CN107603410A - Floor coatings aqueous epoxy resin emulsion and preparation method thereof - Google Patents

Abstract

The invention belongs to aqueous epoxy floor coating field, synthetic intermediate is reacted by polyethylene glycol and phthalic anhydride esterification of derivatives, then the non-ionic reaction type emulsifying agent to epoxy resin with preferable emulsification is prepared using the intermediate and epoxy resin progress ring-opening polymerization, in conjunction with phase inversion, non-ionic reaction type emulsifying agent and epoxy resin are fully premixed, deionized water and defoamer are added dropwise again, stable aqueous epoxy resin emulsion is finally made.Preparation method simple possible of the present invention, building-up process is easily controllable, and whole technological process is nontoxic without any organic solvent, safety and environmental protection；The floor coatings excellent combination property that the aqueous epoxy resin emulsion is prepared, with mechanical performances such as excellent wearability, impact resistance, hardness, adhesive force, and the chemical property such as excellent water resistance, solvent resistance, corrosion resistance, paint film uniform ground, glossiness are high, good decorating effect and easy cleaning maintenance, construction and application especially suitable for the seal coat of industry ground slab, floating coat, finish paint.

Description

Water-based epoxy resin emulsion for floor coating and preparation method thereof

technical field

The invention belongs to the field of epoxy resin water-based floor paint, and in particular relates to a water-based epoxy resin emulsion for floor paint and a preparation method thereof.

Background technique

With the development of the economy and the continuous improvement of people's living standards, people pay more and more attention to epoxy flooring, and the requirements for ground protection and decoration in public places are also constantly improving. At present, my country's industrial floor coatings are still traditional Solvent-based and solvent-free epoxy floor paints are mainly used, although solvent-based and solvent-free epoxy floor paints have good hardness, strength, wear resistance, water resistance, chemical resistance, weather resistance, and durability However, traditional solvent-based epoxy floor coatings contain more volatile organic compounds and pollute the environment; some reactive diluents in solvent-free epoxy floor coatings have certain toxicity and endanger human health.

In recent years, in order to meet the requirements of relevant environmental protection standards at home and abroad, the application of waterborne epoxy resin has been greatly developed. In the process of production and construction, it has the characteristics of slight odor, no organic solvent, no toxicity, no VOC (volatile organic compound) emission, etc. Therefore, it can take into account the development of water-based epoxy resin with high performance and high environmental protection requirements in industrial floor coatings It has attracted more and more attention and research from relevant scientific and technical personnel at home and abroad.

Contents of the invention

The purpose of the invention is to provide a water-based epoxy resin emulsion for floor paint and a preparation method thereof, the method uses water as a dispersion medium, has no volatile solvent, is safe, non-toxic and environmentally friendly; the emulsion is applied to floor paint for its mechanical properties and Excellent chemical resistance.

In order to achieve the above object, the technical scheme adopted in the present invention is as follows: water-based epoxy resin emulsion for floor paint, which is characterized in that by weight, the emulsion composition includes: 2-10 parts of non-ionic reactive emulsifier, epoxy 35-55 parts of resin, 40-60 parts of deionized water, 0.01-0.05 parts of defoamer.

According to the above scheme, the synthetic raw materials of the non-ionic reactive emulsifier include polyethylene glycol, dibasic anhydride (phthalic anhydride derivatives), and epoxy resin, and the ratio of the amount of substances (molar ratio) is 1:2-2.5 : 2.2-2.75.

According to the above scheme, the epoxy resin is selected from one or more of E20, E35, E44, and E51 and mixed in any proportion.

According to the above scheme, the molecular weight of the polyethylene glycol is one of 2000, 4000, 6000 and 8000.

According to the above scheme, the dibasic acid anhydride is one of tetrahydrophthalic anhydride, methyltetrahydrophthalic anhydride, hexahydrophthalic anhydride, and methylhexahydrophthalic anhydride.

According to the above scheme, the defoamer is selected from BYK-019, BYK-024, BYK-028 and mixed in any proportion.

The preparation method of above-mentioned floor paint water-based epoxy resin emulsion is characterized in that comprising the steps:

Step 1, the synthesis of nonionic reactive emulsifier

According to the ratio of polyethylene glycol, dibasic acid anhydride, and epoxy resin, the ratio of substances is 1:2-2.5:2.2-2.75, and the polyethylene glycol and dibasic acid anhydride are stirred and mixed evenly at 90-120°C. After heat preservation reaction for 3-4 hours, add epoxy resin, heat preservation (90-120 ℃) reaction for 3-4 hours again, when the acid value is less than 1mg KOH/g, cool down and discharge; the epoxy value is between 0.03-0.06;

Step 2, the preparation of aqueous epoxy resin emulsion

In parts by weight: 2-10 parts of non-ionic reactive emulsifier, 35-55 parts of epoxy resin, 40-60 parts of deionized water, 0.01-0.05 parts of defoamer, the non-ionic emulsifier prepared in step 1 After the reactive emulsifier and epoxy resin are stirred and mixed evenly under the conditions of 60-80°C and 600-800r/min, slowly add deionized water and defoamer that have been preheated to 60-75°C and mixed, 0.5- After 1.5 hours of dropwise addition, continue to stir for about 1 hour under the condition of a rotating speed of 1000-1200r/min, cool down and discharge to obtain a water-based epoxy resin emulsion for floor coatings.

The solid content of the water-based epoxy resin emulsion for floor paint prepared by the above method is 40%-60%, the epoxy equivalent is 300-1200g/mol, the average particle size is 200-500nm, and the centrifugal stability is 6000r/min No delamination within 30 minutes at a certain rotational speed, and no delamination within 30 days at a storage stability of 50°C.

The present invention also provides the application of the water-based epoxy resin emulsion with the above-mentioned floor paint, which is characterized in that it is applied in the floor paint, and its application formula includes the following components by weight percentage:

Waterborne epoxy resin curing agent: 20%-25%,

Water-based epoxy resin emulsion for floor coatings: 24%-34%,

Pigment and filler: 10%-30%,

Deionized water: 20%-30%,

Additives: 0.4%-4%.

According to the above scheme, the ratio of the active hydrogen equivalent of the water-based epoxy resin curing agent to the epoxy equivalent of the water-based epoxy resin emulsion of the floor coating is 1:1.2-1.3.

According to the above scheme, the water-based epoxy curing agent is one of WH900 (Air Products), AB-HGA (Zhejiang Anbang New Material Company), H208B (Shanghai Hanzhong Chemical Company) and the like.

According to the above scheme, the pigments and fillers include one or more of titanium dioxide, carbon black, phthalocyanine blue, chrome yellow, talcum powder, barite powder and the like mixed in any proportion.

According to the above scheme, the additives include one or more of substrate wetting agents, defoamers, thickeners, and wetting and dispersing agents mixed in any proportion. 0.1%-1% of the total amount.

According to the above scheme, the substrate wetting agent is a kind of TEGO 240, 270; the defoamer is a kind of BYK-019, BYK-024, BYK-028; the thickener is a kind of Mingling PUR 40, 60 species; wetting and dispersing agent Mingling 490.

According to the above scheme, the floor coating is suitable for one or more of the sealing primer, middle coat and top coat of industrial floors.

Compared with the prior art, the present invention has the following advantages:

(1) The water-based epoxy resin emulsion for floor coatings prepared by the present invention has excellent properties such as wear resistance, hardness, water resistance and corrosion resistance, and is especially suitable for industrial floor coatings. It has good decorative effects and is easy to clean and maintain.

(2) The water-based epoxy resin emulsion for floor paint prepared by the method does not have any organic solvent in the production and construction process, is safe, environmentally friendly and non-toxic, and has a simple preparation process and is easy to control.

(3) The water-based epoxy resin emulsion for floor coatings prepared by this method is especially beneficial to the dispersion of pigments and fillers. It can be cured for a long time at room temperature, has good drying property, long pot life, mild curing conditions, and convenient and feasible construction.

Description of drawings

The present invention can be further illustrated by the non-limiting examples given by the accompanying drawings:

Fig. 1 is the infrared spectrogram of the nonionic reactive emulsifier synthesized in Examples 1 to 4 of the present invention.

Fig. 2 is a particle size distribution diagram of water-based epoxy resin emulsions for floor coatings prepared in Examples 1 to 4 of the present invention.

detailed description

In order to enable those skilled in the art to better understand the present invention, the technical solution of the present invention will be further described below in conjunction with the accompanying drawings and embodiments.

Example 1

The preparation method of floor coating water-based epoxy resin emulsion, comprises the steps:

Step 1, the synthesis of nonionic reactive emulsifier

Stir and mix polyethylene glycol with a molecular weight of 6000 and methyl tetrahydrophthalic anhydride at 105°C. After 3 hours of heat-retaining reaction, add epoxy resin E44, heat again (105°C) and react for 3 hours. Measure the acid value 1mgKOH/g , the non-ionic reactive emulsifier can be prepared by cooling down and discharging, wherein the molar ratio of polyethylene glycol 6000: methyltetrahydrophthalic anhydride: epoxy resin E44 = 1: 2.0: 2.2;

Step 2, the preparation of aqueous epoxy resin emulsion

Stir and mix the non-ionic reactive emulsifier and epoxy resin E51 prepared in step 1 evenly at 70°C and 600-800r/min, then slowly add deionized water (preheated at 70°C) and mixed Defoamer BYK-028, after 0.5-1.5h is added dropwise, then continue to stir for about 1h at the speed of 1000-1200r/min, cool down and discharge to get the water-based epoxy resin emulsion for floor coating, of which In terms of weight percentage (ie parts by weight): non-ionic reactive emulsifier accounts for 5%, epoxy resin E51 accounts for 45%, deionized water accounts for 49.98%, and defoamer accounts for 0.02%.

Example 2-4

Using the water-based epoxy resin emulsion for floor coatings prepared by the same process as in Example 1, the differences are shown in Table 1 and Table 2 below.

Step 1, the synthesis of nonionic reactive emulsifier

Table 1

Step 2, preparation of water-based epoxy resin emulsion for floor coating

Table 2

The non-ionic reactive emulsifier prepared in Examples 1-4 is tested by infrared spectrum, as shown in Figure 1, the Fourier transform infrared spectrum shows that the hydroxyl peak at 3370cm ^-1 is obviously enhanced, and it appears at 1718cm- ¹ The stretching vibration peaks of the ester carbonyl group were eliminated, the stretching vibration peaks of the epoxy group at 1062cm ^-1 and 949cm ^-1 were significantly reduced, and the stretching vibration peaks of the hydroxyl and ester groups were introduced at 3740cm ^-1 and 1718cm ^-1 , thus It is proved that part of the dibasic acid anhydride reacts with polyethylene glycol for transesterification, and undergoes a ring-opening reaction with part of epoxy resin to synthesize the required non-ionic reactive emulsifier.

The water-based epoxy resin emulsion for floor coatings prepared in Examples 1-4 is tested for particle size distribution, as shown in Figure 2, the particle size distribution test chart shows that the average particle size of the emulsion is 383.2nm, and the particle size distribution width It is 0.216, and it forms a normal distribution. The average particle size of the emulsion is small, the particle size distribution is narrow, and the mechanical stability is good.

From the above, it can be seen that the nonionic reactive emulsifier prepared by this method has introduced a large amount of hydrophilic polyether chain segments and lipophilic epoxy groups, so that it has certain surface activity and reactivity, and can have a certain effect on epoxy resin. The emulsification effect can participate in solidification and film formation; and water-based epoxy resin emulsion with small particle size, narrow distribution and stable mechanical properties can be obtained only by using water as the dispersion medium, and the preparation method is safe, environmentally friendly and non-toxic.

Example 5

The water-based epoxy resin emulsion for floor paint prepared in the embodiment 1-4 is formulated into an industrial floor finish paint, and the application formula of its water-based epoxy resin emulsion for floor paint is as follows:

table 3

The pigments and fillers include one or more of titanium dioxide, carbon black, phthalocyanine blue, chrome yellow, talc powder, barite powder and the like mixed in any proportion.

The substrate wetting agent is a kind of TEGO 240, 270; the defoamer is a kind of BYK-019, BYK-024, BYK-028; the thickener is a kind of Mingling PUR 40, 60; Dispersant Mingling 490.

The water-based epoxy resin emulsions prepared in Examples 1-4 are all formulated into industrial floor topcoats according to the application formula Table 3, and the performance index test is carried out according to the water-based epoxy floor coating chemical industry standard HG/T 5057-2016 , the test results are as follows:

Table 4

It can be seen from the above table that the floor coating water-based epoxy resin emulsion prepared by this method has excellent comprehensive properties, and has excellent mechanical properties such as abrasion resistance, impact resistance, hardness, adhesion, etc., as well as excellent water resistance, water resistance, etc. Solvent resistance, corrosion resistance and other chemical properties, short curing time and high gloss, especially suitable for the construction and application of industrial floors, and it has good decorative effects and is easy to clean and maintain.

Each raw material enumerated in the present invention, and the upper and lower limits of each raw material of the present invention, the interval value, and the upper and lower limits of process parameters (such as temperature, time, etc.), the interval value can realize the present invention, do not enumerate one by one here Example.

Above, the water-based epoxy resin emulsion for floor paint provided by the present invention and its preparation method have been described in detail and examples have been cited, but for those of ordinary skill in the art, without departing from the principles of the present invention, Several improvements and modifications can also be made to the present invention, and these improvements and modifications should be included within the protection scope of the claims of the present invention.

Claims (10)

1. The water-based epoxy resin emulsion for floor paint is characterized in that by weight, the emulsion composition includes: 2-10 parts of non-ionic reactive emulsifier, 35-55 parts of epoxy resin, 40-55 parts of deionized water 60 parts, 0.01-0.05 parts of defoamer. 2. the water-based epoxy resin emulsion for floor paint according to claim 1, is characterized in that: the synthetic raw material of described nonionic reactive emulsifier comprises Polyethylene Glycol, dibasic acid anhydride, epoxy resin, and according to material The amount ratio is 1:2-2.5:2.2-2.75. 3. The water-based epoxy resin emulsion for floor paint according to claim 1 or 2, characterized in that: said epoxy resin is selected from one or more of E20, E35, E44, E51 in any proportion the mix of. 4. the water-based epoxy resin emulsion for floor paint according to claim 2, is characterized in that: the molecular weight of described polyethylene glycol is a kind of in 2000,4000,6000,8000; Described dibasic acid anhydride is One of tetrahydrophthalic anhydride, methyltetrahydrophthalic anhydride, hexahydrophthalic anhydride, and methylhexahydrophthalic anhydride. 5. The water-based epoxy resin emulsion for floor paint according to claim 1, characterized in that: the defoamer is selected from one or more of BYK-019, BYK-024, BYK-028 according to any Proportioned mix. 6. the preparation method of floor paint water-based epoxy resin emulsion as claimed in claim 1, is characterized in that comprising the steps: Step 1, the synthesis of nonionic reactive emulsifier According to the ratio of polyethylene glycol, dibasic acid anhydride, and epoxy resin, the ratio of substances is 1:2-2.5:2.2-2.75, and the polyethylene glycol and dibasic acid anhydride are stirred and mixed evenly at 90-120°C. After heat preservation reaction for 3-4 hours, add epoxy resin, heat preservation reaction for 3-4 hours again, when the acid value is less than 1mg KOH/g, cool down and discharge; the epoxy value is between 0.03-0.06; Step 2, the preparation of aqueous epoxy resin emulsion In parts by weight: 2-10 parts of non-ionic reactive emulsifier, 35-55 parts of epoxy resin, 40-60 parts of deionized water, 0.01-0.05 parts of defoamer, the non-ionic emulsifier prepared in step 1 Reactive emulsifier and epoxy resin at 60-80°C, 600-800 After stirring and mixing evenly under the condition of r/min, add the preheated to 60-75°C and mixed deionized water and defoamer dropwise. Continue to stir for about 1 hour, cool down and discharge to obtain the water-based epoxy resin emulsion for floor coating. 7. the preparation method of water-based epoxy resin emulsion for floor paint according to claim 6, is characterized in that the solid content of the water-based epoxy resin emulsion for floor paint made by said method is 40%-60%, The epoxy equivalent is 300-1200g/mol, and the average particle size is 200-500nm. 8. the application of floor paint water-based epoxy resin emulsion as claimed in claim 1 is characterized in that being applied in floor paint, its application formula comprises following component by weight percentage: Water-based epoxy resin curing agent: 20%-25%, Water-based epoxy resin emulsion for floor coatings: 24%-34%, Pigment and filler: 10%-30%, Deionized water: 20%-30%, Additives: 0.4%-4%. 9. the application of water-based epoxy resin emulsion for floor paint according to claim 8, is characterized in that the active hydrogen equivalent of described water-based epoxy resin curing agent and the epoxy equivalent of water-based epoxy resin emulsion for floor paint The ratio is 1:1.2-1.3. 10. the application of water-based epoxy resin emulsion for floor paint according to claim 8, is characterized in that said pigments and fillers include titanium dioxide, carbon black, phthalocyanine blue, chrome yellow, talcum powder, barite powder One or more are mixed in any proportion; the auxiliary agent includes one or more of substrate wetting agents, defoamers, thickeners, wetting and dispersing agents mixed in any proportion, more When mixed, they all account for 0.1%-1% of the total amount of paint.