TWI417267B - Self-leveling composition - Google Patents

Description

Self-leveling composition

The present invention relates to a self-leveling composition for use as a floor lining or the like.

The self-leveling material (SL material) can be widely used as a floor lining because it can be naturally flowed to form a horizontal surface and hardened by being mixed with water into the floor. At present, gypsum systems, cement systems, and the like are widely used in SL materials. As a prior art document relating to the above SL material, the following documents exist.

Patent Document 1 discloses a self-leveling composition whose essential components are: cement and/or gypsum, fine aggregate, water reducing agent (fluidizing agent or dispersing agent), disintegrating agent, retarding agent, quick setting agent, In the 14th revision, the water-soluble cellulose ether and water having a sieve residue of 100% (mesh of 150 μm) having a sieve residue of 5% by weight or less disclosed in Japanese Pharmacopoeia B1061. However, in order to prevent the separation of the aggregate of the self-leveling composition, it is necessary to improve the viscosity, and there is a problem that the fluidity of the slurry is lowered and the workability is poor. Further, when the flow thickness is 5 mm, it is easily affected by the unevenness of the floor lining, and the surface smoothness of the formed horizontal surface is poor, and when the flow thickness is about 50 mm, there is a risk of sedimentation of the aggregate. Therefore, the self-leveling composition is less desirable.

Moreover, when the aggregate is not added to the self-leveling material, there is a flow loss (flow value decreases with time) due to hydration and agglomeration of the reactant (cement or gypsum, etc.), and the formation level cannot be sufficiently obtained. The working time of the foundation surface question.

[Patent Document 1] Japanese Patent Laid-Open Publication No. 2006-56763

Accordingly, it is an object of the present invention to provide a self-leveling composition which is excellent in service life when formed into a horizontal plane, excellent in fluidity and surface smoothness (nearly wrinkles or cracks), and which can form a horizontal surface having a high surface strength.

The inventors of the present invention conducted active research to achieve the above object, and as a result, it was found that by adding a cellulose ether containing a highly viscous person and a low viscosity to a specific self-leveling composition, it is possible to obtain a long life and flow when forming a horizontal plane. The present invention is completed by a self-leveling composition excellent in properties and surface smoothness and capable of forming a horizontal surface having a high surface hardness.

That is, the present invention provides a self-leveling composition characterized in that it is attached to a self-leveling composition containing gypsum as a main material and containing no aggregate, and a high-viscosity cellulose ether and a low-viscosity cellulose are added. Made of ether. Preferably, the self-leveling composition further comprises a chelating agent. By including a chelating agent, it can be a self-leveling composition which forms a horizontal surface in which surface smoothness is further improved.

According to the present invention, there can be provided a self-leveling composition which is obtained by adding a highly viscous cellulose ether and a low-viscosity cellulose ether to a self-leveling composition of a gypsum-free main material. Excellent fluidity in the formation of a horizontal plane, long service life, excellent surface smoothness in the formed horizontal plane, and high formation in the resulting horizontal plane Surface hardness. Further, it is possible to provide a self-leveling composition which can prevent cracks on the surface by further adding a chelating agent, and can form a horizontal surface in which surface smoothness is further improved.

Next, the present invention will be described in more detail.

In the self-leveling composition of the present invention, powdered gypsum can be used as a main material. As the gypsum, α-type calcined gypsum, type II anhydrite, and β-type calcined gypsum can be exemplified.

The self-leveling composition of the present invention does not contain an aggregate. If the self-leveling composition contains aggregates, in order to prevent the precipitation of the aggregate, the slurry must have a certain fixed value or more. If the water is mixed into the self-leveling composition when the floor level is formed, the obtained slurry is obtained. The fluidity of the material is reduced. Therefore, especially when the flow thickness is 5 mm or less, the slurry is easily affected by the unevenness of the bottom layer of the floor, and the surface smoothness is deteriorated. Further, when the flow thickness is about 50 mm, there is also precipitation of the aggregate. Danger.

At least two kinds of cellulose ethers may be added to the self-leveling composition of the present invention. Specific examples of the cellulose ether include methylcellulose, hydroxypropylmethylcellulose, hydroxyethylmethylcellulose, hydroxyethylcellulose, hydroxypropylcellulose, and hydroxyethylethylcellulose. Prime.

Among the above cellulose ethers, those having high viscosity and low viscosity are used, and in the present invention, a highly viscous cellulose ether and a low-viscosity cellulose ether are used in combination. Preferably, when a 2% by weight aqueous solution is prepared, the high viscosity cellulose ether has a temperature of 40,000 to 100,000 mPa when measured by a cloth viscometer at 20 ° C and 20 rpm. s viscosity. Further, when expressed by molecular weight, it has a weight average molecular weight (mole molecular weight) of from 5 × 10 ⁵ to 7 × 10 ⁵ (g/mol). On the other hand, when it is preferred to prepare a 2% by weight aqueous solution, the low viscosity cellulose ether has a temperature of 200 to 1,000 mPa when measured by a cloth viscometer at 20 ° C and 20 rpm. s viscosity. Further, when expressed by molecular weight, it has a weight average molecular weight (mole molecular weight) of from 1 × 10 ⁵ to 2 × 10 ⁵ (g/mol).

The total amount (A+B) of the above-mentioned high-viscosity cellulose ether compounding amount (A) and the low-viscosity cellulose ether compounding amount (B) is preferably 0.02 to 0.7 parts by weight. Further, the blending amount (A, B) of the highly viscous cellulose ether and the low-viscosity cellulose ether is preferably 0.01 to 0.6 parts by weight per 100 parts by weight of the gypsum. If the total amount of the highly viscous and low-viscosity cellulose ether is less than 0.02 parts by weight per 100 parts by weight of the gypsum, sufficient material separation resistance cannot be confirmed in the obtained self-leveling composition, and The slurry causes uneven strength of the horizontal plane after hardening of the self-leveling composition. Further, the above-mentioned slurry may sometimes be a cause of weathering or cracking. On the other hand, if the amount used is more than 0.7 parts by weight per 100 parts by weight of gypsum, the viscosity of the slurry is too high, resulting in a lack of fluidity of the slurry, and self-leveling as an important characteristic of the self-leveling composition. Impaired. The above-mentioned excessively high viscosity sometimes causes the wrinkles on the horizontal surface to further impair the appearance or decrease the strength. The ratio of the above-mentioned high-viscosity cellulose ether (A) to the above-mentioned blending amount (B) of the low-viscosity cellulose ether, A:B by weight ratio is preferably 1:0.02 to 1:50, more preferably 1:0.1 to 1:10.

When the self-leveling composition of the present invention forms a floor level, it is preferable to further add a chelating agent in order to reduce the occurrence of a film on the surface or to prevent the occurrence of cracks. Specific examples of the chelating agent include ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, hydroxyethylethylenediaminetriacetic acid, nitrilotriacetic acid, and dihydroxyethylglycine. Among them, preferred is diethylenetriaminepentaacetic acid which can effectively delay the solidification of the aqueous slurry of the self-leveling composition of the present invention.

The amount of the chelating agent is preferably from 0.02 to 0.5 parts by weight per 100 parts by weight of the gypsum. When the compounding amount of the chelating agent is less than 0.02 parts by weight, the effect of preventing the formation of the surface film cannot be sufficiently exhibited. On the other hand, when the amount is more than 0.5 part by weight, since the chelating agent is used in a large amount, the production cost is increased, which is not preferable.

Correspondingly, a cement, a water reducing agent (fluidizing agent or dispersing agent), an antifoaming agent, a retarder, a quick setting agent, an inorganic extender, and a synthetic resin may be appropriately added to the self-leveling composition of the present invention. One type or more.

As the above cement, various Portland cement, early strength Portland cement, medium heat Portland cement, blast furnace cement, cerium oxide cement, lime fly ash cement, alumina cement and control cement can be used. cement. The above-mentioned cement is added to improve the water resistance of the formed floor lining, but the amount thereof is preferably 5 to 50 parts by weight per 100 parts by weight of the gypsum.

As the above water reducing agent (fluidizing agent or dispersing agent), if it is a general marketer, There is no particular limitation on its use. Usually, a water reducing agent such as a polycarboxylic acid type, a melamine type or a naphthalene type can be used. The amount of the water reducing agent is preferably from 0.01 to 5 parts by weight per 100 parts by weight of the gypsum. In the case of a self-leveling composition, since it is necessary to obtain excellent fluidity with as little water as possible, a water reducing agent may be added, but if the amount is too small, the effect cannot be obtained, and if it is too large, sometimes It can cause a slurry or solid-liquid separation, and the strength of the formed horizontal surface is reduced, or weathering occurs.

As the antifoaming agent, a polyether type, a polyoxymethylene type, an alcohol type, a mineral oil type, a vegetable oil type, a nonionic surfactant, or the like can be used.

As the retarder, a citrate such as sodium citrate, a borate such as succinate, acetate, malate or borax, sucrose, hexametaphosphate, ethylenediaminetetraacetate, starch, and protein decomposition can be used. Things and so on. The amount of the retarder is set to the extent that the amount of the retardation function can be exerted. Specifically, it is preferred to add 0.005 to 1 part by weight of retarder per 100 parts by weight of gypsum.

Examples of the quick-setting admixture include a soluble calcium salt such as calcium chloride, calcium nitrite, calcium nitrate, calcium bromide or calcium iodide; a chloride such as ferric chloride or magnesium chloride; and a sulfate such as potassium sulfate; Formate such as potassium oxide, sodium hydroxide, carbonate, thiocarbonate, formic acid and calcium formate. As the inorganic extender, talc, calcium carbonate or the like can be used.

As the above synthetic resin, those which are preferably in the form of a powder may be a vinyl acetate resin, a vinyl versatate resin, a vinyl acetate-vinyl versatate copolymer, an acrylic resin, a vinyl acetate-acrylic acid copolymer, or a vinyl acetate. Ester-tertiary ethylene carbonate An ester-acrylate copolymer, a styrene-butadiene copolymer, or the like. The synthetic resin is added to increase the surface hardness of the formed floor lining, but the amount thereof is preferably 0.05 to 1 part by weight per 100 parts by weight of the gypsum.

The self-leveling composition of the present invention can be uniformly mixed with water, and the resulting slurry is poured into the floor surface of the floor to be spread, placed, hardened, and dried to form a floor lining. As the base surface of the floor, metals such as plaster, cement, wood, plastic tiles or sheets, ceramics, and stainless steel can be exemplified.

The water content is preferably from 20 to 50 parts by weight per 100 parts by weight of the gypsum. If the amount of water is too small, sufficient fluidity may not be obtained, and the obtained slurry may be difficult to spread, and workability may be lowered. On the other hand, if the amount is too large, the strength of the obtained floor lining may be lowered. Therefore, it is less desirable to add water from the above range.

[Examples]

Hereinafter, the examples are given to more specifically describe the present invention, but the present invention is not limited to the examples.

<Use materials>

Gypsum: α-type calcined gypsum

Cement: ordinary Portland cement

Water reducing agent: polycarboxylic acid system

Retarder: sodium citrate (reagent)

Chelating agent: diethylenetriamine pentaacetic acid (DTPA, reagent)

Accelerator: Sulfate (reagent)

Cellulose ether: high viscosity cellulose ether (viscosity 50,000 mPa.s) viscous cellulose ether (viscosity 4,000 mPa.s) low viscosity cellulose ether (viscosity 300 mPa.s)

(The viscosity is based on the measurement method and the values measured under the measurement conditions.)

Defoamer: Polyether

Synthetic resin: vinyl acetate-acrylic acid copolymer

Aggregate: 矽 sand (particle size is 0.05~0.8mm)

[Example 1]

As shown in Table 1, each material was combined and further mixed with a specific amount of cement by adding 0.05 parts by weight of highly viscous cellulose ether and 0.12 parts by weight of low-viscosity cellulose ether per 100 parts by weight of gypsum. A water reducing agent, a retarder, a quick-setting admixture, a synthetic resin, and an antifoaming agent (total of 1.0 to 1.5 parts by weight per 100 parts by weight of gypsum), thereby obtaining a powdery self-leveling composition. Next, as shown in Table 1, 45 parts by weight of water per 100 parts by weight of gypsum was placed in a stirring crucible, and the self-leveling composition obtained in the above step was slowly added while stirring, and the mixture was used. to The test equipment specified in Japanese Industrial Standard JIS R 5201, 8.1, was mixed for 3 minutes to obtain a slurry-like self-leveling composition.

[Embodiment 2]

As shown in Table 1, a self-leveling composition was obtained in the same manner as in Example 1 except that 0.08 part by weight of the chelating agent was further added per 100 parts by weight of gypsum.

[Example 3]

As shown in Table 1, except that the amount of the above-mentioned high-viscosity cellulose ether was 0.1 part by weight and the amount of the low-viscosity cellulose ether was 0.03 part by weight, the same procedure as in Example 1 was obtained. Self-leveling composition.

[Example 4]

As shown in Table 1, except that the amount of the above-mentioned high-viscosity cellulose ether was set to 0.04 part by weight, and the amount of the low-viscosity cellulose ether was set to 0.3 part by weight, the same procedure as in Example 2 was obtained. Self-leveling composition.

[Comparative Example 1]

As shown in Table 2, the same as in Example 1 except that the amount of the above-mentioned high-viscosity cellulose ether was 0.11 part by weight, and no low-viscosity cellulose ether was added. The method obtains a self-leveling composition.

[Comparative Example 2]

As shown in Table 2, except that 0.18 parts by weight of the viscous cellulose ether was added to each 100 parts by weight of gypsum, and no high-viscosity cellulose ether and low-viscosity cellulose ether were added, the same as in Example 1. A self-leveling composition was obtained in the same manner.

[Comparative Example 3]

As shown in Table 2, a self-leveling composition was obtained in the same manner as in Example 1 except that the amount of the above-mentioned low-viscosity cellulose ether was changed to 0.5 part by weight, and no high-viscosity cellulose ether was added.

[Comparative Example 4]

As shown in Table 2, except that 0.08 parts by weight of the viscous cellulose ether was re-added per 100 parts by weight of gypsum, the amount of the above-mentioned high-viscosity cellulose ether was set to 0.03 part by weight, and no low-viscosity fiber was added. A self-leveling composition was obtained in the same manner as in Example 1 except for the ether.

[Comparative Example 5]

As shown in Table 2, except that 0.12 parts by weight of the viscous cellulose ether was re-added per 100 parts by weight of gypsum, the amount of the above-mentioned low-viscosity cellulose ether was set to 0.1. A self-leveling composition was obtained in the same manner as in Example 1 except that the high-viscosity cellulose ether was not added.

[Comparative Example 6]

As shown in Table 2, except that 50 parts by weight of the aggregate was added with respect to 100 parts by weight of gypsum, the amount of the above-mentioned high-viscosity cellulose ether was set to 0.1 part by weight, and the amount of the low-viscosity cellulose ether was adjusted. A self-leveling composition was obtained in the same manner as in Example 1 except that the retarder was set to be 0.09 parts by weight per 100 parts by weight of the gypsum.

The self-leveling compositions obtained in Examples 1 to 4 and Comparative Examples 1 to 6 were evaluated by performing the respective tests shown below. The test results and evaluation criteria (appropriate values) of the self-leveling compositions obtained in Examples 1 to 4 and Comparative Examples 1 to 6 are also shown in Tables 1 and 2, respectively.

[flow value]

The measurement was carried out in accordance with the Japanese Architectural Society's standard specification JASS 15 M-103.

[viscosity]

Using a viscosity measuring instrument Viscotester VT-04 (trade name, manufactured by RION Co., Ltd., shear rate: 4 sec ^-1 ), a specific amount of the slurry was injected into the above-mentioned measuring special cup to measure the viscosity of each slurry.

[flow speed]

The slurry input portion (height 100 mm × length 50 mm × width 100 mm) of an acrylic measuring instrument having a height of 100 mm × a total length of 500 mm × a width of 100 mm placed in a level was placed directly after filling a cup of the slurry. Seven minutes after the start of the introduction, the acrylic plate gate forming one surface of the slurry input portion was instantaneously lifted, and the time until the slurry reached the end portion of the measuring device was measured, and the flow velocity was calculated according to the following formula. Flow speed (mm/s) = slurry moving distance (450mm) / measuring time (s)

[Lifetime]

The service life was measured by the same method as the above-described flow value measurement method according to JASS 15 M-103. A specific amount of each slurry was poured into a vertically standing vinyl chloride tube and placed directly. When the specific time is reached, the tube is lifted, the diffusion of the slurry is stopped, and the diameter in both directions of the slurry which is diffused in the horizontal direction is measured, and the average value is calculated. The time to ensure that the average value is 190 mm or more is set as the service life.

[Surface hardness]

Each slurry was poured into a box-shaped container having a height of 20 mm × a length of 100 mm × a width of 100 mm. After being allowed to stand at room temperature for 48 hours and hardened, the hardened body was placed in a dryer at 40 ° C and dried until it was measured, and then the hardened body was taken out from the dryer, and a rubber hardness meter (manufactured by TECLOCK Co., Ltd.) was used. "TYPE D", trade name) was extruded onto the surface of the hardened body to measure the surface hardness.

[Surface smoothness (surface state: presence or absence of wrinkles or cracks)]

Each slurry was poured into a plastic container having a length of 30 cm × a width of 50 cm until the thickness became 10 mm. After 30 minutes, about 250 cc of the slurry was further poured into the center of the container from the top, and placed directly. After 4 weeks, the surface smoothness of the hardened body was periodically confirmed by touch and vision.

Surface smoothness (wrinkles and cracks) was determined according to the following evaluation criteria.

<pleats>

A: every 1,500 cm ² , there are 0 wrinkles having a width of 0.5 mm or more and a length of 5 mm or more; B: every 1,500 cm ² , there are one wrinkle having a width of 0.5 mm or more and a length of 5 mm or more; C: every 1,500 Cm ² , there are 2 to 5 pleats having a width of 0.5 mm or more and a length of 5 mm or more; D: for every 1,500 cm ² , there are 6 or more pleats having a width of 0.5 mm or more and a length of 5 mm or more; , B is good, C is bad, and D is very bad.

<crack>

A: ^2, the presence of a leak in each 1,500cm 0; B: ^2, the presence of a crack each 1,500cm; C: 1,500cm ^2, the presence of cracks per 2-5; D: each 1,500cm ^2, the presence of six or more cracks The above A is particularly good, B is good, C is bad, and D is very poor.

In the self-leveling compositions of Examples 1 to 4, the evaluation results relating to all of the above test items were excellent or good. That is, as shown in Examples 1 to 4, by adding high-viscosity cellulose ether and low-viscosity cellulose ether to the gypsum without adding the aggregate, the fluidity is excellent and the service life is obtained when the horizontal plane is formed. A self-leveling composition that is long, has excellent surface smoothness, and can form a horizontal surface with a high surface hardness.

Further, the surface smoothness of the self-leveling compositions of Examples 2 and 4 (as evidenced by the absence of cracks) became better than the self-leveling compositions of Examples 1 and 3. That is, the self-leveling compositions of Examples 2 and 4 were more excellent in surface smoothness by the addition of a chelating agent. On the other hand, the self-leveling compositions of Comparative Examples 1 and 2 have a low flow velocity, a short service life, and poor surface smoothness; the surface hardness of the self-leveling composition of Comparative Example 3 is low; and the self-leveling property of Comparative Example 4 The composition has a low flow velocity, a short service life, and poor surface smoothness; the surface smoothness of the self-leveling composition of Comparative Example 5 is poor; the self-leveling composition of Comparative Example 6 has a low flow velocity, a low surface hardness, and a smooth surface. Bad sex.

According to the present invention, it is possible to provide a self-leveling composition which is excellent in service life when formed into a horizontal plane, excellent in fluidity and surface smoothness (nearly wrinkles or cracks), and which can form a horizontal surface having a high surface strength.

Claims (4)

A self-leveling composition characterized in that a high-viscosity cellulose ether and a low-viscosity cellulose ether are added to a self-leveling composition containing gypsum as a main material and no aggregate material, In the case of making a 2% by weight aqueous solution, the high viscosity cellulose ether has a temperature of 40,000 to 100,000 mPa when measured at 20 ° C and 20 rpm using a cloth viscometer. The viscosity of s; in the case of 2% by weight aqueous solution, using a cloth viscometer, measured at 20 ° C, 20 rpm, low viscosity cellulose ether has 200 ~ 1,000 mPa. s viscosity. For example, the self-leveling composition of claim 1 wherein the blending amount of the high-viscosity cellulose ether (A) and the blending amount of the low-viscosity cellulose ether (B) (A+B) are relative to each 100 parts by weight of gypsum is 0.02-0.7 parts by weight, the ratio of the above-mentioned blending amount of the high-viscosity cellulose ether (A) to the above-mentioned blending amount (B) of the low-viscosity cellulose ether is A:B=1:0.02~1 :50. The self-leveling composition according to any one of claims 1 to 3, further comprising a chelating agent, which is ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid, hydroxyethylethylene Amine triacetic acid, nitrilotriacetic acid, or dihydroxyethylglycine. The self-leveling composition of claim 4, wherein the chelating agent is formulated in an amount of from 0.02 to 0.5 parts by weight per 100 parts by weight of the gypsum.