CN114686152B - 一种灌注/压注型环氧树脂结构胶及其应用 - Google Patents
一种灌注/压注型环氧树脂结构胶及其应用 Download PDFInfo
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- CN114686152B CN114686152B CN202210433500.9A CN202210433500A CN114686152B CN 114686152 B CN114686152 B CN 114686152B CN 202210433500 A CN202210433500 A CN 202210433500A CN 114686152 B CN114686152 B CN 114686152B
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- epoxy resin
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- bisphenol
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- -1 modified phenolic amine Chemical class 0.000 claims abstract description 38
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 24
- 150000001412 amines Chemical class 0.000 claims abstract description 17
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- 238000010276 construction Methods 0.000 claims description 17
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical group CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
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- 229920001451 polypropylene glycol Polymers 0.000 claims description 8
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- 125000005375 organosiloxane group Chemical group 0.000 claims description 4
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical group CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 3
- HHRACYLRBOUBKM-UHFFFAOYSA-N 2-[(4-tert-butylphenoxy)methyl]oxirane Chemical compound C1=CC(C(C)(C)C)=CC=C1OCC1OC1 HHRACYLRBOUBKM-UHFFFAOYSA-N 0.000 claims description 3
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 3
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 2
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
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- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- YTZKOQUCBOVLHL-UHFFFAOYSA-N tert-butylbenzene Chemical compound CC(C)(C)C1=CC=CC=C1 YTZKOQUCBOVLHL-UHFFFAOYSA-N 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- JOLVYUIAMRUBRK-UHFFFAOYSA-N 11',12',14',15'-Tetradehydro(Z,Z-)-3-(8-Pentadecenyl)phenol Natural products OC1=CC=CC(CCCCCCCC=CCC=CCC=C)=C1 JOLVYUIAMRUBRK-UHFFFAOYSA-N 0.000 description 1
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- SFJRUJUEMVAZLM-UHFFFAOYSA-N 2-[(2-methylpropan-2-yl)oxymethyl]oxirane Chemical compound CC(C)(C)OCC1CO1 SFJRUJUEMVAZLM-UHFFFAOYSA-N 0.000 description 1
- YLKVIMNNMLKUGJ-UHFFFAOYSA-N 3-Delta8-pentadecenylphenol Natural products CCCCCCC=CCCCCCCCC1=CC=CC(O)=C1 YLKVIMNNMLKUGJ-UHFFFAOYSA-N 0.000 description 1
- YXALYBMHAYZKAP-UHFFFAOYSA-N 7-oxabicyclo[4.1.0]heptan-4-ylmethyl 7-oxabicyclo[4.1.0]heptane-4-carboxylate Chemical compound C1CC2OC2CC1C(=O)OCC1CC2OC2CC1 YXALYBMHAYZKAP-UHFFFAOYSA-N 0.000 description 1
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- JOLVYUIAMRUBRK-UTOQUPLUSA-N Cardanol Chemical compound OC1=CC=CC(CCCCCCC\C=C/C\C=C/CC=C)=C1 JOLVYUIAMRUBRK-UTOQUPLUSA-N 0.000 description 1
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- 229910019142 PO4 Inorganic materials 0.000 description 1
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- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5026—Amines cycloaliphatic
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
-
- 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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- E—FIXED CONSTRUCTIONS
- E02—HYDRAULIC ENGINEERING; FOUNDATIONS; SOIL SHIFTING
- E02D—FOUNDATIONS; EXCAVATIONS; EMBANKMENTS; UNDERGROUND OR UNDERWATER STRUCTURES
- E02D3/00—Improving or preserving soil or rock, e.g. preserving permafrost soil
- E02D3/12—Consolidating by placing solidifying or pore-filling substances in the soil
-
- E—FIXED CONSTRUCTIONS
- E02—HYDRAULIC ENGINEERING; FOUNDATIONS; SOIL SHIFTING
- E02D—FOUNDATIONS; EXCAVATIONS; EMBANKMENTS; UNDERGROUND OR UNDERWATER STRUCTURES
- E02D37/00—Repair of damaged foundations or foundation structures
-
- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04G—SCAFFOLDING; FORMS; SHUTTERING; BUILDING IMPLEMENTS OR AIDS, OR THEIR USE; HANDLING BUILDING MATERIALS ON THE SITE; REPAIRING, BREAKING-UP OR OTHER WORK ON EXISTING BUILDINGS
- E04G23/00—Working measures on existing buildings
- E04G23/02—Repairing, e.g. filling cracks; Restoring; Altering; Enlarging
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/346—Applications of adhesives in processes or use of adhesives in the form of films or foils for building applications e.g. wrap foil
Abstract
本发明属于建筑材料领域,具体涉及一种灌注/压注型环氧树脂结构胶及其应用。所述灌注/压注型环氧树脂结构胶,由A、B组分构成,A、B组分质量比为2:1~3:1;按质量份数计,A组分含有双酚A型环氧树脂50~70份、双酚F型环氧树脂10~15份、稀释剂20~50份、偶联剂1~10份;B组分包含卞醇5~20份、基础胺10~30份、改性酚醛胺30~80份、固化促进剂3~10份;所述改性酚醛胺粘度不高于1000mPa.s,热变形温度不低于60℃,固化温度低至5℃。本发明提供的环氧树脂结构胶色泽浅、粘接强度高,粘度低,可涂刷或灌封作业,也可加压浇注,渗透性好,能够扩散至0.2mm以下缝宽的微细裂纹内。
Description
技术领域
本发明属于建筑材料领域,具体涉及一种灌注/压注型环氧树脂结构胶及其应用。
背景技术
因具备粘接强度高、尺寸收缩率低、性能调节空间大等诸多优势,环氧树脂自面世以来被广泛应用于电子、电器、建筑、化工等众多行业。常规环氧树脂粘度较大,一般需要搭配稀释剂使用,普通惰性(如丙酮、甲乙酮、磷酸酯等)或非惰性稀释剂(如丁基缩水甘油醚)对其有着明显降粘效果,但往往会损失固化物耐温性与机械强度;脂环族稀释剂(如3,4-环氧环己基甲基-3,4-环氧环己基甲酸酯)分子链上含有稳定的六元闭环结构,有利于提升产物玻璃化转变温度,但价格相对过高。再者,环氧制品的性能很大程度上取决于固化剂,酸酐固化剂多需加热至中温或高温方可反应,不利于户外常温施工,产物硬度高,但偏脆,抗冲击强度低;而基础胺(如多烯烃多胺)、聚醚胺常温(23℃)即可固化,改性胺(如酮亚胺、酚醛胺)则在更低温度(5℃)下仍拥有良好活性,但反应物略显柔性,硬度、耐热、模量等均不及酸酐类,因此原材料组配对最终产品的性能、性价比和适用领域影响颇大。
对于混凝土或岩层微小裂缝(缝宽0.01~10mm)修补加固用灌注或压注浆料而言,通常应有着极低的粘度和高浸润渗透性,以利于扩散填充至砼基础施工缝、冷接缝、岩基缝,以及更为狭窄的由于应力、冷热收缩等原因导致的纤细裂纹(缝宽0.01~1mm)内部;同时由于裂隙带大多存在渗/漏水情况,所以最好还能够在潮湿状态甚至水下直接施工,且与原基础可靠粘接(干粘强度一般要求3~4MPa以上,湿粘强度应在2~3MPa以上)。
早期的化学灌浆料大多以有机溶剂对环氧树脂进行稀释。如专利CN102433057B、CN104628994A、CN102585441B、CN105238218B等皆掺入大量丙酮、糠醛,粘度可低至10~30mPa.s,但由于二者的高挥发性或毒副性,对操作人员存在伤害,欧美等发达国家已明令禁止将糠醛作为涂料、胶粘剂行业添加物。
CN102070873A、CN102838960B利用非醛-酮体系,以缩水甘油醚/酯型环氧化合物实现了低粘度,环境友好性得以改善,但大剂量小分子聚醚胺的使用可能导致夏季高温作业时出现“爆聚”,或冬季低温下反应过慢,以及固化物断裂伸长率高、耐热性差、潮湿环境容易脱粘等潜在风险。
CN107384129A尝试以双酚F型环氧混掺来降低双酚A型环氧的粘度,但出于一道涂装即可获得较厚漆膜的考虑,同时添加了20~25份云母粉。实际上,无机粉料的加入不仅提升了粘度,降低了双酚F环氧的使用效果和性价比(双酚F型环氧价格远高于双酚A型),还可能成为环氧树脂低温结晶的晶核,进而诱发其析出分相,造成组分比例失调,这也许是该组合物需要现配现用、难以长时间存储的原因之一。
CN111410821A公开了一种针对集中渗漏水缺陷的灌浆材料及灌浆方法,其稀释剂由10~14%环氧氯丙烷、45~55%脂肪醇、6~10%多聚醚酯、25~35%三氯丙烷混合而成。此灌浆料在有水环境下与原混凝土基面粘接强度高,能够对渗漏水通道起到较好的止水补强效果。但选用的环氧氯丙烷和三氯丙烷,具有较强致癌、致畸、麻醉性,氯离子水解后还会对钢筋、砼结构产生电化学腐蚀,且只适合灌注涌水量高达200~300m3/h的大型裂缝,小裂隙很可能存在渗透深度问题。
CN108047657B提供了一种高强高流动性三组分环氧树脂灌浆材料及其制备方法,该料C组分由大量无机粉体构成,其粘度大、渗透性有限,主要用于填充厘米级以上间隙。
CN113061323A公开了一种灌浆材料,具有初始粘度低、干/湿粘结强度高等优势,但如此低粘度(71~102mPa.s)下,其中的无机填料(氧化铝、氧化锌)将在短时间内随即沉底,只能现配现用;此外,较为单一的聚醚胺类固化剂,也可能使得产物的抗冲击韧性和耐温稳定性存在不足。
总体而言,现阶段针对厘米级以下特定裂缝封堵加固用途的灌注/压注型环氧胶粘产品及其配制、应用技术虽已日益成熟,但依旧面临着毒副性大、韧性不足、粘度过高、渗透性差、难以潮湿状态直接施工、低温反应慢等诸多缺陷。
发明内容
本发明目的在于提供一款针对毫米级以下特定裂缝防渗、加固用途的压注型环氧树脂结构胶,其有着存储稳定、低粘高渗、适合灌浆且可在低温及潮湿基面固化等特性。
为解决当前问题,本发明通过如下技术方案实现:
一种灌注/压注型环氧树脂结构胶,由A、B双组分构成,其质量比为2:1~3:1;按质量份数计,其中A组分含有双酚A型环氧树脂50~70份、双酚F型环氧树脂10~15份、稀释剂20~50份、偶联剂1~10份;B组分包含卞醇5~20份、基础胺10~30份、改性酚醛胺30~80份、固化促进剂3~10份。
优选的,所述双酚A型、双酚F型环氧树脂的环氧当量均为180~230g/mol。
发明人多次研究发现,在此当量范围内的环氧树脂室温下具有较低粘度和良好流动性。
优选的,所述双酚F型环氧树脂与双酚A型环氧树脂的质量比F/A为15~30%。
双酚F型与双酚A型按一定比例互配,有利于改善冬季或低温下的抗冻融稳定,预防结晶沉淀。若F型加量过低(<15%),则不足以破坏双酚A型环氧的纯度和分子规整性,无法有效抑制结晶,但F型加量过高(>30%),不仅增加成本,还会加速晶体析出,故F/A值优选15~30%为宜。
优选的,所述稀释剂为纯度高于98%、粘度低于40mPa.s的缩水甘油醚、缩水甘油酯、缩水甘油胺中的至少一类,其分子链中活性官能团数量为1~3个;优选拥有一定分子链长和柔韧性的聚丙二醇二缩水甘油醚与含刚性芳香基团的对叔丁苯基缩水甘油醚按一定比例的混合物。为使固化物刚柔相济,进一步优选聚丙二醇二缩水甘油醚与对叔丁苯基缩水甘油醚按(0.4~0.9):1质量比的混合物。
优选的,所述偶联剂为有机硅氧烷、硅酸酯、钛酸酯、铝酸酯、锆酸酯中的至少一类,优选有机硅氧烷类,进一步优选KH530或KH560中的至少一种。
优选的,所述基础胺为脂肪胺、脂环胺、芳香胺及其衍生物中的至少一种,优选脂环胺;为确保与混凝土基础有良好的亲和浸润性、适中的反应活性及强度,进一步优选色泽浅、粘度低、气味小、亲水性异佛二酮二胺(IPDA)。
优选的,所述改性酚醛胺粘度不高于1000mPa.s,热变形温度不低于60℃,固化温度可低至5℃;为确保B组分具备低粘度、冬季低温或高寒场景下的反应活性,以及固化物在夏季炎热条件下的尺寸稳定等综合属性,进一步优选多种不同粘度、耐热性及凝胶时间的改性酚醛胺的混合物。
优选的,所述改性酚醛胺为脂环胺改性的酚醛胺,其分子链中含有酚羟基、伯胺基和仲胺基。
通过反复对比,我们选用以脂环胺、酚/醛为主要原料经两步法缩聚后改性而成的酚醛胺作为主固化剂,优选常州山峰化工有限公司产PAA-3626(粘度880mPa.s、热变形温度60℃、凝胶时间15min)、SX-4823LA(粘度1000mPa.s、热变形温度85℃、凝胶时间17min),其二者按照质量比(2-3):(3-6)搭配,分子链软/硬段长度适中,且均含有酚羟基、伯胺基、仲胺基,可赋予产物优越硬度与较高韧性,并可在水下固化。为进一步降低B组分整体粘度,调控操作期,平衡反应发热,同时掺入高柔韧的腰果酚改性脂肪胺Y-5307(粘度100mPa.s、热变形温度65℃、凝胶时间50min)以及小分子卞醇、IPDA等。
优选的,所述固化促进剂选自分子链中含有-OH、-COOH、-SO3H、-CONH2-、-SO2NH2-、-SO3NHR等官能团的化合物;为改善常温或低温反应速率,进一步优选2,4,6-三(二甲基胺基甲基)苯酚(DMP-30)。
优选的,各固化剂、促进剂互配后,可使得B组分粘度调控在40mPa.s以下,且与混凝土有着良好亲和性,其活性基团能够与H2O结合,消耗基面水分,使之形成相对干燥界面,从而实现潮湿基面固化并较强粘接。
基于本发明第二个方面,提出了所述灌浆材料的制备方法,包括以下步骤:
按照重量份,将双酚A型环氧、双酚F型环氧、稀释剂、偶联剂搅拌混匀,得组分A;
再将卞醇、基础胺、改性酚醛胺、固化促进剂搅拌混匀,得组分B;
将组分A、B按2:1~3:1质量比混均后浇铸至预定模具内养护成型。
根据本发明第三个方面,提出了所述灌注/压注型环氧树脂结构胶在建筑工程领域的应用。
对于混凝土或岩层特定裂隙(缝宽0.01~10mm)修补加固用灌注(尤其是压注)型浆料而言,通常需有着极低粘度和高浸润性,以利于渗透扩散至砼基础施工缝、冷接缝、岩基缝,以及更为狭窄的由于应力、冷热收缩等原因导致的纤细裂纹(缝宽0.01~1mm)内部;同时由于裂隙带大多存在渗/漏水情况,所以最好还能够在潮湿状态甚至水下直接施工,且与原基础可靠粘接(干粘强度3~4MPa以上,湿粘强度2~3MPa以上)。
下面对本发明做进一步解释:
选取相近或相同环氧当量,但更小体积位阻的双酚F环氧对双酚A环氧掺杂,在降低粘度、增进相容的同时避免其低温结晶化,确保存储稳定;相对小分子量的聚丙二醇二缩水甘油醚、对叔丁苯基缩水甘油醚不仅对A组分进一步降粘,利用自身的长链柔性和苯基刚性,以及缩水甘油醚结构的可反应性,在与胺类固化剂聚合后成为三维交联网络的内在组成,使固化网络兼具强度、耐温、抗冲等各项属性;此外,环氧开环产生的大量羟基,加之偶联剂中甲氧基硅水解生成的硅羟基,与基础的羟基一同形成若干物理氢键,从而实现胶液固化物对混凝土裂隙边缘“手拉手式”桥接。
多种改性酚醛胺组合,有效规避了各自缺陷(如SX-4823LA硬度高、耐温好、反应快,但粘度较大、韧性稍低;Y-5307则粘度低、韧性优越、反应偏慢),赋予了“1+1>2”的增益能力。异佛二酮二胺、卞醇对改性酚醛胺进一步稀释后,可使B组分粘度降至40mPa.s以下;改性酚醛胺平缓的凝胶速率降低了高活性异佛二酮二胺、卞醇的反应放热,避免其“爆聚”,而异佛二酮二胺、卞醇良好的与水混溶性,反向促进了改性酚醛胺及环氧体系对亲水基础的浸润和深度渗透,推动改性酚醛胺与基面水分结合,以形成相对干燥界面,使得潮湿状态甚至水下直接施工成为可能。
总之,通过对本发明各原料的精心筛选和科学复配,以组分间的协同、配合,实现了低粘、高渗、强粘接等综合性能的较好平衡。
与现有技术相比,本发明有益效果在于:
一、体系中不含糠醛、甲醛、丙酮、乙酰丙酮等有毒、低闪点组分,生产及作业过程零VOC释放,对环境友好,适合封闭空间作业,无需特意排风通气。
二、所用原料价格适中,组配合理,多因素协同增益使得结构胶具备较佳的综合性能。
a.通过双酚A型与双酚F型互掺,有效降低了环氧树脂的低温结晶倾向,A组分在高寒地区仍可呈均一澄清状态。“不同类型的环氧树脂混用,可抑制其结晶”虽已成为行业公知,但对其混合比、整体粘度、成核微晶种类及数量等参数有着较高考量。F/A比值过高或过低均难以规避其结晶化,且双酚F型环氧价格偏贵,用量过大将直接拉高其物料成本;再者,一味追求降低粘度反而会加快结晶速度;其次,某些沉淀性填充料(尤其是超细粉末)很可能成为晶体生长增殖的成核剂,需尽量避免引入。本发明公开的方案中,F/A比值严格控制在(10~15)/(50~70)之间,并通过稀释剂、偶联剂的调配,使得A组分粘度在600~800mPa.s,且无任何增粘、成核类粉体,环氧体系具备良好的存储稳定和高性价比。
b.对叔丁苯基缩水甘油醚、异佛二酮二胺、卞醇等分子中的苯基、环己基闭环结构,相对于丁基缩水甘油醚、脂肪族多烯多胺、低分子量聚醚胺,有着更好的耐温性、力学强度和模量,利用其中的活性基团与环氧结构开环聚合后,成为大分子交联网络主链中的一部分,可使固化物拥有较高耐温特性,50℃不软化。
c.长链聚丙二醇二缩水甘油醚在稀释降粘的同时,也可凭借其单键长链的高旋转自由度为固化物提供良好韧性,确保其在冷热冲击和机械冲击下的力学强度;最为特别的是,通过优选组合市面已商业化的数种不同物性酚醛胺,使得凝胶化过程中,减缓因异佛二酮二胺、卞醇等活性小分子高放热引发的反应加速,避免夏季施工时可能出现的“爆聚”问题,其自身的低温、水下固化特性,也实现了B组分在5~40℃宽温区范围内,干燥或潮湿基面乃至水下直接施工的可能性。
三、本发明提供的环氧树脂结构胶色泽浅、粘接强度高,施工配料简便,相对于三组分体系(如CN103554843B、CN102898075、CN108047657B)混合粘度更低,可涂刷或灌封作业,也可加压浇注,渗透性好,可扩散至0.2mm以下缝宽的微细裂纹内;应用前景广阔,包括但不限于混凝土或岩层裂缝修补、格构式或封闭式湿法外包钢结构加固补强等。
附图说明
图1为本发明实施例1与对比例5树脂浇铸体色泽差异;其中,实施例1(L组)呈正常浅黄色,后期配色/着色性佳,对比例5(R组)因糠醛氧化,呈红棕色。
图2为本发明实施例1与对比例5之对应A组分在5℃下抗冻融稳定性差异;其中,实施例1之A组分(L)澄清透明,对比例5之A组分(R)因环氧树脂低温结晶析出,呈浑浊状。
具体实施方式
以下将结合实施例对本发明构思及产生的技术效果进行清楚、完整地描述,以便充分理解本发明目的、特征和效果。显然,所描述的实施例只是本发明的一部分而非全部,基于下述实施例,同领域技术人员在不付出创造性劳动的前提下所获得的其他实施例,均属于本发明保护范围。
低粘度环氧树脂结构胶性能测试参考《混凝土裂缝用环氧灌浆料(JC/T1041-2007)》《混凝土结构加固设计规范(GB50367-2006)》《工程结构加固材料安全性鉴定技术规范(GB50728-2011)》《树脂浇铸体性能试验方法(GB/T2567-2008)》等标准执行,胶液配制、试样成型与养护温度23±2℃、相对湿度50±5%。改性酚醛胺PAA-3626、Y-5307、SX-4823LA由常州山峰化工有限公司提供,其余原料均通过正常途径采购。
各实施例之低粘度环氧树脂结构胶制备工艺如下:
①将50~70份双酚A型环氧、10~15份双酚F型环氧、20~50份环保稀释剂、1~10份偶联剂以1000r/min高速搅拌3~5min混至均一,得组分A;
②将5~20份卞醇、10~30份基础胺、30~80份改性酚醛胺、3~10份固化促进剂以1000r/min高速搅拌3~5min混至均一,得组分B;
③将组分A、B按2:1~3:1质量比以500r/min高速搅拌3~5min充分混均后浇铸至预定模具内成型,养护14d后检测其性能。
各实施例及对比例原料组配(重量份)如下表1所示。
各实施例及对比例之树脂浇铸体性能参数如下表2所示。
从附图1、2及表2不难看出:对比例1、3、4、5及各实施例均有着较低粘度,可灌入不低于0.1mm宽度的极细裂纹,对比例2由于未添加Y-5307、卞醇等予以稀释,整体粘度偏高,注胶缝宽需在1mm以上,而且影响了压缩强度和抗冻融冲击强度。实施例以不同类型环氧树脂掺杂,破坏了分子链的规整性和纯度,可有效弱化其低温结晶趋势,避免高寒环境下析出导致A组分原料配比失衡。PAA-3626、Y-5307、SX-4823LA改性酚醛胺组合,使得体系最低固化温度下降5℃,并可在干湿基面乃至水下施工,且对混凝土、钢材粘接良好。由于对叔丁苯基缩水甘油醚、卞醇、异佛二酮二胺、KH530等均内含苯基或环己基封闭六元环结构,各实施例固化物有着更高刚度和耐热性(50℃不发软),物理强度和模量较对比例4、5提升35~40%;长链聚丙二醇二缩水甘油醚、Y-5307等组合确保了良好的抗冲击韧性,-25~+35℃下历时400h冷热循环后钢-钢拉剪强度仍高于96%。
值得注意的是,对比例1仅采用单一的改性酚醛胺(Y-5307)与其他固化剂互配,虽体系粘度较低,但不再具备低温(5℃)反应活性,各项强度及热稳定性均低于实施例1;而以相对更为粘稠的PAA-3626、SX-4823LA取代Y-5307后(对比例2),粘度上升明显,渗透性减弱,虽大部分指标优于对比例1,但因SX-4823LA显硬脆且掺量过高,抗冻融韧性不及实施例2及对比例1。据此可以清晰反映出,三种不同物性酚醛胺应在适度范围内与其他固化剂合理组配,方可获得最佳效果。此外,若以脂肪族稀释剂(丁基缩水甘油醚)替代长链聚丙二醇二缩水甘油醚以及刚性对叔丁苯基缩水甘油醚,对比例3固化物各项强度、粘接性能,尤其是抗冷热冲击韧性皆弱于实施例1。
对比例4、5中均以醛-酮为稀释溶剂,降粘能力稍明显,但低闪点的丙酮在聚合阶段挥发造成失重达2.7%、3.8%,势必加剧结构胶的尺寸收缩;而糠醛的易氧化性,使其呈红棕乃至深黑色,降低了后期的配色/着色性,同时也潜在毒害污染。固化剂体系以三乙烯四胺、593完全代替PAA-3626、SX-4823LA等改性酚醛胺后,韧性、耐温性、强度及模量等各项指标皆存在不同程度下降,且难以适应潮湿基面与低温施工。
实验中我们还发现,若将环氧树脂F/A比值降至约0.13(对比例4),10℃时将出现类似对比例5之A组分的结晶析出(附图2);而当F/A提升至0.6时,对A组分降粘显著,但低温下仍存在轻微结晶,且物料成本将拉高10~20%。
Claims (11)
1.一种灌注/压注型环氧树脂结构胶,其特征在于,由A、B组分构成,A、B组分质量比为2:1~3:1;按质量份数计, A组分含有双酚A型环氧树脂50~70份、双酚F型环氧树脂10~15份、稀释剂20~50份、偶联剂1~10份;B组分包含卞醇5~20份、基础胺10~30份、改性酚醛胺30~80份、固化促进剂3~10份;所述改性酚醛胺粘度不高于1000mPa.s,热变形温度不低于60℃,固化温度低至5℃;所述改性酚醛胺为PAA-3626、SX-4823LA、Y-5307三种组合,PAA-3626、SX-4823LA按照质量比(2-3):(3-6)搭配;
所述稀释剂为聚丙二醇二缩水甘油醚与对叔丁苯基缩水甘油醚的混合物。
2.根据权利要求1所述的灌注/压注型环氧树脂结构胶,其特征在于,所述双酚A型、双酚F型环氧树脂的环氧当量均为180~230g/mol。
3.根据权利要求1所述的灌注/压注型环氧树脂结构胶,其特征在于,所述稀释剂为纯度高于98%、粘度低于40mPa.s的缩水甘油醚。
4.根据权利要求1所述的灌注/压注型环氧树脂结构胶,其特征在于,所述偶联剂为有机硅氧烷、硅酸酯、钛酸酯、铝酸酯、锆酸酯中的至少一种。
5.根据权利要求4所述的灌注/压注型环氧树脂结构胶,其特征在于,所述偶联剂为有机硅氧烷类。
6.根据权利要求1所述的灌注/压注型环氧树脂结构胶,其特征在于,所述基础胺为脂肪胺、脂环胺、芳香胺及其衍生物中的至少一种。
7.根据权利要求6所述的灌注/压注型环氧树脂结构胶,其特征在于,所述基础胺为脂环胺。
8.根据权利要求6所述的灌注/压注型环氧树脂结构胶,其特征在于,所述基础胺为异佛二酮二胺。
9.根据权利要求1所述的灌注/压注型环氧树脂结构胶,其特征在于,所述固化促进剂选自分子链中含有-OH、-COOH、-SO3H的化合物。
10.根据权利要求9所述的灌注/压注型环氧树脂结构胶,其特征在于,所述固化促进剂为2,4,6-三(二甲基胺基甲基)苯酚。
11.根据权利要求1-10任一项所述的灌注/压注型环氧树脂结构胶在建筑工程领域的应用。
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