阅读说明：本技术 一种防火涂料及其制备方法 (Fireproof coating and preparation method thereof ) 是由 胡明 唐帆 钱金均 于 2021-08-13 设计创作，主要内容包括：本发明属于涂料技术领域。本发明提供了一种防火涂料,包含多元醇50～60份、有机酸50～60份、单体30～40份、硅丙乳液20～30份、溶剂30～40份、流平剂5～10份、填料10～15份。本发明还提供了防火涂料的制备方法,将多元醇、有机酸和单体进行酯化反应,反应过程中采取分步升温的方式,使酯化反应充分进行；然后将酯化反应得到的中间组分和剩余原料混合,即可得到防火涂料。本发明提供的制备方法简单高效,可以有效的将涂料进行分散,得到成品后不会出现结块等现象,适合大规模的制备。(The invention belongs to the technical field of coatings. The invention provides a fireproof coating, which comprises 50-60 parts of polyol, 50-60 parts of organic acid, 30-40 parts of monomer, 20-30 parts of silicone-acrylic emulsion, 30-40 parts of solvent, 5-10 parts of flatting agent and 10-15 parts of filler. The invention also provides a preparation method of the fireproof coating, wherein the polyhydric alcohol, the organic acid and the monomer are subjected to esterification reaction, and the esterification reaction is fully performed by adopting a step-by-step heating mode in the reaction process; and then mixing the intermediate component obtained by the esterification reaction with the rest raw materials to obtain the fireproof coating. The preparation method provided by the invention is simple and efficient, can effectively disperse the coating, does not cause the phenomena of agglomeration and the like after obtaining a finished product, and is suitable for large-scale preparation.)

1. The fireproof coating is characterized by being prepared from the following raw materials in parts by mass: 50-60 parts of polyol, 50-60 parts of organic acid, 30-40 parts of monomer, 20-30 parts of silicone-acrylic emulsion, 30-40 parts of solvent, 5-10 parts of flatting agent and 10-15 parts of filler.

2. The fire retardant coating of claim 1, wherein the polyol comprises one or more of 1, 3-propanediol, 1, 4-butanediol, glycerol, and pentaerythritol.

3. The fire retardant coating of claim 1 or 2, wherein the organic acid is isophthalic acid, terephthalic acid, adipic acid or glutaric acid;

the monomer is tung oil, linseed oil or catalpa oil.

4. The fire retardant coating of claim 3, wherein the solvent is diethylene glycol methyl ether, diethylene glycol ethyl ether or diethylene glycol butyl ether;

the filler is talcum powder, zinc stearate or kaolin.

5. The method for preparing the fireproof coating of any one of claims 1 to 4, wherein the method comprises the following steps:

(1) mixing polyalcohol, organic acid and monomer, and performing esterification reaction to obtain an intermediate component;

(2) and mixing the intermediate component with the rest raw materials to obtain the fireproof coating.

6. The method according to claim 5, wherein the esterification reaction in the step (1) is carried out under stirring at a rotation speed of 150 to 200 rpm.

7. The production process according to claim 5 or 6, wherein the esterification reaction in the step (1) is a first esterification reaction, a second esterification reaction and a third esterification reaction which are sequentially carried out;

the target temperature of the first-step esterification reaction is 100-150 ℃, the temperature rise rate of the first-step esterification reaction is 4-6 ℃/min, and the heat preservation time after the first-step esterification reaction reaches the target temperature is 1-2 h.

8. The method according to claim 7, wherein the target temperature of the second esterification reaction is 180 to 200 ℃, the temperature increase rate from the first esterification reaction to the second esterification reaction is 2 to 3 ℃/min, and the holding time after the target temperature of the second esterification reaction is reached is 2 to 3 hours.

9. The preparation method of claim 8, wherein the target temperature of the third esterification reaction is 230-260 ℃, the temperature rising rate from the second esterification reaction to the third esterification reaction is 1-2 ℃/min, and the heat preservation time after the target temperature of the third esterification reaction is reached is 3-5 h.

10. The method according to claim 5, 6, 8 or 9, wherein the mixing in the step (2) is performed under stirring at a rotation speed of 1000 to 1500rpm for 1 to 2 hours.

Technical Field

The invention relates to the technical field of coatings, in particular to a fireproof coating and a preparation method thereof.

Background

Since the world, the building steel structure has the advantages of light weight, quick construction, flexible arrangement and the like compared with the traditional building materials, and is widely adopted. The steel can be regarded as a building material which can not be burnt, but the steel has some defects which are difficult to avoid in the aspect of fire prevention as the building material, and the mechanical properties of the steel, such as yield point, tensile strength, elastic modulus and the like, are all sharply reduced due to the increase of temperature. The fire resistance limit of a general unprotected steel structure is about 15 minutes, the steel structure usually loses the bearing capacity at the temperature of 450-650 ℃, and large deformation occurs, so that the steel column and the steel beam bend and even the structure collapses. The collapse of a building is easily caused by the fire failure of steel, and once a steel structure building without protection or with insufficient protection breaks out a fire, extra accidents are often caused, so that the loss of personnel and economy is caused.

Disclosure of Invention

The invention aims to overcome the defects in the prior art and provides a fireproof coating and a preparation method thereof.

In order to achieve the above object, the present invention provides the following technical solutions:

the invention provides a fireproof coating which is prepared from the following raw materials in parts by mass: 50-60 parts of polyol, 50-60 parts of organic acid, 30-40 parts of monomer, 20-30 parts of silicone-acrylic emulsion, 30-40 parts of solvent, 5-10 parts of flatting agent and 10-15 parts of filler.

Preferably, the polyhydric alcohol comprises one or more of 1, 3-propylene glycol, 1, 4-butylene glycol, glycerol and pentaerythritol.

Preferably, the organic acid is isophthalic acid, terephthalic acid, adipic acid or glutaric acid;

the monomer is tung oil, linseed oil or catalpa oil.

Preferably, the solvent is diethylene glycol methyl ether, diethylene glycol ethyl ether or diethylene glycol butyl ether;

the filler is talcum powder, zinc stearate or kaolin.

The invention also provides a preparation method of the fireproof coating, which comprises the following steps:

(1) mixing polyalcohol, organic acid and monomer, and performing esterification reaction to obtain an intermediate component;

(2) and mixing the intermediate component with the rest raw materials to obtain the fireproof coating.

Preferably, the esterification reaction in the step (1) is carried out under a stirring condition, and the rotation speed of the stirring is 150-200 rpm.

Preferably, the esterification reaction in the step (1) is to sequentially perform a first esterification reaction, a second esterification reaction and a third esterification reaction;

the target temperature of the first-step esterification reaction is 100-150 ℃, the temperature rise rate of the first-step esterification reaction is 4-6 ℃/min, and the heat preservation time after the first-step esterification reaction reaches the target temperature is 1-2 h.

Preferably, the target temperature of the second esterification reaction is 180-200 ℃, the heating rate from the first esterification reaction to the second esterification reaction is 2-3 ℃/min, and the heat preservation time after the second esterification reaction reaches the target temperature is 2-3 h.

Preferably, the target temperature of the esterification reaction in the third step is 230-260 ℃, the heating rate from the temperature rise of the esterification reaction in the second step to the temperature rise of the esterification reaction in the third step is 1-2 ℃/min, and the heat preservation time after the esterification reaction in the third step reaches the target temperature is 3-5 h.

Preferably, the mixing in the step (2) is performed in a stirring state, the rotation speed of the stirring is 1000-1500 rpm, and the stirring time is 1-2 h.

The invention provides a fireproof coating, which comprises polyol, organic acid, a monomer, a silicone-acrylate emulsion, a solvent, a leveling agent and a filler. The invention also provides a preparation method of the fireproof coating, wherein the polyhydric alcohol, the organic acid and the monomer are subjected to esterification reaction, and the esterification reaction is fully performed by adopting a step-by-step heating mode in the reaction process; and then mixing the intermediate component obtained by the esterification reaction with the rest raw materials to obtain the fireproof coating. The preparation method provided by the invention is simple and efficient, can effectively disperse the coating, does not cause the phenomena of agglomeration and the like after obtaining a finished product, and is suitable for large-scale preparation.

Detailed Description

The invention provides a fireproof coating which is prepared from the following raw materials in parts by mass: 50-60 parts of polyol, 50-60 parts of organic acid, 30-40 parts of monomer, 20-30 parts of silicone-acrylic emulsion, 30-40 parts of solvent, 5-10 parts of flatting agent and 10-15 parts of filler.

In the present invention, the amount of the polyol is 50 to 60 parts, preferably 52 to 58 parts, and more preferably 54 to 56 parts.

In the present invention, the polyhydric alcohol preferably contains one or more of 1, 3-propanediol, 1, 4-butanediol, glycerol, and pentaerythritol.

In the present invention, the organic acid is 50 to 60 parts, preferably 52 to 58 parts, and more preferably 54 to 56 parts.

In the present invention, the organic acid is preferably isophthalic acid, terephthalic acid, adipic acid or glutaric acid.

In the present invention, the monomer is 30 to 40 parts, preferably 32 to 38 parts, and more preferably 34 to 36 parts.

In the present invention, the monomer is preferably tung oil, linseed oil or catalpa oil.

In the invention, the silicone-acrylic emulsion is 20-30 parts, preferably 22-28 parts, and more preferably 24-26 parts.

According to the invention, the silicone-acrylate emulsion is added, so that the corrosion resistance and the anti-fouling capability of the coating can be effectively improved, and the failure of the whole coating caused by the damage of a local coating after the coating is finished can be prevented.

In the present invention, the solvent is 30 to 40 parts, preferably 32 to 38 parts, and more preferably 34 to 36 parts.

In the present invention, the solvent is preferably diethylene glycol methyl ether, diethylene glycol ethyl ether, or diethylene glycol butyl ether.

In the invention, the leveling agent is 5-10 parts, preferably 6-9 parts, and more preferably 7-8 parts.

In the present invention, the leveling agent is preferably BYK306 or AFCONA 3777.

In the present invention, the filler is 10 to 15 parts, preferably 11 to 14 parts, and more preferably 12 to 13 parts.

In the present invention, the filler is preferably talc, zinc stearate or kaolin.

In the invention, pigment can be added into the fireproof coating according to needs, and the pigment is preferably 5-10 parts, more preferably 6-9 parts, and more preferably 7-8 parts.

The invention also provides a preparation method of the fireproof coating, which comprises the following steps:

(1) mixing polyalcohol, organic acid and monomer, and performing esterification reaction to obtain an intermediate component;

(2) and mixing the intermediate component with the rest raw materials to obtain the fireproof coating.

In the present invention, the esterification reaction in the step (1) is preferably performed under a stirring condition, and the rotation speed of the stirring is preferably 150 to 200rpm, more preferably 160 to 190rpm, and even more preferably 170 to 180 rpm.

In the present invention, the esterification reaction in the step (1) is preferably carried out by sequentially carrying out a first esterification reaction, a second esterification reaction and a third esterification reaction.

In the invention, the target temperature of the first esterification reaction is preferably 100-150 ℃, more preferably 110-140 ℃, and more preferably 120-130 ℃; the temperature rise rate of the first-step esterification reaction is preferably 4-6 ℃/min, more preferably 4.4-5.6 ℃/min, and even more preferably 4.8-5.2 ℃/min; the heat preservation time after the first-step esterification reaction reaches the target temperature is preferably 1-2 h, more preferably 1.2-1.8 h, and even more preferably 1.4-1.6 h.

In the invention, the target temperature of the second esterification reaction is preferably 180-200 ℃, more preferably 183-197 ℃, and more preferably 186-194 ℃; the heating rate from the first esterification reaction to the second esterification reaction is preferably 2-3 ℃/min, more preferably 2.2-2.8 ℃/min, and even more preferably 2.4-2.6 ℃/min; the heat preservation time after the second esterification reaction reaches the target temperature is preferably 2-3 h, more preferably 2.2-2.8 h, and even more preferably 2.4-2.6 h.

In the invention, the target temperature of the esterification reaction in the third step is preferably 230-260 ℃, more preferably 240-250 ℃, and more preferably 243-247 ℃; the heating rate from the second esterification reaction to the third esterification reaction is preferably 1-2 ℃/min, more preferably 1.2-1.8 ℃/min, and even more preferably 1.4-1.6 ℃/min; the heat preservation time after the esterification reaction in the third step reaches the target temperature is preferably 3-5 h, more preferably 3.5-4.5 h, and even more preferably 3.8-4.2 h.

In the invention, through esterification reaction, acid, alcohol and monomer are subjected to esterification reaction, and the obtained alkyd resin can effectively improve the flash point of the coating, thereby improving the fire resistance of the coating.

In the invention, the mixing in the step (2) is preferably carried out in a stirring state, and the rotation speed of the stirring is preferably 1000-1500 rpm, more preferably 1100-1400 rpm, and more preferably 1200-1300 rpm; the stirring time is preferably 1-2 h, more preferably 1.2-1.8 h, and even more preferably 1.4-1.6 h.

The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.

Example 1

55 parts of 1, 3-propylene glycol, 55 parts of isophthalic acid, 35 parts of tung oil, 25 parts of silicone-acrylic emulsion, 35 parts of diethylene glycol monomethyl ether, 7 parts of BYK306 and 13 parts of talcum powder.

The preparation method comprises the following steps: mixing 1, 3-propylene glycol, isophthalic acid and tung oil, controlling the stirring speed at 200rpm, heating to 135 ℃ according to the heating rate of 5 ℃/min, and preserving heat for 1.5 hours after the temperature reaches 135 ℃ to complete the first-step esterification reaction; after the heat preservation is finished, controlling the heating rate to be 2.5 ℃/min, heating to 190 ℃, and preserving the heat for 2.5h after the temperature reaches 190 ℃ to finish the second esterification reaction; after the heat preservation is finished, controlling the heating rate to be 1.5 ℃/min, heating to 245 ℃, and preserving heat for 4 hours after the temperature reaches 245 ℃ to finish the third step of esterification reaction to obtain an intermediate component;

and mixing the intermediate component and the rest raw materials, and stirring at the rotating speed of 1500rpm for 1.5h to obtain the fireproof coating.

The fire-retardant coating prepared in this example was subjected to a performance test and the results are reported in table 1.

Example 2

52 parts of 1, 4-butanediol, 54 parts of terephthalic acid, 32 parts of linseed oil, 20 parts of silicone-acrylic emulsion, 30 parts of diethylene glycol ethyl ether, 9 parts of AFCONA3777 and 14 parts of zinc stearate.

The preparation method comprises the following steps: mixing 1, 4-butanediol, terephthalic acid and linseed oil, controlling the stirring speed to be 150rpm, heating to 110 ℃ according to the heating rate of 4 ℃/min, and preserving heat for 1.4h after the temperature reaches 110 ℃ to finish the first-step esterification reaction; after the heat preservation is finished, controlling the heating rate to be 2.2 ℃/min, heating to 190 ℃, and preserving the heat for 2h after the temperature reaches 190 ℃ to finish the second esterification reaction; after the heat preservation is finished, controlling the heating rate to be 1.8 ℃/min, heating to 240 ℃, preserving the heat for 3h after the temperature reaches 240 ℃, and finishing the third step of esterification reaction to obtain an intermediate component;

and mixing the intermediate component and the rest raw materials, and stirring at the rotating speed of 1400rpm for 1.4h to obtain the fireproof coating.

The fire-retardant coating prepared in this example was subjected to a performance test and the results are reported in table 1.

Example 3

54 parts of glycerol, 56 parts of adipic acid, 34 parts of catalpol oil, 24 parts of silicone-acrylic emulsion, 34 parts of butyl diglycol, 9 parts of BYK306 and 11 parts of kaolin.

The preparation method comprises the following steps: mixing glycerol, adipic acid and catalpa oil, controlling the stirring speed at 170rpm, heating to 120 ℃ according to the heating rate of 4.8 ℃/min, and preserving heat for 1.4h after the temperature reaches 120 ℃ to complete the first-step esterification reaction; after the heat preservation is finished, controlling the heating rate to be 2.4 ℃/min, heating to 186 ℃, and preserving the heat for 2.4h after the temperature reaches 186 ℃ to finish the second esterification reaction; after the heat preservation is finished, controlling the heating rate to be 1.4 ℃/min, heating to 243 ℃, preserving the heat for 3.8 hours after the temperature reaches 243 ℃, and finishing the esterification reaction in the third step to obtain an intermediate component;

and mixing the intermediate component and the rest raw materials, and stirring at the rotating speed of 1200rpm for 1.4h to obtain the fireproof coating.

The fire-retardant coating prepared in this example was subjected to a performance test and the results are reported in table 1.

Example 4

56 parts of pentaerythritol, 56 parts of glutaric acid, 36 parts of tung oil, 26 parts of silicone-acrylic emulsion, 36 parts of diethylene glycol monomethyl ether, 8 parts of BYK306 and 12 parts of talcum powder.

The preparation method comprises the following steps: mixing pentaerythritol, glutaric acid and tung oil, controlling the stirring speed to be 180rpm, heating to 130 ℃ according to the heating rate of 5.2 ℃/min, and preserving heat for 1.6 hours after the temperature reaches 130 ℃ to complete the first-step esterification reaction; after the heat preservation is finished, controlling the heating rate to be 2.6 ℃/min, heating to 194 ℃, and preserving the heat for 2.6h after the temperature reaches 194 ℃ to finish the second step of esterification reaction; after the heat preservation is finished, controlling the heating rate to be 1.6 ℃/min, heating to 247 ℃, preserving the heat for 4.2h after the temperature reaches 247 ℃, and finishing the esterification reaction in the third step to obtain an intermediate component;

and mixing the intermediate component and the rest raw materials, and stirring at the rotating speed of 1300rpm for 1.6h to obtain the fireproof coating.

The fire-retardant coating prepared in this example was subjected to a performance test and the results are reported in table 1.

Example 5

58 parts of 1, 3-propylene glycol, 58 parts of adipic acid, 38 parts of linseed oil, 28 parts of silicone-acrylic emulsion, 38 parts of diethylene glycol ethyl ether, 8 parts of AFCONA3777 and 12 parts of zinc stearate.

The preparation method comprises the following steps: mixing 1, 3-propylene glycol, adipic acid and linseed oil, controlling the stirring speed to be 190rpm, heating to 140 ℃ according to the heating rate of 5.6 ℃/min, and preserving heat for 1.8h after the temperature reaches 140 ℃ to complete the first-step esterification reaction; after the heat preservation is finished, controlling the heating rate to be 2.8 ℃/min, heating to 197 ℃, and preserving the heat for 2.8h after the temperature reaches 197 ℃ to finish the second esterification reaction; after the heat preservation is finished, controlling the heating rate to be 1.8 ℃/min, heating to 250 ℃, and preserving heat for 4.5 hours after the temperature reaches 250 ℃ to finish the third step of esterification reaction to obtain an intermediate component;

and mixing the intermediate component and the rest raw materials, and stirring at the rotating speed of 1400rpm for 1.8h to obtain the fireproof coating.

The fire-retardant coating prepared in this example was subjected to a performance test and the results are reported in table 1.

Comparative example 1

This comparative example is different from example 1 in that 55 parts of an epoxy resin was used in place of 1, 3-propanediol, isophthalic acid and tung oil in example 1, and the remaining raw materials, amounts and preparation methods were the same as in example 1.

The coatings prepared in this comparative example were subjected to performance testing and the results are reported in table 1.

Comparative example 2

The difference between the comparative example and example 1 is that no silicone-acrylic emulsion is added in the comparative example, and the rest of the raw materials, the amount and the preparation method are the same as those in example 1.

The coatings prepared in this comparative example were subjected to performance testing and the results are reported in table 1.

Comparative example 3

The comparative example is different from example 1 in that 1, 3-propanediol is 10 parts, and the rest of raw materials, the amount and the preparation method are the same as those of example 1.

The coatings prepared in this comparative example were subjected to performance testing and the results are reported in table 1.

TABLE 1 test results

The embodiment shows that the fireproof coating provided by the invention has the advantages that the fire resistance can reach 3.8h, the fireproof performance is excellent, the bonding strength can reach 0.86Mpa, the water resistance can reach 34h, and the cold and heat cycle resistance can reach 35 times; as can be seen from comparative example 1, the combination of the polyhydric alcohol, the monomer and the carboxylic acid in the invention can effectively improve the fire resistance of the coating; as can be seen from the comparative example 2, the addition of the silicone-acrylate emulsion is the basis for improving the surface integrity of the coating after film formation, and the failure of the coating protection effect caused by cracking of the coating can be greatly reduced; as can be seen from comparative example 3, too much or too little acid and alcohol both affect the properties of the coating, not only the fire resistance, but also the film formation and integrity of the coating, so the coating was formulated within the range of raw materials provided by the present invention. In conclusion, the coating provided by the invention has high fire resistance limit and no reduction of other properties, and is a fireproof coating with excellent comprehensive properties.

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.