阅读说明：本技术 一种高硬度防滑混凝土地坪硬化剂的制备及使用方法 (Preparation and use method of high-hardness anti-skid concrete floor hardening agent ) 是由 吴春春 李跃 张继 杨辉 于 2020-12-14 设计创作，主要内容包括：本发明涉及混凝土地坪技术,旨在提供一种高硬度防滑混凝土地坪硬化剂的制备及使用方法。包括：向乙醇中加入四氯化硅、去离子水,持续搅拌后冷凝回流；向纳米级氧化硅溶胶中加入中空二氧化硅微球,搅拌均匀后超声分散；将两混合物掺混后搅拌、陈化；再与异丙醇混合均匀,得到地坪硬化剂组分；在使用前加入作为硬化促进剂的二月桂酸二丁基锡,搅拌后得到高硬度防滑混凝土地坪硬化剂。本发明能够提高地坪在积水状态下的湿摩擦系数,达到防滑的效果。与使用常规工艺制备的基于硅醇盐水解预聚的纳米地坪硬化剂的成品地坪相比,使用本发明产品的地坪,保持光泽度不变,但湿摩擦系数大幅提高。(The invention relates to a concrete floor technology, and aims to provide a preparation and use method of a high-hardness anti-slip concrete floor hardening agent. The method comprises the following steps: adding silicon tetrachloride and deionized water into ethanol, continuously stirring, and condensing and refluxing; adding hollow silica microspheres into the nano-scale silica sol, stirring uniformly and then performing ultrasonic dispersion; mixing the two mixtures, stirring and aging; then evenly mixing the mixture with isopropanol to obtain a terrace hardener component; adding dibutyltin dilaurate serving as a hardening accelerator before use, and stirring to obtain the high-hardness anti-skid concrete floor hardening agent. The invention can improve the wet friction coefficient of the terrace in the ponding state and achieve the antiskid effect. Compared with the finished terrace of the nano terrace hardener prepared by the conventional process and based on silicon alkoxide hydrolysis prepolymerization, the terrace prepared by the invention keeps the glossiness unchanged, but greatly improves the wet friction coefficient.)

1. The preparation method of the high-hardness antiskid concrete floor hardening agent is characterized by comprising the following steps:

(1) adding 40-50 parts by mass of silicon tetrachloride into 20 parts by mass of ethanol under the stirring conditions of 0 ℃ and 400rpm, and continuously stirring for 10 min; then adding 5-10 parts by mass of deionized water, continuously stirring for 8 hours after the addition is finished, and then condensing and refluxing for 12 hours at 60 ℃;

(2) under the condition of stirring, adding 5-10 parts of hollow silicon dioxide microspheres into 40-60 parts by mass of nano-scale silica sol, uniformly stirring, and ultrasonically dispersing for 30 min;

(3) adding 50 parts by mass of the mixed solution obtained in the step (2) into the mixture obtained in the step (1) under stirring; stirring for 30min, and aging at 25 deg.C for 2 days;

(4) uniformly mixing the aged composite sol with 10 parts by mass of isopropanol to obtain a component A of the floor hardening agent;

(5) before the floor hardening agent is used in a floor construction site, dibutyltin dilaurate serving as a hardening accelerator B component is added into a floor hardening agent A component, and the mass ratio of dibutyltin dilaurate to the floor hardening agent A component is 3 per mill; stirring for 30min to obtain the high-hardness antiskid concrete floor hardening agent.

2. The method according to claim 1, wherein the stirring speed in the step (2) is 100-200 r/min.

3. The method as claimed in claim 1, wherein the silica sol of step (2) has a solid content of 20%, the particle size of the sol particles is 3-5 nm, and the solvent used in the sol is propylene glycol methyl ether.

4. The method according to claim 1, wherein the hollow silica microspheres in the step (2) have a particle size of 100 to 200 nm; micropores are densely distributed on the shell structure of the hollow silica microspheres, and the pore diameter of each micropore is 2-10 nm.

5. The use method of the high-hardness antiskid terrace hardener prepared by the method in claim 1 is characterized by comprising the following steps:

(1) polishing a self-leveling cement floor with the concrete strength grade of C20 or C30 by using a 200-mesh polishing sheet, pouring the high-hardness moisture-proof floor hardening agent on the surface of the floor according to the using amount of 1 kilogram per square meter, and uniformly coating the high-hardness moisture-proof floor hardening agent;

(2) covering the terrace surface with a plastic film, standing for 2 hours, and then uncovering; after naturally drying for 8 hours, polishing the floor for 2 times by using a 200-300-mesh polishing sheet, polishing the floor for 1 time by using a 500-600-mesh polishing sheet, and polishing the floor for 1 time by using a 1000-mesh polishing sheet.

Technical Field

The invention relates to a concrete floor technology, in particular to a preparation and application method of a high-hardness anti-slip floor hardening agent.

Background

Terrace is hardThe curing agent is a siloxane oligomer solution which penetrates into concrete and reacts with active hydroxyl in the concrete to form an integrated structure, so that the effect of reinforcing and compacting the concrete is achieved. Because of its high hardness and high wear resistance, it is widely used, and various concrete floor hardeners are also appeared. For example, according to the preparation method of the permeation type self-leveling cement antistatic wear-resistant floor coating disclosed in the Chinese patent application CN201610826985.2, the antistatic property of the floor is improved by adding a conductive material. Chinese patent CN201511024168.7Al₂O₃The sol type wear-resistant concrete sealing hardener has the advantages that silane coupling agent and wax powder are added into the sealant to compact pores in concrete and improve the surface glossiness and hydrophobic property of the concrete.

With the development of economy and the improvement of the living standard of people, the requirements of people on high-quality large-scale terraces are higher and higher. The floor is very important for the terrace in the public place, not only needs to be wear-resistant and dustproof, but also has anti-skid performance, and is an important means for avoiding accidents caused by falling down due to wet skid. Particularly in rainy areas such as the middle and lower reaches of Yangtze river, the terrace surface is often in a wet and slippery ponding state, which is easy to cause safety accidents.

The existing terrace technology usually adopts a nano terrace hardener based on silicon alkoxide hydrolysis prepolymerization, has the advantages of high hardness, chemical pollution resistance, good durability and the like, and can be applied to the surfaces of various terraces such as concrete, cement and the like. After the hardening accelerator is added, a hardening layer is formed on the surface of the concrete or cement in a penetration mode, so that the hardening and dust removal effects of the cement are achieved. Is a novel high-performance terrace material. But after the terrace is finely polished, the surface roughness is greatly reduced, and in addition, the concrete surface is densified through a terrace curing agent, so that the friction coefficient is easily reduced in a water accumulation state.

Different from the current floor hardening agent, the invention adopts silica sol and hollow silica microspheres as raw materials to prepare the floor hardening agent, and increases the anti-skid performance of the floor by combining micro-nano structures.

Disclosure of Invention

The invention aims to solve the technical problem of overcoming the defects in the prior art and provides a preparation and use method of a high-hardness antiskid concrete floor hardening agent.

In order to solve the technical problem, the solution of the invention is as follows:

the preparation method of the high-hardness antiskid concrete floor hardening agent comprises the following steps:

(1) adding 40-50 parts by mass of silicon tetrachloride into 20 parts by mass of ethanol under the stirring conditions of 0 ℃ and 400rpm, and continuously stirring for 10 min; then adding 5-10 parts by mass of deionized water, continuously stirring for 8 hours after the addition is finished, and then condensing and refluxing for 12 hours at 60 ℃;

(2) under the condition of stirring, adding 5-10 parts of hollow silicon dioxide microspheres into 40-60 parts by mass of nano-scale silica sol, uniformly stirring, and ultrasonically dispersing for 30 min;

(3) adding 50 parts by mass of the mixed solution obtained in the step (2) into the mixture obtained in the step (1) under stirring; stirring for 30min, and aging at 25 deg.C for 2 days;

(4) uniformly mixing the aged composite sol with 10 parts by mass of isopropanol to obtain a component A of the floor hardening agent;

(5) before the floor hardening agent is used in a floor construction site, dibutyltin dilaurate serving as a hardening accelerator B component is added into a floor hardening agent A component, and the mass ratio of dibutyltin dilaurate to the floor hardening agent A component is 3 per mill; stirring for 30min to obtain the high-hardness antiskid concrete floor hardening agent.

In the invention, the stirring speed in the step (2) is 100-200 r/min.

In the invention, the solid content of the silica sol in the step (2) is 20%, the particle size of the sol particles is 3-5 nm, and the solvent used by the sol is propylene glycol methyl ether.

In the invention, the particle size of the hollow silica microspheres in the step (2) is 100-200 nm; micropores are densely distributed on the shell structure of the hollow silica microspheres, and the pore diameter of each micropore is 2-10 nm.

The invention further provides a use method of the high-hardness anti-slip terrace hardening agent prepared by the method, which comprises the following steps:

(1) polishing a self-leveling cement floor with the concrete strength grade of C20 or C30 by using a 200-mesh polishing sheet, pouring the high-hardness moisture-proof floor hardening agent on the surface of the floor according to the using amount of 1 kilogram per square meter, and uniformly coating the high-hardness moisture-proof floor hardening agent;

(2) covering the terrace surface with a plastic film, standing for 2 hours, and then uncovering; after naturally drying for 8 hours, polishing the floor for 2 times by using a 200-300-mesh polishing sheet, polishing the floor for 1 time by using a 500-600-mesh polishing sheet, and polishing the floor for 1 time by using a 1000-mesh polishing sheet.

Description of the inventive principles:

according to the invention, a micro-nano structure is formed by the hollow silica microspheres with moderate sizes and the silica nanoparticles in the silica sol, so that the roughness of the microstructure of the terrace can be improved without reducing the macroscopic flatness (the surface glossiness is unchanged) of the terrace. And due to the fact that the diameter size of the hollow silica microspheres is 100-200 nm, the micro roughness can be improved under the condition that the macro flatness is not reduced due to fine polishing. On the other hand, the hollow silica microspheres on the floor surface have a good effect on absorbing moisture, and can play a good anti-skidding effect.

Compared with the prior art, the invention has the technical effects that:

1. according to the invention, hollow silica microspheres are used as a microstructure regulator, and form a micro-nano structure with nano silica particles in silica sol; the wet friction coefficient of the terrace in the ponding state can be improved, and the anti-skidding effect is achieved.

2. After the hardening accelerator product is applied, the lubricating effect brought by water in water accumulation can be reduced on the premise that the surface macroscopic flatness of the floor surface is kept unchanged (the glossiness of the floor surface is not reduced) even if the floor surface is subjected to fine polishing. Compared with the finished terrace of the nano terrace hardener prepared by the conventional process and based on silicon alkoxide hydrolysis prepolymerization, the glossiness of the terrace is unchanged, but the wet friction coefficient is greatly improved.

Drawings

FIG. 1 is a scanning electron micrograph of hollow silica microspheres;

FIG. 2 is a graph showing the distribution of hollow silica microspheres and pore sizes.

Detailed Description

In the invention, the nano silica sol and the hardening accelerator are all commercial products. For example, the nano silica sol in the following examples is prepared from GL-006 of Jinhuageling functional coating materials research institute, Inc.; the solid content of the silica sol is 20%, the particle size of sol particles is 3-5 nm, and the solvent used by the sol is propylene glycol methyl ether. The hollow silica microspheres are self-made, the preparation method refers to the record of the publication of 'preparation of slow-release self-repairing microspheres and application thereof in coating' (a zeitan master article, 2020-P39), and the morphology and pore size distribution are shown in figures 1 and 2. The particle size of the hollow silicon dioxide microspheres is 100-200 nm; micropores are densely distributed on the shell structure of the hollow silica microspheres, and the pore diameter of each micropore is 2-10 nm. The hardening accelerator is dibutyltin dilaurate, and the mass content is 95%.

The invention is further described below by way of examples.

Example 1

(1) Adding 40 parts by mass of silicon tetrachloride into 20 parts by mass of ethanol under the stirring conditions of 0 ℃ and 400rpm, and continuously stirring for 10 min; then adding 10 parts by mass of deionized water, continuously stirring for 8 hours after the addition is finished, and then condensing and refluxing for 12 hours at 60 ℃;

(2) and adding 10 parts of hollow silica microspheres into 40 parts by mass of silica sol at a speed of 200r/min under the stirring condition, uniformly stirring, and performing ultrasonic dispersion for 30 min.

(3) Adding 50 parts by mass of the mixed solution obtained in the step (2) into the mixture obtained in the step (1) under stirring; stirring for 30min, and aging at 25 deg.C for 2 days;

(4) and uniformly mixing the aged composite sol and 10 parts by mass of isopropanol to obtain a component A of the floor hardening agent.

(5) Before use, adding dibutyltin dilaurate accounting for 3 per mill of the mass ratio of the component A into the component A of the floor hardening agent, and stirring for 30min to finally obtain the high-hardness antiskid concrete floor hardening agent.

The use method of the high-hardness anti-slip terrace hardener obtained by the invention comprises the following steps:

the self-leveling cement floor with the concrete strength grade of C20 or C30 is polished to be smooth by a 200-mesh polishing sheet, and the high-hardness moisture-proof floor hardening agent is poured on the surface of the floor according to the using amount of 1 kilogram per square meter and is uniformly coated. Covering the terrace with a plastic film, standing for 2 hours, and then uncovering the plastic film; after naturally drying for 8 hours, the floor is polished for 2 times by using the 200-300-mesh polishing sheet, then the floor is polished for 1 time by using the 500-600-mesh polishing sheet, and then the floor is polished for 1 time by using the 1000-mesh polishing sheet.

Example 2

(1) Adding 50 parts by mass of silicon tetrachloride into 20 parts by mass of ethanol under the stirring conditions of 0 ℃ and 400rpm, and continuously stirring for 10 min; then adding 5 parts by mass of deionized water, continuously stirring for 8 hours after the addition is finished, and then condensing and refluxing for 12 hours at 60 ℃;

(2) under the stirring condition of 100r/min, 5 parts of hollow silica microspheres are added into 60 parts by mass of silica sol, and the mixture is ultrasonically dispersed for 30min after being uniformly stirred.

(3) Adding 50 parts by mass of the mixed solution obtained in the step (2) into the mixture obtained in the step (1) under stirring; stirring for 30min, and aging at 25 deg.C for 2 days;

(4) and uniformly mixing the aged composite sol and 10 parts by mass of isopropanol to obtain a component A of the floor hardening agent.

(5) Before use, adding dibutyltin dilaurate accounting for 3 per mill of the mass ratio of the component A into the component A of the floor hardening agent, and stirring for 30min to finally obtain the high-hardness antiskid concrete floor hardening agent.

The method of using the obtained high hardness antiskid floor hardener is as in example 1.

Example 3

(1) Adding 48 parts by mass of silicon tetrachloride into 20 parts by mass of ethanol under the stirring conditions of 0 ℃ and 400rpm, and continuously stirring for 10 min; then adding 7.5 parts by mass of deionized water, continuously stirring for 8 hours after the addition is finished, and then condensing and refluxing for 12 hours at 60 ℃;

(2) adding 7 parts of hollow silica microspheres into 50 parts by mass of silica sol under the stirring condition of 150r/min, and performing ultrasonic dispersion for 30min after uniform stirring.

(3) Adding 50 parts by mass of the mixed solution obtained in the step (2) into the mixture obtained in the step (1) under stirring; stirring for 30min, and aging at 25 deg.C for 2 days;

(4) and uniformly mixing the aged composite sol and 10 parts by mass of isopropanol to obtain a component A of the floor hardening agent.

(5) Before use, adding dibutyltin dilaurate accounting for 3 per mill of the mass ratio of the component A into the component A of the floor hardening agent, and stirring for 30min to finally obtain the high-hardness antiskid concrete floor hardening agent.

The method of using the obtained high hardness antiskid floor hardener is as in example 1.

Comparative example 1

(1) Adding 40 parts by mass of silicon tetrachloride into 20 parts by mass of ethanol under the stirring conditions of 0 ℃ and 400rpm, and continuously stirring for 10 min; then adding 10 parts by mass of deionized water, continuously stirring for 8 hours after the addition is finished, and then condensing and refluxing for 12 hours at 60 ℃;

(2) adding 50 parts by mass of silica sol to the mixture obtained in the step (1) under stirring to obtain a mixed solution; stirring for 30min, and aging at 25 deg.C for 2 days;

(3) and uniformly mixing the aged composite sol with 10 parts by mass of isopropanol to obtain a terrace hardener component, wherein the component is similar to a nano terrace hardener prepared by a conventional process and based on silicon alkoxide hydrolysis prepolymerization.

(4) Before use, dibutyltin dilaurate accounting for 3 per mill of the mass ratio of the concrete floor hardener is added into the floor hardener, and the mixture is stirred for 30min to finally obtain the concrete floor hardener.

Referring to the use method of example 1, the product was used for floor surface construction.

Table 1 shows a comparison of the properties of the hardened concrete blocks of the different examples, the contact angles of the samples being measured by a contact angle measuring instrument.

TABLE 1

Sample (I)	Example 1	Example 2	Example 3	Comparative example 1
					Coefficient of wet friction	0.73	0.75	0.70	0.40
Mohs hardness	7	7	8	7

Wherein, the wet friction coefficient of the concrete sample block is tested according to the method specified by the national standard GB/T4100-2015, and the Mohs hardness is tested according to the method specified by EN 101: 1991. As can be seen from the data in the table, in the range of the test requirements, compared with the sample (comparative example 1) without adding the hollow silica microspheres, the wet friction coefficient of the terrace sample prepared by the invention is obviously improved (both are more than 0.7), while the comparison sample block only reaches 0.4.