CN107286284A - 一种皂化丙烯酸酯共聚保温材料的制备方法 - Google Patents
一种皂化丙烯酸酯共聚保温材料的制备方法 Download PDFInfo
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- 239000012774 insulation material Substances 0.000 title claims abstract description 15
- 238000007334 copolymerization reaction Methods 0.000 title claims abstract description 13
- 125000005396 acrylic acid ester group Chemical group 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 47
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 24
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 14
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- ONIKNECPXCLUHT-UHFFFAOYSA-N 2-chlorobenzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1Cl ONIKNECPXCLUHT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 5
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- FYHXNYLLNIKZMR-UHFFFAOYSA-N calcium;carbonic acid Chemical compound [Ca].OC(O)=O FYHXNYLLNIKZMR-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000004519 grease Substances 0.000 claims description 6
- ZCTXEAQXZGPWFG-UHFFFAOYSA-N imidurea Chemical compound O=C1NC(=O)N(CO)C1NC(=O)NCNC(=O)NC1C(=O)NC(=O)N1CO ZCTXEAQXZGPWFG-UHFFFAOYSA-N 0.000 claims description 6
- 238000007127 saponification reaction Methods 0.000 claims description 6
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims description 5
- JSGVZVOGOQILFM-UHFFFAOYSA-N 3-methoxy-1-butanol Chemical class COC(C)CCO JSGVZVOGOQILFM-UHFFFAOYSA-N 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 229920000642 polymer Polymers 0.000 abstract description 8
- 239000004793 Polystyrene Substances 0.000 abstract description 6
- 229920002223 polystyrene Polymers 0.000 abstract description 6
- 239000002131 composite material Substances 0.000 abstract description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 abstract description 2
- 230000000977 initiatory effect Effects 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
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- 239000002994 raw material Substances 0.000 description 3
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- MSJFJOQCWAVXBU-UHFFFAOYSA-L C=CC1=CC=CC=C1.C([O-])([O-])=O.[Ca+2] Chemical compound C=CC1=CC=CC=C1.C([O-])([O-])=O.[Ca+2] MSJFJOQCWAVXBU-UHFFFAOYSA-L 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- -1 calcium carbonate alcohol Amine Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- GFAUNYMRSKVDJL-UHFFFAOYSA-N formyl chloride Chemical compound ClC=O GFAUNYMRSKVDJL-UHFFFAOYSA-N 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000006902 nitrogenation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 229920006389 polyphenyl polymer Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- 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
- C08F212/00—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 an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/14—Monomers containing only one unsaturated aliphatic radical containing one ring substituted by heteroatoms or groups containing heteroatoms
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- 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
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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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- 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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- 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
- C08K2003/265—Calcium, strontium or barium carbonate
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- Compositions Of Macromolecular Compounds (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract
本发明公开了一种皂化丙烯酸酯共聚保温材料的制备方法,本发明将碳酸钙通过有机化改性,然后将苯乙烯通过苯甲酰氯处理,与有机化碳酸钙混合,在过硫酸铵引发作用下聚合,得到共聚保温材料,本发明的复合材料通过丙烯酸酯改性后,可以有效的提高碳酸钙的有机化,特别适用于作为聚合物的填充材料,能够与聚合物很好的相容,能够提高其与聚合物的分散性,有效的降低团聚,提高碳酸钙与聚合物复合材料的稳定性强度,本发明的材料中加入的聚苯乙烯可以有效的提高成品材料的保温性能。
Description
技术领域
本发明属于材料领域,具体涉及一种皂化丙烯酸酯共聚保温材料的制备方法。
背景技术
建筑涂料具有装饰、保护和居住性改进等功能,涂饰物质表面,能改变其颜色、花纹、光泽、质感等,提高物体的美观价值,能保护被涂饰物的表面,防止来自外界的光、氧、化学物质、溶剂等的侵蚀,提高被涂覆物的使用寿命;
申请号 201510947707.8,公开了一种外墙保温材料,包括下述重量份的原料:聚苯乙烯粒子25-45 份,硅酸盐水泥20-30份,碳酸钙5-10份,发泡剂1-3份,硅酸钠0.1-0.7份,水20-40份,其是将聚苯乙烯粒子、碳酸钙共混成型,
申请号 201310671029.8,公开了一种外墙保温材料,该外墙保温材料的原料包括以下组分及重量份含量:聚苯乙烯粒子30-60份、膨胀珍珠岩20-50份、水玻璃35-85份、锂基膨润土10-40份、煅烧高岭土5-25份、碳酸钙3-10份、阻燃剂3-15 份,其是将各原料共混,搅拌均匀,再成型的方法;
可以看出,传统的复合材料中将聚苯乙烯、碳酸钙共混大多为简单的搅拌、热压等方式处理成型,容易造成碳酸钙在聚苯乙烯中的团聚,降低成品的稳定性强度。
发明内容
本发明的目的在于针对现有技术的缺陷和不足,提供一种皂化丙烯酸酯共聚保温材料的制备方法。
为实现上述目的,本发明采用以下技术方案:
一种皂化丙烯酸酯共聚保温材料的制备方法,包括以下步骤:
(1)取碳酸钙,与三乙醇胺混合,加入到混合料重量10-14倍的去离子水中,超声3-4分钟,加入混合料重量2-3倍的、68-70%的氢氧化钠溶液,升高稳定为65-70℃,保温搅拌30-40分钟,得碳酸钙醇胺分散液;(2)取双咪唑烷基脲,加入到其重量40-50倍的叔丁醇中,搅拌均匀,与丙烯酸混合,升高温度为70-75℃,保温搅拌1-2小时,蒸馏除去叔丁醇,加入到上述碳酸钙醇胺分散液,搅拌反应3-4小时,得皂化碳酸钙酯分散液;
(3)取苯乙烯,加入到其重量5-8倍的3-甲氧基丁醇中,送入到80-90℃的恒温水浴中,加入苯甲酰氯,保温搅拌30-40分钟,出料,冷却至常温,得酰氯苯乙烯单体;
(4)取上述酰氯苯乙烯单体,加入到其重量10-14倍的去离子水中,搅拌均匀,加入过硫酸铵,升高温度为70-75℃,加入皂化碳酸钙酯分散液,通入氮气,保温搅拌4-7小时,过滤,将沉淀用无水乙醇、去离子水依次洗涤,真空60-70℃下干燥1-2小时,得皂化丙烯酸酯共聚保温材料;
所述的碳酸钙、三乙醇胺、双咪唑烷基脲、丙烯酸、苯乙烯、苯甲酰氯、过硫酸铵的重量比为20-30:1-2:2-3:9-12:80-100:3-6:4-5。
本发明的优点:
本发明将碳酸钙通过有机化改性,然后将苯乙烯通过苯甲酰氯处理,与有机化碳酸钙混合,在过硫酸铵引发作用下聚合,得到共聚保温材料,本发明的复合材料通过丙烯酸酯改性后,可以有效的提高碳酸钙的有机化,特别适用于作为聚合物的填充材料,能够与聚合物很好的相容,能够提高其与聚合物的分散性,有效的降低团聚,提高碳酸钙与聚合物复合材料的稳定性强度,本发明的材料中加入的聚苯乙烯可以有效的提高成品材料的保温性能。
具体实施方式
实施例1
一种皂化丙烯酸酯共聚保温材料的制备方法,包括以下步骤:
(1)取碳酸钙,与三乙醇胺混合,加入到混合料重量14倍的去离子水中,超声3分钟,加入混合料重量3倍的、70%的氢氧化钠溶液,升高稳定为70℃,保温搅拌30分钟,得碳酸钙醇胺分散液;(2)取双咪唑烷基脲,加入到其重量40倍的叔丁醇中,搅拌均匀,与丙烯酸混合,升高温度为75℃,保温搅拌1小时,蒸馏除去叔丁醇,加入到上述碳酸钙醇胺分散液,搅拌反应4小时,得皂化碳酸钙酯分散液;
(3)取苯乙烯,加入到其重量8倍的3-甲氧基丁醇中,送入到90℃的恒温水浴中,加入苯甲酰氯,保温搅拌40分钟,出料,冷却至常温,得酰氯苯乙烯单体;
(4)取上述酰氯苯乙烯单体,加入到其重量14倍的去离子水中,搅拌均匀,加入过硫酸铵,升高温度为75℃,加入皂化碳酸钙酯分散液,通入氮气,保温搅拌4小时,过滤,将沉淀用无水乙醇、去离子水依次洗涤,真空70℃下干燥1小时,得皂化丙烯酸酯共聚保温材料;
所述的碳酸钙、三乙醇胺、双咪唑烷基脲、丙烯酸、苯乙烯、苯甲酰氯、过硫酸铵的重量比为30:1:3:9:80-100:3:4。
Claims (1)
1.一种皂化丙烯酸酯共聚保温材料的制备方法,其特征在于,包括以下步骤:
(1)取碳酸钙,与三乙醇胺混合,加入到混合料重量10-14倍的去离子水中,超声3-4分钟,加入混合料重量2-3倍的、68-70%的氢氧化钠溶液,升高稳定为65-70℃,保温搅拌30-40分钟,得碳酸钙醇胺分散液;(2)取双咪唑烷基脲,加入到其重量40-50倍的叔丁醇中,搅拌均匀,与丙烯酸混合,升高温度为70-75℃,保温搅拌1-2小时,蒸馏除去叔丁醇,加入到上述碳酸钙醇胺分散液,搅拌反应3-4小时,得皂化碳酸钙酯分散液;
(3)取苯乙烯,加入到其重量5-8倍的3-甲氧基丁醇中,送入到80-90℃的恒温水浴中,加入苯甲酰氯,保温搅拌30-40分钟,出料,冷却至常温,得酰氯苯乙烯单体;
(4)取上述酰氯苯乙烯单体,加入到其重量10-14倍的去离子水中,搅拌均匀,加入过硫酸铵,升高温度为70-75℃,加入皂化碳酸钙酯分散液,通入氮气,保温搅拌4-7小时,过滤,将沉淀用无水乙醇、去离子水依次洗涤,真空60-70℃下干燥1-2小时,得皂化丙烯酸酯共聚保温材料;
所述的碳酸钙、三乙醇胺、双咪唑烷基脲、丙烯酸、苯乙烯、苯甲酰氯、过硫酸铵的重量比为20-30:1-2:2-3:9-12:80-100:3-6:4-5。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN101466799A (zh) * | 2006-06-09 | 2009-06-24 | 欧米亚发展集团 | 无机和/或有机微粒与纳米碳酸钙颗粒的复合物 |
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| CN101466799A (zh) * | 2006-06-09 | 2009-06-24 | 欧米亚发展集团 | 无机和/或有机微粒与纳米碳酸钙颗粒的复合物 |
| CN1887780A (zh) * | 2006-07-17 | 2007-01-03 | 江西省中科新型建材有限公司 | 纳米改性砂浆外墙保温节能材料 |
| CN104945956A (zh) * | 2015-06-05 | 2015-09-30 | 安徽雪城超细碳酸钙有限公司 | 一种具有隔热保温作用的改性碳酸钙及其制备方法 |
| CN106590057A (zh) * | 2016-11-29 | 2017-04-26 | 安徽九子山塑业有限公司 | 一种耐磨损的丙烯酸酯改性的碳酸钙填料及其制备方法 |
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Application publication date: 20171024 |