CN107245244A - 一种pvc用插层复合热稳定剂的制备方法 - Google Patents
一种pvc用插层复合热稳定剂的制备方法 Download PDFInfo
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- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 20
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—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
- C08L27/02—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 not modified by chemical after-treatment
- C08L27/04—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 not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C08K2003/164—Aluminum halide, e.g. aluminium chloride
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- C08K2003/166—Magnesium halide, e.g. magnesium chloride
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Abstract
本发明属于PVC添加剂制备技术领域,具体涉及一种PVC用插层复合热稳定剂的制备方法。本发明通过没食子酸与硝酸镧反应,制得没食子酸镧,再以氯化镁、氯化铝、氯化锌为原料,并掺杂没食子酸镧进入层间距中,制得三元锌镁铝水滑石,再用乙酰丙酮钙对三元锌镁铝水滑石进行插层改性,最后与季戊四醇研磨混合,并均匀分散在环氧大豆油中,制得PVC用插层复合热稳定剂。本发明制备步骤简单,所得热稳定剂低毒,无粉尘污染,具有较好的耐紫外老化性能和抗着色效能。
Description
技术领域
本发明属于PVC添加剂制备技术领域,具体涉及一种PVC用插层复合热稳定剂的制备方法。
背景技术
热稳定剂是聚氯乙烯(PVC)加工过程中必不可少的添加剂。PVC热稳定剂是一种能增加溶液、胶体、固体、混合物的稳定性能化学物。它可以减慢反应,保持化学平衡,降低表面张力,防止光、热分解或氧化分解等作用。PVC热稳定剂是由无尘复合铅以共生反应技术为基础,保证了基元热稳定成份(如二、三盐,金属皂类)在反应体体系内以初生态的晶粒尺寸和各种润滑剂进行混合,确保产品中个组份充分均匀混合,广泛应用聚氯乙烯制品。
铅盐类热稳定剂是最早用于PVC的稳定剂,由于其热稳定效能良好、性价比相对高等原因,目前仍然是用量最大的一类热稳定剂;但其毒性大,可通过呼吸道、消化道及皮肤进入人体,使脑、肝、肾等组织产生病变,易引起粉尘污染,使用时需添加的浓度高,因此随着全球环保意识的日益增强,PVC热稳定剂的无铅镉化进程逐步加快,铅盐类热稳定剂的应用受到限制。有机锡类热稳定剂具有热稳定效能高、无(低)毒、透明性优良等特点,是目前应用最广、效果最好的PVC热稳定剂之一;有机锡稳定剂的研究主要为引入特定的有机基团以进一步提高其热稳定效能,以及将不饱和有机锡化合物与苯乙烯等共聚以提高稳定剂的相对分子质量,从而提高热稳定剂与PVC树脂的相容性,但其成本高,加工时有异味,有金属存在时易交叉着色。钙锌稳定剂是一类无毒且具有良好润滑性的热稳定剂,传统的钙锌稳定剂的主要成分是硬脂酸、月桂酸、油酸、异辛酸、苯甲酸等的钙/锌盐,还有的采用一些新型钙锌化合物作为热稳定剂的主要成分,如环氧脂肪酸钙锌、甘油锌、二聚酸钙锌、氨基酸锌等。但还普遍存在耐紫外老化性能和抗着色效能较差,分散性不佳的问题。
因此,如何实现一种低毒(无毒)、无粉尘污染、耐紫外老化性能和抗着色效能好的热稳定剂是业内亟待解决的技术问题。
发明内容
本发明所要解决的技术问题:针对传统热稳定剂毒性大,易引起粉尘污染,且耐紫外老化性能和抗着色效能较差,分散性不佳的弊端,提供了一种PVC用插层复合热稳定剂的制备方法。
为解决技术问题,本发明采用如下所述的技术方案是:
(1)取没食子酸加入去离子水中搅拌15~20min,再加入六水合硝酸镧,在95~100℃下搅拌10~15min,得混合液;
(2)将混合液与氢氧化钠溶液混合,在75~80℃下搅拌20~30min,过滤得滤饼,将滤饼水洗干燥后得没食子酸镧;
(3)取氯化镁、氯化铝、氯化锌、没食子酸镧加入去离子水中,搅拌20~30min,得原料液;
(4)向原料液中加入碳酸钠和氢氧化钠溶液,在40~50℃下搅拌15~20min,静置8~10后离心分离,得沉淀;
(5)将沉淀与去离子水加入水热反应釜中,加热至110~120℃,反应20~24h,冷却后过滤得滤渣,将滤渣水洗干燥后得掺镧锌镁铝水滑石;
(6)将掺镧锌镁铝水滑石加入乙醇溶液中搅拌1~2h,再加入乙酰丙酮钙,在70~80℃下搅拌3~5h,冷却后过滤得过滤物,将过滤物水洗干燥后得插层水滑石;
(7)取插层水滑石与季戊四醇研磨过筛后加入环氧大豆油中,加热至80~120℃搅拌反应3~5h,得PVC用插层复合热稳定剂。
步骤(1)所述的没食子酸、去离子水、六水合硝酸镧的重量份为3.5~7.0份没食子酸,50~100份去离子水,6~12份六水合硝酸镧。
步骤(2)所述的氢氧化钠溶液的质量分数为1~3%,使用量为混合液体积的1.2~4.8倍。
步骤(3)所述的氯化镁、氯化铝、氯化锌、没食子酸镧、去离子水的重量份为28.5~57.0份氯化镁,26.6~53.2份氯化铝,27.2~54.5份氯化锌,0.3~0.6份没食子酸镧、200~300份去离子水。
步骤(4)所述的碳酸钠用量为原料液质量的2~8%。
步骤(4)所述的氢氧化钠溶液的质量分数为5~10%,用量为原料液质量的30~70%。
步骤(6)所述的乙酰丙酮钙用量为掺镧锌镁铝水滑石质量的15~60%。
步骤(7)所述的插层水滑石、季戊四醇、环氧大豆油的重量份为5~10份插层水滑石,0.8~1.6份季戊四醇,20~60份环氧大豆油。
本发明的有益技术效果是:本发明通过没食子酸与硝酸镧反应,制得没食子酸镧,再以氯化镁、氯化铝、氯化锌为原料,并掺杂没食子酸镧进入层间距中,制得三元锌镁铝水滑石,再用乙酰丙酮钙对三元锌镁铝水滑石进行插层改性,将乙酰丙酮钙引入水滑石结构中,增大水滑石的层间距使其有更大的反应空间,暴露更多的活性中心,增强对PVC降解产生的氯化氢的吸收作用,从而阻止了氯化氢对PVC的自催化作用,达到对PVC降解的抑制,显著提高PVC的热稳定性,同时还可提高水滑石与PVC间的分散性和相容性,最后与季戊四醇研磨混合,并均匀分散在环氧大豆油中,制得PVC用插层复合热稳定剂,有效解决了传统热稳定剂毒性大,易引起粉尘污染,且耐紫外老化性能和抗着色效能较差,分散性不佳的问题;本发明制备步骤简单,所得热稳定剂低毒,无粉尘污染,具有较好的耐紫外老化性能和抗着色效能。
具体实施方式
为便于理解本发明,本发明列举实施例如下。本领域技术人员应该明了,所述实施例仅仅是帮助理解本发明,不应视为对本发明的具体限制。
称取3.5~7.0g没食子酸,加入到50~100mL去离子水中,以300~400r/min搅拌15~20min,再加入6~12g六水合硝酸镧,在95~100℃恒温水浴下继续搅拌10~15min,得混合液;以1~2mL/min速率向混合液中滴加120~240mL质量分数为1%氢氧化钠溶液,滴加完毕,在75~80℃恒温水浴下,以300~400r/min搅拌反应20~30min,反应后过滤得滤饼,用去离子水洗涤滤饼至洗涤液呈中性,再将洗涤后的滤饼置于干燥箱中,在85~90℃下干燥2~3h,得没食子酸镧;然后称取28.5~57.0g氯化镁,26.6~53.2g氯化铝,27.2~54.5g氯化锌,0.3~0.6g没食子酸镧,依次加入200~300mL去离子水中,以300~400r/min搅拌20~30min,得原料液;向原料液中分别加入10~20g碳酸钠,100~200mL质量分数为10%氢氧化钠溶液,在40~50℃恒温水浴下,以300~400r/min搅拌15~20min,并保温静置8~10h,静置后转入离心机中,以6000~8000r/min离心分离得沉淀;将沉淀与200~300mL去离子水装入1L水热反应釜中,加热至110~120℃,反应20~24h,自然冷却至室温后过滤得滤渣,用去离子水洗涤滤渣3~5次,再将洗涤后的滤渣置于干燥箱中,在70~80℃下干燥3~4h,得掺镧锌镁铝水滑石;再将掺镧锌镁铝水滑石加入到300~500mL质量分数为50%乙醇溶液中,以300~400r/min搅拌1~2h,再加入23.8~47.6g乙酰丙酮钙,在70~80℃恒温水浴下继续搅拌3~5h,冷却至室温后过滤得过滤物,用去离子水洗涤过滤物3~5次,再将洗涤后的过滤物置于干燥箱中,在105~110℃下干燥至恒重,得插层水滑石;最后分别称取5~10g插层水滑石,0.8~1.6g季戊四醇,装入研钵中研磨20~30min,并过100目筛,得混合粉末,将混合粉末加入到30~50mL环氧大豆油中,加热至80~120℃,并以500~600r/min搅拌反应3~5h,反应后冷却至室温,得PVC用插层复合热稳定剂。
实例1
称取3.5g没食子酸,加入到50mL去离子水中,以300r/min搅拌15min,再加入6g六水合硝酸镧,在95℃恒温水浴下继续搅拌10min,得混合液;以1mL/min速率向混合液中滴加120mL质量分数为1%氢氧化钠溶液,滴加完毕,在75℃恒温水浴下,以300r/min搅拌反应20min,反应后过滤得滤饼,用去离子水洗涤滤饼至洗涤液呈中性,再将洗涤后的滤饼置于干燥箱中,在85℃下干燥2h,得没食子酸镧;然后称取28.5g氯化镁,26.6g氯化铝,27.2g氯化锌,0.3g没食子酸镧,依次加入200mL去离子水中,以300r/min搅拌20min,得原料液;向原料液中分别加入10g碳酸钠,100mL质量分数为10%氢氧化钠溶液,在40℃恒温水浴下,以300r/min搅拌15min,并保温静置8h,静置后转入离心机中,以6000r/min离心分离得沉淀;将沉淀与200mL去离子水装入1L水热反应釜中,加热至110℃,反应20h,自然冷却至室温后过滤得滤渣,用去离子水洗涤滤渣3次,再将洗涤后的滤渣置于干燥箱中,在70℃下干燥3h,得掺镧锌镁铝水滑石;再将掺镧锌镁铝水滑石加入到300mL质量分数为50%乙醇溶液中,以300r/min搅拌1h,再加入23.8g乙酰丙酮钙,在70℃恒温水浴下继续搅拌3h,冷却至室温后过滤得过滤物,用去离子水洗涤过滤物3次,再将洗涤后的过滤物置于干燥箱中,在105℃下干燥至恒重,得插层水滑石;最后分别称取5g插层水滑石,0.8g季戊四醇,装入研钵中研磨20min,并过100目筛,得混合粉末,将混合粉末加入到30mL环氧大豆油中,加热至80℃,并以500r/min搅拌反应3h,反应后冷却至室温,得PVC用插层复合热稳定剂。
将本发明制得的PVC用插层复合热稳定剂添加至PVC树脂中,控制添加量为PVC树脂质量的3%,添加完毕,在温度为138℃下熔融塑炼60s,再在温度为170℃下压制成型即可。本发明热稳定剂能有效防止早期着色,抗着色效能好并具有长期稳定性,添加本发明热稳定剂的PVC树脂在紫外箱中老化30天,拉伸强度达25.5MPa,断裂伸长率达105%,具有较好的耐紫外老化性能,值得推广与使用。
实例2
称取5.2g没食子酸,加入到80mL去离子水中,以350r/min搅拌18min,再加入9g六水合硝酸镧,在98℃恒温水浴下继续搅拌13min,得混合液;以2mL/min速率向混合液中滴加180mL质量分数为1%氢氧化钠溶液,滴加完毕,在78℃恒温水浴下,以350r/min搅拌反应25min,反应后过滤得滤饼,用去离子水洗涤滤饼至洗涤液呈中性,再将洗涤后的滤饼置于干燥箱中,在88℃下干燥3h,得没食子酸镧;然后称取42.0g氯化镁,39.9g氯化铝,41.2g氯化锌,0.5g没食子酸镧,依次加入250mL去离子水中,以350r/min搅拌25min,得原料液;向原料液中分别加入15g碳酸钠,150mL质量分数为10%氢氧化钠溶液,在45℃恒温水浴下,以350r/min搅拌18min,并保温静置9h,静置后转入离心机中,以7000r/min离心分离得沉淀;将沉淀与250mL去离子水装入1L水热反应釜中,加热至115℃,反应22h,自然冷却至室温后过滤得滤渣,用去离子水洗涤滤渣4次,再将洗涤后的滤渣置于干燥箱中,在75℃下干燥4h,得掺镧锌镁铝水滑石;再将掺镧锌镁铝水滑石加入到400mL质量分数为50%乙醇溶液中,以350r/min搅拌2h,再加入35.2g乙酰丙酮钙,在75℃恒温水浴下继续搅拌4h,冷却至室温后过滤得过滤物,用去离子水洗涤过滤物4次,再将洗涤后的过滤物置于干燥箱中,在108℃下干燥至恒重,得插层水滑石;最后分别称取8g插层水滑石,1.2g季戊四醇,装入研钵中研磨25min,并过100目筛,得混合粉末,将混合粉末加入到40mL环氧大豆油中,加热至100℃,并以550r/min搅拌反应4h,反应后冷却至室温,得PVC用插层复合热稳定剂。
将本发明制得的PVC用插层复合热稳定剂添加至PVC树脂中,控制添加量为PVC树脂质量的4%,添加完毕,在温度为140℃下熔融塑炼61s,再在温度为173℃下压制成型即可。本发明热稳定剂能有效防止早期着色,抗着色效能好并具有长期稳定性,添加本发明热稳定剂的PVC树脂在紫外箱中老化33天,拉伸强度达30.4MPa,断裂伸长率达256%,具有较好的耐紫外老化性能,值得推广与使用。
实例3
称取7.0g没食子酸,加入到100mL去离子水中,以400r/min搅拌20min,再加入12g六水合硝酸镧,在100℃恒温水浴下继续搅拌15min,得混合液;以2mL/min速率向混合液中滴加240mL质量分数为1%氢氧化钠溶液,滴加完毕,在80℃恒温水浴下,以400r/min搅拌反应30min,反应后过滤得滤饼,用去离子水洗涤滤饼至洗涤液呈中性,再将洗涤后的滤饼置于干燥箱中,在90℃下干燥3h,得没食子酸镧;然后称取57.0g氯化镁,53.2g氯化铝,54.5g氯化锌,0.6g没食子酸镧,依次加入300mL去离子水中,以400r/min搅拌30min,得原料液;向原料液中分别加入20g碳酸钠,200mL质量分数为10%氢氧化钠溶液,在50℃恒温水浴下,以400r/min搅拌20min,并保温静置10h,静置后转入离心机中,以8000r/min离心分离得沉淀;将沉淀与300mL去离子水装入1L水热反应釜中,加热至120℃,反应24h,自然冷却至室温后过滤得滤渣,用去离子水洗涤滤渣5次,再将洗涤后的滤渣置于干燥箱中,在80℃下干燥4h,得掺镧锌镁铝水滑石;再将掺镧锌镁铝水滑石加入到500mL质量分数为50%乙醇溶液中,以400r/min搅拌2h,再加入47.6g乙酰丙酮钙,在80℃恒温水浴下继续搅拌5h,冷却至室温后过滤得过滤物,用去离子水洗涤过滤物5次,再将洗涤后的过滤物置于干燥箱中,在110℃下干燥至恒重,得插层水滑石;最后分别称取10g插层水滑石,1.6g季戊四醇,装入研钵中研磨30min,并过100目筛,得混合粉末,将混合粉末加入到50mL环氧大豆油中,加热至120℃,并以600r/min搅拌反应5h,反应后冷却至室温,得PVC用插层复合热稳定剂。
将本发明制得的PVC用插层复合热稳定剂添加至PVC树脂中,控制添加量为PVC树脂质量的4%,添加完毕,在温度为142℃下熔融塑炼62s,再在温度为175℃下压制成型即可。本发明热稳定剂能有效防止早期着色,抗着色效能好并具有长期稳定性,添加本发明热稳定剂的PVC树脂在紫外箱中老化36天,拉伸强度达35.6MPa,断裂伸长率达400%,具有较好的耐紫外老化性能,值得推广与使用。
Claims (8)
1.一种PVC用插层复合热稳定剂的制备方法,其特征在于具体制备步骤为:
(1)取没食子酸加入去离子水中搅拌15~20min,再加入六水合硝酸镧,在95~100℃下搅拌10~15min,得混合液;
(2)将混合液与氢氧化钠溶液混合,在75~80℃下搅拌20~30min,过滤得滤饼,将滤饼水洗干燥后得没食子酸镧;
(3)取氯化镁、氯化铝、氯化锌、没食子酸镧加入去离子水中,搅拌20~30min,得原料液;
(4)向原料液中加入碳酸钠和氢氧化钠溶液,在40~50℃下搅拌15~20min,静置8~10后离心分离,得沉淀;
(5)将沉淀与去离子水加入水热反应釜中,加热至110~120℃,反应20~24h,冷却后过滤得滤渣,将滤渣水洗干燥后得掺镧锌镁铝水滑石;
(6)将掺镧锌镁铝水滑石加入乙醇溶液中搅拌1~2h,再加入乙酰丙酮钙,在70~80℃下搅拌3~5h,冷却后过滤得过滤物,将过滤物水洗干燥后得插层水滑石;
(7)取插层水滑石与季戊四醇研磨过筛后加入环氧大豆油中,加热至80~120℃搅拌反应3~5h,得PVC用插层复合热稳定剂。
2.如权利要求2所述的一种PVC用插层复合热稳定剂的制备方法,其特征在于,步骤(1)所述的没食子酸、去离子水、六水合硝酸镧的重量份为3.5~7.0份没食子酸,50~100份去离子水,6~12份六水合硝酸镧。
3.如权利要求2所述的一种PVC用插层复合热稳定剂的制备方法,其特征在于,步骤(2)所述的氢氧化钠溶液的质量分数为1~3%,使用量为混合液体积的1.2~4.8倍。
4.如权利要求2所述的一种PVC用插层复合热稳定剂的制备方法,其特征在于,步骤(3)所述的氯化镁、氯化铝、氯化锌、没食子酸镧、去离子水的重量份为28.5~57.0份氯化镁,26.6~53.2份氯化铝,27.2~54.5份氯化锌,0.3~0.6份没食子酸镧、200~300份去离子水。
5.如权利要求2所述的一种PVC用插层复合热稳定剂的制备方法,其特征在于,步骤(4)所述的碳酸钠用量为原料液质量的2~8%。
6.如权利要求2所述的一种PVC用插层复合热稳定剂的制备方法,其特征在于,步骤(4)所述的氢氧化钠溶液的质量分数为5~10%,用量为原料液质量的30~70%。
7.如权利要求2所述的一种PVC用插层复合热稳定剂的制备方法,其特征在于,步骤(6)所述的乙酰丙酮钙用量为掺镧锌镁铝水滑石质量的15~60%。
8.如权利要求2所述的一种PVC用插层复合热稳定剂的制备方法,其特征在于,步骤(7)所述的插层水滑石、季戊四醇、环氧大豆油的重量份为5~10份插层水滑石,0.8~1.6份季戊四醇,20~60份环氧大豆油。
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110723744A (zh) * | 2018-07-17 | 2020-01-24 | 靖江市康高特塑料科技有限公司 | 一种改善水滑石初期白度的水热合成方法 |
CN111471257A (zh) * | 2020-04-01 | 2020-07-31 | 安徽大学 | 一种新型钙锌铝稳定剂及其制备方法 |
CN114656825A (zh) * | 2022-03-09 | 2022-06-24 | 青岛爱尔家佳新材料股份有限公司 | 一种用于新能源汽车的阻燃聚脲及其制备方法 |
CN116444910A (zh) * | 2023-04-28 | 2023-07-18 | 安徽江淮汽车集团股份有限公司 | 一种抗菌性能和voc性能良好的ps复合材料及其制备方法 |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101007878A (zh) * | 2006-01-25 | 2007-08-01 | 扬州科宇化工有限公司 | Pvc用水滑石-稀土-钙锌稳定剂及其制备方法 |
CN101508636A (zh) * | 2009-03-27 | 2009-08-19 | 北京化工大学 | 一种乙酰丙酮基复合热稳定剂 |
CN101508796A (zh) * | 2009-03-25 | 2009-08-19 | 江西宏远化工有限公司 | 三元水滑石-稀土-钙/锌无毒复合热稳定剂及其制备方法 |
CN101602863A (zh) * | 2009-06-22 | 2009-12-16 | 温州天盛塑料助剂有限公司 | 用于pvc加工的环保型无尘钙锌复合热稳定剂 |
CN101942111A (zh) * | 2009-07-06 | 2011-01-12 | 邵阳天堂助剂化工有限公司 | 一种锌镁铝水滑石基pvc复合热稳定剂的制造方法及应用 |
CN104277368A (zh) * | 2014-09-17 | 2015-01-14 | 湖南稀土金属材料研究院 | 稀土类水滑石复合热稳定剂及热稳定聚氯乙烯 |
CN106633490A (zh) * | 2016-11-10 | 2017-05-10 | 周荣 | 一种聚氯乙烯抗静电薄膜的制备方法 |
-
2017
- 2017-06-17 CN CN201710460456.XA patent/CN107245244A/zh active Pending
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101007878A (zh) * | 2006-01-25 | 2007-08-01 | 扬州科宇化工有限公司 | Pvc用水滑石-稀土-钙锌稳定剂及其制备方法 |
CN101508796A (zh) * | 2009-03-25 | 2009-08-19 | 江西宏远化工有限公司 | 三元水滑石-稀土-钙/锌无毒复合热稳定剂及其制备方法 |
CN101508636A (zh) * | 2009-03-27 | 2009-08-19 | 北京化工大学 | 一种乙酰丙酮基复合热稳定剂 |
CN101602863A (zh) * | 2009-06-22 | 2009-12-16 | 温州天盛塑料助剂有限公司 | 用于pvc加工的环保型无尘钙锌复合热稳定剂 |
CN101942111A (zh) * | 2009-07-06 | 2011-01-12 | 邵阳天堂助剂化工有限公司 | 一种锌镁铝水滑石基pvc复合热稳定剂的制造方法及应用 |
CN104277368A (zh) * | 2014-09-17 | 2015-01-14 | 湖南稀土金属材料研究院 | 稀土类水滑石复合热稳定剂及热稳定聚氯乙烯 |
CN106633490A (zh) * | 2016-11-10 | 2017-05-10 | 周荣 | 一种聚氯乙烯抗静电薄膜的制备方法 |
Non-Patent Citations (4)
Title |
---|
叶志强等: "硬脂酸镧的制备与动力学研究", 《稀土》 * |
唐颂超主编: "《高分子材料成型加工(第3板)》", 31 May 2013, 中国轻工业出版社 * |
徐同考等: "《塑料改性实用技术》", 31 October 2014, 中国轻工业出版社 * |
武卫莉等: "《电线电缆加工工艺学》", 31 October 2012, 哈尔滨工业大学出版社 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110723744A (zh) * | 2018-07-17 | 2020-01-24 | 靖江市康高特塑料科技有限公司 | 一种改善水滑石初期白度的水热合成方法 |
CN111471257A (zh) * | 2020-04-01 | 2020-07-31 | 安徽大学 | 一种新型钙锌铝稳定剂及其制备方法 |
CN111471257B (zh) * | 2020-04-01 | 2023-06-27 | 安徽大学 | 一种钙锌铝稳定剂及其制备方法 |
CN114656825A (zh) * | 2022-03-09 | 2022-06-24 | 青岛爱尔家佳新材料股份有限公司 | 一种用于新能源汽车的阻燃聚脲及其制备方法 |
CN116444910A (zh) * | 2023-04-28 | 2023-07-18 | 安徽江淮汽车集团股份有限公司 | 一种抗菌性能和voc性能良好的ps复合材料及其制备方法 |
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