阅读说明：本技术 用于粘贴软石材料的双组分粘接剂及其制备方法 (Bi-component adhesive for adhering soft stone material and preparation method thereof ) 是由 沈思源 潘杨 夏小燕 沈阳 于 2021-11-08 设计创作，主要内容包括：本发明涉及软石材料技术领域,具体涉及用于粘贴软石材料的双组分粘接剂及其制备方法,所述双组份粘接剂包括重量比为1-10：1的组分A和组分B,其中,以所述组分A的总量计,所述组分A包括：15-25wt％的重质碳酸钙；0.5-3wt％的淀粉醚；1-5wt％的木质纤维；余量为石英砂；以所述组分B的总量计,所述组分B包括：0.3-1wt％的羟乙基纤维素；0.1-0.7wt％的聚乙烯醇、25-40wt％的丙烯酸乳液；0.03-0.09wt％的AMP-95；20-45wt的TFX；2-5wt％的成膜助剂；1-5wt％的乙二醇；0.1-0.5wt％的防腐杀菌剂；余量为水。(The invention relates to the technical field of soft stone materials, in particular to a two-component adhesive for sticking soft stone materials and a preparation method thereof, wherein the two-component adhesive comprises the following components in percentage by weight of 1-10: 1, wherein the component a comprises, based on the total amount of the component a: 15-25 wt% of ground calcium carbonate; 0.5-3 wt% of starch ether; 1-5 wt% of wood fibers; the balance being quartz sand; (ii) said component B comprises, based on the total amount of said component B: 0.3 to 1 wt% of hydroxyethyl cellulose; 0.1-0.7 wt% of polyvinyl alcohol and 25-40 wt% of acrylic emulsion; 0.03-0.09 wt% AMP-95; 20-45wt TFX; 2-5 wt% of a film-forming aid; 1-5 wt% ethylene glycol; 0.1-0.5 wt% of an antiseptic bactericide; the balance being water.)

1. The two-component adhesive for adhering soft stone materials is characterized by comprising the following components in percentage by weight of 1-10: 1, wherein the component a comprises, based on the total amount of the component a: 15-25 wt% of ground calcium carbonate; 0.5-3 wt% of starch ether; 1-5 wt% of wood fibers; the balance being quartz sand;

(ii) said component B comprises, based on the total amount of said component B: 0.3 to 1 wt% of hydroxyethyl cellulose; 0.1-0.7 wt% polyvinyl alcohol; 25-40 wt% of an acrylic emulsion; 0.03-0.09 wt% AMP-95; 20-45wt of a polymeric elastic water-resistant emulsion; 2-5 wt% of a film-forming aid; 1-5 wt% ethylene glycol; 0.1-0.5 wt% of an antiseptic bactericide; the balance being water.

2. The two-component adhesive according to claim 1, wherein the weight ratio of the component a to the component B is 2 to 5: 1.

3. the two-component adhesive according to claim 1, wherein the component a comprises, based on the total amount of the component a: 18-22 wt% of ground calcium carbonate; 1-2 wt% of starch ether; 2-3 wt% of wood fibers; the balance being quartz sand.

4. The two-component adhesive as claimed in claim 1, wherein the ground calcium carbonate has a mesh size of 120-500 meshes.

5. The two-component adhesive according to claim 1, wherein the quartz sand has a mesh size of 70 to 120 mesh.

6. The two-component adhesive according to any one of claims 1 to 5, wherein the component B comprises, based on the total amount of the component B: 0.5-0.7 wt% hydroxyethyl cellulose; 0.3-0.5 wt% of polyvinyl alcohol and 30-35 wt% of acrylic emulsion; 0.05-0.07 wt% AMP-95; 30-35wt TFX; 2.5-4 wt% of a film-forming aid; 2-4 wt% of ethylene glycol; 0.2-0.4 wt% of antiseptic bactericide; the balance being water.

7. The two-component adhesive according to claim 6, wherein the acrylic emulsion is an anionic acrylic emulsion;

the pH value of the anionic acrylic emulsion is 6-7, the viscosity at 25 ℃ is 50-500 mPa.s, the solid content is 49-51%, the glass transition temperature is 28.2 ℃, and the lowest film forming temperature is 20 ℃.

8. The two-component adhesive of claim 6, wherein the coalescent is selected from the group consisting of lauryl alcohol esters.

9. The two-component adhesive of claim 6, wherein the polyvinyl alcohol is PE 100.

10. A method of making the two-component adhesive of any one of claims 1-9, comprising:

preparation of component A:

after the ground limestone, the starch ether and the wood fiber are uniformly mixed with the first part of quartz sand, adding the second part of quartz sand and uniformly mixing to obtain a component A;

preparation of component B:

uniformly mixing hydroxyethyl cellulose and polyvinyl alcohol in water, then adding acrylic emulsion and TFX, uniformly mixing, then adding AMP-95, a film-forming aid, ethylene glycol and an antiseptic bactericide, and uniformly mixing to obtain a component B.

Technical Field

The invention relates to the technical field of soft stone materials, in particular to a bi-component adhesive for sticking soft stone materials and a preparation method thereof.

Background

The soft stone material has rich textures and unique flexibility, is light in weight and high in bending strength, can meet the design requirements of special-shaped buildings and a plurality of application scenes, and can bear the thermal stress deformation of building structures and different heat-insulating base layers; the coating has a plurality of excellent performances such as safety, durability, rapid construction and the like; the problems that floor tiles and stone are poor in use feeling, wood floors are polluted by environment and short in service life are solved, and all in all, the soft stone material has wide application prospect in the field of decoration.

At present, when the soft stone material is produced, an adhesive is coated on one side of the soft stone material and then the soft stone material is directly adhered to a wall of a user; however, no adhesive dedicated to soft stone materials is available at present, and when the conventional building adhesive is used for soft stone materials, the soft stone materials are bubbled, alkali is returned, and even the soft stone materials are peeled off from wall surfaces.

Disclosure of Invention

The invention aims to overcome the problems that the adhesive in the prior art is easy to cause bubbling, alkali return and even peeling from a wall surface, and provides a two-component adhesive for adhering soft stone materials and a preparation method thereof.

In order to achieve the above object, a first aspect of the present invention provides a two-component adhesive for adhering soft stone materials, the two-component adhesive comprising, by weight, 1 to 10: 1, wherein the component a comprises, based on the total amount of the component a: 15-25 wt% of ground calcium carbonate; 0.5-3 wt% of starch ether; 1-5 wt% of wood fibers; the balance being quartz sand;

(ii) said component B comprises, based on the total amount of said component B: 0.3 to 1 wt% of hydroxyethyl cellulose; 0.1-0.7 wt% of polyvinyl alcohol and 25-40 wt% of acrylic emulsion; 0.03-0.09 wt% AMP-95; 20-45wt TFX; 2-5 wt% of a film-forming aid; 1-5 wt% ethylene glycol; 0.1-0.5 wt% of an antiseptic bactericide; the balance being water.

The inventor of the invention finds that the weight ratio of the component A and the component B is controlled within a reasonable range, the construction slurry is not smooth due to excessive component A, the viscosity of the adhesive is low, and soft stones are easy to fall off; too little component A can cause insufficient thickness of sagging cloth pulp, and the weight ratio of the component A to the component B is 2-5: 1, for example, may be 2: 1. 3: 1. 4: 1. 5: 1 or any value in the range consisting of any two of the ratios described above.

Preferably, the component A comprises, based on the total amount of the component A: 18-22 wt% of ground calcium carbonate; 1-2 wt% of starch ether; 2-3 wt% of wood fibers; the balance being quartz sand.

According to the invention, under the preferable conditions, the mesh number of the heavy calcium carbonate is 120-500 meshes, and under the preferable conditions, the pores of the construction surface can be filled, the curve deviation of the construction surface can be corrected, and a foundation is laid for obtaining a uniform and smooth paint surface.

Under the preferable conditions, the mesh number of the quartz sand is 70-120 meshes, and under the preferable conditions, the construction performance of the adhesive can be optimized, and the strength of the two-component adhesive after curing is improved.

According to the invention, by compounding the hydroxyethyl cellulose, the polyvinyl alcohol, the acrylic emulsion and the polymer elastic waterproof emulsion in a specific ratio, the bonding effect and the water retention effect of the adhesive can be increased, the anti-permeability performance of the adhesive is improved, the bonding strength of the adhesive to soft stone materials is improved, the bonding life of the adhesive is prolonged, and the phenomena of bubbling, alkali return and wall surface peeling of the soft stone materials are avoided. Preferably, the component B comprises, based on the total amount of the component B: 0.5-0.7 wt% hydroxyethyl cellulose; 0.3-0.5 wt% of polyvinyl alcohol and 30-35 wt% of acrylic emulsion; 0.05-0.07 wt% AMP-95; 30-35wt TFX; 2.5-4 wt% of a film-forming aid; 2-4 wt% of ethylene glycol; 0.2-0.4 wt% of antiseptic bactericide; the balance being water.

According to the invention, under the preferable conditions, the acrylic emulsion is anionic acrylic emulsion, the pH value of the acrylic emulsion is 6-7, the viscosity at 25 ℃ is 50-500mPa & s, the solid content (150 ℃,20min) is 49-51%, the glass transition temperature is 20 ℃, and the lowest film forming temperature is 20 ℃; the inventor of the invention finds that the acrylic emulsion provided by the invention has high viscosity and can be well compatible with wood fiber and quartz sand.

In some preferred embodiments of the present invention, the method for preparing the acrylic emulsion comprises the steps of: emulsifying acrylic monomers, 3-5% of emulsifier and 20% of water in a pre-emulsifying kettle for 30-40min to obtain non-layered emulsion, then adding the rest 30-32% of water, the rest 6-10% of emulsifier and buffer in a polymerization reaction kettle, heating to 78-80 ℃, adding 20% of emulsion and 30% of initiator to react for 20-30min, then dropwise adding the rest 80% of emulsion and the rest 70% of initiator, and completing dripping within 3-4 h; and then, keeping the temperature of the polymerization reaction kettle at 85-90 ℃ for reaction for 1-2h, cooling to 45-50 ℃, and adding a pH regulator to regulate the pH of the reaction system to 6-7 to obtain the acrylic emulsion.

In the invention, the acrylic monomer comprises an acrylic hard monomer, an acrylic soft monomer and an acrylic functional monomer; wherein the acrylic hard monomer is at least one selected from methyl acrylate, methyl methacrylate, ethyl methacrylate, n-butyl methacrylate, vinyl acetate and styrene; the acrylic acid soft monomer is selected from at least one of butyl acrylate, ethyl acrylate, n-octyl acrylate, isooctyl methacrylate and dodecyl methacrylate; the functional monomer is at least one of acrylonitrile, acrylic acid, methacrylic acid, N-hydroxymethyl acrylamide, hydroxyethyl acrylate, hydroxypropyl methacrylate, itaconic acid, hydroxyethyl methacrylate and maleic anhydride,

further preferably, the weight ratio of the acrylic hard monomer, the acrylic soft monomer and the acrylic functional monomer is 3/6/1.

The kind of (B) can be selected according to actual requirements, and under the preferable conditions, the film-forming assistant is selected from dodecyl alcohol ester.

In some preferred embodiments of the present invention, the polyvinyl alcohol is PE100, and the PE100 is capable of wetting the substrate to improve surface tension and permeability, thereby improving the adhesion of the two-part adhesive to soft stone materials.

In a second aspect, the present invention provides a method for preparing the two-component adhesive of the first aspect, the method comprising:

preparation of component A:

after the ground limestone, the starch ether and the wood fiber are uniformly mixed with the first part of quartz sand, adding the second part of quartz sand and uniformly mixing to obtain a component A;

preparation of component B:

uniformly mixing hydroxyethyl cellulose and polyvinyl alcohol in water, then adding acrylic emulsion and TFX, uniformly mixing, then adding AMP-95, a film-forming aid, ethylene glycol and an antiseptic bactericide, and uniformly mixing to obtain a component B.

Through the technical scheme, the adhesive disclosed by the invention does not contain alkaline components, does not have the phenomena of alkali return and alkali spitting, has strong adhesive capacity to soft stone materials, and is not easy to bulge and peel.

Detailed Description

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.

The present invention will be described in detail below by way of examples. In the following examples, the starch ether was a commercially available product having a type of 8860 (hereinafter referred to as "starch ether 8860"); hydroxyethyl cellulose is a commercially available product (hereinafter referred to as HS3 ten thousand) of a Kelaien company with a model number of HS30000 YP 2; the polymer elastic waterproof emulsion is a product sold in the model of TFX (TFX for short) by Jiangsu sunrise chemical Co., Ltd; the antiseptic bactericide is a commercial product (hereinafter referred to as D29) with the model number of D29 of Hoffman company.

Example 1

A two-component adhesive for adhering soft stone materials comprises 4: 1, wherein the component a comprises, based on the total amount of the component a: 20 wt% of 200 mesh heavy calcium carbonate; 1.5 wt% starch ether 8860; 2.5 wt% wood fibres; the balance is 7# quartz sand;

(ii) said component B comprises, based on the total amount of said component B: 0.6 wt% hydroxyethyl cellulose HS3 ten thousand; 0.4 wt% of polyvinyl alcohol PE100 and 32 wt% of acrylic emulsion; 0.06 wt% AMP-95; 32wt TFX; 3 wt% of a film forming aid; 3 wt% ethylene glycol; 0.3 wt% of D29; the balance being water.

The preparation method of the two-component adhesive comprises the following steps:

preparation of component A:

uniformly mixing 200-mesh heavy calcium carbonate, starch ether 8860 and wood fiber with 26% of quartz sand (based on the total amount of the component A), adding the rest 50% of quartz sand (based on the total amount of the component A) and uniformly mixing to obtain a component A;

preparation of component B:

the preparation method of the acrylic emulsion comprises the following steps: emulsifying 450g of acrylic monomer (consisting of methyl methacrylate, butyl acrylate and hydroxyethyl methacrylate according to a weight ratio of 3:6: 1) 30g of emulsifier OP-10 and 104g of water in a pre-emulsification kettle at normal temperature for 30min to obtain a non-layered emulsion, then adding 396g of water, 20g of emulsifier OP-10 and buffer sodium bicarbonate into a polymerization reaction kettle, heating to 80 ℃, then adding 58.4g of emulsion and 0.45g of initiator sodium bicarbonate to react for 20-30min, then dropwise adding 525.6g of the emulsion and 1.05g of initiator sodium bicarbonate, and finishing dripping within 3 h; then keeping the temperature of the polymerization reaction kettle at 90 ℃ for 2 hours for reaction, then cooling to 50 ℃, adding a pH regulator to regulate the pH of the reaction system to 6-7, and obtaining acrylic emulsion;

the acrylic emulsion is anionic acrylic emulsion, has pH of 6.5, viscosity of 350 mPa.s at 25 deg.C, solid content of 50% (150 deg.C, 20min), glass transition temperature of 28.2 deg.C, and minimum film-forming temperature of 20 deg.C.

Hydroxyethyl cellulose HS3, polyvinyl alcohol PE100 and water are stirred for 15min at the rotating speed of 800r/min, then acrylic emulsion and TFX are added and stirred for 5min at the rotating speed of 400r/min, and then AMP-95, dodecyl alcohol ester, ethylene glycol and D29 are added and stirred for 5min at the rotating speed of 400r/min, so that a component B is obtained.

Examples 2 to 3 and comparative examples 1 to 2

Following the procedure of the examples, except that the weight ratio of component A to component B was varied, as shown in Table 1.

Examples 4 to 9

According to the method of the examples, the proportions of the materials in the component A are different, as shown in Table 1.

Test example

The tensile bond strength after soaking, the tensile bond strength after heat aging, the tensile bond strength after freeze thawing and the tensile bond strength after freeze thawing of the bi-component adhesive were tested according to the method of JC/T547-2005, and the experimental results are shown in Table 1.

TABLE 1

Examples 10 to 17

According to the method of the examples, the amounts of the materials in component B were varied, specifically as shown in Table 2, and the results are shown in Table 3.

TABLE 2

Comparative example 3

The procedure of example 1 was followed except that the acrylic monomers were not included in the acrylic monomers during the preparation of the acrylic emulsion, and the results are shown in Table 3;

comparative example 4

The procedure of example 1 was followed except that the acrylic acid monomers were not contained in the acrylic acid emulsion preparation process, and the results are shown in Table 3.

Comparative example 5

The procedure of example 1 was followed except that the acrylic monomer was not included in the acrylic acid functional monomer during the preparation of the acrylic emulsion, and the results are shown in Table 3.

TABLE 3

The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.