉碎制备而成，所述固体树脂由如下质量百分比的组份混合制备得到：苯酚55-65％、甲醛30-40％、酸性催化剂1.0％～1.5％、水3-5％、疏水剂0.1-0.5％。
2.根据权利要求1所述的粉体酚醛树脂，其特征在于，所述固体树脂由如下质量百分比的组份混合制备得到：苯酚55～65％、甲醛30～40％、酸性催化剂1.0％～1.5％、水3～5％、消泡剂0.05～0.2％、疏水剂0.1～0.5％。
3.根据权利要求1或2所述的粉体酚醛树脂，其特征在于，所述酸性催化剂为草酸或柠檬酸。
4.根据权利要求1或2所述的粉体酚醛树脂，其特征在于，所述疏水剂选自含氟硅油、反应型疏水界面改性剂中的一种或几种混合。
5.根据权利要求2所述的粉体酚醛树脂，其特征在于，所述消泡剂选自有机硅类或聚醚类消泡剂。
6.如权利要求1-5所述的粉体酚醛树脂的制备方法，其特征在于，包括如下步骤：
(1)将一定量的苯酚、酸性催化剂和甲醛溶液投入反应容器中，在100～102℃温度下回流反应一定时间，
(2)然后常压脱水至温度达到145～155℃，再进行真空脱水至温度达到165～175℃，保温真空一段时间，直至取样检测游离酚和流动度的指标达到要求，
(3)加入疏水剂搅拌均匀后，放料制片即可获得热塑性酚醛树脂，再加入六次甲基四胺一起进行打粉，最终得到砂轮用粉体酚醛树脂。
7.根据权利要求6所述的制备方法，其特征在于，所述步骤(1)中，在100～102℃下回流反应1.5～2.5小时，在90～95℃条件下加入甲醛。
8.根据权利要求6所述的制备方法，其特征在于，所述步骤(2)中，在165～175℃保温1.5-2.5小时，检测游离酚达到≤1.5％、流动度达到25～35mm时，符合要求。
9.根据权利要求6所述的制备方法，其特征在于，在所述步骤(2)的真空脱水至温度达到165～175℃后，加入适量消泡剂，继续保温真空一段时间。
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| CN112430298A (zh) * | 2020-11-23 | 2021-03-02 | 山东仁丰特种材料股份有限公司 | 快速固化有机硅改性酚醛树脂的制备方法 |
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