CN116715989A - Solvent-free system colored sand suspending agent, preparation method thereof and colored sand coating - Google Patents
Solvent-free system colored sand suspending agent, preparation method thereof and colored sand coating Download PDFInfo
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- CN116715989A CN116715989A CN202310676089.2A CN202310676089A CN116715989A CN 116715989 A CN116715989 A CN 116715989A CN 202310676089 A CN202310676089 A CN 202310676089A CN 116715989 A CN116715989 A CN 116715989A
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- color sand
- suspending agent
- solvent
- free system
- glycidyl ether
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- 239000004576 sand Substances 0.000 title claims abstract description 125
- 239000000375 suspending agent Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000576 coating method Methods 0.000 title claims description 39
- 239000011248 coating agent Substances 0.000 title claims description 29
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 45
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000000178 monomer Substances 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 18
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
- -1 acrylic acid furan ester Chemical class 0.000 claims abstract description 12
- 239000003999 initiator Substances 0.000 claims abstract description 12
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 17
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 16
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 14
- LCXXNKZQVOXMEH-UHFFFAOYSA-N Tetrahydrofurfuryl methacrylate Chemical compound CC(=C)C(=O)OCC1CCCO1 LCXXNKZQVOXMEH-UHFFFAOYSA-N 0.000 claims description 11
- 229920005989 resin Polymers 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 11
- HRWYHCYGVIJOEC-UHFFFAOYSA-N 2-(octoxymethyl)oxirane Chemical group CCCCCCCCOCC1CO1 HRWYHCYGVIJOEC-UHFFFAOYSA-N 0.000 claims description 9
- 239000003085 diluting agent Substances 0.000 claims description 8
- 125000005250 alkyl acrylate group Chemical group 0.000 claims description 7
- 229910000278 bentonite Inorganic materials 0.000 claims description 7
- 239000000440 bentonite Substances 0.000 claims description 7
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 6
- 239000003822 epoxy resin Substances 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- 239000000945 filler Substances 0.000 claims description 5
- XNYMEGZIZQYIEX-UHFFFAOYSA-N furan;prop-2-enoic acid Chemical compound C=1C=COC=1.OC(=O)C=C XNYMEGZIZQYIEX-UHFFFAOYSA-N 0.000 claims description 5
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 5
- ATZHWSYYKQKSSY-UHFFFAOYSA-N tetradecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C(C)=C ATZHWSYYKQKSSY-UHFFFAOYSA-N 0.000 claims description 5
- VEPKQEUBKLEPRA-UHFFFAOYSA-N VX-745 Chemical compound FC1=CC(F)=CC=C1SC1=NN2C=NC(=O)C(C=3C(=CC=CC=3Cl)Cl)=C2C=C1 VEPKQEUBKLEPRA-UHFFFAOYSA-N 0.000 claims description 4
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 claims description 4
- MUTNCGKQJGXKEM-UHFFFAOYSA-N tamibarotene Chemical group C=1C=C2C(C)(C)CCC(C)(C)C2=CC=1NC(=O)C1=CC=C(C(O)=O)C=C1 MUTNCGKQJGXKEM-UHFFFAOYSA-N 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 2
- ZNAOFAIBVOMLPV-UHFFFAOYSA-N hexadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C(C)=C ZNAOFAIBVOMLPV-UHFFFAOYSA-N 0.000 claims description 2
- 229920002521 macromolecule Polymers 0.000 claims description 2
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims description 2
- XZHNPVKXBNDGJD-UHFFFAOYSA-N tetradecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C=C XZHNPVKXBNDGJD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000725 suspension Substances 0.000 abstract description 16
- 150000001875 compounds Chemical class 0.000 abstract description 7
- 230000000694 effects Effects 0.000 description 17
- 239000000203 mixture Substances 0.000 description 12
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 8
- 238000010276 construction Methods 0.000 description 8
- 238000007667 floating Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- 239000013530 defoamer Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- RBNPOMFGQQGHHO-UHFFFAOYSA-N glyceric acid Chemical compound OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JTHZUSWLNCPZLX-UHFFFAOYSA-N 6-fluoro-3-methyl-2h-indazole Chemical compound FC1=CC=C2C(C)=NNC2=C1 JTHZUSWLNCPZLX-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 208000003464 asthenopia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229960001506 brilliant green Drugs 0.000 description 1
- HXCILVUBKWANLN-UHFFFAOYSA-N brilliant green cation Chemical compound C1=CC(N(CC)CC)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](CC)CC)C=C1 HXCILVUBKWANLN-UHFFFAOYSA-N 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PZDUWXKXFAIFOR-UHFFFAOYSA-N hexadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCOC(=O)C=C PZDUWXKXFAIFOR-UHFFFAOYSA-N 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- YNXCGLKMOXLBOD-UHFFFAOYSA-N oxolan-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CCCO1 YNXCGLKMOXLBOD-UHFFFAOYSA-N 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention relates to a solvent-free system color sand suspending agent, which comprises a high molecular compound with the following chemical structure:wherein R is 1 Is a straight-chain alkyl group with 12-18 carbon atoms or an isomeric alkyl group thereof; r is R 2 And R is 3 Each of which is a hydrogen atom or a methyl group; wherein m and n represent the degree of polymerization, and m is not less than 1, n is not less than 1, m and n are integers; the preparation method comprises the following steps: adding glycidyl ether and an initiator into a reaction container under a continuous stirring state, stirring until the glycidyl ether and the initiator are dissolved uniformly, adding an acrylic acid alkyl ester monomer and an acrylic acid furan ester monomer, continuously stirring uniformly, vacuumizing the reaction container, filling nitrogen for a plurality of times, and sealing after the reaction container is filled with nitrogen; and then carrying out two-stage heating polymerization reaction to obtain the solvent-free system color sand suspending agent. The color sand suspending agent has excellent suspension characteristics on color sand, shows overall uniformity on treated and untreated color sand, and has good market prospect.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a solvent-free system colored sand suspending agent, a preparation method thereof and a colored sand coating.
Background
The existing terraces are various in types, but most of the terraces are single-color terraces such as brilliant green and light gray. In order to improve the decorative effect of the terrace and improve visual fatigue, a type of colored sand terrace is developed on the market: the natural mineral colored sand particles or artificial synthetic polymer colored particles are used for producing the components of the floor paint directly or through later stage throwing, so that the beautiful effect of uniform colored sand distribution after solidification is achieved.
In the pre-dispersed color sand terrace paint, whether the color sand is uniformly distributed in the system and whether the color is uniformly distributed on the surface directly influences the beautiful effect of the terrace. How to improve the uniform distribution of the color sand in the system and maintain good suspension property is a key factor for determining the quality of the color sand terrace. At present, two types of processed color sand and unprocessed color sand exist in the market, however, even the processed color sand is difficult to ensure good suspension in a system to realize uniform color sand consistency of a surface layer, and particularly, the large-area construction is difficult to avoid the fluctuation of a certain ground, so that the accumulation of the color sand is easy to form, color overflow is caused, and the defects of scraping printing, floating color and the like are formed.
Disclosure of Invention
In order to realize the suspension uniformity of the color sand in a solvent-free system, improve the batch stability of the color sand production and construction and obtain the uniformity and consistency of the color sand for large-area construction, the invention provides a solvent-free system color sand suspending agent, a preparation method thereof and a color sand coating. The color sand suspending agent has excellent color sand suspending property, shows overall uniformity for processed and unprocessed color sand, and has good market prospect.
In order to achieve the above object, the present invention is realized by the following technical scheme:
a solvent-free system color sand suspending agent comprises a macromolecular compound with the following chemical structure:
wherein R is 1 Is a straight-chain alkyl group with 12-18 carbon atoms or an isomeric alkyl group thereof; r is R 2 And R is 3 Each of which is a hydrogen atom or a methyl group; wherein m and n represent the degree of polymerization, and m.gtoreq.1, n.gtoreq.1, m and n are integers.
Preferably, R 1 Is a straight-chain alkyl group having 16 to 18 carbon atoms.
Furthermore, the solvent-free system color sand suspending agent also comprises glycidyl ether which is used as a reactive diluent of the color sand coating to participate in resin curing.
The preparation method of the solvent-free system color sand suspending agent comprises the following steps:
adding glycidyl ether and an initiator into a reaction container under a continuous stirring state, stirring until the glycidyl ether and the initiator are dissolved uniformly, adding an acrylic acid alkyl ester monomer and an acrylic acid furan ester monomer, continuously stirring uniformly, vacuumizing the reaction container, filling nitrogen for a plurality of times, and sealing after the reaction container is filled with nitrogen; then carrying out two-stage heating polymerization reaction to obtain a solvent-free system color sand suspending agent;
the alkyl acrylate monomer comprises one or more of dodecyl acrylate, dodecyl methacrylate, tetradecyl acrylate, tetradecyl methacrylate, hexadecyl acrylate, hexadecyl methacrylate, octadecyl acrylate and octadecyl methacrylate; the acrylic acid furan ester monomer is tetrahydrofurfuryl acrylate or tetrahydrofurfuryl methacrylate.
Further, the glycidyl ether is octyl glycidyl ether; the initiator is azobisisobutyronitrile.
Further, the mass ratio of the alkyl acrylate monomer to the furan acrylate monomer to the glycidyl ether to the initiator is (55-65): (35-45): 100:1.
Preferably, the mass ratio of the alkyl acrylate monomer to the furan acrylate monomer to the glycidyl ether to the initiator is 59:40:100:1.
Further, the two-stage heating polymerization reaction is to perform first-stage polymerization at 68-75 ℃ for 3-8 hours and then second-stage polymerization at 75-85 ℃ for 2-5 hours.
The third aspect of the invention provides a colored sand coating, comprising the following first materials in parts by weight: 25-35 parts of resin, 2-4 parts of diluent, 10-20 parts of colored sand, 0.5-1.5 parts of solvent-free system colored sand suspending agent according to claim 1 or 2, 40-68 parts of filler, 0.5-0.8 part of dispersing agent, 0.3-0.6 part of defoaming agent, 0.1-0.3 part of leveling agent and 0-1 part of color paste;
the color sand coating also comprises a curing agent, and the first material and the curing agent are uniformly mixed according to the mass ratio (3-6): 1 for use.
Further, the filler comprises one or more of heavy calcium carbonate powder, precipitated barium sulfate and bentonite; preferably, the filler is a mixture of heavy calcium carbonate powder, precipitated barium sulfate and bentonite, wherein the mass ratio of the three is 40 (20-25) (0.5-0.8); the curing agent is polyetheramine; the resin is epoxy resin or polyurethane.
The beneficial technical effects are as follows:
according to the invention, an alkyl acrylate monomer (long-chain alkyl) and a furan acrylate monomer are used as polymerization units, azobisisobutyronitrile is used for initiating free radical polymerization, a solvent-free system color sand suspending agent is prepared, and the obtained product comprises glycidyl ether which is added into the color sand coating as a whole besides the suspending agent with the structure of the invention, wherein the glycidyl ether is used as an active diluent to participate in the solidification of resin; the polymer has better floating capability on treated or untreated colored sand in epoxy, polyurethane and other systems, and can ensure that the colored sand shows an overall uniform and consistent suspended colored sand effect in a solvent-free system;
the copolymer of the color sand suspending agent disclosed by the invention has the structural characteristics of meeting the requirements of good adsorption on resin color sand, assisting the color sand to show excellent suspension stability in a solvent-free system, realizing rapid migration of color sand particles to the surface of the coating in the construction process, forming uniform color sand distribution, realizing the overall uniform and attractive color sand effect, and ensuring that the color sand coating added with the color sand suspending agent is uniform in suspension of the color sand in large-area construction, and has no defects of any floating color, joint printing and the like.
Drawings
Fig. 1 is a physical diagram of suspension effect of the color sand coating of the formula P1 and the formula P4 after curing.
Fig. 2 is a physical diagram of suspension effect of the color sand coating of the formula P2, the formula P3 and the formula P5 after curing.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The numerical values set forth in these examples do not limit the scope of the present invention unless specifically stated otherwise. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values.
In addition, the terms "first", "second", etc. are used to define the polymerization process, and are merely for convenience of distinguishing the polymerization steps, and unless otherwise stated, the terms have no special meaning, and thus should not be construed as limiting the scope of the present invention.
The experimental methods in the following examples, for which specific conditions are not noted, are generally determined according to national standards; if the national standard is not corresponding, the method is carried out according to the general international standard or the standard requirements set by related enterprises. Unless otherwise indicated, all parts are parts by weight and all percentages are percentages by weight.
The solvent-free system color sand suspending agent obtained by polymerization in the following example comprises a high molecular compound with a chemical structure shown in the following formula I:
wherein R is 1 Is a straight-chain alkyl group with 12-18 carbon atoms or an isomeric alkyl group thereof; r is R 2 And R is 3 Each of which is a hydrogen atom or a methyl group; wherein m and n represent the degree of polymerization, and m is not less than 1, n is not less than 1, m and n are integers;
the solvent-free system color sand suspending agent also comprises glycidyl ether.
Example 1
The preparation method of the solvent-free system color sand suspending agent comprises the following steps:
preparing materials: octyl glycidyl ether (CAS number 2461-15-6), azodiisobutyronitrile (CAS number 78-76-1), dodecyl acrylate (CAS number 2156-97-0), tetrahydrofurfuryl methacrylate (CAS number 2455-24-5), the mass ratio of the four is 100:1:65:35;
under the continuous stirring state, octyl shrink is added into the reaction vessel according to the proportionStirring the water glycerol ether and the azodiisobutyronitrile until the water glycerol ether and the azodiisobutyronitrile are dissolved uniformly, adding the dodecyl acrylate and the tetrahydrofurfuryl methacrylate, continuously stirring uniformly, vacuumizing the reaction container, filling nitrogen for three times, and sealing after the reaction container is filled with nitrogen; then carrying out two-stage heating polymerization reaction, carrying out first-stage polymerization and then carrying out second-stage polymerization, wherein the temperature of the first-stage polymerization is 68 ℃ and the polymerization time is 7h, the temperature of the second-stage polymerization is 82 ℃ and the polymerization time is 3h, and obtaining the solvent-free system color sand suspending agent, namely the high molecular compound with the chemical structure shown in the formula I in the embodiment 1 Is n-dodecyl, R 2 Is a hydrogen atom, R 3 Is methyl.
Example 2
The preparation method of the solvent-free system color sand suspending agent comprises the following steps:
preparing materials: octyl glycidyl ether (CAS number 2461-15-6), azodiisobutyronitrile (CAS number 78-76-1), tetradecyl methacrylate (CAS number 2549-53-3), tetrahydrofurfuryl acrylate (CAS number 2399-48-6), the mass ratio of the four is 100:1:60:40;
under the continuous stirring state, octyl glycidyl ether and azodiisobutyronitrile are added into a reaction container according to the proportion, after stirring until the mixture is uniformly dissolved, tetradecyl methacrylate and tetrahydrofurfuryl acrylate are added, after continuously stirring uniformly, the reaction container is vacuumized, then nitrogen is filled for three times, and after the reaction container is filled with nitrogen, the reaction container is sealed; then carrying out two-stage heating polymerization reaction, carrying out first-stage polymerization and then carrying out second-stage polymerization, wherein the temperature of the first-stage polymerization is 70 ℃, the polymerization time is 6h, the temperature of the second-stage polymerization is 80 ℃, and the polymerization time is 4h to obtain the solvent-free system color sand suspending agent, namely the suspending agent comprises a high molecular compound with a chemical structure shown as the formula I in the embodiment, wherein R in the formula I 1 Is n-tetradecyl, R 2 Is methyl, R 3 Is a hydrogen atom.
Example 3
The preparation method of the solvent-free system color sand suspending agent comprises the following steps:
preparing materials: octyl glycidyl ether (CAS number 2461-15-6), azodiisobutyronitrile (CAS number 78-76-1), hexadecyl acrylate (CAS number 13402-02-3), tetrahydrofurfuryl methacrylate (CAS number 2455-24-5), the mass ratio of the four is 100:1:59:40;
under the continuous stirring state, octyl glycidyl ether and azodiisobutyronitrile are added into a reaction container according to the proportion, after stirring until the mixture is uniformly dissolved, hexadecyl acrylate and tetrahydrofurfuryl methacrylate are added, after continuously stirring uniformly, the reaction container is vacuumized, then nitrogen is filled for three times, and after the reaction container is filled with nitrogen, the reaction container is sealed; then carrying out two-stage heating polymerization reaction, carrying out first-stage polymerization and then carrying out second-stage polymerization, wherein the temperature of the first-stage polymerization is 70 ℃, the polymerization time is 6h, the temperature of the second-stage polymerization is 80 ℃, and the polymerization time is 4h to obtain the solvent-free system color sand suspending agent, namely the suspending agent comprises a high molecular compound with a chemical structure shown as the formula I in the embodiment, wherein R in the formula I 1 Is normal hexadecyl, R 2 Is a hydrogen atom, R 3 Is methyl.
Example 4
The preparation method of the solvent-free system color sand suspending agent comprises the following steps:
preparing materials: octyl glycidyl ether (CAS number 2461-15-6), azobisisobutyronitrile (CAS number 78-76-1), stearyl acrylate (CAS number 4813-57-4), tetrahydrofurfuryl methacrylate (CAS number 2455-24-5), the mass ratio of the four being 100:1:59:40;
under the continuous stirring state, octyl glycidyl ether and azodiisobutyronitrile are added into a reaction container according to the proportion, after the mixture is stirred until the mixture is uniformly dissolved, octadecyl acrylate and tetrahydrofurfuryl methacrylate are added, after the mixture is continuously uniformly stirred, the reaction container is vacuumized, then nitrogen is filled for three times, and after the reaction container is filled with nitrogen, the reaction container is sealed; then carrying out two-stage heating polymerization reaction, carrying out first-stage polymerization and then carrying out second-stage polymerization, wherein the temperature of the first-stage polymerization is 75 ℃, the polymerization time is 3h, the temperature of the second-stage polymerization is 82 ℃, and the polymerization time is 2h to obtain the solvent-free system color sand suspending agent, namely the suspending agent comprises a high molecular compound with a chemical structure shown as the formula I in the embodiment, wherein R in the formula I 1 Is normal octadecyl, R 2 Is a hydrogen atom, R 3 Is methyl.
Example 5
The suspending agents of the embodiment 1 are respectively applied to color sand coatings, wherein the color sand coatings comprise the following first materials in parts by weight: 30 parts of bisphenol A type epoxy resin E51 resin, 3 parts of 690 diluent, 40 parts of heavy calcium carbonate, 24 parts of precipitated barium sulfate, 0.6 part of dispersing agent tech-598, 0.5 part of defoamer tech-369, 0.2 part of leveling agent tech-257N, 1 part of color paste, 15 parts of color sand (untreated), 0.7 part of bentonite and 1 part of color sand suspending agent of example 1;
uniformly mixing the first material with a curing agent (alicyclic amine 9035 curing agent) according to a mass ratio of 6:1, coating the mixture on a substrate ceramic tile, and curing at normal temperature. The color sand coating of this example is designated as P2.
Example 6
The suspending agents of the embodiment 2 are respectively applied to color sand coatings, wherein the color sand coatings comprise the following first materials in parts by weight: 30 parts of bisphenol A type epoxy resin E51 resin, 3 parts of 690 diluent, 40 parts of heavy calcium carbonate, 24 parts of precipitated barium sulfate, 0.6 part of dispersing agent tech-598, 0.5 part of defoamer tech-369, 0.2 part of leveling agent tech-257N, 1 part of color paste, 15 parts of color sand (hydrophobically modified color sand product provided by Shanghai Dekun), 0.7 part of bentonite and 1 part of color sand suspending agent of example 2;
uniformly mixing the first material with a curing agent (alicyclic amine 9035 curing agent) according to a mass ratio of 6:1, coating the mixture on a substrate ceramic tile, and curing at normal temperature. The color sand coating of this example is designated as P3.
Example 7
The suspending agents of the embodiment 3 are respectively applied to color sand coatings, wherein the color sand coatings comprise the following first materials in parts by weight: 30 parts of bisphenol A type epoxy resin E51 resin, 3 parts of 690 diluent, 40 parts of heavy calcium carbonate, 24 parts of precipitated barium sulfate, 0.6 part of dispersing agent tech-598, 0.5 part of defoamer tech-369, 0.2 part of leveling agent tech-257N, 1 part of color paste, 15 parts of color sand (untreated), 0.7 part of bentonite and 1 part of color sand suspending agent of example 3;
uniformly mixing the first material with a curing agent (alicyclic amine 9035 curing agent) according to a mass ratio of 6:1, coating the mixture on a substrate ceramic tile, and curing at normal temperature. The color sand coating of this example is designated as P4.
Example 8
The suspending agents of the embodiment 4 are respectively applied to color sand coatings, wherein the color sand coatings comprise the following first materials in parts by weight: 30 parts of bisphenol A type epoxy resin E51 resin, 3 parts of 690 diluent, 40 parts of heavy calcium carbonate, 24 parts of precipitated barium sulfate, 0.6 part of dispersing agent tech-598, 0.5 part of defoamer tech-369, 0.2 part of leveling agent tech-257N, 1 part of color paste, 15 parts of color sand (treated, same as the color sand in example 6), 0.7 part of bentonite and 1 part of color sand suspending agent in example 4;
uniformly mixing the first material with a curing agent (alicyclic amine 9035 curing agent) according to a mass ratio of 6:1, coating the mixture on a substrate ceramic tile, and curing at normal temperature. The color sand coating of this example is designated as P5.
Comparative example 1
The formulation of the color sand coating of this comparative example 1 was the same as that of example 7, except that the color sand suspending agent of example 3 was not added. The color sand coating of this comparative example was designated as P1.
The effect evaluation was carried out on the color sand coating materials of examples 5 to 8 and comparative example 1, and the results are shown in Table 1.
Table 1 evaluation of the color sand coating effect of examples 5 to 8 and comparative example 1
(Note: the diameter of the colored sand used above ranges from 30 to 70 mesh)
As can be seen from Table 1, compared with the formulations P1 and P4, the coating P1 without the colored sand suspending agent has the problems of slow migration and suspension speed and small particle number of the colored sand within 30 minutes in the initial stage of construction, the colored sand particles on the hardened surface are not obvious, the particles are sparse, and especially the suspension and migration effects of the untreated colored sand are poor; the suspending agent of the embodiment 3 adopted in the invention P4 has a good suspension migration floating effect on the color sand, and the suspension speed is high and the color sand can be uniformly distributed. The physical diagrams of the suspension effects of the P1 and P4 colored sand coatings after curing are shown in FIG. 1, and it is obvious that the suspension agent of the invention adopted by P4 can obtain the performances of uniform and integral colored sand, uniform distribution, no floating color and excellent suspension effect.
The formulas P2-P5 are respectively added with the colored sand suspending agents of the examples 1, 2, 3 and 4, wherein the solid diagrams of the colored sand suspending effects of the cured colored sand coatings of the formulas P2, P3 and P5 are shown in figure 2, and the polymer compound with the structure of formula I of the invention has excellent suspending performance and uniform dispersion performance on the colored sand, and the colored sand can be completely and rapidly suspended, migrated and floated within 30 minutes in the initial stage of construction, and the hardened colored sand is uniform and uniform in whole and uniformly distributed without floating color; the treated colored sand (P3 and P5) can be quickly and completely suspended, migrated and floated in 10 minutes, and the cured colored sand is uniformly distributed, so that the suspension effect is excellent.
Therefore, the color sand coating provided by the embodiment of the invention has the advantages that the color sand suspending agent provided by the embodiment of the invention is added, so that the color sand can quickly migrate and float up after construction and is uniformly dispersed, and the color sand after solidification is uniform and unified as a whole, and the suspension effect is excellent.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The solvent-free system color sand suspending agent is characterized by comprising a macromolecular compound with the following chemical structure:
wherein R is 1 Is a straight-chain alkyl group with 12-18 carbon atoms or an isomeric alkyl group thereof; r is R 2 And R is 3 Each of which is a hydrogen atom or a methyl group; wherein m and n represent the degree of polymerization, andm is greater than or equal to 1, n is greater than or equal to 1, and m and n are integers.
2. The solvent-free system color sand suspending agent as claimed in claim 1, wherein R 1 Is a straight-chain alkyl group having 16 to 18 carbon atoms.
3. A solvent-free system color sand suspending agent as claimed in claim 1 or 2, wherein the solvent-free system color sand suspending agent further comprises glycidyl ether.
4. A method for preparing a solvent-free system color sand suspending agent according to any one of claims 1 to 3, comprising the steps of:
adding glycidyl ether and an initiator into a reaction container under a continuous stirring state, stirring until the glycidyl ether and the initiator are dissolved uniformly, adding an acrylic acid alkyl ester monomer and an acrylic acid furan ester monomer, continuously stirring uniformly, vacuumizing the reaction container, filling nitrogen for a plurality of times, and sealing after the reaction container is filled with nitrogen; then carrying out two-stage heating polymerization reaction to obtain a solvent-free system color sand suspending agent;
the alkyl acrylate monomer comprises one or more of dodecyl acrylate, dodecyl methacrylate, tetradecyl acrylate, tetradecyl methacrylate, hexadecyl acrylate, hexadecyl methacrylate, octadecyl acrylate and octadecyl methacrylate;
the acrylic acid furan ester monomer is tetrahydrofurfuryl acrylate or tetrahydrofurfuryl methacrylate.
5. The method of claim 4, wherein the glycidyl ether is octyl glycidyl ether; the initiator is azobisisobutyronitrile.
6. The preparation method according to claim 4, wherein the mass ratio of the alkyl acrylate monomer, the furan acrylate monomer, the glycidyl ether and the initiator is (55-65): (35-45): 100:1.
7. The preparation method according to claim 6, wherein the mass ratio of the alkyl acrylate monomer, the furan acrylate monomer, the glycidyl ether and the initiator is 59:40:100:1.
8. The process according to claim 4, wherein the two-stage heating polymerization is performed after the first stage polymerization at 68 to 75℃for 3 to 8 hours and the second stage polymerization at 75 to 85℃for 2 to 5 hours.
9. The color sand coating is characterized by comprising the following first materials in parts by weight: 25-35 parts of resin, 2-4 parts of diluent, 10-20 parts of colored sand, 0.5-1.5 parts of solvent-free system colored sand suspending agent according to any one of claims 1-3, 40-68 parts of filler, 0.5-0.8 part of dispersing agent, 0.3-0.6 part of defoaming agent, 0.1-0.3 part of leveling agent and 0-1 part of color paste;
the color sand coating also comprises a curing agent, and the first material and the curing agent are uniformly mixed according to the mass ratio (3-6): 1 for use.
10. The colored sand coating of claim 9, wherein the filler comprises one or more of heavy calcium carbonate powder, precipitated barium sulfate, bentonite; the curing agent is alicyclic amine 9035 curing agent; the resin is epoxy resin or polyurethane.
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