WO2023040076A1 - 一种建筑用丙烯酸酯密封胶及其制备方法 - Google Patents

一种建筑用丙烯酸酯密封胶及其制备方法 Download PDF

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WO2023040076A1
WO2023040076A1 PCT/CN2021/136044 CN2021136044W WO2023040076A1 WO 2023040076 A1 WO2023040076 A1 WO 2023040076A1 CN 2021136044 W CN2021136044 W CN 2021136044W WO 2023040076 A1 WO2023040076 A1 WO 2023040076A1
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hollow ceramic
parts
sealant
emulsion
construction
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PCT/CN2021/136044
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English (en)
French (fr)
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王�忠
樊民
毕建华
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海南红杉科创实业有限公司
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    • 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
    • C09J201/00—Adhesives based on unspecified macromolecular compounds
    • 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
    • C09J11/04—Non-macromolecular additives inorganic
    • 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

Definitions

  • the invention relates to the technical field of sealant, in particular to an acrylic sealant for construction and a preparation method thereof.
  • Water-based acrylate sealant has the characteristics of environmental protection, good weather resistance, good elasticity, and low price. At the same time, because the structure of acrylate has high polarity and high saturation, it has excellent resistance to mineral oil and high temperature oxidation resistance. . Based on the above advantages, acrylate materials have become one of the four major sealants for building structures. Compared with traditional silicone and polysulfide sealants, acrylate materials are more in line with the relevant policies of my country to vigorously promote green building materials.
  • the force between the monomers of the acrylate sealing material before curing is van der Waals force.
  • the curing process of the acrylate sealing material is accompanied by the process of dehydration and crosslinking. After curing, the force between the monomers becomes a covalent bond force.
  • the bodies are connected in the form of covalent bonds, forming a stable three-dimensional network structure, the distance between molecules changes from 0.3 to 0.4nm to about 0.15nm, and the distance between monomers in the resin decreases, which leads to a macroscopic polymerization time. The volume shrinks.
  • the problem of high shrinkage of acrylate sealant is serious, and its adverse consequences include: (1) When applied to the exterior wall of a prefabricated building, a weak layer of sealant will be formed on the edge of the wall panel, making it a weak point of force , it is easy to form cracks during displacement, causing water leakage problems; (2) When the acrylic sealant is applied to the built-in lightweight partition wall, the shrinkage of the sealant will cause depressions at the joints of the wall, which will increase when the wall paint is applied. The unevenness of the wall surface will affect the beauty of the building. Therefore, solving the problem of high shrinkage of acrylate sealant is the only way to promote its large-scale application.
  • the technical problem to be solved by the present invention is to provide an acrylic sealant for construction and a preparation method thereof.
  • the acrylic sealant for construction provided by the present invention has better shrinkage resistance.
  • the invention provides an acrylic sealant for construction, which is prepared from raw materials comprising the following components in parts by weight:
  • the modified hollow ceramic microspheres are obtained by modifying the hollow ceramic microspheres with a modifier
  • the modifiers include maleic anhydride and stearic acid.
  • the modified hollow ceramic microspheres are prepared from raw materials including the following components by weight:
  • the modified hollow ceramic microspheres are prepared according to the following method:
  • the mixing temperature is 70-80°C, and the mixing time is 10-20 minutes;
  • step b) after the reaction, further include: washing, filtering and drying.
  • the acrylic emulsion includes at least one of pure acrylic emulsion, styrene-acrylic emulsion, silicon-acrylic emulsion, fluorocarbon emulsion, elastic emulsion and vinegar-acrylic emulsion.
  • the particle size of the hollow ceramic microspheres is 20-250 ⁇ m.
  • the coupling agent includes at least one of vinyltriethoxysilane, vinyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane and benzyltriethoxysilane;
  • the film-forming aids include at least one of alcohol ester dodecane, benzyl alcohol and propylene glycol;
  • the thixotropic agent includes at least one of fumed silica, precipitated silica, organic bentonite and kaolin.
  • the other additives include at least one of dispersants, preservatives and defoamers.
  • the dispersant includes at least one of dispersant 5027, dispersant SN-5040 and dispersant KYC9611;
  • the preservative includes isothiazolinone LXE;
  • the defoamer included 750 mineral oil.
  • the present invention also provides a kind of preparation method of acrylic sealant for construction, comprising the following steps:
  • the invention provides an acrylic sealant for construction, which is prepared from raw materials comprising the following components in parts by weight: 85-95 parts of acrylic emulsion; 1-10 parts of modified hollow ceramic microspheres; 0-5 parts of coupling agent ; 0.2 to 5 parts of film-forming aids; 0.1 to 5 parts of thixotropic agents; 0.1 to 5 parts of other additives; the modified hollow ceramic microspheres are obtained by modifying hollow ceramic microspheres with modifiers; Modifiers include maleic anhydride and stearic acid.
  • hollow ceramic microspheres modified by specific components are added to the acrylate sealant for construction.
  • the modification of the surface allows specific organic groups to be grafted on the surface of the hollow ceramic microspheres, so that the hollow ceramic microspheres and acrylate A bridge is formed between the sealing materials, thereby effectively improving the compatibility between the hollow ceramic microspheres and the acrylate sealant, thereby reducing the loss of mechanical properties such as elasticity caused by the addition of fillers.
  • the modified hollow ceramic microspheres cooperate with other components to further improve the shrinkage resistance of the acrylate sealant for construction.
  • the invention provides an acrylic sealant for construction, which is prepared from raw materials comprising the following components in parts by weight:
  • the modified hollow ceramic microspheres are obtained by modifying the hollow ceramic microspheres with a modifier
  • the modifiers include maleic anhydride and stearic acid.
  • the raw materials for preparing the acrylate sealant for construction provided by the invention include acrylic emulsion.
  • the parts by weight of the acrylic emulsion are 85-95 parts. In some embodiments of the present invention, the parts by weight of the acrylic emulsion are 93 parts, 91.8 parts, 90.6 parts, 89.5 parts, 88.3 parts, 87.2 parts or 86.2 parts.
  • the acrylic emulsion includes at least one of pure acrylic emulsion, styrene-acrylic emulsion, silicon-acrylic emulsion, fluorocarbon emulsion, elastic emulsion and vinegar-acrylic emulsion.
  • the acrylic emulsion includes styrene-acrylic emulsion and elastic emulsion.
  • the mass ratio of the styrene-acrylic emulsion to the elastic emulsion is 2:8.
  • the raw materials for the preparation of the acrylate sealant for construction provided by the invention also include modified hollow ceramic microspheres.
  • the parts by weight of the modified hollow ceramic microspheres are 1-10 parts. In some embodiments of the present invention, the weight parts of the modified hollow ceramic microspheres are 1.3 parts, 2.5 parts, 3.8 parts, 5 parts, 3.7 parts or 3.6 parts.
  • the modified hollow ceramic microspheres are obtained by modifying the hollow ceramic microspheres with a modifier; the modifier includes maleic anhydride and stearic acid.
  • the modified hollow ceramic microspheres are prepared from raw materials comprising the following components in parts by weight:
  • the particle size of the hollow ceramic microspheres is 45-150 ⁇ m.
  • the present invention has no special limitation on the source of the hollow ceramic microspheres, which may be generally commercially available hollow ceramic microspheres.
  • the parts by weight of the hollow ceramic microspheres are 45 parts.
  • the weight part of the absolute ethanol is 50 parts.
  • the number of parts by weight of the stearic acid is 3 parts.
  • the parts by weight of the maleic anhydride are 2 parts.
  • the modified hollow ceramic microspheres are prepared according to the following method:
  • the mixing temperature is 70-80° C., and the mixing time is 10-20 minutes. In some embodiments, the temperature of the mixing is 75° C., and the mixing time is 10 minutes.
  • the temperature of the reaction is 75°C.
  • the reaction time is 1.5-2.5 hours. In some embodiments, the reaction time is 2 hours.
  • washing, filtering and drying are also included.
  • the present invention has no special limitation on the washing, filtering and drying methods, and the washing, filtering and drying methods known to those skilled in the art can be used.
  • the raw materials for the preparation of the acrylate sealant for construction provided by the invention also include a coupling agent.
  • the parts by weight of the coupling agent are 0-5 parts. In some embodiments of the present invention, the parts by weight of the coupling agent are 0 parts, 1.3 parts, 2.5 parts or 3.7 parts.
  • the coupling agent includes vinyltriethoxysilane, vinyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane (KH-550) and benzyl at least one of triethoxysilanes.
  • the raw materials for the preparation of the acrylate sealant for construction provided by the invention also include film-forming aids.
  • the weight part of the film-forming aid is 0.2-5 parts. In some embodiments of the present invention, the weight part of the film-forming aid is 2.7 parts, 2.6 parts or 2.5 parts.
  • the coalescence aid includes at least one of alcohol ester dodecane, benzyl alcohol and propylene glycol.
  • the raw materials for the preparation of the acrylate sealant for construction provided by the invention also include a thixotropic agent.
  • the parts by weight of the thixotropic agent are 0.1-5 parts. In some embodiments of the present invention, the weight part of the thixotropic agent is 1.9 parts, 1.8 parts or 1.7 parts.
  • the thixotropic agent includes at least one of fumed silica, precipitated silica, organobentonite and kaolin.
  • the raw materials for the preparation of the acrylate sealant for construction provided by the invention also include other additives.
  • the parts by weight of the other additives are 0.1-5 parts. In some embodiments, the parts by weight of the other additives are 2.4 parts, 2.3 parts or 2.2 parts.
  • the other additives include at least one of dispersants, preservatives and defoamers.
  • the dispersant includes at least one of dispersant 5027, dispersant SN-5040 and dispersant KYC9611.
  • the weight part of the dispersant is 1.1 parts or 1.0 parts.
  • the preservative includes isothiazolinone LXE. In some embodiments of the present invention, the weight part of the preservative is 0.5 parts.
  • the defoamer includes 750 mineral oil. In some embodiments of the present invention, the weight part of the defoamer is 0.8 part or 0.7 part.
  • the mass ratio of the dispersant, preservative and defoamer is 3-5:1-3:2-4. In some embodiments, the mass ratio of the dispersant, preservative and defoamer is 4:2:3.
  • the present invention also provides a kind of preparation method of acrylic sealant for construction as described above, comprising the following steps:
  • the acrylic emulsion and the dispersant are stirred and mixed to obtain the first emulsion.
  • the rotation speed of the stirring and mixing is 500-600 r/min, and the time is 4-6 minutes. In some embodiments, the rotational speed of the stirring and mixing is 550 r/min. In some embodiments, the stirring and mixing time is 5 minutes.
  • the first emulsion After the first emulsion is obtained, the first emulsion, the coalescent and the preservative are stirred and mixed to obtain the second emulsion.
  • the first emulsion, the coalescent, the coupling agent and the preservative are stirred and mixed to obtain the second emulsion.
  • the rotation speed of the stirring and mixing is 500-600 r/min, and the time is 4-6 minutes. In some embodiments, the rotational speed of the stirring and mixing is 550 r/min. In some embodiments, the stirring and mixing time is 5 minutes.
  • the modified hollow ceramic microspheres are stirred and mixed with the second emulsion, and then mixed with an antifoaming agent to obtain a mixed material liquid.
  • the rotational speed of the stirring and mixing is 1300-1500 r/min, and the time is 10-20 min. In some embodiments, the rotational speed of the stirring and mixing is 1400 r/min. In some embodiments, the stirring and mixing time is 10 minutes.
  • the organic groups on the modified hollow ceramic microspheres fully contact with the acrylate emulsion and form a certain chemical connection.
  • a defoamer is added to eliminate air bubbles in the mixed material liquid.
  • the thixotropic agent is added to the mixed material liquid in stages, and stirred to obtain the acrylate sealant for construction.
  • the thixotropic agent is added into the mixed material liquid in three stages, and the interval between each stage is 4-6 minutes. In some embodiments, each interval is 4 minutes.
  • the thixotropic agent is added into the mixed feed solution in stages while being stirred while adding.
  • the stirring speed is 1300-1500 r/min, and the stirring time is 8-15 minutes. In some embodiments, the stirring speed is 1400r/min. In some embodiments, the stirring time is 10 minutes.
  • the present invention has no special limitation on the sources of raw materials used above, and may be generally commercially available.
  • the particle size of the hollow ceramic microsphere is 45-150 ⁇ m.
  • Modified hollow ceramic microspheres are prepared according to the following steps:
  • Acrylic sealant for construction is prepared according to the following steps:
  • the coupling agent is ⁇ -aminopropyltriethoxysilane (KH550);
  • the dispersant is SN-5040;
  • the preservative is isothiazolinone LXE;
  • the thixotropic agent is fumed silica
  • the film-forming aid is alcohol ester twelve;
  • the defoamer is 750 mineral oil.
  • the test method for the linear shrinkage of the material is: in a rectangular frame mold with a length ⁇ width ⁇ height of 100mm ⁇ 10mm ⁇ 1mm, apply a release agent (non-reactive silicone oil), and apply the above-mentioned prepared acrylate sealant for construction Squeeze them into the mold and scrape them flat, cure them for 7 days under standard curing conditions (temperature (23 ⁇ 2)°C, humidity 50% ⁇ 5%), take out the sealant and measure the length, and calculate the shrinkage according to formula (1).
  • a release agent non-reactive silicone oil
  • the length unit after curing is mm.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Sealing Material Composition (AREA)

Abstract

本发明涉及密封胶技术领域，尤其涉及一种建筑用丙烯酸酯密封胶及其制备方法。建筑用丙烯酸酯密封胶的制备原料包括：丙烯酸乳液85～95份；改性中空陶瓷微球1～10份；偶联剂0～5份；成膜助剂0.2～5份；触变剂0.1～5份；其他助剂0.1～5份；所述改性中空陶瓷微球由改性剂对中空陶瓷微球进行改性得到；所述改性剂包括马来酸酐和硬脂酸。本发明在建筑用丙烯酸酯密封胶中添加了特定组分改性的中空陶瓷微球，有效改善了中空陶瓷微球与丙烯酸酯密封胶的相容性，进而减少因填料的加入而引起的弹性等力学性能的损失。同时，改性中空陶瓷微球配合其他组分协同作用，进一步提高了建筑用丙烯酸酯密封胶的抗收缩性能。

Description

一种建筑用丙烯酸酯密封胶及其制备方法 技术领域
本发明涉及密封胶技术领域，尤其涉及一种建筑用丙烯酸酯密封胶及其制备方法。
背景技术
水性丙烯酸酯密封胶具有绿色环保、耐候性好、弹性好、价格低等特点，同时，由于丙烯酸酯的结构具有高极性和高饱和性，使得其具有优越的耐矿物油和耐高温氧化性能。基于以上优势，丙烯酸酯材料成为建筑结构四大密封胶之一，相对于传统的硅酮、聚硫类密封胶来说，丙烯酸酯材料更加符合我国大力推广绿色建材的相关政策。
目前，建筑用丙烯酸酯密封胶的改性多集中在粘接性、耐久性、固化速度及耐沾污性等方面，未有论文和专利针对建筑用丙烯酸酯密封材料的抗收缩性进行专门的介绍和研究。
丙烯酸酯密封材料在固化之前单体间的作用力是范德华力，丙烯酸酯密封材料的固化过程伴随着失水、交联的过程，固化后单体间的作用力变为共价键力，单体间以共价键形式相连，形成了稳定的三维网状结构，分子间距离由0.3～0.4nm变为0.15nm左右，树脂中单体间的距离减小，从而在宏观上导致了聚合时体积产生收缩。
丙烯酸酯密封胶的高收缩性问题严重，其造成的不良后果包括：(1)应用于装配式建筑外墙时会在墙板的边缘部分形成密封胶的薄弱层，使其形成受力薄弱点，容易在位移时形成开裂，造成漏水问题；(2)当丙烯酸酯密封胶运用到内置轻质隔墙板时，密封胶收缩会造成墙面连接处的凹陷，涂刷墙面涂料时会增导致墙面的不平整，会影响到建筑物的美观。因此，解决丙烯酸酯密封胶高收缩率的问题是推广其大规模应用的必经之路。
发明内容
有鉴于此，本发明要解决的技术问题在于提供一种建筑用丙烯酸酯密封胶及其制备方法，本发明提供的建筑用丙烯酸酯密封胶抗收缩性能较优。
本发明提供了一种建筑用丙烯酸酯密封胶，由包括以下重量份组分的原料制备得到：
Figure PCTCN2021136044-appb-000001
所述改性中空陶瓷微球由改性剂对中空陶瓷微球进行改性得到；
所述改性剂包括马来酸酐和硬脂酸。
优选的，所述改性中空陶瓷微球由包括以下重量份组分的原料制备得到：
Figure PCTCN2021136044-appb-000002
优选的，所述改性中空陶瓷微球按照以下方法制备得到：
a)将中空陶瓷微球与无水乙醇混合，得到分散料液；
b)将所述分散料液、马来酸酐和硬脂酸混合，在70～80℃下进行反应，得到改性中空陶瓷微球。
优选的，步骤a)中，所述混合的温度为70～80℃，时间为10～20min；
步骤b)中，所述反应后，还包括：洗涤、过滤和干燥。
优选的，所述丙烯酸乳液包括纯丙乳液、苯丙乳液、硅丙乳液、氟碳乳液、弹性乳液和醋丙乳液中的至少一种。
优选的，所述中空陶瓷微球的粒径为20～250μm。
优选的，所述偶联剂包括乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷和苯甲基三乙氧基硅烷中的至少一种；
所述成膜助剂包括醇酯十二、苯甲醇和丙二醇中的至少一种；
所述触变剂包括气相二氧化硅、沉淀二氧化硅、有机膨润土和高岭土中的至少一种。
优选的，所述其他助剂包括分散剂、防腐剂和消泡剂中的至少一种。
优选的，所述分散剂包括分散剂5027、分散剂SN-5040和分散剂KYC9611中的至少一种；
所述防腐剂包括异噻唑啉酮LXE；
所述消泡剂包括750矿物油。
本发明还提供了一种建筑用丙烯酸酯密封胶的制备方法，包括以下步骤：
A)将丙烯酸乳液和分散剂搅拌混合，得到第一乳液；
B)将所述第一乳液、成膜助剂和防腐剂搅拌混合，得到第二乳液；
C)将改性中空陶瓷微球与所述第二乳液搅拌混合后，与消泡剂混合，得到混合料液；
D)将触变剂分段加入所述混合料液中，搅拌，得到建筑用丙烯酸酯密封胶。
本发明提供了一种建筑用丙烯酸酯密封胶，由包括以下重量份组分的原料制备得到：丙烯酸乳液85～95份；改性中空陶瓷微球1～10份；偶联剂0～5份；成膜助剂0.2～5份；触变剂0.1～5份；其他助剂0.1～5份；所述改性中空陶瓷微球由改性剂对中空陶瓷微球进行改性得到；所述改性剂包括马来酸酐和硬脂酸。本发明在建筑用丙烯酸酯密封胶中添加了特定组分改性的中空陶瓷微球，表面的改性使得中空陶瓷微球表面接枝上特定的有机基团，使得中空陶瓷微球与丙烯酸酯密封材料之间形成桥梁，从而有效改善了中空陶瓷微球与丙烯酸酯密封胶的相容性，进而减少因填料的加入而引起的弹性等力学性能的损失。同时，改性中空陶瓷微球配合其他组分协同作用，进一步提高了建筑用丙烯酸酯密封胶的抗收缩性能。
具体实施方式
下面将结合本发明实施例，对本发明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做出创造性劳动前提下所获 得的所有其他实施例，都属于本发明保护的范围。
本发明提供了一种建筑用丙烯酸酯密封胶，由包括以下重量份组分的原料制备得到：
Figure PCTCN2021136044-appb-000003
所述改性中空陶瓷微球由改性剂对中空陶瓷微球进行改性得到；
所述改性剂包括马来酸酐和硬脂酸。
本发明提供的建筑用丙烯酸酯密封胶的制备原料包括丙烯酸乳液。所述丙烯酸乳液的重量份数为85～95份。在本发明的某些实施例中，所述丙烯酸乳液的重量份数为93份、91.8份、90.6份、89.5份、88.3份、87.2份或86.2份。
在本发明的某些实施例中，所述丙烯酸乳液包括纯丙乳液、苯丙乳液、硅丙乳液、氟碳乳液、弹性乳液和醋丙乳液中的至少一种。
在本发明的某些实施例中，所述丙烯酸乳液包括苯丙乳液和弹性乳液。在本发明的某些实施例中，所述苯丙乳液和弹性乳液的质量比为2：8。
本发明提供的建筑用丙烯酸酯密封胶的制备原料还包括改性中空陶瓷微球。所述改性中空陶瓷微球的重量份数为1～10份。在本发明的某些实施例中，所述改性中空陶瓷微球的重量份数为1.3份、2.5份、3.8份、5份、3.7份或3.6份。
本发明中，所述改性中空陶瓷微球由改性剂对中空陶瓷微球进行改性得到；所述改性剂包括马来酸酐和硬脂酸。
在本发明的某些实施例中，所述改性中空陶瓷微球由包括以下重量份组分的原料制备得到：
Figure PCTCN2021136044-appb-000004
Figure PCTCN2021136044-appb-000005
在本发明的某些实施例中，所述中空陶瓷微球的粒径为45～150μm。本发明对所述中空陶瓷微球的来源并无特殊的限制，可以为一般市售的中空陶瓷微珠。
在本发明的某些实施例中，所述中空陶瓷微球的重量份数为45份。
在本发明的某些实施例中，所述无水乙醇的重量份数为50份。
在本发明的某些实施例中，所述硬脂酸的重量份数为3份。
在本发明的某些实施例中，所述马来酸酐的重量份数为2份。
在本发明的某些实施例中，所述改性中空陶瓷微球按照以下方法制备得到：
a)将中空陶瓷微球与无水乙醇混合，得到分散料液；
b)将所述分散料液、马来酸酐和硬脂酸混合，在70～80℃下进行反应，得到改性中空陶瓷微球。
所述改性中空陶瓷微球的制备方法中，采用的原料组分和配比同上，在此不再赘述。
步骤a)中：
在本发明的某些实施例中，所述混合的温度为70～80℃，时间为10～20min。在某些实施例中，所述混合的温度为75℃，时间为10min。
步骤b)中：
在本发明的某些实施例中，所述反应的温度为75℃。
在本发明的某些实施例中，所述反应的时间为1.5～2.5h。在某些实施例中，所述反应的时间为2h。
在本发明的某些实施例中，所述反应后，还包括：洗涤、过滤和干燥。
本发明对所述洗涤、过滤和干燥的方法并无特殊的限制，采用本领域技术人员熟知的洗涤、过滤和干燥的方法即可。
本发明提供的建筑用丙烯酸酯密封胶的制备原料还包括偶联剂。所述偶联剂的重量份数为0～5份。在本发明的某些实施例中，所述偶联剂的重量份数为0份、1.3份、2.5份或3.7份。
在本发明的某些实施例中，所述偶联剂包括乙烯基三乙氧基硅烷、乙烯基 三甲氧基硅烷、γ-氨丙基三乙氧基硅烷(KH-550)和苯甲基三乙氧基硅烷中的至少一种。
本发明提供的建筑用丙烯酸酯密封胶的制备原料还包括成膜助剂。所述成膜助剂的重量份数为0.2～5份。在本发明的某些实施例中，所述成膜助剂的重量份数为2.7份、2.6份或2.5份。
在本发明的某些实施例中，所述成膜助剂包括醇酯十二、苯甲醇和丙二醇中的至少一种。
本发明提供的建筑用丙烯酸酯密封胶的制备原料还包括触变剂。所述触变剂的重量份数为0.1～5份。在本发明的某些实施例中，所述触变剂的重量份数为1.9份、1.8份或1.7份。
在本发明的某些实施例中，所述触变剂包括气相二氧化硅、沉淀二氧化硅、有机膨润土和高岭土中的至少一种。
本发明提供的建筑用丙烯酸酯密封胶的制备原料还包括其他助剂。所述其他助剂的重量份数为0.1～5份。在某些实施例中，所述其他助剂的重量份数为2.4份、2.3份或2.2份。
在本发明的某些实施例中，所述其他助剂包括分散剂、防腐剂和消泡剂中的至少一种。
在本发明的某些实施例中，所述分散剂包括分散剂5027、分散剂SN-5040和分散剂KYC9611中的至少一种。
在本发明的某些实施例中，所述分散剂的重量份数为1.1份或1.0份。
在本发明的某些实施例中，所述防腐剂包括异噻唑啉酮LXE。在本发明的某些实施例中，所述防腐剂的重量份数为0.5份。
在本发明的某些实施例中，所述消泡剂包括750矿物油。在本发明的某些实施例中，所述消泡剂的重量份数为0.8份或0.7份。
在本发明的某些实施例中，所述分散剂、防腐剂和消泡剂的质量比为3～5：1～3：2～4。在某些实施例中，所述分散剂、防腐剂和消泡剂的质量比为4：2：3。
本发明还提供了一种上文所述的建筑用丙烯酸酯密封胶的制备方法，包括以下步骤：
A)将丙烯酸乳液和分散剂搅拌混合，得到第一乳液；
B)将所述第一乳液、成膜助剂和防腐剂搅拌混合，得到第二乳液；
C)将改性中空陶瓷微球与所述第二乳液搅拌混合后，与消泡剂混合，得到混合料液；
D)将触变剂分段加入所述混合料液中，搅拌，得到建筑用丙烯酸酯密封胶。
本发明提供的建筑用丙烯酸酯密封胶的制备方法中，采用的原料组分和配比同上，在此不再赘述。
本发明先将丙烯酸乳液和分散剂搅拌混合，得到第一乳液。
在本发明的某些实施例中，所述搅拌混合的转速为500～600r/min，时间为4～6min。在某些实施例中，所述搅拌混合的转速为550r/min。在某些实施例中，所述搅拌混合的时间为5min。
得到第一乳液后，将所述第一乳液、成膜助剂和防腐剂搅拌混合，得到第二乳液。
在本发明的某些实施例中，将所述第一乳液、成膜助剂、偶联剂和防腐剂搅拌混合，得到第二乳液。
在本发明的某些实施例中，所述搅拌混合的转速为500～600r/min，时间为4～6min。在某些实施例中，所述搅拌混合的转速为550r/min。在某些实施例中，所述搅拌混合的时间为5min。
得到第二乳液后，将改性中空陶瓷微球与所述第二乳液搅拌混合后，与消泡剂混合，得到混合料液。
在本发明的某些实施例中，所述搅拌混合的转速为1300～1500r/min，时间为10～20min。在某些实施例中，所述搅拌混合的转速为1400r/min。在某些实施例中，所述搅拌混合的时间为10min。
本发明中，改性中空陶瓷微球与所述第二乳液搅拌混合的过程中，改性中空陶瓷微球上的有机基团与丙烯酸酯乳液充分接触并产生一定的化学连接。
本发明中，加入消泡剂用于消除混合料液中的气泡。
得到混合料液后，将触变剂分段加入所述混合料液中，搅拌，得到建筑用丙烯酸酯密封胶。
在本发明的某些实施例中，触变剂分三段加入所述混合料液中，每段间隔的时间为4～6min。在某些实施例中，每段间隔的时间为4min。
在本发明的某些实施例中，将触变剂分段加入所述混合料液的过程中边加入边搅拌。
在本发明的某些实施例中，完成触变剂的分段加入后，搅拌的转速为1300～1500r/min，时间为8～15min。在某些实施例中，所述搅拌的转速为1400r/min。在某些实施例中，所述搅拌的时间为10min。
本发明对上文采用的原料来源并无特殊的限制，可以为一般市售。
为了进一步说明本发明，以下结合实施例对本发明提供的一种建筑用丙烯酸酯密封胶及其制备方法进行详细描述，但不能将其理解为对本发明保护范围的限定。
以下实施例中所用的原料均为市售。
实施例1～9和对比例1
中空陶瓷微球的粒径为45～150μm。
改性中空陶瓷微球按照以下步骤制备：
在可加热的反应釜中加入45重量份的中空陶瓷微珠，加入50重量份无水乙醇，在75℃下搅拌10min，得到分散料液；
在所述分散料液中加入2重量份的马来酸酐和3重量份的硬脂酸，继续在75℃下反应2h后，洗涤、过滤、干燥，即得改性中空陶瓷微球。
建筑用丙烯酸酯密封胶按照以下步骤制备：
1)在搅拌机中加入苯丙乳液和弹性乳液，再加入分散剂，550r/min下搅拌5min，得到第一乳液；
2)在所述第一乳液中加入成膜助剂、偶联剂和防腐剂，550r/min下搅拌5min，得到第二乳液；
3)将所述改性中空陶瓷微球加入所述第二乳液中，1400r/min下搅拌10min，加入消泡剂去除气泡，得到混合料液；
4)将触变剂分3段加入所述混合料液中，每段间隔的时间为4min，所述加入的过程中边加入边搅拌；触变剂添加完成后，1400r/min下搅拌10min，即可获得建筑用丙烯酸酯密封胶。
建筑用丙烯酸酯密封胶的制备原料中：
偶联剂为γ-氨丙基三乙氧基硅烷(KH550)；
分散剂为SN-5040；
防腐剂为异噻唑啉酮LXE；
触变剂为气相二氧化硅；
成膜助剂为醇酯十二；
消泡剂为750矿物油。
建筑用丙烯酸酯密封胶的制备原料组分及配比如表1所示。
表1实施例1～9和对比例1的建筑用丙烯酸酯密封胶的制备原料的重量份组分及配比
Figure PCTCN2021136044-appb-000006
对实施例1～9和对比例1制备的建筑用丙烯酸酯密封胶进行性能检测：
表干时间依据GB/T 13477《建筑密封材料试验方法》第五部分：表干时间的测定。断裂伸长率依据GB/T 13477.8—2003《建筑密封材料试验方法第8部分：拉伸粘结性的测定》中的方法进行测试。拉伸强度依据GB/T 528《硫化橡胶或热塑性橡胶拉伸应力应变性能的测定》进行测试。
材料的线收缩率测试方法为：在长×宽×高为100mm×10mm×1mm的长方框模具中，涂好脱模剂(非反应性硅油)，将上述制备的建筑用丙烯酸酯密封胶分别挤入模具中刮平，在标准固化条件下(温度(23±2)℃，湿度50％±5％)固化7d，取出密封胶测量长度，按公式(1)计算收缩率。
Figure PCTCN2021136044-appb-000007
公式(1)中，固化后的长度单位为mm。
检测结果如表2所示。
表2实施例1～9和对比例1的建筑用丙烯酸酯密封胶的性能检测结果
Figure PCTCN2021136044-appb-000008
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (10)

  1. 一种建筑用丙烯酸酯密封胶，由包括以下重量份组分的原料制备得到：
    Figure PCTCN2021136044-appb-100001
    所述改性中空陶瓷微球由改性剂对中空陶瓷微球进行改性得到；
    所述改性剂包括马来酸酐和硬脂酸。
  2. 根据权利要求1所述的建筑用丙烯酸酯密封胶，其特征在于，所述改性中空陶瓷微球由包括以下重量份组分的原料制备得到：
    Figure PCTCN2021136044-appb-100002
  3. 根据权利要求2所述的建筑用丙烯酸酯密封胶，其特征在于，所述改性中空陶瓷微球按照以下方法制备得到：
    a)将中空陶瓷微球与无水乙醇混合，得到分散料液；
    b)将所述分散料液、马来酸酐和硬脂酸混合，在70～80℃下进行反应，得到改性中空陶瓷微球。
  4. 根据权利要求3所述的建筑用丙烯酸酯密封胶，其特征在于，步骤a)中，所述混合的温度为70～80℃，时间为10～20min；
    步骤b)中，所述反应后，还包括：洗涤、过滤和干燥。
  5. 根据权利要求1所述的建筑用丙烯酸酯密封胶，其特征在于，所述丙烯酸乳液包括纯丙乳液、苯丙乳液、硅丙乳液、氟碳乳液、弹性乳液和醋丙乳液中的至少一种。
  6. 根据权利要求1所述的建筑用丙烯酸酯密封胶，其特征在于，所述中 空陶瓷微球的粒径为20～250μm。
  7. 根据权利要求1所述的建筑用丙烯酸酯密封胶，其特征在于，所述偶联剂包括乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、γ-氨丙基三乙氧基硅烷和苯甲基三乙氧基硅烷中的至少一种；
    所述成膜助剂包括醇酯十二、苯甲醇和丙二醇中的至少一种；
    所述触变剂包括气相二氧化硅、沉淀二氧化硅、有机膨润土和高岭土中的至少一种。
  8. 根据权利要求1所述的建筑用丙烯酸酯密封胶，其特征在于，所述其他助剂包括分散剂、防腐剂和消泡剂中的至少一种。
  9. 根据权利要求8所述的建筑用丙烯酸酯密封胶，其特征在于，所述分散剂包括分散剂5027、分散剂SN-5040和分散剂KYC9611中的至少一种；
    所述防腐剂包括异噻唑啉酮LXE；
    所述消泡剂包括750矿物油。
  10. 一种建筑用丙烯酸酯密封胶的制备方法，包括以下步骤：
    A)将丙烯酸乳液和分散剂搅拌混合，得到第一乳液；
    B)将所述第一乳液、成膜助剂和防腐剂搅拌混合，得到第二乳液；
    C)将改性中空陶瓷微球与所述第二乳液搅拌混合后，与消泡剂混合，得到混合料液；
    D)将触变剂分段加入所述混合料液中，搅拌，得到建筑用丙烯酸酯密封胶。
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