CN103694445B - 一种喷涂聚脲弹性材料的制备方法 - Google Patents

一种喷涂聚脲弹性材料的制备方法 Download PDF

Info

Publication number
CN103694445B
CN103694445B CN201310673022.XA CN201310673022A CN103694445B CN 103694445 B CN103694445 B CN 103694445B CN 201310673022 A CN201310673022 A CN 201310673022A CN 103694445 B CN103694445 B CN 103694445B
Authority
CN
China
Prior art keywords
performed polymer
ethyl
dmba
described step
diaminocarbazole
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310673022.XA
Other languages
English (en)
Other versions
CN103694445A (zh
Inventor
刘连河
和海清
王德成
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
QINGDAO ADVANCED MARINE MATERIAL TECHNOLOGY Co Ltd
Original Assignee
QINGDAO ADVANCED MARINE MATERIAL TECHNOLOGY Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by QINGDAO ADVANCED MARINE MATERIAL TECHNOLOGY Co Ltd filed Critical QINGDAO ADVANCED MARINE MATERIAL TECHNOLOGY Co Ltd
Priority to CN201310673022.XA priority Critical patent/CN103694445B/zh
Publication of CN103694445A publication Critical patent/CN103694445A/zh
Application granted granted Critical
Publication of CN103694445B publication Critical patent/CN103694445B/zh
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08—Processes
    • C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
    • C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
    • C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
    • C08G18/3819—Low-molecular-weight compounds having heteroatoms other than oxygen having nitrogen
    • C08G18/3842—Low-molecular-weight compounds having heteroatoms other than oxygen having nitrogen containing heterocyclic rings having at least one nitrogen atom in the ring
    • C08G18/3844—Low-molecular-weight compounds having heteroatoms other than oxygen having nitrogen containing heterocyclic rings having at least one nitrogen atom in the ring containing one nitrogen atom in the ring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C08G18/50—Polyethers having heteroatoms other than oxygen
    • C08G18/5021—Polyethers having heteroatoms other than oxygen having nitrogen
    • C08G18/5054—Polyethers having heteroatoms other than oxygen having nitrogen containing heterocyclic rings having at least one nitrogen atom in the ring
    • C08G18/5057—Polyethers having heteroatoms other than oxygen having nitrogen containing heterocyclic rings having at least one nitrogen atom in the ring containing one nitrogen atom in the ring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666—Compounds of group C08G18/48 or C08G18/52
    • C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/02—Polyureas

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Polyurethanes Or Polyureas (AREA)

Abstract

一种喷涂聚脲弹性材料的制备方法，是以IPDI、DEG、DMBA、聚醚胺D-2000为原料制备预聚体，加入三乙胺进行中和反应生成盐，加入N-乙基-3,6-二氨基咔唑的水溶液进行乳化扩链，制得聚脲乳液，有效延长了凝胶时间，增强了拉伸强度。

Description

一种喷涂聚脲弹性材料的制备方法
技术领域
本发明涉及一种喷涂聚脲弹性材料的制备方法，属化工领域。
技术背景
喷涂聚脲弹性材料是近二十年发展起来的一种无污染、高性能、快速固化、固含量达到95%以上的防护涂料，该涂料能在里面、曲面等多种结构上喷涂施工，同时，由于快速固化，使得聚脲弹性体对水分、湿气、温度等不敏感，由于其良好的固化特性，聚脲已广泛应用于防水、防腐等传统材料不能胜任的领域。
发明内容
本发明的目的是提供一种喷涂聚脲弹性材料的制备方法，有效延长了凝胶时间，增强了拉伸强度。
为实现以上目的，本发明的一种喷涂聚脲弹性材料的制备方法，步骤如下：
(1)异佛尔酮二异氰酸酯(IPDI)、聚醚胺D-2000、一缩二乙二醇(DEG)、二羟甲基丁酸(DMBA)为原料制备预聚体，反应2h；(2)降温至40℃，加入三乙胺进行中和反应生成盐，反应3-5min；(3)在N-乙基-3,6-二硝基咔唑中加入镁粉，再缓慢加入浓盐酸，回流至黄色沉淀变为白色沉淀，过滤后用水溶解，用质量浓度为10%的氢氧化钠中和上述溶液，至pH大于10，过滤后重结晶得到N-乙基-3,6-二氨基咔唑；(4)将N-乙基-3,6-二氨基咔唑加入到步骤(2)的盐溶液进行乳化扩链1h，得到聚脲乳液。
进一步的，所述的步骤(1)中预聚体原料的配比为：IPDI与聚醚胺D-2000、DEG、DMBA的摩尔比为1.3:1-1.4:1，DEG占预聚体质量的2%-3%，DMBA占预聚体质量的5%-6%。
进一步的，所述的步骤(2)中三乙胺的物质的量与DMBA的物质的量相同。
进一步的，所述的步骤(3)中N-乙基-3,6-二硝基咔唑与镁粉的质量比为1:2。
进一步的，所述的步骤(4)中N-乙基-3,6-二氨基咔唑的用量为预聚体质量的0.1%；水的用量为预聚体总质量的2倍。
本发明产生的有益效果为，本发明以N-乙基-3,6-二硝基咔唑为扩链剂合成了聚脲，凝胶时间明显延长，拉伸强度也有明显增强。
实施例
实施例1：
(1)异佛尔酮二异氰酸酯(IPDI)、聚醚胺D-2000、一缩二乙二醇(DEG)、二羟甲基丁酸(DMBA)为原料制备预聚体，反应2h，IPDI与聚醚胺D-2000、DEG、DMBA的摩尔比为1.3:1，DEG占预聚体质量的2%，DMBA占预聚体质量的5%；
(2)降温至40℃，加入三乙胺进行中和反应生成盐，反应3min，三乙胺的物质的量与DMBA的物质的量相同；
(3)在N-乙基-3,6-二硝基咔唑中加入镁粉，所述N-乙基-3,6-二硝基咔唑与镁粉的质量比为1:2，再缓慢加入浓盐酸，回流至黄色沉淀变为白色沉淀，过滤后用水溶解，用质量浓度为10%的氢氧化钠中和上述溶液，至pH大于10，过滤后重结晶得到N-乙基-3,6-二氨基咔唑；
(4)将N-乙基-3,6-二氨基咔唑的水溶液加入到步骤(2)的盐溶液进行乳化扩链1h，N-乙基-3,6-二氨基咔唑的用量为预聚体质量的0.1%，水的用量为预聚体总质量的2倍，得到聚脲乳液。
经测得，本发明的聚脲弹性材料的凝胶时间为98s，拉伸强度为71.5MPa。
实施例2：
(1)异佛尔酮二异氰酸酯(IPDI)、聚醚胺D-2000、一缩二乙二醇(DEG)、二羟甲基丁酸(DMBA)为原料制备预聚体，反应2h，IPDI与聚醚胺D-2000、DEG、DMBA的摩尔比为1.4:1，DEG占预聚体质量的2%，DMBA占预聚体质量的5%；
(2)降温至40℃，加入三乙胺进行中和反应生成盐，反应3min，三乙胺的物质的量与DMBA的物质的量相同；
(3)在N-乙基-3,6-二硝基咔唑中加入镁粉，所述N-乙基-3,6-二硝基咔唑与镁粉的质量比为1:2，再缓慢加入浓盐酸，回流至黄色沉淀变为白色沉淀，过滤后用水溶解，用质量浓度为10%的氢氧化钠中和上述溶液，至pH大于10，过滤后重结晶得到N-乙基-3,6-二氨基咔唑；
(4)将N-乙基-3,6-二氨基咔唑的水溶液加入到步骤(2)的盐溶液进行乳化扩链1h，N-乙基-3,6-二氨基咔唑的用量为预聚体质量的0.1%，水的用量为预聚体总质量的2倍，得到聚脲乳液。
经测得，本发明的聚脲弹性材料的凝胶时间为104s，拉伸强度为75.3MPa。

Claims (1)

1.一种喷涂聚脲弹性材料的制备方法，其特征在于：步骤如下：
(1)IPDI、聚醚胺D-2000、DEG、DMBA为原料制备预聚体，反应2h；
(2)降温至40℃，加入三乙胺进行中和反应生成盐，反应3-5min；
(3)在N-乙基-3,6-二硝基咔唑中加入镁粉，再缓慢加入浓盐酸，回流至黄色沉淀变为白色沉淀，过滤后用水溶解，用质量浓度为10%的氢氧化钠中和上述溶液，至pH大于10，过滤后重结晶得到N-乙基-3,6-二氨基咔唑；
(4)将N-乙基-3,6-二氨基咔唑的水溶液加入到步骤(2)的盐溶液进行中乳化扩链1h，得到聚脲乳液；
所述的步骤(1)中预聚体原料的配比为：IPDI与聚醚胺D-2000、DEG、DMBA的摩尔比为1.3:1-1.4:1，DEG占预聚体质量的2%-3%，DMBA占预聚体质量的5%-6%；
所述的步骤(2)中三乙胺的物质的量与DMBA的物质的量相同；
所述的步骤(3)中N-乙基-3,6-二硝基咔唑与镁粉的质量比为1:2；
所述的步骤(4)中N-乙基-3,6-二氨基咔唑的用量为预聚体质量的0.1%；
所述的步骤(4)中水的用量为预聚体总质量的2倍。
CN201310673022.XA 2013-12-12 2013-12-12 一种喷涂聚脲弹性材料的制备方法 Active CN103694445B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310673022.XA CN103694445B (zh) 2013-12-12 2013-12-12 一种喷涂聚脲弹性材料的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310673022.XA CN103694445B (zh) 2013-12-12 2013-12-12 一种喷涂聚脲弹性材料的制备方法

Publications (2)

Publication Number Publication Date
CN103694445A CN103694445A (zh) 2014-04-02
CN103694445B true CN103694445B (zh) 2016-02-17

Family

ID=50356122

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310673022.XA Active CN103694445B (zh) 2013-12-12 2013-12-12 一种喷涂聚脲弹性材料的制备方法

Country Status (1)

Country Link
CN (1) CN103694445B (zh)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104311785A (zh) * 2014-09-24 2015-01-28 徐广苓 一种阻燃型自交联喷涂聚脲弹性乳液的制备方法
CN106832175B (zh) * 2017-02-17 2019-10-18 华南理工大学 一种基于咔唑衍生物的双羟基荧光扩链剂及其制备与应用
CN107603440B (zh) * 2017-08-22 2021-07-09 山西省建筑科学研究院 聚脲型建筑用反射隔热涂料的制备方法
CN113234377A (zh) * 2021-05-21 2021-08-10 徐州双聚环保新材料有限公司 无溶剂免底涂封孔喷涂速干弹性体聚氨酯、ⅲ型聚脲防水涂料

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101407692A (zh) * 2008-11-14 2009-04-15 上海维凯化学品有限公司 一种耐紫外线的喷涂聚脲弹性体材料及其制备方法
CN102311700A (zh) * 2010-06-29 2012-01-11 拜耳材料科技(中国)有限公司 脂肪族聚脲涂料、制备方法及其应用

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101407692A (zh) * 2008-11-14 2009-04-15 上海维凯化学品有限公司 一种耐紫外线的喷涂聚脲弹性体材料及其制备方法
CN102311700A (zh) * 2010-06-29 2012-01-11 拜耳材料科技(中国)有限公司 脂肪族聚脲涂料、制备方法及其应用

Also Published As

Publication number Publication date
CN103694445A (zh) 2014-04-02

Similar Documents

Publication Publication Date Title
CN103694445B (zh) 一种喷涂聚脲弹性材料的制备方法
KR102043383B1 (ko) N-아실 산성 아미노산이나 그의 염의 화학적 제조 방법 및 응용
CN102743888A (zh) 一种新型泡泡液产品组合物及其制造方法
CN102977320A (zh) 一种端羟基聚丁二烯改性水性聚氨酯的方法
MX2019011094A (es) Composicion adhesiva y metodo para preparar la misma.
MX2015016073A (es) Metodo de fabricacion de sales antitranspirantes.
EP4321147A3 (en) Antiperspirant compositions
CN104592056B (zh) 一种n-羟基正辛酰胺的制备工艺
CN106748873A (zh) 一种维生素b5机械研磨固相制备方法
CN102816204A (zh) 阿斯巴甜的制备工艺
CN103894105A (zh) 一种n-长链酰基含羟基氨基酸表面活性剂及制造方法
CN101816622A (zh) 一种泡泡剂型染发剂及其制备方法
CN103571392B (zh) 一种汽车内饰件用防腐蚀热熔胶
CN102898610A (zh) 羟乙基封端聚二甲基硅氧烷改性水性聚氨酯的制备方法
WO2014121647A1 (zh) 一种n-甲基牛磺酸钠的制备方法
CN107033096A (zh) 2‑巯基‑6‑氯苯并恶唑的合成方法
CN103031732A (zh) 一种水性聚氨酯皮革黏合剂的制备方法
CN107793288A (zh) 一种2,4,5‑三氟溴苯的制备方法
CN103739815B (zh) 一种阻燃型喷涂聚脲弹性乳液的制备方法
CN102178615A (zh) 一种沐浴液
CN103951579B (zh) 一种正十二碳二酰基双天冬氨酸铵盐的合成方法
CN104311785A (zh) 一种阻燃型自交联喷涂聚脲弹性乳液的制备方法
CN104371496A (zh) 一种阴极水溶性电泳漆乳液及其制备方法
CN102977834A (zh) 一种水性聚氨酯皮革黏合剂
CN107488126A (zh) 通过双氧水合成2‑氨基‑3,5二溴苯甲醛的方法

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CP02 Change in the address of a patent holder

Address after: 266000 Qingdao science and technology, Huangdao District, Shandong, No. two road, No. 167

Patentee after: Qingdao Advanced Marine Material Technology Co., Ltd.

Address before: 266101, Qingdao Road, Zhuzhou District, Shandong, Laoshan, 143

Patentee before: Qingdao Advanced Marine Material Technology Co., Ltd.

CP02 Change in the address of a patent holder