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CN114701220A - 一种pvc防滑保温篷布的生产工艺 - Google Patents

一种pvc防滑保温篷布的生产工艺 Download PDF

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CN114701220A
CN114701220A CN202210345194.3A CN202210345194A CN114701220A CN 114701220 A CN114701220 A CN 114701220A CN 202210345194 A CN202210345194 A CN 202210345194A CN 114701220 A CN114701220 A CN 114701220A
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tarpaulin
pvc
neck flask
parts
slip
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宋佳华
赵铁虎
何大磊
于志创
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Jiangsu Gaiya Polymer New Material Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B3/00Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form
    • B32B3/02Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions
    • B32B3/08Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar shape; Layered products comprising a layer having particular features of form characterised by features of form at particular places, e.g. in edge regions characterised by added members at particular parts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B33/00Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
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    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/22Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
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    • B32B7/00Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04Interconnection of layers
    • B32B7/12Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0002Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
    • D06N3/0015Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
    • D06N3/0036Polyester fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06NWALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/04Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06N3/06Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds with polyvinylchloride or its copolymerisation products
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00Coating on the layer surface
    • B32B2255/02Coating on the layer surface on fibrous or filamentary layer
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2255/00Coating on the layer surface
    • B32B2255/26Polymeric coating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02Synthetic macromolecular fibres
    • B32B2262/0276Polyester fibres
    • B32B2262/0284Polyethylene terephthalate [PET] or polybutylene terephthalate [PBT]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/30Properties of the layers or laminate having particular thermal properties
    • B32B2307/304Insulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/30Properties of the layers or laminate having particular thermal properties
    • B32B2307/306Resistant to heat
    • B32B2307/3065Flame resistant or retardant, fire resistant or retardant
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00Properties of the layers or laminate
    • B32B2307/70Other properties
    • B32B2307/714Inert, i.e. inert to chemical degradation, corrosion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
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    • B32B2307/00Properties of the layers or laminate
    • B32B2307/70Other properties
    • B32B2307/744Non-slip, anti-slip
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract

本发明公开了一种PVC防滑保温篷布的生产工艺,涉及保温篷布领域,通过将PVC防护涂料涂覆在涤纶帆布的外侧面上,并置于烘箱中进行烘干,将发泡卷材和电发热丝通过压敏胶胶合到涤纶帆布的内侧面上,使电发热丝位于发泡卷材与涤纶帆布之间,得到该PVC防滑保温篷布,解决了现有的篷布保温性能和耐老化性能差,使用时温度过高或经过白天阳光照射后会发生损坏,遮盖效果下降,降低经济效益,且阻燃效果差的问题;通过在涤纶帆布外侧涂覆PVC防护树脂,从而使篷布增加保温性能,并通过涂覆工艺在表面形成防滑层,增加篷布的防滑性能,并通过制备得到了防老化剂和阻燃剂,使篷布在具备防滑保温的同时具备抗老化和阻燃性能。

Description

一种PVC防滑保温篷布的生产工艺
技术领域
本发明涉及保温篷布技术领域,具体涉及一种PVC防滑保温篷布的生产工艺。
背景技术
篷布是一种高强度、具有良好韧性及柔软程度的防水材料,常被用作帆布(油画布)、带聚氨酯涂层的涤纶或制作成聚乙烯类塑料,篷布通常在角部或边缘有坚固的索环,以方便用来穿绳索捆绑、悬挂或覆盖。
篷布具有良好的防水、防霉性能,同时抗拉强度高、耐酸碱腐蚀,洗刷折叠方便,能够用于雨天货物的遮盖或者户外帐篷搭建,比如火车、汽车、轮船上货物的遮盖,临时堆砌货物的遮盖等。
现有的篷布保温性能和耐老化性能差,使用时温度过高或经过白天阳光照射后会发生损坏,遮盖效果下降,损害货物,降低经济效益,且阻燃效果差。
发明内容
为了克服上述的技术问题,本发明的目的在于提供了一种PVC防滑保温篷布的生产工艺:
(1)准备涤纶帆布、发泡卷材和发热丝,将PVC防护涂料涂覆在涤纶帆布的外侧面上,并置于烘箱中进行烘干,将发泡卷材和电发热丝通过压敏胶胶合到涤纶帆布的内侧面上,使电发热丝位于发泡卷材与涤纶帆布之间,得到该PVC防滑保温篷布,解决了现有篷布耐老化性能差和阻燃效果差的问题;
(2)将六氯环三磷腈、间醋氨酚和K2CO3溶于盛有丙酮的三口烧瓶中,得到中间体A,取中间体A、甲醇和NaOH水溶液于三口瓶中,得到中间体B,取9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、CCl4和溶剂丙酮置于三口烧瓶中,将中间体B和三乙胺溶于溶剂丙酮并滴加到三口瓶中,得到该阻燃剂,解决了现有的篷布阻燃效果差的问题;
(3)在单口烧瓶中加入十二胺、甲醇,边搅拌边滴加丙烯酸甲酯,加入甲醇、乙二胺,得到中间体F,将β-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯加入四口烧瓶中,将氢氧化钠溶液用恒压滴液漏斗滴加,得到中间体H,将中间体H置干燥的三口瓶中,加入三氯甲烷,滴加二氯亚砜,得到中间体J,将中间体F加入干燥的三口烧瓶中,加入三氯甲烷,再加入三乙胺,将中间体J加入到三口瓶中,得到该防老化剂,解决了现有的篷布耐老化性能差,使用时温度过高或经过白天阳光照射后会发生损坏,遮盖效果下降,损害货物,降低经济效益的问题。
本发明的目的可以通过以下技术方案实现:
一种PVC防滑保温篷布的生产工艺,该PVC防滑保温篷布由以下步骤制备得到:
S1:准备涤纶帆布、发泡卷材和发热丝;
S2:将PVC防护涂料涂覆在涤纶帆布的外侧面上,并置于烘箱中进行烘干;
S3:将发泡卷材和电发热丝通过压敏胶胶合到涤纶帆布的内侧面上,使电发热丝位于发泡卷材与涤纶帆布之间,得到该PVC防滑保温篷布;
所述PVC防护涂料包括以下重量份的组分:
PVC树脂100-120份、增塑剂50-70份、稳定剂2-8份、阻燃剂5-15份、防霉剂10-16份、防老化剂3-9份和颜料2-10份。
作为本发明进一步的方案:所述阻燃剂由以下步骤制备得到:
S21:将六氯环三磷腈、间醋氨酚和K2CO3溶于盛有丙酮的三口烧瓶中,搅拌使其充分溶解,并通氮气保护气,逐渐将温度升至70-80℃,反应96-100h,用20mL的水,50mL的乙醇,50mL的正己烷分别洗涤3-4次,置于真空烘箱干燥中70-80℃,烘干48-50h,得到中间体A;
化学反应式如下所示:
Figure BDA0003580638930000031
S22:取中间体A、甲醇和NaOH水溶液于三口瓶中,90-95℃下加热回流24-36h,放入真空烘箱干燥中80-85℃,烘干48-56h,得到中间体B;
化学反应式如下所示:
Figure BDA0003580638930000041
S23:取9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、CCl4和溶剂丙酮置于三口烧瓶中,通N2保护气,将三口烧瓶放置于40-50℃的恒温油浴锅中反应1-3h,将中间体B和三乙胺溶于溶剂丙酮中,置于恒压漏斗中,并滴加到三口瓶中反应3-5h,控制滴加速度为1-2滴/s,置于真空烘箱干燥中70-80℃,烘干48-50h,得到该阻燃剂。
化学反应式如下所示:
Figure BDA0003580638930000051
作为本发明进一步的方案:步骤S21中所述六氯环三磷腈、间醋氨酚、K2CO3和丙酮的用量比为0.347g:1.088g:0.429g:60mL,步骤S22中所述中间体A、甲醇和NaOH水溶液的用量比为0.518g:30mL:5.8g,所述NaOH水溶液的质量分数为21%,步骤S23中所述9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、CCl4、中间体B和三乙胺的用量比为20g:20g:40-50g:10g。
作为本发明进一步的方案:所述防老化剂由以下步骤制备得到:
S41:在单口烧瓶中加入十二胺、甲醇,使十二胺溶解,边搅拌边滴加丙烯酸甲酯,滴加速度控制为1-2滴/s,25-30℃下恒温反应24-26h,在60℃、133.3Pa的条件下减压蒸馏,得到中间体E;
S42:在单口烧瓶中加入中间体E、甲醇,边搅拌边滴加乙二胺,滴加速度控制为1-2滴/s,25-30℃下恒温反应24-36h,在70℃、266.6Pa的条件下减压蒸馏,得到中间体F;
S43:将β-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯加入四口烧瓶中,然后加入无水乙醇溶解,放入恒温磁力搅拌水浴后开始升温,同时打开冷凝水,待温度升到60-70℃,通入氮气,将氢氧化钠溶液用恒压滴液漏斗滴加,滴加速度控制为1-2滴/s,在氮气保护下连续反应3-5h,冷却至室温,用盐酸中和至pH值为3,在40-50℃真空条件下干燥24-36h,得到中间体H;
S44:将中间体H置干燥的三口瓶中,加入三氯甲烷,置于50-60℃的恒温磁力搅拌水浴中,打开冷凝水同时通入氮气保护,用滴液漏斗滴加二氯亚砜,滴加速度控制为1-2滴/s,继续反应5-7h,在60℃、133Pa的条件下进行减压蒸馆,得到中间体J;
S45:将中间体F加入干燥的三口烧瓶中,加入三氯甲烷,再加入三乙胺置于恒温磁力搅拌水浴中,通过加入冰控制温度为0-2℃同时通氮气保护,将中间体J加入到三口瓶中,升温至40-50℃,恒温反应12-24h,在60℃、133Pa的条件下进行减压蒸馏,得到该防老化剂。
作为本发明进一步的方案:步骤S41中所述十二胺、甲醇和丙烯酸甲酯的用量比为9g:40g:35g,步骤S42中所述中间体E、甲醇和乙二胺的用量比为12.5g:70g:130g。
作为本发明进一步的方案:步骤S43中所述β-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯、无水乙醇和氢氧化钠溶液的用量比为30g:50mL:50g,所述氢氧化钠溶液的质量分数为30%。
作为本发明进一步的方案:步骤S44中所述中间体H、三氯甲烷和二氯亚砜的用量比为5.56g:50mL:4mL。
作为本发明进一步的方案:步骤S45中所述中间体F、三氯甲烷、三乙胺和中间体J的用量比为1.06g:50mL:1.7mL:3.69g。
本发明的有益效果:
(1)本发明是通过将PVC防护涂料涂覆在涤纶帆布的外侧面上,并置于烘箱中进行烘干,将发泡卷材和电发热丝通过压敏胶胶合到涤纶帆布的内侧面上,使电发热丝位于发泡卷材与涤纶帆布之间,得到该PVC防滑保温篷布,通过在涤纶帆布外侧涂覆PVC防护树脂,从而使篷布增加保温性能,并通过涂覆工艺在表面形成防滑层,增加篷布的防滑性能,并通过制备得到了防老化剂和阻燃剂,使篷布在具备防滑保温的同时具备抗老化和阻燃性能;
(2)将六氯环三磷腈、间醋氨酚和K2CO3溶于盛有丙酮的三口烧瓶中,得到中间体A,取中间体A、甲醇和NaOH水溶液于三口瓶中,得到中间体B,取9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、CCl4和溶剂丙酮置于三口烧瓶中,将中间体B和三乙胺溶于溶剂丙酮并滴加到三口瓶中,得到该阻燃剂,选择磷杂菲和磷腈化合物作为反应物中的磷酸酯和亲核试剂,以磷杂菲结构为侧基的聚酯,包括磷杂菲基均聚酯和磷杂菲基共聚酯,磷杂菲中苯环的引入可以有效地提高聚酯的热稳定性,且可以促进聚酯化合物的成炭,且磷杂菲官能团具有大体积结构的非共面性特点,分子结构内极性P-H键的活泼性和有机溶解性赋予了其广泛的相互作用性,分解过程中的典型降解自由基更是赋予了其高效的阻燃性能,从而达到了提高篷布阻燃性的目的;
(3)又通过“发散法”合成以十二胺为核心的新抗氧剂骨架,通过酰氯和氨基的酰胺化缩合反应将两个具有抗氧化功能的基团引入到超支化大分子的骨架上,从而支化程度较高的该防老化剂,该防老化剂结构中的官能团既有类似抗氧剂1076的烷基长链,又具有类似于抗氧剂1098的酰胺键结构,从而使篷布具备优异的抗老化性能。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1:
本实施例为一种PVC防滑保温篷布的生产工艺,该PVC防滑保温篷布由以下步骤制备得到:
S1:准备涤纶帆布、发泡卷材和发热丝;
S2:将PVC防护涂料涂覆在涤纶帆布的外侧面上,并置于烘箱中进行烘干;
S3:将发泡卷材和电发热丝通过压敏胶胶合到涤纶帆布的内侧面上,使电发热丝位于发泡卷材与涤纶帆布之间,得到该PVC防滑保温篷布;
PVC防护涂料包括以下重量份的组分:
PVC树脂100份、增塑剂50份、稳定剂2份、阻燃剂5份、防霉剂10份、防老化剂3份和颜料2份;
阻燃剂由以下步骤制备得到:
S21:将0.347g的六氯环三磷腈、1.088g的间醋氨酚和0.429g的K2CO3溶于盛有60mL丙酮的三口烧瓶中,搅拌使其充分溶解,并通氮气保护气,逐渐将温度升至70℃,反应96h,用20mL的水,50mL的乙醇,50mL的正己烷分别洗涤3次,置于真空烘箱干燥中70℃,烘干48h,得到中间体A;
S22:取0.518g的中间体A、30mL的甲醇和5.8g的NaOH水溶液于三口瓶中,90℃下加热回流24h,放入真空烘箱干燥中80℃,烘干48h,得到中间体B;
S23:取20g的9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、20g的CCl4和溶剂丙酮置于三口烧瓶中,通N2保护气,将三口烧瓶放置于40℃的恒温油浴锅中反应1h,将40g中间体B和10g三乙胺溶于溶剂丙酮中,置于恒压漏斗中,并滴加到三口瓶中反应3h,控制滴加速度为1滴/s,置于真空烘箱干燥中70℃,烘干48h,得到该阻燃剂;
防老化剂由以下步骤制备得到:
S41:在单口烧瓶中加入9g的十二胺、40g的甲醇,使十二胺溶解,边搅拌边滴加35g的丙烯酸甲酯,滴加速度控制为1滴/s,25℃下恒温反应24h,在60℃、133.3Pa的条件下减压蒸馏,得到中间体E;
S42:在单口烧瓶中加入12.5g的中间体E、70g的甲醇,边搅拌边滴加130g的乙二胺,滴加速度控制为1滴/s,25℃下恒温反应24h,在70℃、266.6Pa的条件下减压蒸馏,得到中间体F;
S43:称量30g的β-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯于四口烧瓶中,然后加入50mL的无水乙醇溶解,放入恒温磁力搅拌水浴后开始升温,同时打开冷凝水,待温度升到600℃,通入氮气,将50g的氢氧化钠溶液用恒压滴液漏斗滴加,滴加速度控制为1滴/s,在氮气保护下连续反应3h,冷却至室温,用盐酸中和至pH值为3,在40℃真空条件下干燥24h,得到中间体H;
S44:称量5.56g的中间体H置干燥的三口瓶中,加入50mL三氯甲烷,置于50℃的恒温磁力搅拌水浴中,打开冷凝水同时通入氮气保护,用滴液漏斗滴加4mL的二氯亚砜,滴加速度控制为1滴/s,继续反应5h,在60℃、133Pa的条件下进行减压蒸馆,得到中间体J;
S45:称量1.06g的中间体F于干燥的三口烧瓶中,加入50mL的三氯甲烷,再加入1.7mL三乙胺置于恒温磁力搅拌水浴中,通过加入冰控制温度为0℃同时通氮气保护,将3.69g的中间体J加入到三口瓶中,升温至40℃,恒温反应12h,在60℃、133Pa的条件下进行减压蒸馏,得到该防老化剂。
实施例2:
本实施例与实施例1的区别在于:
PVC防护涂料包括以下重量份的组分:
PVC树脂100份、增塑剂70份、稳定剂8份、阻燃剂15份、防霉剂16份、防老化剂9份和颜料10份;
阻燃剂由以下步骤制备得到:
S21:将0.347g的六氯环三磷腈、1.088g的间醋氨酚和0.429g的K2CO3溶于盛有60mL丙酮的三口烧瓶中,搅拌使其充分溶解,并通氮气保护气,逐渐将温度升至80℃,反应100h,用20mL的水,50mL的乙醇,50mL的正己烷分别洗涤3-4次,置于真空烘箱干燥中80℃,烘干50h,得到中间体A;
S22:取0.518g的中间体A、30mL的甲醇和5.8g的NaOH水溶液于三口瓶中,95℃下加热回流36h,放入真空烘箱干燥中85℃,烘干56h,得到中间体B;
S23:取20g的9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、20g的CCl4和溶剂丙酮置于三口烧瓶中,通N2保护气,将三口烧瓶放置于50℃的恒温油浴锅中反应1h,将50g中间体B和10g三乙胺溶于溶剂丙酮中,置于恒压漏斗中,并滴加到三口瓶中反应3h,控制滴加速度为1滴/s,置于真空烘箱干燥中70℃,烘干48h,得到该阻燃剂;
防老化剂由以下步骤制备得到:
S41:在单口烧瓶中加入9g的十二胺、40g的甲醇,使十二胺溶解,边搅拌边滴加35g的丙烯酸甲酯,滴加速度控制为2滴/s,30℃下恒温反应26h,在60℃、133.3Pa的条件下减压蒸馏,得到中间体E;
S42:在单口烧瓶中加入12.5g的中间体E、70g的甲醇,边搅拌边滴加130g的乙二胺,滴加速度控制为2滴/s,30℃下恒温反应36h,在70℃、266.6Pa的条件下减压蒸馏,得到中间体F;
S43:称量30g的β-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯于四口烧瓶中,然后加入50mL的无水乙醇溶解,放入恒温磁力搅拌水浴后开始升温,同时打开冷凝水,待温度升到70℃,通入氮气,将50g的氢氧化钠溶液用恒压滴液漏斗滴加,滴加速度控制为2滴/s,在氮气保护下连续反应5h,冷却至室温,用盐酸中和至pH值为3,在50℃真空条件下干燥36h,得到中间体H;
S44:称量5.56g的中间体H置干燥的三口瓶中,加入50mL三氯甲烷,置于60℃的恒温磁力搅拌水浴中,打开冷凝水同时通入氮气保护,用滴液漏斗滴加4mL的二氯亚砜,滴加速度控制为2滴/s,继续反应7h,在60℃、133Pa的条件下进行减压蒸馆,得到中间体J;
S45:称量1.06g的中间体F于干燥的三口烧瓶中,加入50mL的三氯甲烷,再加入1.7mL三乙胺置于恒温磁力搅拌水浴中,通过加入冰控制温度为2℃同时通氮气保护,将3.69g的中间体J加入到三口瓶中,升温至50℃,恒温反应14h,在60℃、133Pa的条件下进行减压蒸馏,得到该防老化剂。
实施例3:
本实施例与实施例1的区别在于:
PVC防护涂料包括以下重量份的组分:
PVC树脂120份、增塑剂70份、稳定剂8份、阻燃剂15份、防霉剂16份、防老化剂9份和颜料10份;
阻燃剂由以下步骤制备得到:
S21:将0.347g的六氯环三磷腈、1.088g的间醋氨酚和0.429g的K2CO3溶于盛有60mL丙酮的三口烧瓶中,搅拌使其充分溶解,并通氮气保护气,逐渐将温度升至80℃,反应100h,用20mL的水,50mL的乙醇,50mL的正己烷分别洗涤4次,置于真空烘箱干燥中80℃,烘干50h,得到中间体A;
S22:取0.518g的中间体A、30mL的甲醇和5.8g的NaOH水溶液于三口瓶中,95℃下加热回流36h,放入真空烘箱干燥中85℃,烘干56h,得到中间体B;
S23:取20g的9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、20g的CCl4和溶剂丙酮置于三口烧瓶中,通N2保护气,将三口烧瓶放置于50℃的恒温油浴锅中反应3h,将50g中间体B和10g三乙胺溶于溶剂丙酮中,置于恒压漏斗中,并滴加到三口瓶中反应5h,控制滴加速度为2滴/s,置于真空烘箱干燥中80℃,烘干50h,得到该阻燃剂;
防老化剂由以下步骤制备得到:
S41:在单口烧瓶中加入9g的十二胺、40g的甲醇,使十二胺溶解,边搅拌边滴加35g的丙烯酸甲酯,滴加速度控制为2滴/s,30℃下恒温反应26h,在60℃、133.3Pa的条件下减压蒸馏,得到中间体E;
S42:在单口烧瓶中加入12.5g的中间体E、70g的甲醇,边搅拌边滴加130g的乙二胺,滴加速度控制为2滴/s,30℃下恒温反应36h,在70℃、266.6Pa的条件下减压蒸馏,得到中间体F;
S43:称量30g的β-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯于四口烧瓶中,然后加入50mL的无水乙醇溶解,放入恒温磁力搅拌水浴后开始升温,同时打开冷凝水,待温度升到70℃,通入氮气,将50g的氢氧化钠溶液用恒压滴液漏斗滴加,滴加速度控制为2滴/s,在氮气保护下连续反应5h,冷却至室温,用盐酸中和至pH值为3,在50℃真空条件下干燥36h,得到中间体H;
S44:称量5.56g的中间体H置干燥的三口瓶中,加入50mL三氯甲烷,置于60℃的恒温磁力搅拌水浴中,打开冷凝水同时通入氮气保护,用滴液漏斗滴加4mL的二氯亚砜,滴加速度控制为2滴/s,继续反应7h,在60℃、133Pa的条件下进行减压蒸馆,得到中间体J;
S45:称量1.06g的中间体F于干燥的三口烧瓶中,加入50mL的三氯甲烷,再加入1.7mL三乙胺置于恒温磁力搅拌水浴中,通过加入冰控制温度为2℃同时通氮气保护,将3.69g的中间体J加入到三口瓶中,升温至50℃,恒温反应24h,在60℃、133Pa的条件下进行减压蒸馏,得到该防老化剂。
对比例1:
对比例1与实施例1的区别在于不添加防老化剂。
对比例2:
对比例2与实施例1的区别在于使用市购防老化剂。
性能检测
将实施例1-3以及对比例1-2的篷布进行检测,在120℃下老化处理1000h后,参照GB/T528-1998的标准在50mm/min下测试抗老化PVC篷布老化前后的拉伸强度、断裂伸长率,计算抗老化PVC篷布的老化后拉伸强度保持率和老化后断裂伸长率保持率,其中,老化后拉伸强度保持率=老化后的拉伸强度/老化前的拉伸强度×100%,老化后断裂伸长率保持率=老化后的断裂伸长率/老化前的断裂伸长率×100%;
检测结果如下表所示:
Figure BDA0003580638930000141
由上表可知,实施例的老化后拉伸强度保持率达到了90.5-91.1%,不添加防老化剂的对比例1的老化后拉伸强度保持率为70.2%,使用市购防老化剂的对比例2的老化后拉伸强度保持率为85.6%,实施例的老化后断裂伸长率保持率达到了87.5-88.9%,不添加防老化剂的对比例1的老化后断裂伸长率保持率为74.1%,使用市购防老化剂的对比例2的老化后断裂伸长率保持率为82.6%,实施例的迁移率为0.34-0.45%,不添加防老化剂的对比例1的迁移率为0.75%,使用市购防老化剂的对比例2的迁移率为0.64%,实施例的各项数据均优于对比例,说明本发明所制备的防老化剂添加到篷布中,可以使制备得到的篷布具备更加优异的抗老化性能。
在本说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。

Claims (8)

1.一种PVC防滑保温篷布的生产工艺,其特征在于,该PVC防滑保温篷布由以下步骤制备得到:
S1:准备涤纶帆布、发泡卷材和发热丝;
S2:将PVC防护涂料涂覆在涤纶帆布的外侧面上,并置于烘箱中进行烘干;
S3:将发泡卷材和电发热丝通过压敏胶胶合到涤纶帆布的内侧面上,使电发热丝位于发泡卷材与涤纶帆布之间,得到该PVC防滑保温篷布;
所述PVC防护涂料包括以下重量份的组分:
PVC树脂100-120份、增塑剂50-70份、稳定剂2-8份、阻燃剂5-15份、防霉剂10-16份、防老化剂3-9份和颜料2-10份。
2.根据权利要求1所述的一种PVC防滑保温篷布的生产工艺,其特征在于,所述阻燃剂由以下步骤制备得到:
S21:将六氯环三磷腈、间醋氨酚和K2CO3溶于盛有丙酮的三口烧瓶中,得到中间体A;
S22:取中间体A、甲醇和NaOH水溶液于三口瓶中,得到中间体B;
S23:取9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、CCl4和溶剂丙酮置于三口烧瓶中,将中间体B和三乙胺溶于溶剂丙酮并滴加到三口瓶中,得到该阻燃剂。
3.根据权利要求2所述的一种PVC防滑保温篷布的生产工艺,其特征在于,步骤S21中所述六氯环三磷腈、间醋氨酚、K2CO3和丙酮的用量比为0.347g:1.088g:0.429g:60mL,步骤S22中所述中间体A、甲醇和NaOH水溶液的用量比为0.518g:30mL:5.8g,所述NaOH水溶液的质量分数为21%,步骤S23中所述9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物、CCl4、中间体B和三乙胺的用量比为20g:20g:40-50g:10g。
4.根据权利要求1所述的一种PVC防滑保温篷布的生产工艺,其特征在于,所述防老化剂由以下步骤制备得到:
S41:在单口烧瓶中加入十二胺、甲醇,边搅拌边滴加丙烯酸甲酯,得到中间体E;
S42:在单口烧瓶中加入中间体E、甲醇,边搅拌边滴加乙二胺,得到中间体F;
S43:将β-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯加入四口烧瓶中,然后加入无水乙醇溶解,将氢氧化钠溶液用恒压滴液漏斗滴加,得到中间体H;
S44:将中间体H置干燥的三口瓶中,加入三氯甲烷,用滴液漏斗滴加二氯亚砜,得到中间体J;
S45:将中间体F加入干燥的三口烧瓶中,加入三氯甲烷,再加入三乙胺,将中间体J加入到三口瓶中,得到该防老化剂。
5.根据权利要求4所述的一种PVC防滑保温篷布的生产工艺,其特征在于,步骤S41中所述十二胺、甲醇和丙烯酸甲酯的用量比为9g:40g:35g,步骤S42中所述中间体E、甲醇和乙二胺的用量比为12.5g:70g:130g。
6.根据权利要求4所述的一种PVC防滑保温篷布的生产工艺,其特征在于,步骤S43中所述β-(3,5-二叔丁基-4-羟基苯基)丙酸甲酯、无水乙醇和氢氧化钠溶液的用量比为30g:50mL:50g,所述氢氧化钠溶液的质量分数为30%。
7.根据权利要求4所述的一种PVC防滑保温篷布的生产工艺,其特征在于,步骤S44中所述中间体H、三氯甲烷和二氯亚砜的用量比为5.56g:50mL:4mL。
8.根据权利要求4所述的一种PVC防滑保温篷布的生产工艺,其特征在于,步骤S45中所述中间体F、三氯甲烷、三乙胺和中间体J的用量比为1.06g:50mL:1.7mL:3.69g。
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