WO2023011303A1 - Polyamide wax composition, preparation method therefor, and application thereof - Google Patents

Polyamide wax composition, preparation method therefor, and application thereof Download PDF

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Publication number
WO2023011303A1
WO2023011303A1 PCT/CN2022/108508 CN2022108508W WO2023011303A1 WO 2023011303 A1 WO2023011303 A1 WO 2023011303A1 CN 2022108508 W CN2022108508 W CN 2022108508W WO 2023011303 A1 WO2023011303 A1 WO 2023011303A1
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polyamide wax
parts
wax composition
composition
waterproof coating
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PCT/CN2022/108508
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French (fr)
Chinese (zh)
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王仁杰
李忠人
贺小钢
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江苏凯伦建材股份有限公司
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Publication of WO2023011303A1 publication Critical patent/WO2023011303A1/en

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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
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/65—Additives macromolecular
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
    • C08J3/095—Oxygen containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
    • C08J3/096—Nitrogen containing compounds
    • 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
    • C09D175/04—Polyurethanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers

Definitions

  • the invention belongs to the field of building waterproofing, and in particular relates to a polyamide wax composition and a preparation method and application thereof.
  • polyamide wax is one of the more common thixotropic agents.
  • Polyamide wax is mainly composed of two parts, non-polar aliphatic hydrocarbon part and polar amide functional group.
  • the oxygen atom in the amide group has a large electronegativity, and it is easy to form a hydrogen bond with the hydrogen atom of the hydrocarbon group.
  • the hydrogen bond can be formed between molecules or within the molecule.
  • the intramolecular hydrogen bond makes the molecule curl up, and the whole molecule is basically non-polar to the outside world.
  • Polyamide wax is easy to form intramolecular hydrogen bonds under normal storage conditions. Therefore, before use, polyamide wax needs to be subjected to high-speed shearing and high-temperature activation treatment at about 120°C in a solvent to fully disperse the polyamide wax into a uniform dispersion.
  • the purpose of the present invention is to overcome the deficiencies in the prior art, to provide a new polyamide wax composition, the polyamide wax composition can be achieved by simply stirring at a low speed and/or at a lower activation temperature of the polyamide wax Activation treatment greatly improves construction convenience and saves construction cost.
  • the present invention also provides a preparation method of the polyamide wax composition.
  • the present invention also provides a method for activating polyamide wax dependent on the above polyamide wax composition.
  • the present invention also provides an application of the above-mentioned polyamide wax composition in polyurethane waterproof coatings.
  • a polyamide wax composition which comprises polyamide wax and a mixed solvent for dispersing the polyamide wax, the mixed solvent is composed of isopropanol and N-methylpyrrolidone.
  • the mass ratio of the isopropanol to the N-methylpyrrolidone is 1:0.5-2.5.
  • the mass ratio of the isopropanol to the N-methylpyrrolidone is 1:1.1-2.3.
  • polyamide wax accounts for 30-50%
  • isopropanol accounts for 20-30%
  • N-methylpyrrolidone accounts for 25-45%.
  • Another technical solution provided by the present invention a preparation method of the above-mentioned polyamide wax composition, the preparation method comprising: weighing polyamide wax, isopropanol and N-methylpyrrolidone according to the formula, mixing and dispersing, A polyamide wax composition is obtained.
  • a method for activating polyamide wax comprising: mixing the polyamide wax combination described above at a mixing temperature below 60°C and/or at a stirring speed below 200rpm Each component in the product, obtains the polyamide wax containing activation.
  • the mixing time can be shortened to 0.5-2h, and the activation of the polyamide wax can be realized.
  • the mixing temperature is 40-60° C.
  • the stirring speed is 100-200 rpm.
  • the polyamide wax composition of the present invention can make polyamide wax can realize activation under lower activation temperature and/or stirring speed, overcomes needing to adopt specific high-speed shearing equipment (shearing) in the prior art preferably The speed needs to reach 1500rpm or more) and the disadvantages of the activation temperature of about 120°C reduce the construction difficulty and construction cost.
  • an application of the above-mentioned polyamide wax composition in polyurethane waterproof coatings includes: before being added to polyurethane waterproof coatings, the polyamide wax composition is carried out as follows Operation: Mix and disperse at a mixing temperature below 60°C and/or at a stirring speed below 200rpm.
  • a single-component polyurethane waterproof coating characterized in that, in parts by mass, the raw materials of the single-component polyurethane waterproof coating include: 25-50 parts of polyurethane prepolymer, the above-mentioned 0.1-2 parts of the polyamide wax composition, 2-5 parts of reactive diluent, 0.1-0.3 parts of wetting and dispersing agent, 20-30 parts of heavy filler, 10-20 parts of nano-scale filler, 0.1-0. 0.3 parts, catalyst 0.05-0.2 parts, physical defoamer 0.1-0.3 parts, chemical defoamer 0.1-0.3 parts;
  • the preparation method of described one-component polyurethane waterproof coating comprises:
  • the polyamide wax composition containing activated polyamide wax obtained according to the above-mentioned activation method is mixed with the polyurethane prepolymer, and then the remaining raw materials are added, mixed, and defoamed to prepare a one-component polyurethane waterproof coating.
  • the polyurethane prepolymer is prepared by reacting polyol with polyisocyanate and then reacting with chain extender, and the NCO content is controlled at 2.5-5.0% (mass percentage). That is to say, the raw materials of the polyurethane prepolymer include: polyol, polyisocyanate and chain extender.
  • the polyols are at least two selected from polyether diols, polyester diols, and polyether triols, specifically, they can be selected from, for example, polyether diols Alcohol 2000, polyether glycol 1000, polyether 400, etc.
  • the polyisocyanate is selected from the group consisting of toluene diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), modified MDI,
  • TDI toluene diisocyanate
  • IPDI isophorone diisocyanate
  • MDI diphenylmethane diisocyanate
  • HMDI dicyclohexylmethane diisocyanate
  • HDI hexamethylene diisocyanate
  • LLI lysine diisocyanate
  • the chain extender is selected from clearlink 1000 4,4'bis-sec-butylaminodicyclohexylmethane, clearlink3000 3,3'-dimethyl 4,4'-bis-sec One or more combinations of butylaminodicyclohexylmethane, jefflink754, jefflink555, jefflink 7027, jeffamin HK-511.
  • the reactive diluent may be zoldine RD20 reactive diluent from Angus Company in the United States, Incozol LV reactive diluent from ICL Company in the United Kingdom, etc.
  • the wetting and dispersing agent can be at least one of titanate, silane, carboxylic acid and other dispersants, for example, it can be Hangzhou Linan Adjuvant f108.
  • the dehydrating agent is at least one of molecular sieves or isocyanate small-molecule water-removing agents, specifically micro-nano molecular sieves from Luoyang Jianlong, p-toluenesulfonyl isocyanate small-molecule water-removing agents from BASF, Germany, and group Calcium oxide of Xin heavy calcium, etc.
  • the heavy filler is at least one selected from titanium dioxide, heavy calcium, kaolin, talc and the like.
  • nano-scale fillers are selected from gypsum whiskers, fumed silica, nano-calcium carbonate, nano-aluminum nitride, nano-boron nitride, nano-aluminum borate, etc., and can be one, two or more Various.
  • the catalyst is selected from the group consisting of dibutyltin dilaurate, stannous octoate, environmentally friendly non-butyltin catalysts, bismuth carboxylate catalysts, zinc naphthenate, pentamethyldipropylenetriamine, tetramethyl At least one of ethylenediamine and bismorpholines.
  • a composite catalyst in which at least two are combined is preferred, and a combination of at least three is further preferred.
  • the physical defoamer can be a polysiloxane defoamer, a silicone defoamer, and the specific defoamer can be the defoamer of Deqian Chemical 5500, 066N of Byk Chemical, Chemical defoamer calcium oxide, magnesium oxide, calcium hydroxide, latent curing agent, etc.
  • the present invention has the following advantages compared with the prior art:
  • the present invention is based on the disadvantages of high-speed shearing and high-temperature activation treatment at about 120°C when polyamide wax is used as a thixotropic agent.
  • the conditions adopted for the activation of polyamide wax can be made simpler, only conventional stirring equipment and/or lower activation temperature ( It can be activated in the range of 40-60 °C, of course, the temperature is higher, but the corresponding energy consumption and equipment requirements will be increased), so that the polyamide wax can be added to the polyurethane waterproof coating
  • it When used as a thixotropic agent, it reduces the requirements for operating equipment, reduces energy consumption, saves costs, and is conducive to on-site construction and configuration of waterproof coatings; at the same time, it also endows polyurethane waterproof coatings with improved anti-sag performance without increasing viscosity.
  • the viscosity is moderate, and it can be applied at low temperature in winter and high temperature in summer.
  • polyamide wax compositions adopted in the following examples have all carried out the activation of polyamide wax: the N-methylpyrrolidone of 1.25kg isopropanol, 1.75kg is mixed with 2kg polyamide wax and stirred under 60 °C of water baths ( 200rpm) for 1h to obtain a polyamide wax composition containing activated polyamide wax.
  • 337kg of polyurethane prepolymer mixture prepared by the above method about 251kg of dehydrated filler processed by the above method, 20kg of zoldine RD20 reactive diluent from Angus Company of the United States, 2kg of BYK 066N defoamer, 1kg of Hubei Wuda Organic Silicon Company Silane coupling agent WD50, 0.5kg dibutyltin dilaurate from Beijing Akema, 0.3kg pentamethyldipropylene triamine from American Air Chemicals, 0.2kg zinc isooctanoate from American leading chemical company, 0.5kg from German BASF P-toluenesulfonyl isocyanate small molecule dehydrating agent, keep stirring, dispersing, grinding and defoaming at below 25°C by twin-screw mixer, vacuum degree of -0.09 ⁇ 0.1MPa, and test the fineness by scraper fineness meter to reach more than 50um, that is It can be discharged and filled.
  • Viscosity at low shear rate at 25°C is 17000mpa.s, solid content is 98.2%, surface dry time is 5 hours, hard drying time is 18 hours, 7-day tensile strength is 2.8MPa, elongation at break is 640%, tear strength is 17N/mm.
  • the situation after scrape coating is as follows: 1 mm thick coating at 25 °C does not flow, and the base surface temperature is 60 °C and 1 mm thick coating does not flow at one time.
  • Luoyang Jianlong micro-nano molecular sieve 1kg magnesium oxide chemical defoamer, 100kg Suzhou Lida superfine LD600, 190kg Hunan Jinjian B-type nano powder, and 10kg gypsum whiskers produced by China University of Mining and Technology through the kneader at 160 °C, -0.1MPA vacuum dehydration to a moisture content below 0.05%, and then stored in a buffer tank for later use.
  • the viscosity at 25°C is 16100mpa.s, the solid content is 98.7%, the surface dry time is 6 hours, the hard drying time is 19 hours, the 7-day tensile strength is 2.6MPa, the elongation at break is 660%, and the tear strength is 17.5N/mm.
  • the situation after scrape coating is as follows: 1.5mm thick coating at 25°C does not flow, and the base surface temperature is 60°C and 1mm thick coating does not flow at one time.
  • 347kg of polyurethane prepolymer mixture prepared by the above method about 410kg of dehydrated filler treated by the above method, 50kg of Incozol LV reactive diluent from British ICL company, 1kg of Deqian Chemical 5500 defoamer and 1kg of BYK 066N, 3kg f108 Hangzhou Lin'an auxiliary agent, 0.5kg American leading organic bismuth, 0.1kg American air chemical pentamethyldipropylenetriamine and 5kg Deshan PM20L, kept stirring, dispersing, grinding and removing by twin-screw mixer below 25°C Bubble, -0.09 ⁇ 0.1MPa vacuum degree, through the scraper fineness tester to test the fineness to more than 50um, the material can be discharged and filled.
  • the viscosity at 25°C is 35900mpa.s, the solid content is 98.9%, the surface dry time is 7 hours, the dry time is 20 hours, the tensile strength is 2.4MPa after 7 days, the elongation at break is 590%, and the tear strength is 16.7N/mm.
  • the situation after scrape coating is as follows: the base surface temperature is 25°C and a thick coating of 2mm does not flow, and the base surface temperature is 60°C and a thick coating of 1mm does not flow.
  • Comparative Example 1 is a comparative example that is directly added without pre-activation treatment on the basis of Example 1 (the polyamide wax is dispersed in the later mixing process):
  • the viscosity at 25°C is 28000mpa.s, the solid content is 98.2%, the surface dry time is 5 hours, the hard drying time is 18 hours, the 7-day tensile strength is 2.3MPa, the elongation at break is 580%, and the tear strength is 16N/mm.
  • the situation after scrape coating is as follows: 1 mm thick coating at 25 ° C does not flow, and the base surface temperature is 60 ° C 1 mm thick coating flows.
  • Comparative example 2 adjusts the comparative example of the solvent component of polyamide wax composition on the basis of embodiment 1:
  • the viscosity at 25°C is 33300mpa.s, the solid content is 98.1%, the surface dry time is 5 hours, the hard drying time is 17 hours, the 7-day tensile strength is 2.4MPa, the elongation at break is 592%, and the tear strength is 17N/mm.
  • the situation after scrape coating is as follows: 0.75mm thick coating once at 25°C does not flow, 1mm thick coating once at 25°C flows, base surface temperature 60°C 1mm thick coating flows.
  • Example 2 Basically the same as Example 1, the only difference is: 3kg of N-methylpyrrolidone and 2kg of polyamide wax were mixed and stirred (200rpm) in a water bath at 60°C for 1 hour to obtain a pretreated polyamide wax composition. Others are the same as embodiment 1.
  • the viscosity at 25°C is 23600mpa.s, the solid content is 98.2%, the surface dry time is 5 hours, the hard drying time is 17 hours, the 7-day tensile strength is 2.3MPa, the elongation at break is 623%, and the tear strength is 17N/mm.
  • the situation after scrape coating is as follows: 1 mm thick coating at 25 ° C does not flow, and the base surface temperature is 60 ° C 1 mm thick coating flows.
  • Example 2 Basically the same as Example 1, the only difference is that: 3 kg of isopropanol and 2 kg of polyamide wax were mixed and stirred (200 rpm) in a water bath at 60° C. for 1 hour to obtain a pretreated polyamide wax composition. Others are the same as embodiment 1.
  • the viscosity at 25°C is 21300mpa.s, the solid content is 98.1%, the surface dry time is 5 hours, the hard drying time is 17 hours, the 7-day tensile strength is 2.5MPa, the elongation at break is 598%, and the tear strength is 18N/mm.
  • the situation after scrape coating is as follows: 1 mm thick coating at 25 ° C does not flow, and the base surface temperature is 60 ° C 1 mm thick coating flows.

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Abstract

Discloses are a polyamide wax composition, a preparation method therefor, and an application thereof. The composition comprises polyamide wax and a mixed solvent for dispersing the polyamide wax, the mixed solvent consisting of isopropanol and n-methyl pyrrolidone. The polyamide wax composition containing the activated polyamide wax can be obtained by mixing at a mixing temperature of 60°C or less and/or a stirring speed of 200 rpm or less, can significantly reduce the construction difficulty and the construction cost during a preparation process of a waterproof polyurethane coating, endows the waterproof polyurethane coating with excellent anti-sagging properties, and can achieve excellent anti-sagging effects on a high-temperature base in time.

Description

一种聚酰胺蜡组合物及其制备方法和应用A kind of polyamide wax composition and its preparation method and application 技术领域technical field
本发明属于建筑防水领域，具体涉及一种聚酰胺蜡组合物及其制备方法和应用。The invention belongs to the field of building waterproofing, and in particular relates to a polyamide wax composition and a preparation method and application thereof.
背景技术Background technique
目前市面上的聚氨酯要具备抗流挂性能通常要加入触变剂，聚酰胺蜡是其中较为常见的触变剂。聚酰胺蜡主要由两部分构成，非极性的脂肪烃部分和极性的酰胺基官能团。酰胺基中的氧原子电负性大，易和烃基部分的氢原子形成氢键，氢键可在分子间或分子内形成，分子内氢键使分子呈卷曲状，整个分子基本对外界显非极性状态，难以建立起立体网状结构，进而无法实现触变作用；分子间氢键能在涂料体系里形成一个立体网状结构，这种结构的建立使涂料具备抗流挂性能。而聚酰胺蜡常规储存条件下易形成分子内氢键，因此，聚酰胺蜡在使用之前均需要在溶剂中进行高速剪切和120℃左右的高温活化处理，使聚酰胺蜡充分分散成分散均匀、呈拉直状态的分子个体，进而使其与聚氨酯体系更加相容，能够使多数胶体有效分散且产生流变活化的网络结构，从而提供优异的触变性能，实现黏度建立、流挂控制及颜填料悬浮控制。但是，高速剪切和较高温度的活化处理方式，对生产设备要求高，同时由于还需要在现场进行处理，极大地增加了施工难度与施工成本。Currently, thixotropic agents are usually added to polyurethanes on the market to have anti-sag properties, and polyamide wax is one of the more common thixotropic agents. Polyamide wax is mainly composed of two parts, non-polar aliphatic hydrocarbon part and polar amide functional group. The oxygen atom in the amide group has a large electronegativity, and it is easy to form a hydrogen bond with the hydrogen atom of the hydrocarbon group. The hydrogen bond can be formed between molecules or within the molecule. The intramolecular hydrogen bond makes the molecule curl up, and the whole molecule is basically non-polar to the outside world. It is difficult to establish a three-dimensional network structure, and thus unable to achieve thixotropy; intermolecular hydrogen bonds can form a three-dimensional network structure in the coating system, and the establishment of this structure makes the coating have anti-sagging properties. Polyamide wax is easy to form intramolecular hydrogen bonds under normal storage conditions. Therefore, before use, polyamide wax needs to be subjected to high-speed shearing and high-temperature activation treatment at about 120°C in a solvent to fully disperse the polyamide wax into a uniform dispersion. , molecular individuals in a straightened state, and thus make it more compatible with the polyurethane system, which can effectively disperse most colloids and generate a rheologically activated network structure, thereby providing excellent thixotropic properties, achieving viscosity establishment, sagging control and Pigment suspension control. However, the high-speed shearing and high-temperature activation treatment method requires high production equipment, and at the same time, it also needs to be processed on site, which greatly increases the construction difficulty and construction cost.
发明内容Contents of the invention
本发明的目的是克服现有技术的不足，提供一种新的聚酰胺蜡组合物，该聚酰胺蜡组合物能够通过简单地低速搅拌和/或在较低的活化温度下实现聚酰胺蜡的活化处理，极大地提升了施工便利性以及节约了施工成本。The purpose of the present invention is to overcome the deficiencies in the prior art, to provide a new polyamide wax composition, the polyamide wax composition can be achieved by simply stirring at a low speed and/or at a lower activation temperature of the polyamide wax Activation treatment greatly improves construction convenience and saves construction cost.
本发明同时还提供了一种上述聚酰胺蜡组合物的的制备方法。The present invention also provides a preparation method of the polyamide wax composition.
本发明同时还提供了一种依赖于上述聚酰胺蜡组合物的聚酰胺蜡的活化方法。The present invention also provides a method for activating polyamide wax dependent on the above polyamide wax composition.
本发明同时还提供了一种上述聚酰胺蜡组合物在聚氨酯防水涂料中的应用。The present invention also provides an application of the above-mentioned polyamide wax composition in polyurethane waterproof coatings.
为达到上述目的，本发明采用的一种技术方案是：In order to achieve the above object, a kind of technical scheme that the present invention adopts is:
一种聚酰胺蜡组合物，该组合物包含聚酰胺蜡以及用于分散聚酰胺蜡的混合溶剂，所述混合溶剂由异丙醇和N-甲基吡咯烷酮构成。A polyamide wax composition, which comprises polyamide wax and a mixed solvent for dispersing the polyamide wax, the mixed solvent is composed of isopropanol and N-methylpyrrolidone.
根据本发明的一些优选方面，所述异丙醇与所述N-甲基吡咯烷酮的投料质量比为1∶0.5-2.5。According to some preferred aspects of the present invention, the mass ratio of the isopropanol to the N-methylpyrrolidone is 1:0.5-2.5.
进一步地，所述异丙醇与所述N-甲基吡咯烷酮的投料质量比为1∶1.1-2.3。Further, the mass ratio of the isopropanol to the N-methylpyrrolidone is 1:1.1-2.3.
根据本发明的一些优选方面，该组合物中，以质量百分含量计，聚酰胺蜡占30-50％，异丙醇占20-30％，N-甲基吡咯烷酮占25-45％。According to some preferred aspects of the present invention, in the composition, by mass percentage, polyamide wax accounts for 30-50%, isopropanol accounts for 20-30%, and N-methylpyrrolidone accounts for 25-45%.
本发明提供的又一技术方案：一种上述所述的聚酰胺蜡组合物的制备方法，所述制备方法包括：按配方称取聚酰胺蜡、异丙醇和N-甲基吡咯烷酮，混合分散，获得聚酰胺蜡组合物。Another technical solution provided by the present invention: a preparation method of the above-mentioned polyamide wax composition, the preparation method comprising: weighing polyamide wax, isopropanol and N-methylpyrrolidone according to the formula, mixing and dispersing, A polyamide wax composition is obtained.
本发明提供的又一技术方案：一种聚酰胺蜡的活化方法，所述活化方法包括：在60℃以下的混合温度下和/或200rpm以下的搅拌速度下混合上述所述的聚酰胺蜡组合物中的各成分，获得含有活化的聚酰胺蜡。Another technical solution provided by the present invention: a method for activating polyamide wax, the activation method comprising: mixing the polyamide wax combination described above at a mixing temperature below 60°C and/or at a stirring speed below 200rpm Each component in the product, obtains the polyamide wax containing activation.
根据本发明，混合的时间可以缩短至0.5-2h，就可以实现聚酰胺蜡的活化。According to the present invention, the mixing time can be shortened to 0.5-2h, and the activation of the polyamide wax can be realized.
根据本发明的一些优选且具体的方面，混合温度为40-60℃，搅拌速度为100-200rpm。According to some preferred and specific aspects of the present invention, the mixing temperature is 40-60° C., and the stirring speed is 100-200 rpm.
本发明的聚酰胺蜡组合物可以使得聚酰胺蜡在较低的活化温度和/或搅拌速度下即可实现活化，较好地克服了现有技术中需要采用特定的高速剪切设备(剪切速度需达到1500rpm以上)以及120℃左右的活化温度的弊端，降低了施工难以以及施工成本。The polyamide wax composition of the present invention can make polyamide wax can realize activation under lower activation temperature and/or stirring speed, overcomes needing to adopt specific high-speed shearing equipment (shearing) in the prior art preferably The speed needs to reach 1500rpm or more) and the disadvantages of the activation temperature of about 120°C reduce the construction difficulty and construction cost.
本发明提供的又一技术方案：一种上述所述的聚酰胺蜡组合物在聚氨酯防水涂料中的应用，所述应用包括：在添加至聚氨酯防水涂料之前，对该聚酰胺蜡组合物进行如下操作：在60℃以下的混合温度下和/或200rpm以下的搅拌速度下混合分散。Another technical solution provided by the present invention: an application of the above-mentioned polyamide wax composition in polyurethane waterproof coatings, the application includes: before being added to polyurethane waterproof coatings, the polyamide wax composition is carried out as follows Operation: Mix and disperse at a mixing temperature below 60°C and/or at a stirring speed below 200rpm.
本发明提供的又一技术方案：一种单组分聚氨酯防水涂料，其特征在于，以质量份数计，所述单组分聚氨酯防水涂料的原料包括：聚氨酯预聚体25-50份、上述所述的聚酰胺蜡组合物0.1-2份、活性稀释剂2-5份、润湿分散剂0.1-0.3份，重质填料20-30份、纳米级填料10-20份、脱水剂0.1-0.3份、催化剂0.05-0.2份、物理消泡剂0.1-0.3份、化学消泡剂0.1-0.3份；Another technical solution provided by the present invention: a single-component polyurethane waterproof coating, characterized in that, in parts by mass, the raw materials of the single-component polyurethane waterproof coating include: 25-50 parts of polyurethane prepolymer, the above-mentioned 0.1-2 parts of the polyamide wax composition, 2-5 parts of reactive diluent, 0.1-0.3 parts of wetting and dispersing agent, 20-30 parts of heavy filler, 10-20 parts of nano-scale filler, 0.1-0. 0.3 parts, catalyst 0.05-0.2 parts, physical defoamer 0.1-0.3 parts, chemical defoamer 0.1-0.3 parts;
所述单组分聚氨酯防水涂料的制备方法包括：The preparation method of described one-component polyurethane waterproof coating comprises:
将根据上述所述的活化方法获得的含有活化的聚酰胺蜡的聚酰胺蜡组合物与聚氨酯预聚体混合，然后加入剩余原料，混合，脱泡，制成单组分聚氨酯防水涂料。The polyamide wax composition containing activated polyamide wax obtained according to the above-mentioned activation method is mixed with the polyurethane prepolymer, and then the remaining raw materials are added, mixed, and defoamed to prepare a one-component polyurethane waterproof coating.
根据本发明的一些具体方面，所述聚氨酯预聚体由多元醇与多异氰酸酯反应后再与扩链剂反应而制成，控制NCO含量为2.5-5.0％(质量百分含量)。也即该聚氨酯预聚体的原料包括：多元醇、多异氰酸酯和扩链剂。According to some specific aspects of the present invention, the polyurethane prepolymer is prepared by reacting polyol with polyisocyanate and then reacting with chain extender, and the NCO content is controlled at 2.5-5.0% (mass percentage). That is to say, the raw materials of the polyurethane prepolymer include: polyol, polyisocyanate and chain extender.
根据本发明的一些优选且具体的方面，所述多元醇为选自聚醚二元醇、聚酯二元醇、聚醚三元醇中的至少两种，具体可以选自例如聚醚二元醇2000、聚醚二元醇1000、聚醚400等等。根据本发明的一些优选且具体的方面，所述多异氰酸酯为选自括甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、二苯基甲烷二异氰酸酯(MDI)、改性MDI、二环己基甲烷二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)、赖氨酸二异氰酸酯(LDI)中的一种或多种的组合，具体例如可以选自巴斯夫MDI-MI、万华IPDI、巴斯夫改性MDI103C、巴斯夫MDI-50、巴斯夫TDI等等。According to some preferred and specific aspects of the present invention, the polyols are at least two selected from polyether diols, polyester diols, and polyether triols, specifically, they can be selected from, for example, polyether diols Alcohol 2000, polyether glycol 1000, polyether 400, etc. According to some preferred and specific aspects of the present invention, the polyisocyanate is selected from the group consisting of toluene diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), modified MDI, One or more combinations of dicyclohexylmethane diisocyanate (HMDI), hexamethylene diisocyanate (HDI), lysine diisocyanate (LDI), for example, can be selected from BASF MDI-MI, Wanhua IPDI, BASF modified MDI103C, BASF MDI-50, BASF TDI and so on.
根据本发明的一些优选且具体的方面，所述扩链剂为选自clearlink 1000 4,4’双仲丁氨基 二环己基甲烷，clearlink3000 3,3’-二甲基4,4’-双仲丁氨基二环己基甲烷，jefflink754，jefflink555，jefflink 7027，jeffamin HK-511中的一种或者多种的组合。According to some preferred and specific aspects of the present invention, the chain extender is selected from clearlink 1000 4,4'bis-sec-butylaminodicyclohexylmethane, clearlink3000 3,3'-dimethyl 4,4'-bis-sec One or more combinations of butylaminodicyclohexylmethane, jefflink754, jefflink555, jefflink 7027, jeffamin HK-511.
根据本发明的一些具体方面，所述活性稀释剂可以为美国angus公司的zoldine RD20活性稀释剂、英国ICL公司的Incozol LV活性稀释剂等。According to some specific aspects of the present invention, the reactive diluent may be zoldine RD20 reactive diluent from Angus Company in the United States, Incozol LV reactive diluent from ICL Company in the United Kingdom, etc.
根据本发明的一些具体方面，所述润湿分散剂可以为钛酸酯类，硅烷类，羧酸类等分散剂的至少一种，例如可以为杭州临安助剂f108。According to some specific aspects of the present invention, the wetting and dispersing agent can be at least one of titanate, silane, carboxylic acid and other dispersants, for example, it can be Hangzhou Linan Adjuvant f108.
根据本发明的一些具体方面，脱水剂为分子筛或者异氰酸酯小分子除水剂的至少一种，具体可以为洛阳建龙的微纳分子筛，德国巴斯夫的对甲苯磺酰异氰酸酯小分子除水剂，群鑫重钙的氧化钙等。According to some specific aspects of the present invention, the dehydrating agent is at least one of molecular sieves or isocyanate small-molecule water-removing agents, specifically micro-nano molecular sieves from Luoyang Jianlong, p-toluenesulfonyl isocyanate small-molecule water-removing agents from BASF, Germany, and group Calcium oxide of Xin heavy calcium, etc.
根据本发明的一些具体方面，重质填料选自钛白粉、重钙、高岭土、滑石粉等中的至少一种。According to some specific aspects of the present invention, the heavy filler is at least one selected from titanium dioxide, heavy calcium, kaolin, talc and the like.
根据本发明的一些具体方面，纳米级填料选自石膏晶须，气相二氧化硅，纳米碳酸钙，纳米氮化铝，纳米氮化硼，纳米硼酸铝等，可以为一种、两种或更多种。According to some specific aspects of the present invention, nano-scale fillers are selected from gypsum whiskers, fumed silica, nano-calcium carbonate, nano-aluminum nitride, nano-boron nitride, nano-aluminum borate, etc., and can be one, two or more Various.
根据本发明的一些具体方面，催化剂选自二月桂酸二丁基锡、辛酸亚锡、环保非丁基锡催化剂、羧酸铋类催化剂、环烷酸锌、五甲基二亚丙基三胺、四甲基乙二胺、双吗啉类中的至少一种。优选其中的至少两种组合的复合催化剂，进一步可以优选为至少三种的组合。According to some specific aspects of the present invention, the catalyst is selected from the group consisting of dibutyltin dilaurate, stannous octoate, environmentally friendly non-butyltin catalysts, bismuth carboxylate catalysts, zinc naphthenate, pentamethyldipropylenetriamine, tetramethyl At least one of ethylenediamine and bismorpholines. A composite catalyst in which at least two are combined is preferred, and a combination of at least three is further preferred.
根据本发明的一些具体方面，物理消泡剂可以为聚硅氧烷消泡剂，硅酮类消泡剂，具体消泡剂可以为德谦化学5500的消泡剂、毕克化学的066N，化学消泡剂氧化钙，氧化镁，氢氧化钙、潜固化剂等。According to some specific aspects of the present invention, the physical defoamer can be a polysiloxane defoamer, a silicone defoamer, and the specific defoamer can be the defoamer of Deqian Chemical 5500, 066N of Byk Chemical, Chemical defoamer calcium oxide, magnesium oxide, calcium hydroxide, latent curing agent, etc.
由于上述技术方案运用，本发明与现有技术相比具有下列优点：Due to the use of the above-mentioned technical solutions, the present invention has the following advantages compared with the prior art:
本发明基于聚酰胺蜡在作为触变剂应用时需要进行高速剪切和120℃左右的高温活化处理的弊端而作的相应改进，在长期的生产实践中，本发明发明人偶然发现，当采用异丙醇与N-甲基吡咯烷酮相组合作为混合溶剂分散聚酰胺蜡时，能够使得聚酰胺蜡的活化采用的条件变得更简单，仅仅采用常规的搅拌设备和/或较低的活化温度(可在40-60℃区间内，当然温度更高也可以，但是相应对能耗以及设备的要求就会增加)即可实现对聚酰胺蜡的活化，使得在向聚氨酯防水涂料中添加聚酰胺蜡作为触变剂时降低了对操作设备的要求，降低了能耗，节约了成本，有利于现场施工配置防水涂料；同时还赋予了聚氨酯防水涂料在不增加粘度的情况下提升抗流挂性能，具体可实现立面不流淌(一次涂刮1mm不流淌)、高温不流淌(基面60℃一次刮涂1mm不流淌)等特点，粘度适中，而且可在冬季低温、夏季高温下施工。The present invention is based on the disadvantages of high-speed shearing and high-temperature activation treatment at about 120°C when polyamide wax is used as a thixotropic agent. When isopropanol and N-methylpyrrolidone are combined as mixed solvents to disperse polyamide wax, the conditions adopted for the activation of polyamide wax can be made simpler, only conventional stirring equipment and/or lower activation temperature ( It can be activated in the range of 40-60 °C, of course, the temperature is higher, but the corresponding energy consumption and equipment requirements will be increased), so that the polyamide wax can be added to the polyurethane waterproof coating When used as a thixotropic agent, it reduces the requirements for operating equipment, reduces energy consumption, saves costs, and is conducive to on-site construction and configuration of waterproof coatings; at the same time, it also endows polyurethane waterproof coatings with improved anti-sag performance without increasing viscosity. Specifically, it can achieve the characteristics of no flow on the facade (one-time application of 1mm without flow), high-temperature non-flow (the base surface is 60°C and one-time application of 1mm without flow), etc., the viscosity is moderate, and it can be applied at low temperature in winter and high temperature in summer.
具体实施方式Detailed ways
以下结合具体实施例对上述方案做进一步说明；应理解，这些实施例是用于说明本发明 的基本原理、主要特征和优点，而本发明不受以下实施例的范围限制；实施例中采用的实施条件可以根据具体要求做进一步调整，未注明的实施条件通常为常规实验中的条件。Below in conjunction with specific embodiment above-mentioned scheme is described further; It should be understood that these embodiments are to illustrate basic principle, main feature and advantage of the present invention, and the present invention is not limited by the scope of following embodiment; Adopted in the embodiment The implementation conditions can be further adjusted according to specific requirements, and the unspecified implementation conditions are usually the conditions in routine experiments.
下述实施例中未作特殊说明，所有原料均来自于商购或通过本领域的常规方法制备而得。There are no special instructions in the following examples, and all raw materials are commercially available or prepared by conventional methods in the art.
下述实施例中采用的聚酰胺蜡组合物均已进行过聚酰胺蜡的活化：将1.25kg异丙醇、1.75kg的N-甲基吡咯烷酮与2kg聚酰胺蜡混合在60℃水浴下搅拌(200rpm)1h，即得到含有活化的聚酰胺蜡的聚酰胺蜡组合物。The polyamide wax compositions adopted in the following examples have all carried out the activation of polyamide wax: the N-methylpyrrolidone of 1.25kg isopropanol, 1.75kg is mixed with 2kg polyamide wax and stirred under 60 ℃ of water baths ( 200rpm) for 1h to obtain a polyamide wax composition containing activated polyamide wax.
实施例1Example 1
在反应釜内，加入150kg东大聚醚二元醇2000，50kg东大聚醚二元醇1000、50kg东大聚醚400和2kg扩链剂clearlink 1000 4,4’双仲丁氨基二环己基甲烷，在搅拌状态下慢慢升温到120℃，真空脱水2h，测定水分含量。将温度降低到70℃以下，加入50kg巴斯夫MDI-MI和30kg巴斯夫改性MDI103c，然后温度控制在80±2℃，在搅拌下通氮气保护反应1.5h，测定预聚体的NCO含量，达到设定值(NCO含量为3.3％)后，中止反应。加入5kg聚酰胺蜡组合物混合分散1h，即得聚氨酯预聚体混合物，打入缓冲罐。In the reactor, add 150kg Dongda polyether diol 2000, 50kg Dongda polyether diol 1000, 50kg Dongda polyether 400 and 2kg chain extender clearlink 1000 4,4'bis-sec-butylaminodicyclohexyl methane, slowly heated up to 120°C under stirring, dehydrated in vacuum for 2 hours, and measured the moisture content. Lower the temperature below 70°C, add 50kg of BASF MDI-MI and 30kg of BASF modified MDI103c, then control the temperature at 80±2°C, and react with nitrogen protection for 1.5h under stirring, and measure the NCO content of the prepolymer to reach the set value. After a constant value (3.3% NCO content), the reaction was terminated. Add 5 kg of polyamide wax composition and mix and disperse for 1 hour to obtain polyurethane prepolymer mixture, which is poured into a buffer tank.
将150kg苏州立达超微LD600，100kg湖南金箭B型纳米粉0.5kg无锡泽辉化工的氧化镁和0.5kg江苏群鑫的氧化钙通过捏合机于160℃，-0.1MPa真空脱水到0.05％以下的水分含量后，存储于缓冲罐中备用。150kg of Suzhou Lida Super Micro LD600, 100kg of Hunan Jinjian B-type nanopowder, 0.5kg of magnesium oxide from Wuxi Zehui Chemical and 0.5kg of calcium oxide from Jiangsu Qunxin were dehydrated to 0.05% by kneader at 160°C and -0.1MPa vacuum After the moisture content is below, it is stored in the buffer tank for later use.
采用上述方法制备的337kg聚氨酯预聚体混合物、上述方法处理的约251kg的脱水填料、20kg美国angus公司的zoldine RD20活性稀释剂、2kg毕克化学066N的消泡剂，1kg湖北武大有机硅公司的硅烷偶联剂WD50，0.5kg北京阿克玛的二月桂酸二丁基锡，0.3kg美国空气化工的五甲基二亚丙基三胺，0.2kg美国领先化学的异辛酸锌，0.5kg德国巴斯夫的对甲苯磺酰异氰酸酯小分子除水剂，通过双螺杆混合机保持在25℃以下搅拌分散研磨脱泡，-0.09～0.1MPa的真空度，通过刮板细度仪测试细度达到50um以上，即可出料灌装。337kg of polyurethane prepolymer mixture prepared by the above method, about 251kg of dehydrated filler processed by the above method, 20kg of zoldine RD20 reactive diluent from Angus Company of the United States, 2kg of BYK 066N defoamer, 1kg of Hubei Wuda Organic Silicon Company Silane coupling agent WD50, 0.5kg dibutyltin dilaurate from Beijing Akema, 0.3kg pentamethyldipropylene triamine from American Air Chemicals, 0.2kg zinc isooctanoate from American leading chemical company, 0.5kg from German BASF P-toluenesulfonyl isocyanate small molecule dehydrating agent, keep stirring, dispersing, grinding and defoaming at below 25°C by twin-screw mixer, vacuum degree of -0.09～0.1MPa, and test the fineness by scraper fineness meter to reach more than 50um, that is It can be discharged and filled.
实施例1得到的涂料性能测试如下：The coating performance test that embodiment 1 obtains is as follows:
25℃低剪切速率下粘度17000mpa.s，固含量98.2％，表干时间5小时，实干时间18小时，7天拉伸强度2.8MPa，断裂伸长率640％，撕裂强度17N/mm。Viscosity at low shear rate at 25°C is 17000mpa.s, solid content is 98.2%, surface dry time is 5 hours, hard drying time is 18 hours, 7-day tensile strength is 2.8MPa, elongation at break is 640%, tear strength is 17N/mm.
刮涂施工后情况如下：25℃一次厚涂1mm不流淌，基面温度60℃一次厚涂1mm不流淌。The situation after scrape coating is as follows: 1 mm thick coating at 25 °C does not flow, and the base surface temperature is 60 °C and 1 mm thick coating does not flow at one time.
实施例2Example 2
在反应釜内，加入50kg东大聚醚二元醇2000，80kg东大聚醚二元醇1000、80kg东大聚醚400和2kg扩链剂clearlink 1000 4,4’双仲丁氨基二环己基甲烷，在搅拌状态下慢慢升温到120℃，真空脱水2h，测定水分含量。将温度降低到60℃以下，加入70kg巴斯夫MDI-50和 20kg巴斯夫TDI，然后温度控制在80±3℃，在搅拌下通氮气保护反应1.5h。测定预聚体的NCO含量，达到设定值(NCO含量为3.3％)后，中止反应。加入5kg聚酰胺蜡组合物继续混合分散1h，即得聚氨酯预聚体混合物，打入缓冲罐。In the reactor, add 50kg Dongda polyether diol 2000, 80kg Dongda polyether diol 1000, 80kg Dongda polyether 400 and 2kg chain extender clearlink 1000 4,4'bis-sec-butylaminodicyclohexyl methane, slowly heated up to 120°C under stirring, dehydrated in vacuum for 2 hours, and measured the moisture content. Lower the temperature below 60°C, add 70kg BASF MDI-50 and 20kg BASF TDI, then control the temperature at 80±3°C, and react with nitrogen protection for 1.5h under stirring. The NCO content of the prepolymer was measured, and when it reached the set value (the NCO content was 3.3%), the reaction was terminated. Add 5 kg of polyamide wax composition and continue mixing and dispersing for 1 hour to obtain polyurethane prepolymer mixture, which is poured into a buffer tank.
将0.5kg洛阳建龙微纳分子筛，1kg氧化镁化学消泡剂，100kg苏州立达超微LD600，190kg湖南金箭B型纳米粉，10kg中国矿业大学研究生产的石膏晶须通过捏合机于160℃，-0.1MPA真空脱水到0.05％以下的水分含量后，存储于缓冲罐中备用。Put 0.5kg Luoyang Jianlong micro-nano molecular sieve, 1kg magnesium oxide chemical defoamer, 100kg Suzhou Lida superfine LD600, 190kg Hunan Jinjian B-type nano powder, and 10kg gypsum whiskers produced by China University of Mining and Technology through the kneader at 160 ℃, -0.1MPA vacuum dehydration to a moisture content below 0.05%, and then stored in a buffer tank for later use.
采用上述方法制备的307kg聚氨酯预聚体混合物、上述方法处理的约301.5kg的脱水填料、20kg美国angus公司的zoldine RD20活性稀释剂、2kg德谦化学5500的消泡剂，1kg f108杭州临安助剂，0.5kg北京阿克玛的二月桂酸二丁基锡，0.5kg美国空气化工的五甲基二亚丙基三胺，0.5kg美国领先化学的异辛酸锌，1kg德国巴斯夫的对甲苯磺酰异氰酸酯小分子除水剂，通过双螺杆混合机保持在25℃以下搅拌分散研磨脱泡，-0.09～0.1MPa的真空度，通过刮板细度仪测试细度达到50um以上，即可出料灌装。307kg of polyurethane prepolymer mixture prepared by the above method, about 301.5kg of dehydrated filler treated by the above method, 20kg of zoldine RD20 reactive diluent from Angus Company of the United States, 2kg of Deqian Chemical 5500 defoamer, 1kg of f108 Hangzhou Linan auxiliary agent , 0.5kg of dibutyltin dilaurate from Beijing Akema, 0.5kg of pentamethyldipropylenetriamine from American Air Chemicals, 0.5kg of zinc isooctanoate from the leading American chemical industry, 1kg of p-toluenesulfonyl isocyanate from BASF in Germany Molecular dewatering agent is kept under 25°C by twin-screw mixer for stirring, dispersing, grinding and defoaming, with a vacuum degree of -0.09-0.1MPa, and the fineness of which can be tested by a scraper fineness meter to reach 50um or more, and then it can be discharged and filled.
实施例2得到的涂料性能测试如下：The coating performance test that embodiment 2 obtains is as follows:
25℃粘度16100mpa.s，固含量98.7％，表干时间6小时，实干时间19小时，7天拉伸强度2.6MPa，断裂伸长率660％，撕裂强度17.5N/mm。The viscosity at 25°C is 16100mpa.s, the solid content is 98.7%, the surface dry time is 6 hours, the hard drying time is 19 hours, the 7-day tensile strength is 2.6MPa, the elongation at break is 660%, and the tear strength is 17.5N/mm.
刮涂施工后情况如下：25℃一次厚涂1.5mm不流淌，基面温度60℃一次厚涂1mm不流淌。The situation after scrape coating is as follows: 1.5mm thick coating at 25℃ does not flow, and the base surface temperature is 60℃ and 1mm thick coating does not flow at one time.
实施例3Example 3
在反应釜内，加入100kg东大聚醚二元醇2000，20kg东大聚醚二元醇1000、100kg东大聚醚400和2kg扩链剂clearlink 1000 4,4’双仲丁氨基二环己基甲烷，在搅拌状态下慢慢升温到120℃，真空脱水2h，测定水分含量。将温度降低到60℃以下，加入100kg万华IPDI和20kg巴斯夫103C，然后温度控制在80±3℃，在搅拌下通氮气保护反应1.5h。测定预聚体的NCO含量，达到设定值(NCO含量为3.3％)后，中止反应。然后加入5kg聚酰胺蜡组合物继续混合分散1h即得聚氨酯预聚体混合物，打入缓冲罐。In the reactor, add 100kg Dongda polyether diol 2000, 20kg Dongda polyether diol 1000, 100kg Dongda polyether 400 and 2kg chain extender clearlink 1000 4,4'bis-sec-butylaminodicyclohexyl methane, slowly heated up to 120°C under stirring, dehydrated in vacuum for 2 hours, and measured the moisture content. Lower the temperature below 60°C, add 100kg Wanhua IPDI and 20kg BASF 103C, then control the temperature at 80±3°C, and react with nitrogen protection for 1.5h under stirring. The NCO content of the prepolymer was measured, and when it reached the set value (the NCO content was 3.3%), the reaction was terminated. Then add 5 kg of polyamide wax composition and continue mixing and dispersing for 1 hour to obtain polyurethane prepolymer mixture, which is put into a buffer tank.
将2kg洛阳建龙微纳分子筛，3kg氧化镁化学消泡剂，200kg苏州立达超微LD600，200kg湖南金箭B型纳米粉，5kg中国矿业大学研究生产的石膏晶须，通过捏合机于160℃，-0.1MPA真空脱水到0.05％以下的水分含量后，存储于缓冲罐中备用。2kg Luoyang Jianlong micro-nano molecular sieve, 3kg magnesium oxide chemical defoamer, 200kg Suzhou Lida superfine LD600, 200kg Hunan Jinjian B-type nanopowder, 5kg gypsum whiskers researched and produced by China University of Mining and Technology, passed through a kneader at 160 ℃, -0.1MPA vacuum dehydration to a moisture content below 0.05%, and then stored in a buffer tank for later use.
采用上述方法制备的347kg聚氨酯预聚体混合物、上述方法处理的约410kg的脱水填料、50kg英国ICL公司的Incozol LV活性稀释剂，1kg德谦化学5500的消泡剂和1kg毕克化学的066N，3kg f108杭州临安助剂，0.5kg美国领先的有机铋，0.1kg美国空气化工的五甲基二亚 丙基三胺以及5kg德山PM20L，通过双螺杆混合机保持在25℃以下搅拌分散研磨脱泡，-0.09～0.1MPa的真空度，通过刮板细度仪测试细度达到50um以上，即可出料灌。347kg of polyurethane prepolymer mixture prepared by the above method, about 410kg of dehydrated filler treated by the above method, 50kg of Incozol LV reactive diluent from British ICL company, 1kg of Deqian Chemical 5500 defoamer and 1kg of BYK 066N, 3kg f108 Hangzhou Lin'an auxiliary agent, 0.5kg American leading organic bismuth, 0.1kg American air chemical pentamethyldipropylenetriamine and 5kg Deshan PM20L, kept stirring, dispersing, grinding and removing by twin-screw mixer below 25°C Bubble, -0.09 ~ 0.1MPa vacuum degree, through the scraper fineness tester to test the fineness to more than 50um, the material can be discharged and filled.
实施例3得到的涂料性能测试如下：The coating performance test that embodiment 3 obtains is as follows:
25℃粘度35900mpa.s，固含量98.9％，表干时间7小时，实干时间20小时，7天拉伸强度2.4MPa，断裂伸长率590％，撕裂强度16.7N/mm。The viscosity at 25°C is 35900mpa.s, the solid content is 98.9%, the surface dry time is 7 hours, the dry time is 20 hours, the tensile strength is 2.4MPa after 7 days, the elongation at break is 590%, and the tear strength is 16.7N/mm.
刮涂施工后情况如下：基面温度25℃一次厚涂2mm不流淌，基面温度60℃一次厚涂1mm不流淌。The situation after scrape coating is as follows: the base surface temperature is 25°C and a thick coating of 2mm does not flow, and the base surface temperature is 60°C and a thick coating of 1mm does not flow.
对比例1在实施例1基础上不经过预先活化处理而直接加入的对比实施例(使聚酰胺蜡在后期的混合过程进行分散)：Comparative Example 1 is a comparative example that is directly added without pre-activation treatment on the basis of Example 1 (the polyamide wax is dispersed in the later mixing process):
在反应釜内，加入150kg东大聚醚二元醇2000，50kg东大聚醚二元醇1000和50kg东大聚醚400和2kg扩链剂clearlink 1000 4,4’双仲丁氨基二环己基甲烷，在搅拌状态下慢慢升温到120℃，真空脱水2h，测定水分含量。将温度降低到70℃以下，加入50kg巴斯夫MDI-MI和30kg巴斯夫改性MDI103c，然后温度控制在80±2℃，在搅拌下通氮气保护反应1.5h。测定预聚体的NCO含量，达到设定值(NCO含量为3.3％)后，中止反应。加入2kg聚酰胺蜡和1.25kg异丙醇、1.75kg n-甲基吡咯烷酮混合溶液混合分散1h，即得聚氨酯预聚体混合物，打入缓冲罐。In the reactor, add 150kg Dongda Polyether Diol 2000, 50kg Dongda Polyether Diol 1000, 50kg Dongda Polyether 400 and 2kg chain extender clearlink 1000 4,4'bis-sec-butylaminodicyclohexyl methane, slowly heated up to 120°C under stirring, dehydrated in vacuum for 2 hours, and measured the moisture content. Lower the temperature below 70°C, add 50kg of BASF MDI-MI and 30kg of BASF modified MDI103c, then control the temperature at 80±2°C, and react with nitrogen protection for 1.5h under stirring. The NCO content of the prepolymer was measured, and when it reached the set value (the NCO content was 3.3%), the reaction was terminated. Add 2kg of polyamide wax, 1.25kg of isopropanol, and 1.75kg of n-methylpyrrolidone mixed solution and mix and disperse for 1 hour to obtain a polyurethane prepolymer mixture, which is poured into a buffer tank.
其余制备过程同实施例1。All the other preparation processes are the same as in Example 1.
涂料性能测试如下：Coating performance tests are as follows:
25℃粘度28000mpa.s，固含量98.2％，表干时间5小时，实干时间18小时，7天拉伸强度2.3MPa，断裂伸长率580％，撕裂强度16N/mm。The viscosity at 25°C is 28000mpa.s, the solid content is 98.2%, the surface dry time is 5 hours, the hard drying time is 18 hours, the 7-day tensile strength is 2.3MPa, the elongation at break is 580%, and the tear strength is 16N/mm.
刮涂施工后情况如下：25℃一次厚涂1mm不流淌，基面温度60℃一次厚涂1mm流淌。The situation after scrape coating is as follows: 1 mm thick coating at 25 ° C does not flow, and the base surface temperature is 60 ° C 1 mm thick coating flows.
对比例2在实施例1基础上调整聚酰胺蜡组合物的溶剂组分的对比实施例：Comparative example 2 adjusts the comparative example of the solvent component of polyamide wax composition on the basis of embodiment 1:
将1.25kg乙醇、1.75kg的N-甲基吡咯烷酮混合液与2kg聚酰胺蜡混合在60℃水浴下搅拌(200rpm)1h，即得到经过预处理的聚酰胺蜡组合物。Mix 1.25 kg of ethanol, 1.75 kg of N-methylpyrrolidone mixed solution with 2 kg of polyamide wax and stir (200 rpm) in a water bath at 60° C. for 1 hour to obtain a pretreated polyamide wax composition.
在反应釜内，加入150kg东大聚醚二元醇2000，50kg东大聚醚二元醇1000和50kg东大聚醚400和2kg扩链剂clearlink 1000 4,4’双仲丁氨基二环己基甲烷，在搅拌状态下慢慢升温到120℃，真空脱水2h，测定水分含量。将温度降低到70℃以下，加入50kg巴斯夫MDI-MI和30kg巴斯夫改性MDI103c，然后温度控制在80±2℃，在搅拌下通氮气保护反应1.5h。测定预聚体的NCO含量，达到设定值(NCO含量为3.3％)后，中止反应。加入已经经过预处 理的聚酰胺蜡组合物混合分散1h，即得聚氨酯预聚体混合物，打入缓冲罐。In the reactor, add 150kg Dongda Polyether Diol 2000, 50kg Dongda Polyether Diol 1000, 50kg Dongda Polyether 400 and 2kg chain extender clearlink 1000 4,4'bis-sec-butylaminodicyclohexyl methane, slowly heated up to 120°C under stirring, dehydrated in vacuum for 2 hours, and measured the moisture content. Lower the temperature below 70°C, add 50kg of BASF MDI-MI and 30kg of BASF modified MDI103c, then control the temperature at 80±2°C, and react with nitrogen protection for 1.5h under stirring. The NCO content of the prepolymer was measured, and when it reached the set value (the NCO content was 3.3%), the reaction was terminated. Add the pretreated polyamide wax composition and mix and disperse for 1 hour to obtain the polyurethane prepolymer mixture, which is put into a buffer tank.
其余制备过程同实施例1。All the other preparation processes are the same as in Example 1.
涂料性能测试如下：Coating performance tests are as follows:
25℃粘度33300mpa.s，固含量98.1％，表干时间5小时，实干时间17小时，7天拉伸强度2.4MPa，断裂伸长率592％，撕裂强度17N/mm。The viscosity at 25°C is 33300mpa.s, the solid content is 98.1%, the surface dry time is 5 hours, the hard drying time is 17 hours, the 7-day tensile strength is 2.4MPa, the elongation at break is 592%, and the tear strength is 17N/mm.
刮涂施工后情况如下：25℃一次厚涂0.75mm不流淌，25℃一次厚涂1mm流淌，基面温度60℃一次厚涂1mm流淌。The situation after scrape coating is as follows: 0.75mm thick coating once at 25°C does not flow, 1mm thick coating once at 25°C flows, base surface temperature 60°C 1mm thick coating flows.
对比例3Comparative example 3
基本同实施例1，其区别仅在于：将3kg N-甲基吡咯烷酮与2kg聚酰胺蜡混合在60℃水浴下搅拌(200rpm)1h，即得到经过预处理的聚酰胺蜡组合物。其他同实施例1。Basically the same as Example 1, the only difference is: 3kg of N-methylpyrrolidone and 2kg of polyamide wax were mixed and stirred (200rpm) in a water bath at 60°C for 1 hour to obtain a pretreated polyamide wax composition. Others are the same as embodiment 1.
涂料性能测试如下：Coating performance tests are as follows:
25℃粘度23600mpa.s，固含量98.2％，表干时间5小时，实干时间17小时，7天拉伸强度2.3MPa，断裂伸长率623％，撕裂强度17N/mm。The viscosity at 25°C is 23600mpa.s, the solid content is 98.2%, the surface dry time is 5 hours, the hard drying time is 17 hours, the 7-day tensile strength is 2.3MPa, the elongation at break is 623%, and the tear strength is 17N/mm.
刮涂施工后情况如下：25℃一次厚涂1mm不流淌，基面温度60℃一次厚涂1mm流淌。The situation after scrape coating is as follows: 1 mm thick coating at 25 ° C does not flow, and the base surface temperature is 60 ° C 1 mm thick coating flows.
对比例4Comparative example 4
基本同实施例1，其区别仅在于：将3kg异丙醇与2kg聚酰胺蜡混合在60℃水浴下搅拌(200rpm)1h，即得到经过预处理的聚酰胺蜡组合物。其他同实施例1。Basically the same as Example 1, the only difference is that: 3 kg of isopropanol and 2 kg of polyamide wax were mixed and stirred (200 rpm) in a water bath at 60° C. for 1 hour to obtain a pretreated polyamide wax composition. Others are the same as embodiment 1.
涂料性能测试如下：Coating performance tests are as follows:
25℃粘度21300mpa.s，固含量98.1％，表干时间5小时，实干时间17小时，7天拉伸强度2.5MPa，断裂伸长率598％，撕裂强度18N/mm。The viscosity at 25°C is 21300mpa.s, the solid content is 98.1%, the surface dry time is 5 hours, the hard drying time is 17 hours, the 7-day tensile strength is 2.5MPa, the elongation at break is 598%, and the tear strength is 18N/mm.
刮涂施工后情况如下：25℃一次厚涂1mm不流淌，基面温度60℃一次厚涂1mm流淌。The situation after scrape coating is as follows: 1 mm thick coating at 25 ° C does not flow, and the base surface temperature is 60 ° C 1 mm thick coating flows.
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。The above-mentioned embodiments are only to illustrate the technical concept and characteristics of the present invention, and the purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly, and not to limit the protection scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention shall fall within the protection scope of the present invention.
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值，这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说，各个范围的端点值之间、各个范围的端点值和单独的点值之间，以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围，这些数值范围应被视为在本文中具体公开。Neither the endpoints nor any values of the ranges disclosed herein are limited to such precise ranges or values, and these ranges or values are understood to include values approaching these ranges or values. For numerical ranges, between the endpoints of each range, between the endpoints of each range and individual point values, and between individual point values can be combined with each other to obtain one or more new numerical ranges, these values Ranges should be considered as specifically disclosed herein.

Claims (10)

  1. 一种聚酰胺蜡组合物，其特征在于，该组合物包含聚酰胺蜡以及用于分散聚酰胺蜡的混合溶剂，所述混合溶剂由异丙醇和N-甲基吡咯烷酮构成。A polyamide wax composition is characterized in that the composition contains polyamide wax and a mixed solvent for dispersing the polyamide wax, and the mixed solvent is composed of isopropanol and N-methylpyrrolidone.
  2. 根据权利要求1所述的聚酰胺蜡组合物，其特征在于，所述异丙醇与所述N-甲基吡咯烷酮的投料质量比为1∶0.5-2.5。The polyamide wax composition according to claim 1, characterized in that the mass ratio of the isopropanol to the N-methylpyrrolidone is 1:0.5-2.5.
  3. 根据权利要求2所述的聚酰胺蜡组合物，其特征在于，所述异丙醇与所述N-甲基吡咯烷酮的投料质量比为1∶1.1-2.3。The polyamide wax composition according to claim 2, characterized in that the mass ratio of the isopropanol to the N-methylpyrrolidone is 1:1.1-2.3.
  4. 根据权利要求1所述的聚酰胺蜡组合物，其特征在于，该组合物中，以质量百分含量计，聚酰胺蜡占30-50％，异丙醇占20-30％，N-甲基吡咯烷酮占25-45％。The polyamide wax composition according to claim 1, characterized in that, in the composition, in terms of mass percentage, polyamide wax accounts for 30-50%, isopropanol accounts for 20-30%, and N-formazol Base pyrrolidone accounts for 25-45%.
  5. 一种权利要求1-4中任一项所述的聚酰胺蜡组合物的制备方法，其特征在于，所述制备方法包括：按配方称取聚酰胺蜡、异丙醇和N-甲基吡咯烷酮，混合分散，获得聚酰胺蜡组合物。A preparation method of the polyamide wax composition described in any one of claims 1-4, is characterized in that, described preparation method comprises: take polyamide wax, Virahol and N-methylpyrrolidone by formula, Mix and disperse to obtain a polyamide wax composition.
  6. 一种聚酰胺蜡的活化方法，其特征在于，所述活化方法包括：在60℃以下的混合温度下和/或200rpm以下的搅拌速度下混合权利要求1-4中任一项所述的聚酰胺蜡组合物中的各成分，获得含有活化的聚酰胺蜡。A method for activating polyamide wax, characterized in that the activation method comprises: mixing the polyamide wax described in any one of claims 1-4 at a mixing temperature below 60°C and/or at a stirring speed below 200rpm The components in the amide wax composition are used to obtain activated polyamide wax.
  7. 根据权利要求6所述的活化方法，其特征在于，混合的时间为0.5-2h。The activation method according to claim 6, characterized in that the mixing time is 0.5-2h.
  8. 根据权利要求6或7所述的活化方法，其特征在于，混合温度为40-60℃，搅拌速度为100-200rpm。The activation method according to claim 6 or 7, characterized in that the mixing temperature is 40-60° C., and the stirring speed is 100-200 rpm.
  9. 一种权利要求1-4中任一项所述的聚酰胺蜡组合物在聚氨酯防水涂料中的应用，其特征在于，所述应用包括：在添加至聚氨酯防水涂料之前，对该聚酰胺蜡组合物进行如下操作：在60℃以下的混合温度下和/或200rpm以下的搅拌速度下混合分散。An application of the polyamide wax composition described in any one of claims 1-4 in polyurethane waterproof coating, is characterized in that, described application comprises: before being added to polyurethane waterproof coating, this polyamide wax combination The mixture is mixed and dispersed at a mixing temperature below 60° C. and/or at a stirring speed below 200 rpm.
  10. 一种单组分聚氨酯防水涂料，其特征在于，以质量份数计，所述单组分聚氨酯防水涂料的原料包括：聚氨酯预聚体25-50份、权利要求1-4中任一项所述的聚酰胺蜡组合物0.1-2份、活性稀释剂2-5份、润湿分散剂0.1-0.3份，重质填料20-30份、纳米级填料10-20份、脱水剂0.1-0.3份、催化剂0.05-0.2份、物理消泡剂0.1-0.3份、化学消泡剂0.1-0.3份；A single-component polyurethane waterproof coating, characterized in that, in parts by mass, the raw materials of the single-component polyurethane waterproof coating include: 25-50 parts of polyurethane prepolymer, any one of claims 1-4 0.1-2 parts of the polyamide wax composition, 2-5 parts of reactive diluent, 0.1-0.3 parts of wetting and dispersing agent, 20-30 parts of heavy filler, 10-20 parts of nanoscale filler, 0.1-0.3 parts of dehydrating agent parts, catalyst 0.05-0.2 parts, physical defoamer 0.1-0.3 parts, chemical defoamer 0.1-0.3 parts;
    所述单组分聚氨酯防水涂料的制备方法包括：The preparation method of described one-component polyurethane waterproof coating comprises:
    将根据权利要求6-8中任一项所述的活化方法获得的含有活化的聚酰胺蜡的聚酰胺蜡组合物与聚氨酯预聚体混合，然后加入剩余原料，混合，脱泡，制成单组分聚氨酯防水涂料。The polyamide wax composition containing the activated polyamide wax obtained by the activation method according to any one of claims 6-8 is mixed with the polyurethane prepolymer, then the remaining raw materials are added, mixed, and defoamed to make a single Component polyurethane waterproof coating.
PCT/CN2022/108508 2021-08-06 2022-07-28 Polyamide wax composition, preparation method therefor, and application thereof WO2023011303A1 (en)

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