CN113429730B - 一种高强度耐高温给水管及其制备方法 - Google Patents
一种高强度耐高温给水管及其制备方法 Download PDFInfo
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- 239000003508 Dilauryl thiodipropionate Substances 0.000 description 3
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- 235000019304 dilauryl thiodipropionate Nutrition 0.000 description 3
- 229920001903 high density polyethylene Polymers 0.000 description 3
- 239000004700 high-density polyethylene Substances 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 3
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- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 description 3
- 229960004889 salicylic acid Drugs 0.000 description 3
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 2
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Classifications
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/64—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by introduction of functional groups containing oxygen only in singly bound form
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D235/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings
- C07D235/02—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
- C07D235/04—Benzimidazoles; Hydrogenated benzimidazoles
- C07D235/18—Benzimidazoles; Hydrogenated benzimidazoles with aryl radicals directly attached in position 2
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
-
- 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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- 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
- C08K3/34—Silicon-containing compounds
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L9/00—Rigid pipes
- F16L9/12—Rigid pipes of plastics with or without reinforcement
-
- 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
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- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2203/18—Applications used for pipes
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
Abstract
本发明公开了一种高强度耐高温给水管,属于水管技术领域,以解决现有给水管的强度和耐热性差的问题。该给水管包括如下重量份的原料:聚乙烯树脂42.5‑60.8份、改性单体10.3‑20.5份、滑石粉1.2‑4.5份、轻质碳酸钙0.8‑1.1份、引发剂0.2‑0.4份、交联剂2.1‑4.3份、偶联剂0.4‑0.8份、稳定剂0.6‑1份、抗氧剂0.2‑0.5份;本发明还公开了该给水管的制备方法。本发明中引入改性单体和引发剂,使得聚乙烯树脂与改性单体发生自由基聚合反应来增加聚乙烯树脂多样化的性能,改性单体中含有大量苯环和苯并咪唑,环与环之间的共轭可以显著提高结构的耐热性能,从而增强基材的耐高温性。
Description
技术领域
本发明属于水管技术领域,涉及一种高强度耐高温给水管及其制备方法。
背景技术
高密度聚乙烯PE(聚乙烯)材料由于其强度高、耐腐蚀、无毒等特点,被广泛应用于给水管制造领域。因为它不会生锈,所以,是替代普通铁给水管的理想管材。
参照中国专利CN111347699A公开的一种PE给水管的制备方法,所述PE给水管的材料配方包括:聚乙烯树脂(PE)、聚乙烯蜡(PE蜡)、纳米碳黑、茂金属催化剂、抗氧化剂以及纳米银抗菌剂,通过在PE管的配方原料中添加茂金属催化剂与纳米银抗菌剂,提升成品PE管的强度与刚性,并且改善加工性能以及解决PE管管壁后期滋生细菌的问题。但是,传统的PE管由于配方材料单一,使得其用作给水管并长时间使用后,其韧性不足,抗冲击,热稳定差,在受到外界强热时容易发生破损,大大缩短使用寿命,造成安全隐患。
发明内容
本发明的目的在于提供一种高强度耐高温给水管及其制备方法,解决背景技术中提及的给水管强度和耐热性差的问题。
本发明的目的可以通过以下技术方案实现:
一种高强度耐高温给水管,包括如下重量份的原料:
聚乙烯树脂42.5-60.8份、改性单体10.3-20.5份、滑石粉1.2-4.5份、轻质碳酸钙0.8-1.1份、引发剂0.2-0.4份、交联剂2.1-4.3份、偶联剂0.4-0.8份、稳定剂0.6-1份、抗氧剂0.2-0.5份;
该高强度耐高温给水管由如下步骤制成:
步骤A1,将聚乙烯树脂、改性单体、滑石粉、轻质碳酸钙、稳定剂和抗氧剂加入混合机中,在60-80℃混合25-35min,得到混合物a;
步骤A2,向混合物a中加入交联剂、偶联剂、引发剂,在70-100℃反应5-6h,得到混合物b;
反应过程如下:
步骤A3,将混合物b加入双螺杆挤出机中造粒,熔融挤出,经冷却、切割、扩径、包装,得到高强度耐高温给水管。
进一步,步骤A1所述稳定剂为水杨酸、油酸、环烷酸中的任意一种,抗氧剂为二丁基羟基甲苯、硫代二丙酸二月桂酯中的任意一种。
进一步,步骤A2所述交联剂为2,5-二甲基-2,5-二(叔丁过氧基)己烷、过氧化苯二甲酰、过氧化二异丙苯、三聚异氰酸三烯丙酯中的任意一种,偶联剂为三乙醇胺硼酸酯、四正丙基锆酸酯、二硬脂酰氧异丙氧基铝酸酯、氨丙基三乙氧基硅烷中的任意一种,引发剂为偶氮二异丁腈、过氧化二异丙苯、过氧化苯甲酰、过氧化叔丁基二碳酸酯中的任意一种。
其中改性单体由如下步骤制得:
步骤S1,向三口烧瓶中加入4-硝基邻苯二胺、对苯二酰氯和N-甲基吡咯烷酮,搅拌均匀后,在25℃条件下回流反应13-15h,再升温至180℃反应5h,冷却至100℃并倒入冰水中搅拌1h,过滤,滤饼用去离子水洗涤2-3次,再经二甲基乙酰胺重结晶,得到中间体1,其中4-硝基邻苯二胺、对苯二酰氯、N-甲基吡咯烷酮的用量比为0.154-0.156mol:0.072-0.074mol:150.5-152.4mL;
反应过程如下:
步骤S2,向三口烧瓶中加入中间体1、无水乙醇,搅拌均匀后,向其中加入Pd/C催化剂,滴加质量分数85%的水合肼,回流反应12-13h,过滤除去Pd/C催化剂,向滤液中加入去离子水,过滤,滤饼用去离子水洗涤2-3次,用质量分数85%的乙醇溶液重结晶,得到中间体2,其中中间体1、无水乙醇、Pd/C催化剂、水合肼的用量比为0.0176-0.0178mol:151-155mL:0.53-0.55g:42.5-42.7mL;
反应过程如下:
步骤S3,向三口烧瓶中加入4-羟基苯甲醛、K2CO3、丙酮,搅拌均匀后,向其中滴加1,5-二溴戊烷的丙酮溶液,室温下回流反应16-17h,旋转蒸发除去溶剂,产物用二氯甲烷洗涤2-3次,用硫酸镁干燥后,再通过硅胶柱色谱纯化,得到中间体3,其中4-羟基苯甲醛、K2CO3、丙酮、1,5-二溴戊烷的丙酮溶液的用量比为16.4-16.8mmol:28.9-29.1mmol:20.1-20.3mL:5.3-5.4mL,1,5-二溴戊烷的丙酮溶液中1,5-二溴戊烷、丙酮的用量比为49.5-49.6mmol:5-6mL;
反应过程如下:
步骤S4,向三口烧瓶中加入中间体3、K2CO3、乙腈,搅拌均匀后,向其中加入中间体2,升温至100-110℃回流反应13-14h,冷却至室温,过滤,滤液经旋蒸除去溶剂,得到中间体4,其中中间体3、K2CO3、乙腈、中间体2的用量比为15.2-15.6mmol:45.4-45.8mmol:50.3-50.6mL:4.8-4.86g;
反应过程如下:
步骤S5,将乙基三苯基溴化磷加入三口烧瓶中,通入氮气,加入无水四氢呋喃,在-78℃条件下滴加1.3mol/L的正丁基锂溶液,在室温下搅拌1h,再将温度降低至-78℃,向其中滴加中间体4的四氢呋喃溶液,在室温下继续搅拌12h,将反应液倒入正己烷中,静置2h,过滤除去沉淀,滤液旋干,再用正丙醇重结晶,得到改性单体,其中乙基三苯基溴化磷、无水四氢呋喃、正丁基锂溶液、中间体4的四氢呋喃溶液的用量比为10.2-10.5mmol:40.2-40.8mL:7.5-7.8mL:19.8-20.5mL,中间体4的四氢呋喃溶液中四氢呋喃、中间体4的用量比为20mL:7.1-7.4mmol。
反应过程如下:
本发明的有益效果:本发明的目的在于提供一种高强度耐高温给水管及其制备方法,在配方中引入改性单体和引发剂,使得聚乙烯树脂与改性单体发生自由基聚合反应,来增加聚乙烯树脂多样化的性能,改性单体中含有大量苯环和苯并咪唑,环与环之间的共轭可以显著提高结构的耐热性能,从而增强基材的耐高温性,首先4-硝基邻苯二胺与对苯二酰氯反应生成含有氨基酰胺结构的过渡态,接着闭环生成咪唑环的中间体1,中间体1经还原生成中间体2,然后4-羟基苯甲醛与1,5-二溴戊烷反应脱去水生成中间体3,中间体3与中间体2反应脱去HBr生成中间体4,中间体4与乙基三苯基溴化磷在正丁基锂的作用下发生witting反应生成改性单体,由于该改性单体含有双键,在引发剂的作用下生成自由基,可与聚乙烯发生自由基聚合而接枝于聚乙烯支链上,改性单体其分子中含有N-H基团,可形成分子间氢键,苯并咪唑环与相邻的芳环直接相连,具有较强的分子链刚性以及分子间作用力,具备耐热性能,并且化学键的结合不易析出、稳定性好,大大提升聚乙烯树脂耐高温的性能。
其次,通过在高密度聚乙烯树脂中加入轻质碳酸钙,轻质碳酸钙作为填充改性剂,轻质碳酸钙可进入高密度聚乙烯、改性单体、偶联剂混合后的共混体系中,且分散均匀,轻质碳酸钙能很好的传递所承受的外力,消耗冲击能,从而起到很好的改性作用,使给水管获得较好的刚性强度和优异的稳定性。
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
改性单体由如下步骤制得:
步骤S1,向三口烧瓶中加入0.154mol 4-硝基邻苯二胺、0.072mol对苯二酰氯和150.5mL N-甲基吡咯烷酮,搅拌均匀后,在25℃条件下回流反应13h,再升温至180℃反应5h,冷却至100℃并倒入冰水中搅拌1h,过滤,滤饼用去离子水洗涤2次,再经二甲基乙酰胺重结晶,得到中间体1;
步骤S2,向三口烧瓶中加入0.0176mol中间体1、151mL无水乙醇,搅拌均匀后,向其中加入0.53g Pd/C催化剂,滴加42.5mL质量分数85%的水合肼,回流反应12h,过滤除去Pd/C催化剂,向滤液中加入去离子水,过滤,滤饼用去离子水洗涤2次,用质量分数85%的乙醇溶液重结晶,得到中间体2;
步骤S3,向三口烧瓶中加入16.4mmol4-羟基苯甲醛、28.9mmol K2CO3、20.1mL丙酮,搅拌均匀后,向其中滴加5.3mL1,5-二溴戊烷的丙酮溶液,室温下回流反应16h,旋转蒸发除去溶剂,产物用二氯甲烷洗涤2次,用硫酸镁干燥后,再通过硅胶柱色谱纯化,得到中间体3,其中1,5-二溴戊烷的丙酮溶液中1,5-二溴戊烷、丙酮的用量比为49.5mmol:5mL;
步骤S4,向三口烧瓶中加入15.2mmol中间体3、45.4mmol K2CO3、50.3mL乙腈,搅拌均匀后,向其中加入4.8g中间体2,升温至100℃回流反应13h,冷却至室温,过滤,滤液经旋蒸除去溶剂,得到中间体4;
骤S5,将10.2mmol乙基三苯基溴化磷加入三口烧瓶中,通入氮气,加入40.2mL无水四氢呋喃,在-78℃条件下滴加7.5mL 1.3mol/L的正丁基锂溶液,在室温下搅拌1h,再将温度降低至-78℃,向其中滴加19.8mL中间体4的四氢呋喃溶液,在室温下继续搅拌12h,将反应液倒入正己烷中,静置2h,过滤除去沉淀,滤液旋干,再用正丙醇重结晶,得到改性单体,其中中间体4的四氢呋喃溶液中四氢呋喃、中间体4的用量比为20mL:7.1mmol。
实施例2
改性单体由如下步骤制得:
步骤S1,向三口烧瓶中加入0.155mol4-硝基邻苯二胺、0.073mol对苯二酰氯和151.4mL N-甲基吡咯烷酮,搅拌均匀后,在25℃条件下回流反应14h,再升温至180℃反应5h,冷却至100℃并倒入冰水中搅拌1h,过滤,滤饼用去离子水洗涤2次,再经二甲基乙酰胺重结晶,得到中间体1;
步骤S2,向三口烧瓶中加入0.0177mol中间体1、153mL无水乙醇,搅拌均匀后,向其中加入0.54g Pd/C催化剂,滴加42.6mL质量分数85%的水合肼,回流反应12h,过滤除去Pd/C催化剂,向滤液中加入去离子水,过滤,滤饼用去离子水洗涤2次,用质量分数85%的乙醇溶液重结晶,得到中间体2;
步骤S3,向三口烧瓶中加入16.6mmol4-羟基苯甲醛、29mmol K2CO3、20.2mL丙酮,搅拌均匀后,向其中滴加5.3mL1,5-二溴戊烷的丙酮溶液,室温下回流反应16h,旋转蒸发除去溶剂,产物用二氯甲烷洗涤2次,用硫酸镁干燥后,再通过硅胶柱色谱纯化,得到中间体3,其中1,5-二溴戊烷的丙酮溶液中1,5-二溴戊烷、丙酮的用量比为49.5mmol:5mL;
步骤S4,向三口烧瓶中加入15.4mmol中间体3、45.6mmol K2CO3、50.4mL乙腈,搅拌均匀后,向其中加入4.83g中间体2,升温至105℃回流反应13h,冷却至室温,过滤,滤液经旋蒸除去溶剂,得到中间体4;
骤S5,将10.4mmol乙基三苯基溴化磷加入三口烧瓶中,通入氮气,加入40.5mL无水四氢呋喃,在-78℃条件下滴加7.7mL 1.3mol/L的正丁基锂溶液,在室温下搅拌1h,再将温度降低至-78℃,向其中滴加20.3mL中间体4的四氢呋喃溶液,在室温下继续搅拌12h,将反应液倒入正己烷中,静置2h,过滤除去沉淀,滤液旋干,再用正丙醇重结晶,得到改性单体,其中中间体4的四氢呋喃溶液中四氢呋喃、中间体4的用量比为20mL:7.2mmol。
实施例3
改性单体由如下步骤制得:
步骤S1,向三口烧瓶中加入0.156mol4-硝基邻苯二胺、0.074mol对苯二酰氯和152.4mL N-甲基吡咯烷酮,搅拌均匀后,在25℃条件下回流反应15h,再升温至180℃反应5h,冷却至100℃并倒入冰水中搅拌1h,过滤,滤饼用去离子水洗涤3次,再经二甲基乙酰胺重结晶,得到中间体1;
步骤S2,向三口烧瓶中加入0.0178mol中间体1、155mL无水乙醇,搅拌均匀后,向其中加入0.55g Pd/C催化剂,滴加42.7mL质量分数85%的水合肼,回流反应13h,过滤除去Pd/C催化剂,向滤液中加入去离子水,过滤,滤饼用去离子水洗涤3次,用质量分数85%的乙醇溶液重结晶,得到中间体2;
步骤S3,向三口烧瓶中加入16.8mmol4-羟基苯甲醛、29.1mmol K2CO3、20.3mL丙酮,搅拌均匀后,向其中滴加5.4mL1,5-二溴戊烷的丙酮溶液,室温下回流反应17h,旋转蒸发除去溶剂,产物用二氯甲烷洗涤3次,用硫酸镁干燥后,再通过硅胶柱色谱纯化,得到中间体3,其中1,5-二溴戊烷的丙酮溶液中1,5-二溴戊烷、丙酮的用量比为49.6mmol:6mL;
步骤S4,向三口烧瓶中加入15.6mmol中间体3、45.8mmol K2CO3、50.6mL乙腈,搅拌均匀后,向其中加入4.86g中间体2,升温至110℃回流反应14h,冷却至室温,过滤,滤液经旋蒸除去溶剂,得到中间体4;
骤S5,将10.5mmol乙基三苯基溴化磷加入三口烧瓶中,通入氮气,加入40.8mL无水四氢呋喃,在-78℃条件下滴加7.8mL 1.3mol/L的正丁基锂溶液,在室温下搅拌1h,再将温度降低至-78℃,向其中滴加20.5mL中间体4的四氢呋喃溶液,在室温下继续搅拌12h,将反应液倒入正己烷中,静置2h,过滤除去沉淀,滤液旋干,再用正丙醇重结晶,得到改性单体,其中中间体4的四氢呋喃溶液中四氢呋喃、中间体4的用量比为20mL:7.4mmol。
实施例4
一种高强度耐高温给水管,包括如下重量份的原料:
聚乙烯树脂42.5份、改性单体10.3份、滑石粉1.2份、轻质碳酸钙0.8份、偶氮二异丁腈0.2份、2,5-二甲基-2,5-二(叔丁过氧基)己烷2.1份、三乙醇胺硼酸酯0.4份、水杨酸0.6份、二丁基羟基甲苯0.2份;
该高强度耐高温给水管由如下步骤制成:
步骤A1,将聚乙烯树脂、实施例1制备的改性单体、滑石粉、轻质碳酸钙、水杨酸和二丁基羟基甲苯加入混合机中,在60℃混合25min,得到混合物a;
步骤A2,向混合物a中加入2,5-二甲基-2,5-二(叔丁过氧基)己烷、三乙醇胺硼酸酯、偶氮二异丁腈,在70℃反应5h,得到混合物b;
步骤A3,将混合物b加入双螺杆挤出机中造粒,熔融挤出,经冷却、切割、扩径、包装,得到高强度耐高温给水管。
实施例5
一种高强度耐高温给水管,包括如下重量份的原料:
聚乙烯树脂51.3份、改性单体15.8份、滑石粉2.5份、轻质碳酸钙0.9份、偶氮二异丁腈0.3份、过氧化苯二甲酰3.8份、四正丙基锆酸酯0.6份、油酸0.8份、二丁基羟基甲苯0.3份;
该高强度耐高温给水管由如下步骤制成:
步骤A1,将聚乙烯树脂、实施例2制备的改性单体、滑石粉、轻质碳酸钙、油酸和二丁基羟基甲苯加入混合机中,在70℃混合30min,得到混合物a;
步骤A2,向混合物a中加入过氧化苯二甲酰、四正丙基锆酸酯、偶氮二异丁腈,在85℃反应5h,得到混合物b;
步骤A3,将混合物b加入双螺杆挤出机中造粒,熔融挤出,经冷却、切割、扩径、包装,得到高强度耐高温给水管。
实施例6
一种高强度耐高温给水管,包括如下重量份的原料:
聚乙烯树脂60.8份、改性单体20.5份、滑石粉4.5份、轻质碳酸钙1.1份、偶氮二异丁腈0.4份、三聚异氰酸三烯丙酯4.3份、氨丙基三乙氧基硅烷0.8份、环烷酸1份、硫代二丙酸二月桂酯0.5份;
该高强度耐高温给水管由如下步骤制成:
步骤A1,将聚乙烯树脂、实施例3制备的改性单体、滑石粉、轻质碳酸钙、环烷酸和硫代二丙酸二月桂酯加入混合机中,在80℃混合35min,得到混合物a;
步骤A2,向混合物a中加入三聚异氰酸三烯丙酯、氨丙基三乙氧基硅烷、偶氮二异丁腈,在100℃反应6h,得到混合物b;
步骤A3,将混合物b加入双螺杆挤出机中造粒,熔融挤出,经冷却、切割、扩径、包装,得到高强度耐高温给水管。
对比例1
山东中科欧普管道有限公司生产的PE给水管。
对比例2
对比例2的给水管的制备方法参照实施例4,不同点在于不添加轻质碳酸钙。
对比例3
对比例3的给水管的制备方法参照实施例4,不同点在于不添加改性单体和引发剂。
对实施例4-6和对比例1-3得到的给水管做如下性能测试,测试结果见表1:
表1
由表1可知,相较于对比例1-3,实施例4-6制备的给水管有较优的刚性强度和耐热性能。
在说明书的描述中,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 (7)
1.一种高强度耐高温给水管,其特征在于,包括如下重量份的原料:聚乙烯树脂42.5-60.8份、改性单体10.3-20.5份、滑石粉1.2-4.5份、轻质碳酸钙0.8-1.1份、引发剂0.2-0.4份、交联剂2.1-4.3份、偶联剂0.4-0.8份、稳定剂0.6-1份、抗氧剂0.2-0.5份;
其中改性单体由如下步骤制得:
步骤S1,将4-硝基邻苯二胺、对苯二酰氯和N-甲基吡咯烷酮搅拌均匀后,在25℃条件下回流反应13-15h,再升温至180℃反应5h,冷却并倒入冰水中结晶,过滤,滤饼经洗涤、重结晶,得到中间体1;
步骤S2,将中间体1、无水乙醇搅拌均匀后,向其中加入Pd/C催化剂和水合肼,回流反应12-13h,过滤,向滤液中加入去离子水,再过滤,滤饼经洗涤、重结晶,得到中间体2;
步骤S3,将4-羟基苯甲醛、K2CO3、丙酮搅拌均匀后,向其中滴加1,5-二溴戊烷的丙酮溶液,室温下回流反应16-17h,旋转蒸发除去溶剂,产物经洗涤、干燥、纯化,得到中间体3;
步骤S4,将中间体3、K2CO3、乙腈搅拌均匀后,加入中间体2,升温至100-110℃回流反应13-14h,冷却至室温,过滤,滤液旋蒸后,得到中间体4;
步骤S5,将乙基三苯基溴化磷加入三口烧瓶中,通入氮气,加入无水四氢呋喃,在-78℃条件下滴加正丁基锂溶液,在室温下搅拌1h,再将温度降低至-78℃,向其中滴加中间体4的四氢呋喃溶液,在室温下搅拌12h,将反应液倒入正己烷中,静置2h,过滤,滤液旋干,经重结晶,得到改性单体。
2.根据权利要求1所述的一种高强度耐高温给水管,其特征在于:步骤S1所述4-硝基邻苯二胺、对苯二酰氯、N-甲基吡咯烷酮的用量比为0.154-0.156mol:0.072-0.074mol:150.5-152.4mL。
3.根据权利要求1所述的一种高强度耐高温给水管,其特征在于:步骤S2所述中间体1、无水乙醇、Pd/C催化剂、水合肼的用量比为0.0176-0.0178mol:151-155mL:0.53-0.55g:42.5-42.7mL。
4.根据权利要求1所述的一种高强度耐高温给水管,其特征在于:步骤S3所述4-羟基苯甲醛、K2CO3、丙酮、1,5-二溴戊烷的丙酮溶液的用量比为16.4-16.8mmol:28.9-29.1mmol:20.1-20.3mL:5.3-5.4mL,1,5-二溴戊烷的丙酮溶液中1,5-二溴戊烷、丙酮的用量比为49.5-49.6mmol:5-6mL。
5.根据权利要求1所述的一种高强度耐高温给水管,其特征在于:步骤S4所述中间体3、K2CO3、乙腈、中间体2的用量比为15.2-15.6mmol:45.4-45.8mmol:50.3-50.6mL:4.8-4.86g。
6.根据权利要求1所述的一种高强度耐高温给水管,其特征在于:步骤S5所述乙基三苯基溴化磷、无水四氢呋喃、正丁基锂溶液、中间体4的四氢呋喃溶液的用量比为10.2-10.5mmol:40.2-40.8mL:7.5-7.8mL:19.8-20.5mL,中间体4的四氢呋喃溶液中四氢呋喃、中间体4的用量比为20mL:7.1-7.4mmol。
7.根据权利要求1所述的一种高强度耐高温给水管的制备方法,其特征在于:包括如下制备步骤:
步骤A1,将聚乙烯树脂、改性单体、滑石粉、轻质碳酸钙、稳定剂和抗氧剂加入混合机中,在60-80℃混合25-35min,得到混合物a;
步骤A2,向混合物a中加入交联剂、偶联剂、引发剂,在70-100℃反应5-6h,得到混合物b;
步骤A3,将混合物b加入双螺杆挤出机中造粒,熔融挤出,经冷却、切割、扩径、包装,得到高强度耐高温给水管。
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