CN113527722A - Polyamide wax composition and preparation method and application thereof - Google Patents

Polyamide wax composition and preparation method and application thereof Download PDF

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Publication number
CN113527722A
CN113527722A CN202110899915.0A CN202110899915A CN113527722A CN 113527722 A CN113527722 A CN 113527722A CN 202110899915 A CN202110899915 A CN 202110899915A CN 113527722 A CN113527722 A CN 113527722A
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polyamide wax
wax composition
mixing
composition
parts
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CN113527722B (en
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王仁杰
李忠人
周围
贺小钢
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Jiangsu Canlon Building Materials Co Ltd
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Jiangsu Canlon Building Materials Co Ltd
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Priority to CN202311238107.5A priority Critical patent/CN117363086A/en
Priority to CN202110899915.0A priority patent/CN113527722B/en
Publication of CN113527722A publication Critical patent/CN113527722A/en
Priority to PCT/CN2022/108508 priority patent/WO2023011303A1/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/091Making 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
    • C08J3/095Oxygen containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/09Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
    • C08J3/091Making 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
    • C08J3/096Nitrogen containing compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04Polyurethanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2377/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Paints Or Removers (AREA)

Abstract

The invention discloses a polyamide wax composition, a preparation method and application thereof, wherein the composition comprises polyamide wax and a mixed solvent for dispersing the polyamide wax, wherein the mixed solvent is composed of isopropanol and N-methyl pyrrolidone; the composition can be mixed at a mixing temperature of below 60 ℃ and/or a stirring speed of below 200rpm to obtain the polyamide wax composition containing the activated polyamide wax, so that the construction difficulty and the construction cost can be greatly reduced in the preparation process of the polyurethane waterproof coating, the polyurethane waterproof coating is endowed with excellent anti-sagging performance, and the excellent anti-sagging effect can be obtained on a base surface at a higher temperature in time.

Description

Polyamide wax composition and preparation method and application thereof
Technical Field
The invention belongs to the field of building waterproofing, and particularly relates to a polyamide wax composition, and a preparation method and application thereof.
Background
Currently, the polyurethane on the market has anti-sagging performance, and a thixotropic agent is usually added, wherein polyamide wax is a more common thixotropic agent. Polyamide waxes are mainly composed of two parts, a non-polar aliphatic hydrocarbon part and a polar amide functional group. The oxygen atom in the amide group has large electronegativity and is easy to form a hydrogen bond with the hydrogen atom of the alkyl part, the hydrogen bond can be formed between molecules or in molecules, the intra-molecular hydrogen bond enables the molecules to be in a curled shape, the whole molecule basically shows a nonpolar state to the outside, a three-dimensional network structure is difficult to establish, and then the thixotropic effect cannot be realized; the intermolecular hydrogen bond can form a three-dimensional network structure in the coating system, and the establishment of the structure enables the coating to have the anti-sagging performance. The polyamide wax is easy to form intramolecular hydrogen bonds under the conventional storage condition, so that the polyamide wax is fully dispersed into uniformly dispersed molecular individuals in a straightened state by high-speed shearing and high-temperature activation treatment at about 120 ℃ in a solvent before use, is more compatible with a polyurethane system, can effectively disperse most colloids and generate a rheological activated network structure, provides excellent thixotropic property, and realizes viscosity establishment, sagging control and pigment and filler suspension control. However, the high-speed shearing and higher-temperature activation treatment mode has high requirements on production equipment, and meanwhile, the treatment needs to be carried out on site, so that the construction difficulty and the construction cost are greatly increased.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a novel polyamide wax composition, which can realize the activation treatment of polyamide wax by simply stirring at a low speed and/or at a lower activation temperature, greatly improves the construction convenience and saves the construction cost.
The invention also provides a preparation method of the polyamide wax composition.
The invention also provides a method for activating the polyamide wax by the polyamide wax composition.
The invention also provides an application of the polyamide wax composition in polyurethane waterproof paint.
In order to achieve the purpose, the invention adopts a technical scheme that:
a polyamide wax composition comprising a polyamide wax and a mixed solvent for dispersing the polyamide wax, the mixed solvent being composed of isopropyl alcohol and N-methylpyrrolidone.
According to some preferred aspects of the present invention, the feed mass ratio of the isopropanol to the N-methylpyrrolidone is 1: 0.5-2.5.
Further, the feeding mass ratio of the isopropanol to the N-methyl pyrrolidone is 1: 1.1-2.3.
According to some preferred aspects of the invention, the composition comprises 30-50% by weight of the polyamide wax, 20-30% by weight of the isopropyl alcohol, and 25-45% by weight of the N-methylpyrrolidone.
The invention provides another technical scheme that: a method for preparing the polyamide wax composition, the method comprising: weighing the polyamide wax, the isopropanol and the N-methyl pyrrolidone according to the formula, and mixing and dispersing to obtain the polyamide wax composition.
The invention provides another technical scheme that: a method of activating a polyamide wax, the method comprising: the components of the polyamide wax composition described above are mixed at a mixing temperature of 60 ℃ or less and/or at a stirring speed of 200rpm or less to obtain an activated-containing polyamide wax.
According to the invention, the mixing time can be shortened to 0.5-2h, and the activation of the polyamide wax can be realized.
According to some preferred and specific aspects of the present invention, the mixing temperature is 40-60 ℃ and the stirring speed is 100-200 rpm.
The polyamide wax composition can activate the polyamide wax at a lower activation temperature and/or stirring speed, better overcomes the defects that special high-speed shearing equipment (the shearing speed needs to be more than 1500 rpm) and the activation temperature of about 120 ℃ are needed in the prior art, and reduces the construction difficulty and the construction cost.
The invention provides another technical scheme that: the application of the polyamide wax composition in polyurethane waterproof coating comprises the following steps: before being added to the polyurethane waterproofing coating, the polyamide wax composition is subjected to the following operations: mixing and dispersing at a mixing temperature of 60 ℃ or lower and/or at a stirring speed of 200rpm or lower.
The invention provides another technical scheme that: the single-component polyurethane waterproof coating is characterized by comprising the following raw materials in parts by mass: 25-50 parts of polyurethane prepolymer, 0.1-2 parts of the polyamide wax composition, 2-5 parts of active diluent, 0.1-0.3 part of wetting dispersant, 20-30 parts of heavy filler, 10-20 parts of nano filler, 0.1-0.3 part of dehydrating agent, 0.05-0.2 part of catalyst, 0.1-0.3 part of physical defoaming agent and 0.1-0.3 part of chemical defoaming agent;
the preparation method of the single-component polyurethane waterproof coating comprises the following steps:
and mixing the polyamide wax composition containing the activated polyamide wax obtained by the activation method with the polyurethane prepolymer, then adding the rest raw materials, mixing and defoaming to prepare the single-component polyurethane waterproof coating.
According to some specific aspects of the invention, the polyurethane prepolymer is prepared by reacting a polyol with a polyisocyanate and then reacting the reaction product with a chain extender, wherein the NCO content is controlled to be 2.5-5.0% (mass percentage). Namely, the polyurethane prepolymer comprises the following raw materials: a polyol, a polyisocyanate, and a chain extender.
According to some preferred and specific aspects of the present invention, the polyol is at least two selected from polyether diol, polyester diol, polyether triol, and specifically may be selected from, for example, polyether diol 2000, polyether diol 1000, polyether 400, and the like. According to some preferred and specific aspects of the present invention, the polyisocyanate is a combination of one or more selected from the group consisting of Toluene Diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI), modified MDI, dicyclohexylmethane diisocyanate (HMDI), Hexamethylene Diisocyanate (HDI), Lysine Diisocyanate (LDI), and specifically may be selected from basf MDI-MI, royal IPDI, basf modified MDI103C, basf MDI-50, basf TDI, and the like, for example.
According to some preferred and specific aspects of the present invention, the chain extender is one or a combination of more selected from the group consisting of clearlink 10004, 4 ' bis-sec-butylaminodicyclohexylmethane, clearlink 30003, 3 ' -dimethyl 4,4 ' -bis-sec-butylaminodicyclohexylmethane, jefflink754, jefflink555, jefflink 7027, jeffamin HK-511.
According to some particular aspects of the invention, the reactive diluent may be zoldine RD20 reactive diluent from Angus, Incozol LV reactive diluent from ICL, UK, or the like.
According to some embodiments of the present invention, the wetting dispersant may be at least one dispersant selected from titanates, silanes, carboxylic acids, and the like, and may be, for example, the hang state temporary assistant f 108.
According to some specific aspects of the invention, the dehydrating agent is at least one of a molecular sieve or an isocyanate micromolecular dehydrating agent, and specifically can be a micro-nano molecular sieve of Loyang Jianlong, a p-toluenesulfonyl isocyanate micromolecular dehydrating agent of Pasff, Germany, calcium oxide of Tuxin heavy calcium and the like.
According to some particular aspects of the invention, the heavy filler is selected from at least one of titanium dioxide, heavy calcium, kaolin, talc, and the like.
According to some specific aspects of the present invention, the nano-scale filler is selected from one, two or more of gypsum whisker, fumed silica, nano calcium carbonate, nano aluminum nitride, nano boron nitride, nano aluminum borate and the like.
According to some specific aspects of the invention, the catalyst is selected from at least one of dibutyltin dilaurate, stannous octoate, environmentally friendly non-butyltin catalysts, bismuth carboxylate-based catalysts, zinc naphthenate, pentamethyldipropylenetriamine, tetramethylethylenediamine, dimorpholine. The composite catalyst is preferably a combination of at least two of them, and further preferably a combination of at least three of them.
According to some specific aspects of the invention, the physical defoamer may be a polysiloxane defoamer, a silicone defoamer, and the specific defoamer may be a defoamer of courtesy chemistry 5500, 066N of bike chemistry, a chemical defoamer of calcium oxide, magnesium oxide, calcium hydroxide, a latent curing agent, and the like.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
the invention is based on the corresponding improvement of the defect that the polyamide wax needs high-speed shearing and high-temperature activation treatment at about 120 ℃ when being used as a thixotropic agent, in long-term production practice, the present inventors have occasionally found that when a polyamide wax is dispersed using isopropanol in combination with N-methylpyrrolidone as a mixed solvent, the conditions for activation of the polyamide wax can be made simpler, and the activation of the polyamide wax can be achieved only by conventional stirring equipment and/or lower activation temperatures (which can be in the range of 40-60 ℃, although higher temperatures are also possible, but the corresponding requirements on energy consumption and equipment are increased), when the polyamide wax is added into the polyurethane waterproof coating as the thixotropic agent, the requirements on operating equipment are reduced, the energy consumption is reduced, the cost is saved, and the preparation of the waterproof coating in site construction is facilitated; meanwhile, the polyurethane waterproof coating is endowed with improved anti-sagging performance under the condition of not increasing the viscosity, and the characteristics of no flow on the vertical surface (no flow when 1mm is coated once), no flow at high temperature (no flow when 1mm is coated once on the base surface at 60 ℃) and the like can be realized.
Detailed Description
The above-described scheme is further illustrated below with reference to specific examples; it is to be understood that these embodiments are provided to illustrate the general principles, essential features and advantages of the present invention, and the present invention is not limited in scope by the following embodiments; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments.
Not specifically illustrated in the following examples, all starting materials are commercially available or prepared by methods conventional in the art.
The polyamide wax compositions used in the following examples have all been subjected to activation of the polyamide wax: 1.25kg of isopropanol, 1.75kg of N-methylpyrrolidone and 2kg of polyamide wax are mixed and stirred (200 rpm) in a water bath at 60 ℃ for 1h to obtain the polyamide wax composition containing the activated polyamide wax.
Example 1
150kg of Dongda polyether diol 2000, 50kg of Dongda polyether diol 1000, 50kg of Dongda polyether 400 and 2kg of chain extender clearlink 10004, 4' -bis-sec-butylamino dicyclohexyl methane are added into a reaction kettle, the temperature is slowly raised to 120 ℃ under the stirring state, the vacuum dehydration is carried out for 2 hours, and the moisture content is measured. The temperature is reduced to below 70 ℃, 50kg of BASF MDI-MI and 30kg of BASF modified MDI103c are added, then the temperature is controlled to be 80 +/-2 ℃, nitrogen is introduced for protection reaction for 1.5h under stirring, the NCO content of the prepolymer is measured, and the reaction is stopped after the NCO content reaches a set value (NCO content is 3.3%). Adding 5kg of polyamide wax composition, mixing and dispersing for 1h to obtain a polyurethane prepolymer mixture, and pumping the polyurethane prepolymer mixture into a buffer tank.
150kg of Suzhou lida ultramicro LD600, 100kg of Hunan Jinjian B-type nanometer powder, 0.5kg of magnesium oxide in Wuzhenghui chemical industry and 0.5kg of calcium oxide in Jiangsu Tuxin are dehydrated to the moisture content of below 0.05 percent in vacuum at 160 ℃ and 0.1MPa by a kneader and then stored in a buffer tank for later use.
337kg of polyurethane prepolymer mixture prepared by the method, about 251kg of dehydrated filler treated by the method, 20kg of zoldine RD20 reactive diluent of American angus company, 2kg of defoamer of Pico chemical 066N, 1kg of silane coupling agent WD50 of Hubei Wu Dai organosilicon company, 0.5kg of dibutyltin dilaurate of Beijing Akma, 0.3kg of pentamethyldipropylene triamine of American air chemical engineering, 0.2kg of American lead chemical zinc isooctanoate, 0.5kg of small molecule water remover of tosyl isocyanate of Germany BASF, stirring, dispersing, grinding and defoaming at the temperature of below 25 ℃ by a double-screw mixer, and vacuum degree of 0.09-0.1 MPa, wherein the fineness reaches more than 50 microns by a scraper fineness tester, and then discharging and filling can be carried out.
The coatings obtained in example 1 were tested for their properties as follows:
the viscosity is 17000mpa.s at the low shear rate of 25 ℃, the solid content is 98.2 percent, the surface drying time is 5 hours, the actual drying time is 18 hours, the 7-day tensile strength is 2.8MPa, the elongation at break is 640 percent, and the tear strength is 17N/mm.
The conditions after blade coating construction were as follows: the coating thickness is 1mm at 25 ℃ and does not flow, and the coating thickness is 1mm at 60 ℃ and does not flow.
Example 2
Adding 50kg of Dongda polyether glycol 2000, 80kg of Dongda polyether glycol 1000, 80kg of Dongda polyether 400 and 2kg of chain extender clearlink 10004, 4' -bis-sec-butylamino dicyclohexyl methane into a reaction kettle, slowly heating to 120 ℃ under the stirring state, carrying out vacuum dehydration for 2h, and measuring the moisture content. The temperature is reduced to below 60 ℃, 70kg of BASF MDI-50 and 20kg of BASF TDI are added, then the temperature is controlled to be 80 +/-3 ℃, and nitrogen is introduced for protection reaction for 1.5h under stirring. The NCO content of the prepolymer was measured and the reaction was terminated after the NCO content reached the set value (NCO content: 3.3%). Adding 5kg of polyamide wax composition, continuously mixing and dispersing for 1h to obtain a polyurethane prepolymer mixture, and pumping the polyurethane prepolymer mixture into a buffer tank.
0.5kg of Luoyang Jianlong micro-nano molecular sieve, 1kg of magnesium oxide chemical defoaming agent, 100kg of Suzhou zhuo ultramicro LD600, 190kg of Hunan Jinjiangjian B type nano powder and 10kg of gypsum whisker researched and produced by China mining university are dehydrated to the moisture content of below 0.05 percent in vacuum by a kneader at 160 ℃, and then are stored in a buffer tank for later use.
307kg of polyurethane prepolymer mixture prepared by the method, about 301.5kg of dehydrated filler treated by the method, 20kg of zoldine RD20 reactive diluent of American angus company, 2kg of defoamer of moderate chemistry 5500, 1kg of f108 Hangzhou auxiliary agent, 0.5kg of dibutyltin dilaurate of Beijing Akma, 0.5kg of pentamethyldipropylene triamine of American air chemistry, 0.5kg of American lead chemistry zinc isooctanoate, 1kg of p-toluenesulfonyl isocyanate micromolecule dehydrator of German Basff, stirring, dispersing, grinding and defoaming are carried out at the temperature below 25 ℃ by a double-screw mixer, the vacuum degree is 0.09-0.1 MPa, the fineness reaches more than 50 microns by a scraper fineness tester, and discharging and filling are carried out.
The paint properties obtained in example 2 were tested as follows:
16100mpa.s of viscosity at 25 ℃, 98.7 percent of solid content, 6 hours of surface drying time, 19 hours of actual drying time, 2.6MPa of tensile strength after 7 days, 660 percent of elongation at break and 17.5N/mm of tearing strength.
The conditions after blade coating construction were as follows: the coating thickness of 1.5mm at 25 ℃ does not flow, and the coating thickness of 1mm at 60 ℃ does not flow.
Example 3
100kg of Dongda polyether diol 2000, 20kg of Dongda polyether diol 1000, 100kg of Dongda polyether 400 and 2kg of chain extender clearlink 10004, 4' -bis-sec-butylamino dicyclohexyl methane are added into a reaction kettle, the temperature is slowly raised to 120 ℃ under the stirring state, the vacuum dehydration is carried out for 2 hours, and the moisture content is measured. The temperature is reduced to below 60 ℃, 100kg of Wanhua IPDI and 20kg of Basff 103C are added, then the temperature is controlled to be 80 +/-3 ℃, and nitrogen is introduced for protection reaction for 1.5h under stirring. The NCO content of the prepolymer was measured and the reaction was terminated after the NCO content reached the set value (NCO content: 3.3%). Then 5kg of polyamide wax composition is added to be mixed and dispersed for 1 hour to obtain a polyurethane prepolymer mixture, and the mixture is injected into a buffer tank.
2kg of Luoyang Jianlong micro-nano molecular sieve, 3kg of magnesium oxide chemical defoaming agent, 200kg of Suzhou zhuda ultramicro LD600, 200kg of Hunan Jinjiangjian B-type nano powder and 5kg of gypsum whisker researched and produced by China mining university are dehydrated to the moisture content of below 0.05 percent in vacuum at 160 ℃ through a kneader and then stored in a buffer tank for later use.
347kg of polyurethane prepolymer mixture prepared by the method, about 410kg of dehydrated filler treated by the method, 50kg of Incozol LV reactive diluent of British ICL company, 1kg of defoamer of moderate chemistry 5500 and 1kg of midkine chemistry 066N, 3kg of f108 Hangzhou auxiliary agent, 0.5kg of American leading organic bismuth, 0.1kg of American air-chemical pentamethyldipropylene triamine and 5kg of Deshan PM20L are stirred, dispersed, ground and defoamed by a double-screw mixer at the temperature of below 25 ℃, the vacuum degree of 0.09-0.1 MPa is kept, and the fineness is tested to be more than 50 microns by a scraper fineness tester, so that the polyurethane prepolymer can be discharged and poured.
The paint properties obtained in example 3 were tested as follows:
35900mpa.s at 25 ℃, 98.9 percent of solid content, 7 hours of surface drying time, 20 hours of actual drying time, 2.4MPa of 7-day tensile strength, 590 percent of breaking elongation and 16.7N/mm of tearing strength.
The conditions after blade coating construction were as follows: the flow does not occur when the base surface temperature is 25 ℃ and the thickness is 2mm at one time, and the flow does not occur when the base surface temperature is 60 ℃ and the thickness is 1mm at one time.
Comparative example 1 comparative example added directly to example 1 without prior activation treatment (polyamide wax was dispersed during the later mixing):
150kg of Dongda polyether diol 2000, 50kg of Dongda polyether diol 1000, 50kg of Dongda polyether 400 and 2kg of chain extender clearlink 10004, 4' -bis-sec-butylamino dicyclohexyl methane are added into a reaction kettle, the temperature is slowly raised to 120 ℃ under the stirring state, the vacuum dehydration is carried out for 2 hours, and the moisture content is measured. The temperature is reduced to below 70 ℃, 50kg of basf MDI-MI and 30kg of basf modified MDI103c are added, then the temperature is controlled at 80 +/-2 ℃, and nitrogen is introduced for protection reaction for 1.5h under stirring. The NCO content of the prepolymer was measured and the reaction was terminated after the NCO content reached the set value (NCO content: 3.3%). Adding 2kg of polyamide wax, 1.25kg of isopropanol and 1.75kg of n-methyl pyrrolidone mixed solution, mixing and dispersing for 1 hour to obtain a polyurethane prepolymer mixture, and pumping the polyurethane prepolymer mixture into a buffer tank.
The rest of the preparation process is the same as example 1.
The paint performance was tested as follows:
28000mpa.s viscosity at 25 ℃, 98.2 percent of solid content, 5 hours of surface drying time, 18 hours of actual drying time, 2.3MPa of 7-day tensile strength, 580 percent of breaking elongation and 16N/mm of tearing strength.
The conditions after blade coating construction were as follows: the coating thickness is 1mm at 25 ℃ and does not flow, and the coating thickness is 1mm at 60 ℃ on the base surface.
Comparative example 2 comparative example in which the solvent component of the polyamide wax composition was adjusted on the basis of example 1:
1.25kg of ethanol, 1.75kg of N-methyl pyrrolidone mixed solution and 2kg of polyamide wax are mixed and stirred (200 rpm) for 1h in a water bath at the temperature of 60 ℃, and the pretreated polyamide wax composition is obtained.
150kg of Dongda polyether diol 2000, 50kg of Dongda polyether diol 1000, 50kg of Dongda polyether 400 and 2kg of chain extender clearlink 10004, 4' -bis-sec-butylamino dicyclohexyl methane are added into a reaction kettle, the temperature is slowly raised to 120 ℃ under the stirring state, the vacuum dehydration is carried out for 2 hours, and the moisture content is measured. The temperature is reduced to below 70 ℃, 50kg of basf MDI-MI and 30kg of basf modified MDI103c are added, then the temperature is controlled at 80 +/-2 ℃, and nitrogen is introduced for protection reaction for 1.5h under stirring. The NCO content of the prepolymer was measured and the reaction was terminated after the NCO content reached the set value (NCO content: 3.3%). Adding the pretreated polyamide wax composition, mixing and dispersing for 1h to obtain a polyurethane prepolymer mixture, and pumping the polyurethane prepolymer mixture into a buffer tank.
The rest of the preparation process is the same as example 1.
The paint performance was tested as follows:
viscosity at 25 ℃ of 33300mpa.s, solid content of 98.1 percent, surface drying time of 5 hours, actual drying time of 17 hours, 7-day tensile strength of 2.4MPa, elongation at break of 592 percent and tear strength of 17N/mm.
The conditions after blade coating construction were as follows: the coating thickness is 0.75mm at 25 ℃ and does not flow, the coating thickness is 1mm at 25 ℃ and 1mm at 60 ℃ on the base surface.
Comparative example 3
Basically, the method is the same as the method of the embodiment 1, and the method only differs from the method in that: 3kg of N-methyl pyrrolidone and 2kg of polyamide wax are mixed and stirred (200 rpm) for 1h in a water bath at 60 ℃ to obtain the pretreated polyamide wax composition. The rest is the same as example 1.
The paint performance was tested as follows:
23600mpa.s at 25 ℃, 98.2 percent of solid content, 5 hours of surface drying time, 17 hours of actual drying time, 2.3MPa of 7-day tensile strength, 623 percent of elongation at break and 17N/mm of tearing strength.
The conditions after blade coating construction were as follows: the coating thickness is 1mm at 25 ℃ and does not flow, and the coating thickness is 1mm at 60 ℃ on the base surface.
Comparative example 4
Basically, the method is the same as the method of the embodiment 1, and the method only differs from the method in that: 3kg of isopropanol and 2kg of polyamide wax were mixed and stirred (200 rpm) in a water bath at 60 ℃ for 1h to obtain a pretreated polyamide wax composition. The rest is the same as example 1.
The paint performance was tested as follows:
viscosity at 25 ℃ of 21300mpa.s, solid content of 98.1 percent, surface drying time of 5 hours, actual drying time of 17 hours, 7-day tensile strength of 2.5MPa, elongation at break of 598 percent and tear strength of 18N/mm.
The conditions after blade coating construction were as follows: the coating thickness is 1mm at 25 ℃ and does not flow, and the coating thickness is 1mm at 60 ℃ on the base surface.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.

Claims (10)

1. A polyamide wax composition, characterized in that the composition comprises a polyamide wax and a mixed solvent for dispersing the polyamide wax, wherein the mixed solvent is composed of isopropyl alcohol and N-methylpyrrolidone.
2. The polyamide wax composition as claimed in claim 1, wherein the mass ratio of the isopropanol to the N-methylpyrrolidone is 1: 0.5-2.5.
3. The polyamide wax composition as claimed in claim 2, wherein the mass ratio of the isopropanol to the N-methylpyrrolidone is 1: 1.1-2.3.
4. The polyamide wax composition as claimed in claim 1, wherein the polyamide wax composition comprises 30 to 50% by mass of the polyamide wax, 20 to 30% by mass of the isopropyl alcohol, and 25 to 45% by mass of the N-methylpyrrolidone.
5. A method of making the polyamide wax composition of any of claims 1-4, comprising: weighing the polyamide wax, the isopropanol and the N-methyl pyrrolidone according to the formula, and mixing and dispersing to obtain the polyamide wax composition.
6. A method for activating a polyamide wax, the method comprising: mixing the components of the polyamide wax composition according to any of claims 1 to 4 at a mixing temperature below 60 ℃ and/or at a stirring speed below 200rpm to obtain an activated polyamide wax.
7. Activation process according to claim 6, characterised in that the mixing time is between 0.5 and 2 h.
8. The activation method according to claim 6 or 7, wherein the mixing temperature is 40-60 ℃ and the stirring speed is 100-200 rpm.
9. Use of a polyamide wax composition according to any one of claims 1 to 4 in a polyurethane waterproofing coating, characterized in that it comprises: before being added to the polyurethane waterproofing coating, the polyamide wax composition is subjected to the following operations: mixing and dispersing at a mixing temperature of 60 ℃ or lower and/or at a stirring speed of 200rpm or lower.
10. The single-component polyurethane waterproof coating is characterized by comprising the following raw materials in parts by mass: 25-50 parts of polyurethane prepolymer, 0.1-2 parts of polyamide wax composition as defined in any one of claims 1-4, 2-5 parts of active diluent, 0.1-0.3 part of wetting dispersant, 20-30 parts of heavy filler, 10-20 parts of nano filler, 0.1-0.3 part of dehydrating agent, 0.05-0.2 part of catalyst, 0.1-0.3 part of physical defoaming agent and 0.1-0.3 part of chemical defoaming agent;
the preparation method of the single-component polyurethane waterproof coating comprises the following steps:
mixing the polyamide wax composition containing the activated polyamide wax obtained by the activation method according to any one of claims 6 to 8 with a polyurethane prepolymer, then adding the rest raw materials, mixing, defoaming, and preparing the one-component polyurethane waterproof coating.
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