CN107459750B - 一种软质cpvc组合物的成型方法 - Google Patents
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- C08L27/22—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers modified by chemical after-treatment
- C08L27/24—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers modified by chemical after-treatment halogenated
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Abstract
一种软质CPVC组合物的成型方法,属于软质CPVC组合物加工技术领域。1)将CPVC树脂和助剂加入高速搅拌混合机,105~120℃,转速1000~1400r/min,搅拌混合8~15min;放料至低速搅拌机中冷却至50℃以下,得干混料;2)将干混料置于密炼机熔腔中,将液体增塑剂分1~5次加入密炼机中,160~200℃塑炼3~10min,得塑化块;3)将塑化块挤出、造粒,得CPVC树脂粒料;或者,将塑化块经压延制得CPVC软质片材;CPVC树脂、助剂和液体增塑剂质量比100:2~70:25~85。该成型方法解决了制备软质CPVC时由于高比例增塑剂添加导致的组合物难以成型的问题。
Description
技术领域
本发明涉及一种软质CPVC组合物的成型方法,属于软质CPVC组合物加工技术领域。
背景技术
塑料加工(如PVC制品)一般需要进行预混制取干混料,然后再进行塑炼加工。现有的塑料混合工艺有以下3种:1)普通捏合开炼塑化混合工艺流程:称量原材料→普通捏合机捏合(制取干混料)→开放式炼塑机塑化→开炼机冷却下片→平板造粒机切粒。2)高速混合密炼塑化混合工艺流程:称量原材料→高速混合机捏合(制取干混料)→密炼机塑化→开炼机冷却下片→平板造粒机切粒。3)高速混合挤出造粒工艺流程:称量原材料→高速捏合机捏合(制取干混料)→挤出机(单螺杆、双螺杆或双阶挤出机)塑炼→造粒机。由以上3种塑料混合工艺可看出,塑料加工一般需要按照配方用量要求将所用全部原材料进行预混,制得干混料,然后再进行塑炼加工。CPVC的增塑剂吸收速率慢,制备CPVC软制品时,预混过程中,增塑剂尚没有被吸收完全即形成塑化块,难以制得干混料,以至难以制成CPVC软制品。
在申请号为201510331367.6专利“一种耐温125℃等级CPVC电线电缆料及其生产方法”中介绍了这样一种混合料制备工艺:1)将CPVC 树脂加入到高速混合机中,再加入粉体稳定剂,低速混合1~3 分钟后,加入组分一半的增塑剂,混合机由低速转入高速混合3~5分钟后,加入另一半组分的增塑剂,混合机由低速转入高速混合到80~90℃,最后加入碳酸钙、阻燃剂、煅烧陶土、润滑剂,低速混合后转入高速混合,温度到115~125℃后获得混合料。2)将混合料加入到密炼机中,密炼温度为160~170℃,密炼8~10 分钟后获取熟料,通过长径比较大的单螺杆挤出机在170~185℃下造粒,获得耐温125℃等级CPVC 电线电缆料成品母料。使用该制备方法步骤1),由于增塑剂吸收慢,低温下几乎不吸收,CPVC软制品物料呈溶胀状态或糊状(与增塑剂量有关),80~90℃后,物料易形成半塑化弹性块状物,不能形成流动性干混料,不但影响了物料混合的均匀性,还导致混合物难以顺利甚至不能从高速混合机放料口放出,大大影响了生产效率。众所周知,这种未充分混合的料块即使再放入密炼机中塑炼,其混合均匀性亦差,会影响制品的物理机械性能。
发明内容
本发明要解决的技术问题是:克服现有技术的不足,提供一种软质CPVC组合物的成型方法,该方法解决了制备软质CPVC时由于高比例增塑剂添加导致的组合物难以成型的问题。
本发明解决其技术问题所采用的技术方案是:该软质CPVC组合物的成型方法,其特征在于,包括如下步骤:
1)将CPVC树脂和助剂加入高速搅拌混合机,105~120℃,转速1000~1400r/min,搅拌混合8~15min;放料至低速搅拌机中搅拌、冷却至50℃以下放出,得干混料;
2)将干混料置于密炼机熔腔中,将液体增塑剂分1~5次加入密炼机中,160~200℃塑炼3~10min,得塑化块;
3)将塑化块加入挤出机,经挤出、造粒,制得CPVC树脂粒料;或者,将塑化块加入压延机,经压延制得CPVC软质片材;
所述的CPVC树脂、助剂和液体增塑剂的质量比为100: 2~70:25~85;
所述的助剂包括稳定剂和润滑剂。
所述的助剂包括稳定剂和润滑剂,还包括改性剂、填充剂、抗氧剂中的至少一种。
所述的助剂包括稳定剂、润滑剂和填充剂,CPVC树脂、助剂和液体增塑剂的质量比为100: 30~70:40~85。
所述的液体增塑剂为邻苯二甲酸酯类增塑剂、脂肪族二元酸酯类增塑剂、苯甲酸酯类增塑剂、磷酸酯类增塑剂、环氧化合物类增塑剂、石油酯类增塑剂、氯化碳氢化合物类增塑剂、柠檬酸酯类增塑剂、聚酯类增塑剂、苯多酸酯类增塑剂中的一种或两种。
所述的液体增塑剂为邻苯二甲酸酯(简写DOP)。
所述的稳定剂为有机锡稳定剂,润滑剂为石蜡、硬脂酸、硬脂酸镁、聚乙烯蜡、氧化聚乙烯蜡中的两种。
所述的改性剂为双酚A,填充剂为活性碳酸钙。
所述的CPVC 树脂氯含量在质量百分比66 ~75%。
步骤2)的具体操作为:将干混料置于密炼机熔腔中,将液体增塑剂分1~5次加入密炼机中,塑炼3~5min,塑炼温度180~190℃,制得塑化块。
步骤3)所述的挤出机为螺杆挤出机,螺杆挤出机自加料段至挤出段温度为170~190℃。螺杆挤出机自加料段至挤出段温度可设计多个测温点,优选的有4~6个测温点。
步骤3)所述的压延机为L型四辊压延机,压延温度为155~165℃。
对于本发明的说明如下:
申请人经研究发现:软质CPVC无法制得干混料的原因与增塑剂的用量和成型方法有关,CPVC树脂氯含量大于66%。CPVC分子链上的氯具有很强的极性,随着氯含量提高,CPVC分子链间作用力增强,CPVC树脂的耐热性提高,维卡软化温度提高,但是吸收增塑剂的速度随氯含量提高明显下降,优选的CPVC 树脂氯含量在质量百分比66 ~75%。现有的制作硬质CPVC的工艺不能直接用作软质CPVC。硬质CPVC中增塑剂的添加量少,而软质CPVC中需要添加大用量的增塑剂,而CPVC树脂与增塑剂搅拌混合时,由于增塑剂吸收慢,低温下几乎不吸收,大用量的增塑剂导致CPVC软制品物料呈溶胀状态或糊状,难以形成干混料,工艺无法继续进行。申请人通过研究设计添加的增塑剂为液体增塑剂,液体增塑剂分散效果较好,便于与CPVC树脂混合。润滑剂便于组合物的挤出,稳定剂和填充剂会增加增塑剂吸收量,有利于混合。活性碳酸钙的粒径小于0.1微米。
申请人通过研究发现:步骤1)中助剂可根据生产配方需要添加。但本发明步骤1)和2)的顺序不能替换、步骤1)中的原料不能更改。如在步骤1)中添加了液体增塑剂,则会导致步骤1)无法获得干混料。本发明成型方法分三步:在步骤,1)中,先将CPVC软质配方中除增塑剂外的组分加入高速搅拌机(转速为1000~1400r/min)中,高速搅拌至105~115℃,混合时间为6~15min,然后放至低速搅拌釜中搅拌冷却至50℃以下放出,即为干混料;通过制得干混料将材料进行预混合,步骤1)由于没有添加增塑剂的干扰,干混料能够成型、且干混料中的各组分混合均匀。在步骤2)中,先按照密炼机容量称取定量干混料置于密炼机熔腔(密炼机密炼腔室仅有顶部加料口,其他处密封)中,然后将液体增塑剂25~80份根据用量分1~5次加入密炼室塑炼;优选的所述液体增塑剂份3~5次加入,增塑剂每次加入量相等,逐步加入液体增塑剂,能够避免一次性加入大用量的增塑剂导致的CPVC软制品物料呈溶胀状态或糊状现象。在步骤3)中,将塑炼好的塑化块置于压延机上压延成型,或置于带有输送螺杆和保温功能的挤出机料斗中,通过挤出机造粒或加工成型。步骤3)中螺杆挤出机自加料段至挤出段温度为170℃~190℃。螺杆挤出机自加料段至挤出段温度可设计多个测温点,优选的螺杆挤出机自加料段至挤出段有4~6个测温点。
与现有技术相比,本发明的一种软质CPVC组合物的成型方法及其制作方法所具有的有益效果是:该软质CPVC组合物的成型方法解决了制备软质CPVC时由于高比例增塑剂添加导致的组合物难以成型的问题。通过先将配方中除增塑剂外各组分在高低速混合机中制成干混料,然后于密炼机中塑炼混合干混料与增塑剂的方法,解决了用传统工艺制备CPVC软制品配混料时存在的结块、不能制成干混料,导致原材料混合均匀性差和生产效率低的问题,大大促进了具有优良综合性能的CPVC树脂在软制品上的应用。
具体实施方式
实施例1~4是本发明的一种软质CPVC组合物的成型方法及其制作方法的具体实施方式,其中实施例1为最佳实施例。对比例与实施例配方见表1。所用设备:张家港市万塑机械有限公司制造的的100L/200L型高速混合机组;南通科诚橡塑机械有限公司制造的kcd30型3L密炼+30单螺杆造粒机组;大连嘉尔新橡塑机械有限公司制造的倒L型四辊压延机。表1中所用CPVC树脂为潍坊高信科技有限公司所产J-700型CPVC树脂,有机锡稳定剂为美国罗门哈斯生产的产TM-181FS型有机锡,DOP为山东蓝帆塑胶股份有限公司生产的增塑剂,HSt为莱阳化工实验厂生产的硬脂酸,半精炼石蜡为中国大庆石油炼化公司产品,双酚A为上海肯高贸易有限公司产品,微细活性碳酸钙为常州碳酸钙有限公司产品。
表1实施例和对比例配方
实施例1
1)按配比称取除DOP以外的各组分,将称取物料加入加入高速搅拌混合机(转速为1000~1400r/min)中,高速搅拌至110℃,混合时间为10min,然后放料至低速搅拌机中搅拌,转速600~700r/min,冷却至50℃以下放出,即为干混料;
2)称取4kg干混料置于密炼机熔腔中,然后称取0.96kg(25份)DOP一次加入密炼室中塑炼5min,制得塑炼均匀的塑化块;
3)将塑炼好的塑化块置于双螺杆加料斗中,通过单螺杆挤出机挤出热切造粒。根据造粒速度和密炼时间调节密炼频次,实现间歇密炼到连续造粒的转化,保证连续化生产,提高了生产效率。密炼温度为190℃,挤出机自加料段至挤出段温度分别为170℃,180℃,185℃,190℃。CPVC树脂粒料可以根据需要加工成所需制品。
实施例2
1)按配比称取除DOP以外的各组分,将称取物料加入加入高速搅拌混合机(转速为1000~1400r/min)中,高速搅拌至110℃,混合时间为10min,然后放料至低速搅拌机中搅拌,转速600~700r/min,冷却至50℃以下放出,即为干混料;
2)称取4kg干混料置于密炼机熔腔中,然后1.11kg(40份)DOP根据一次加入密炼室中塑炼4min,制得塑炼均匀的塑化块;
3)将塑炼好的塑化块置于双螺杆加料斗中,通过单螺杆挤出机挤出热切造粒。密炼温度为180℃,挤出机自加料段至挤出段温度分别为160℃,170℃,180℃,180℃。CPVC树脂粒料可以根据需要加工成所需制品。
实施例3
1)按配比称取除DOP以外的各组分,将称取物料加入加入高速搅拌机(转速为1000~1400r/min)中,高速搅拌至110℃,混合时间为10min,然后放料至低速搅拌机中搅拌,转速600~700r/min,冷却至50℃以下放出,即为干混料;
2)称取4kg干混料置于密炼机熔腔中,然后1.68kg(60份)DOP根据一次加入密炼室中塑炼3min,制得塑炼均匀的塑化块;
3)将塑炼好的塑化块置于倒L型四辊压延机上,通过压延制得CPVC树脂软质片材。密炼温度为170℃,压延温度为160℃。
实施例4
1)按配比称取除DOP以外的各组分,将称取物料加入加入高速搅拌机(转速为1000~1400r/min)中,高速搅拌至110℃,混合时间为10min,然后放料至低速搅拌机中搅拌,转速600~700r/min,冷却至50℃以下放出,即为干混料;
2)称取4kg干混料置于密炼机熔腔中,然后2.24kg(80份)DOP根据一次加入密炼室中塑炼3min,制得塑炼均匀的塑化块;
3)将塑炼好的塑化块置于倒L型四辊压延机上,通过压延制得CPVC树脂软质片材。密炼温度为160℃,压延温度为155℃。
对比例1
本对比例配方和步骤1)~3)各项操作和参数,均与实施例1相同,区别在于:步骤1)中将包括增塑剂DOP在内的所有原料加入高速搅拌机。然后逐步进行实施例1中步骤1)~3)的操作。
申请人发现:对比例1在进行步骤1)的操作时,由于在步骤1)中添加了大用量的增塑剂DOP,随着温度升高,物料形成半塑化弹性块状物,不能形成流动性干混料充分混合,出料口堵塞,不能顺利出料。最终导致对比例1的步骤1)无法获得干混料,步骤1)无法顺利进行,自然也无法继续进行步骤2)~3)的操作,最终无法获得软质CPVC制品。而本发明实施例1~4能够获得CPVC树脂粒料或者CPVC树脂软质片材,实现了高增塑剂用量时的软质CPVC组合物的成型。
以上所述,仅是本发明的较佳实施例而已,并非是对本发明作其它形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (10)
1.一种软质CPVC组合物的成型方法,其特征在于,包括如下步骤:
1)将CPVC树脂和助剂加入高速搅拌混合机,105~120℃,转速1000~1400r/min,搅拌混合8~15min;放料至低速搅拌机中搅拌、冷却至50℃以下放出,得干混料;
2)将干混料置于密炼机熔腔中,将液体增塑剂分1~5次加入密炼机中,160~200℃塑炼3~10min,得塑化块;
3)将塑化块加入挤出机,经挤出、造粒,制得CPVC树脂粒料;或者,将塑化块加入压延机,经压延制得CPVC软质片材;
所述的CPVC树脂、助剂和液体增塑剂的质量比为100: 2~70:25~85;
所述的助剂包括稳定剂和润滑剂。
2.根据权利要求1所述的一种软质CPVC组合物的成型方法,其特征在于:所述的助剂包括稳定剂和润滑剂,还包括改性剂、填充剂、抗氧剂中的至少一种。
3.根据权利要求2所述的一种软质CPVC组合物的成型方法,其特征在于:所述的助剂包括稳定剂、润滑剂和填充剂,CPVC树脂、助剂和液体增塑剂的质量比为100: 30~70:40~85。
4.根据权利要求1所述的一种软质CPVC组合物的成型方法,其特征在于:所述的液体增塑剂为脂肪族二元酸酯类增塑剂、苯甲酸酯类增塑剂、磷酸酯类增塑剂、环氧化合物类增塑剂、石油酯类增塑剂、氯化碳氢化合物类增塑剂、柠檬酸酯类增塑剂、聚酯类增塑剂、苯多酸酯类增塑剂中的一种或两种。
5.根据权利要求1所述的一种软质CPVC组合物的成型方法,其特征在于:所述的稳定剂为有机锡稳定剂,润滑剂为石蜡、硬脂酸、硬脂酸镁、聚乙烯蜡、氧化聚乙烯蜡中的两种。
6.根据权利要求2所述的一种软质CPVC组合物的成型方法,其特征在于:所述的改性剂为双酚A,填充剂为活性碳酸钙。
7.根据权利要求1所述的一种软质CPVC组合物的成型方法,其特征在于:所述的CPVC树脂氯含量的质量百分比为66 ~75%。
8.根据权利要求1所述的一种软质CPVC组合物的成型方法,其特征在于:步骤2)的具体操作为:将干混料置于密炼机熔腔中,将液体增塑剂分1~5次加入密炼机中,塑炼3~5min,塑炼温度180~190℃,制得塑化块。
9.根据权利要求1所述的一种软质CPVC组合物的成型方法,其特征在于:步骤3)所述的挤出机为螺杆挤出机,螺杆挤出机自加料段至挤出段温度为170~190℃。
10.根据权利要求1所述的一种软质CPVC组合物的成型方法,其特征在于:步骤3)所述的压延机为L型四辊压延机,压延温度为155~165℃。
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