CN108726945B - Preparation method of boron nitride nanotube modified bonding composite material - Google Patents

Preparation method of boron nitride nanotube modified bonding composite material Download PDF

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CN108726945B
CN108726945B CN201810681812.5A CN201810681812A CN108726945B CN 108726945 B CN108726945 B CN 108726945B CN 201810681812 A CN201810681812 A CN 201810681812A CN 108726945 B CN108726945 B CN 108726945B
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boron nitride
parts
nitride nanotube
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composite material
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CN108726945A (en
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苏英
彭凯
贺行洋
陈顺
杨进
王迎斌
曾三海
陈威
秦景燕
卢敏
黄健翔
蒋健
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Hubei Qingyao Environment Co ltd
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Hubei University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04—Portland cements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
    • C01B21/0648—After-treatment, e.g. grinding, purification
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00637—Uses not provided for elsewhere in C04B2111/00 as glue or binder for uniting building or structural materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Structural Engineering (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a preparation method of a boron nitride nanotube modified bonding composite material, which adopts the following components, by weight, 100 parts of portland cement, 5-50 parts of superfine slag powder, 5-20 parts of denitration fly ash, 10-30 parts of steel slag coarse powder, 15-20 parts of water, 10-15 parts of surface-modified boron nitride nanotubes, 3-10 parts of polymer emulsion, 0.6-1.0 part of cellulose ether, 0.05-0.16 part of defoaming agent and 0.2-0.8 part of hyper-dispersant, wherein the components are put into a stirrer and uniformly stirred at a high speed to obtain the bonding composite material, and the surface-modified boron nitride nanotubes are obtained by taking dopamine as a surface modifier for surface modification. The invention has the advantages of simple method, low production cost, high bonding strength, high temperature resistance and good water resistance.

Description

Preparation method of boron nitride nanotube modified bonding composite material
Technical Field
The invention relates to the field of building materials, in particular to a preparation method of a bonding composite material.
Background
Compared with the traditional construction process: the fabricated building has the advantages of high construction efficiency, high industrialization degree, less construction waste and the like. In addition, the assembly type process can be used for houses, containers, long-rented apartments and the like.
With the rise of the assembly type building industry, a series of problems occur to restrict the rapid development of the assembly type building industry. The outer wall members of the fabricated building can generate a plurality of splicing seams after being spliced, and the difficulty of processing the splicing seams is inevitably met. The existing fabricated prefabricated parts have poor bonding strength and poor water resistance. In order to change the current situation, the assembly type materials are researched and modified, a modified bonding composite material meeting the actual construction requirement is provided, and the modified bonding composite material is applied to splicing seams of the assembly type building, so that the assembly type building has good waterproof and bonding performances.
For example, CN101407387B discloses a second-order reactive waterproof adhesive material, which is prepared by stirring and reacting 0.2-1.8 parts of styrene-butadiene rubber, 2.75-4.25 parts of styrene-butadiene-styrene triblock copolymer, 13.75-15.45 parts of coumarone resin, 22.6-25.6 parts of No. 70 matrix asphalt, 17.85-21.3 parts of xylene and 23-27 parts of butyl acetate at high temperature. The scheme contains materials such as asphalt and rubber, high-temperature reaction stirring is needed during preparation, construction difficulty is increased, and meanwhile, the bonding property of the asphalt and rubber is to be improved.
On the other hand, industrial waste is expected to be used in the construction field in many cases, but when used in a waterproof adhesive material, the adhesive material has problems of poor adhesive properties, thermal stability, toughness and mechanical properties due to low active material content, difficulty in forming a structural network after bonding, and high thermal expansion coefficient.
The boron nitride nanotube consists of B and N atoms in sp2The tubular structure formed by hybridization bonding has excellent electrical property, magnetic property, mechanical property and thermal stability, is a new material, is reported to be used for manufacturing various products such as displays, microscopes, cutter molds and the like, is usually used for manufacturing energy-saving bricks by utilizing the thermal stability when being used for building materials, and has no report for preparing bonded composite materials.
Disclosure of Invention
The invention aims to solve the technical problems and provides a preparation method of a boron nitride nanotube modified bonding composite material, which has the advantages of simple method, low production cost, high bonding strength, high temperature resistance and good water resistance.
The technical scheme comprises the following components, by weight, 100 parts of portland cement, 5-50 parts of superfine slag powder, 5-20 parts of denitration fly ash, 10-30 parts of steel slag coarse powder, 15-20 parts of water, 10-15 parts of surface-modified boron nitride nanotubes, 3-10 parts of polymer emulsion, 0.6-1.0 part of cellulose ether, 0.05-0.16 part of defoaming agent and 0.2-0.8 part of hyper-dispersant;
putting the components into a stirrer, and uniformly stirring at a high speed to obtain a bonding composite material;
the surface modified boron nitride nanotube is prepared by the following method:
placing the boron nitride nanotube into PBS buffer solution with the PH of 7-8, adding dopamine accounting for 3-8% of the mass of the boron nitride nanotube, reacting for 30-60 minutes, adding diluted hydrochloric acid to stop, and then filtering and drying to obtain the surface modified boron nitride nanotube.
The boron nitride nanotubes are mechanically ground to a length of 50-150nm and then placed in PBS buffer.
Aiming at the problems in the background art, the inventor uses a large amount of industrial waste materials, such as superfine slag powder, denitration fly ash and steel slag coarse powder, the highest addition amount of the total of the three materials can be equivalent to that of portland cement, the production cost is greatly reduced, the doping of the superfine slag powder has the effect of improving the durability of the composite material, the denitration fly ash has a certain water reducing effect, the fluidity of the composite material can be improved after the doping, the steel slag coarse powder has the effect of accelerating the early hydration speed, but the negative effect of lower early strength can be brought by the addition of the three materials, in order to solve the problems, the inventor considers that the introduction of the boron nitride nanotube plays the role of reinforcing and toughening, and other characteristics of the boron nitride nanotube can be effectively utilized, but if the boron nitride nanotube is directly added into the components, the problem of combination with inorganic materials can exist due to surface inertia, therefore, the inventor considers the surface modification of the boron nitride nanotube, the selection of the modifier is very important, common coupling agents such as silane coupling agents only have the dispersion effect, so the compatibility and the dispersibility with components such as slag, steel slag and the like are limited, based on the fact that the inventor conducts intensive research on various existing surface modifiers, dopamine is used as the surface modifier, and in the invention, the modification of the boron nitride nanotube by selecting the dopamine considers the chemical bond effect formed by the dopamine and the boron nitride, and then the good bonding effect is formed between the dopamine and inorganic materials, so the combination between the boron nitride and the inorganic materials is greatly enhanced, the problem of insufficient interface combination between the boron nitride and the inorganic materials is solved, and unexpected technical effects are generated. The reaction time is controlled to be 30-60 minutes, and then dilute hydrochloric acid is added to stop the reaction.
Further, the boron nitride nanotubes are preferably ground to a length of 50-150nm, and if the length is too long, the boron nitride nanotubes are not easy to modify and have a limited reinforcing effect on a system, and if the length is too short, the boron nitride nanotubes can be agglomerated, so that the reinforcing effect of the boron nitride nanotubes in inorganic materials is influenced.
The superfine slag powder is preferably granulated blast furnace slag powder with the particle size of 5-20 mu m and the Bosch specific surface area of 500-800m2Kg, mass coefficient of 1.7-2.1; the denitration fly ash is preferably waste for denitration of power plant flue gas, and the nitrogen content of the denitration fly ash is<1% of carbon content<1 percent. The steel slag coarse powder is preferably powder with the grain diameter of 16-25 mu m obtained by coarsely grinding steel slag particles;
the polymer emulsion has the functions that the emulsion forms a colloidal system in a material medium, the stability of the material is improved, the polyacrylate emulsion is preferably used, the addition amount is controlled to be 3-10 parts, too much flocculating particles are not easy to generate in the system, and too little flocculating particles are not easy to generate in the system; the cellulose ether has the function of ensuring that the composite material has water retention, preferably hydroxypropyl methyl cellulose ether, and the addition amount is controlled to be 0.6-1.0 part, so that the condensation time of the composite material is longer if the addition amount is too large, and the water retention is poor if the addition amount is too small; the defoaming agent is preferably a silicone defoaming agent; the hyperdispersant is preferably a polyhydroxy acid based hyperdispersant.
Has the advantages that:
the invention has simple process, low production cost, excellent waterproof performance, high bonding strength and high temperature resistance, can be used for a long time at the temperature of between 40 ℃ below zero and 300 ℃, and is particularly suitable for the waterproofing and bonding of the splicing seams of the fabricated building.
Detailed Description
Surface modified boron nitride nanotubes example 1:
and (2) placing the boron nitride nanotube into a PBS (phosphate buffer solution) with the pH of 7-8, adding dopamine accounting for 3% of the mass of the boron nitride nanotube, reacting for 30 minutes, adding diluted hydrochloric acid to terminate, and filtering and drying to obtain the surface-modified boron nitride nanotube 1.
Surface modified boron nitride nanotubes example 2:
and (2) placing the boron nitride nanotube into a PBS (phosphate buffer solution) with the pH of 7-8, adding dopamine accounting for 4% of the mass of the boron nitride nanotube, reacting for 40 minutes, adding diluted hydrochloric acid to terminate, and filtering and drying to obtain the surface-modified boron nitride nanotube 2.
Surface modified boron nitride nanotubes example 3:
and (2) placing the boron nitride nanotube into a PBS (phosphate buffer solution) with the pH of 7-8, adding dopamine accounting for 5% of the mass of the boron nitride nanotube, reacting for 45 minutes, adding diluted hydrochloric acid to terminate, and filtering and drying to obtain the surface-modified boron nitride nanotube 3.
Surface modified boron nitride nanotubes example 4:
and (2) placing the boron nitride nanotube into a PBS (phosphate buffer solution) with the pH of 7-8, adding dopamine accounting for 6% of the mass of the boron nitride nanotube, reacting for 50 minutes, adding diluted hydrochloric acid to terminate, and filtering and drying to obtain the surface-modified boron nitride nanotube 4.
Surface modified boron nitride nanotubes example 5:
and (2) placing the boron nitride nanotube into a PBS (phosphate buffer solution) with the pH of 7-8, adding dopamine accounting for 7% of the mass of the boron nitride nanotube, reacting for 55 minutes, adding diluted hydrochloric acid to terminate, and filtering and drying to obtain the surface-modified boron nitride nanotube 5.
Surface modified boron nitride nanotubes example 6:
and (2) placing the boron nitride nanotube into a PBS (phosphate buffer solution) with the pH of 7-8, adding dopamine accounting for 8% of the mass of the boron nitride nanotube, reacting for 60 minutes, adding diluted hydrochloric acid to terminate, and filtering and drying to obtain the surface-modified boron nitride nanotube 6.
Surface-modified boron nitride nanotubes comparative example 1:
the surface-modified boron nitride nanotubes 7 were obtained in the same manner as in example 1, except that dopamine was replaced with a silane coupling agent.
Bonded composite example 1:
100 parts of 52.5-grade ordinary portland cement, 15 parts of denitration fly ash, 50 parts of superfine slag powder, 20 parts of steel slag coarse powder, 16 parts of water, 3 parts of polymer emulsion, 0.8 part of hydroxypropyl cellulose ether, 0.1 part of defoaming agent, 0.5 part of early-strength type polyhydroxy acid hyper-dispersant and the surface-modified boron nitride nanotube 1 are put into a stirrer together and uniformly stirred at high speed to obtain the bonding composite material 1.
Bonded composite example 2:
100 parts of 42.5-grade ordinary portland cement, 15 parts of denitration fly ash, 40 parts of superfine slag powder, 20 parts of steel slag coarse powder, 16 parts of water, 5 parts of polymer emulsion, 0.8 part of hydroxypropyl cellulose ether, 0.1 part of defoaming agent, 0.5 part of early-strength type polyhydroxy acid hyper-dispersant and the surface-modified boron nitride nanotube 2 are put into a stirrer together and uniformly stirred at a high speed to obtain the bonding composite material 2.
Bonded composite example 3:
100 parts of 52.5-grade ordinary portland cement, 15 parts of denitration fly ash, 30 parts of superfine slag powder, 20 parts of steel slag coarse powder, 16 parts of water, 6 parts of polymer emulsion, 0.8 part of hydroxypropyl cellulose ether, 0.1 part of defoaming agent, 0.5 part of early-strength type polyhydroxy acid hyper-dispersant and the surface-modified boron nitride nanotube 3 are put into a stirrer together and uniformly stirred at high speed to obtain the bonding composite material 3.
Bonded composite example 4:
100 parts of 52.5-grade ordinary portland cement, 15 parts of denitration fly ash, 20 parts of superfine slag powder, 20 parts of steel slag coarse powder, 16 parts of water, 7 parts of polymer emulsion, 0.8 part of hydroxypropyl cellulose ether, 0.1 part of defoaming agent, 0.5 part of early-strength type polyhydroxy acid hyper-dispersant and the surface-modified boron nitride nanotube 4 are put into a stirrer together and uniformly stirred at a high speed to obtain the bonding composite material 4.
Bonded composite example 5:
100 parts of 52.5-grade ordinary portland cement, 15 parts of denitration fly ash, 10 parts of superfine slag powder, 20 parts of steel slag coarse powder, 16 parts of water, 8 parts of polymer emulsion, 0.8 part of hydroxypropyl cellulose ether, 0.1 part of defoaming agent, 0.5 part of early-strength type polyhydroxy acid hyper-dispersant and the surface-modified boron nitride nanotube 5 are put into a stirrer together and uniformly stirred at a high speed to obtain the bonding composite material 5.
Bonded composite example 6:
100 parts of 52.5-grade ordinary portland cement, 15 parts of denitration fly ash, 5 parts of superfine slag powder, 20 parts of steel slag coarse powder, 16 parts of water, 10 parts of composite polymer emulsion, 0.8 part of hydroxypropyl cellulose ether, 0.1 part of defoaming agent, 0.5 part of early-strength polycarboxylic acid hyper-dispersant and the surface-modified boron nitride nanotube 6 are put into a stirrer together and uniformly stirred at high speed to obtain the bonding composite material 6.
Bonded composite comparative example 1:
a comparative bonded composite 1 was obtained as in example 1, except that the surface-modified boron nitride nanotubes 1 were replaced with unmodified boron nitride nanotubes.
Comparative bonded composite example 2
A comparative bonded composite 2 was obtained as in example 1, except that the surface-modified boron nitride nanotubes 1 were replaced with surface-modified boron nitride nanotubes 7.
Comparative bonded composite example 3
A comparative bonded composite 3 was obtained as in example 1, except that the surface-modified boron nitride nanotubes 1 were not added.
Performance data for bonded composites 1-6 and comparative bonded composites 1-3
Figure GDA0002830866200000071
Figure GDA0002830866200000072
And (3) knotting: from the examples and comparative examples, it can be concluded that the composite material doped with dopamine-modified boron nitride nanotubes has good performance, and the softening coefficient (water resistance), bonding strength, permeability and thermal deformation (high temperature resistance) of the composite material all show excellent effects, and meet the performance requirements of the material. The three comparative examples were poor in overall performance, and had respective performance reductions in softening coefficient (water resistance), adhesive strength, permeability, and heat distortion (high temperature resistance) to different degrees.

Claims (5)

1. The preparation method of the boron nitride nanotube modified bonding composite material is characterized by comprising the following components, by weight, 100 parts of portland cement, 5-50 parts of superfine slag powder, 5-20 parts of denitration fly ash, 10-30 parts of steel slag coarse powder, 15-20 parts of water, 10-15 parts of surface-modified boron nitride nanotubes, 3-10 parts of polymer emulsion, 0.6-1.0 part of cellulose ether, 0.05-0.16 part of defoaming agent and 0.2-0.8 part of hyper-dispersant;
putting the components into a stirrer, and uniformly stirring at a high speed to obtain a bonding composite material;
the surface modified boron nitride nanotube is prepared by the following method:
and (2) mechanically grinding the boron nitride nanotube until the length is 50-150nm, placing the boron nitride nanotube into PBS (phosphate buffer solution) with the pH of 7-8, adding dopamine accounting for 3-8% of the mass of the boron nitride nanotube, reacting for 30-60 minutes, adding diluted hydrochloric acid to stop reaction, and filtering and drying to obtain the surface modified boron nitride nanotube.
2. The method for preparing boron nitride nanotube modified cementitious composite as claimed in claim 1, wherein the ultrafine slag powder is granulated blast furnace slag powder with a particle size of 5-20 μm and a Bosch's specific surface area of 500-800m2Kg, mass coefficient of 1.7-2.1.
3. The method for preparing the boron nitride nanotube modified cementitious composite of claim 1, wherein the denitration fly ash is a waste of flue gas denitration of a power plant, and has a nitrogen content of <1% and a carbon content of < 1%.
4. The method of claim 1, wherein the steel slag coarse powder is a powder with a particle size of 16-25 μm obtained by coarse grinding of steel slag particles.
5. The method of preparing a boron nitride nanotube modified cementitious composite of claim 1, wherein the polymer emulsion is an acrylic polymer emulsion; the cellulose ether is hydroxypropyl methyl cellulose ether; the defoaming agent is an organic silicon defoaming agent; the hyper-dispersant is a polyhydroxy acid-based hyper-dispersant.
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