CN113233919A - Novel stone protective agent and preparation method thereof - Google Patents
Novel stone protective agent and preparation method thereof Download PDFInfo
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- CN113233919A CN113233919A CN202110552228.1A CN202110552228A CN113233919A CN 113233919 A CN113233919 A CN 113233919A CN 202110552228 A CN202110552228 A CN 202110552228A CN 113233919 A CN113233919 A CN 113233919A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5018—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with fluorine compounds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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Abstract
The invention belongs to the technical field of stone protection, and particularly relates to a novel stone protective agent and a preparation method thereof. The stone protective agent provided by the invention comprises the following components in parts by weight: 30-35 parts of silicone oil, 15-20 parts of sodium monofluorophosphate, 1-2 parts of tripterygium wilfordii extract, 4-6 parts of curing agent, 1-3 parts of tea polyphenol, 1-3 parts of emulsifier, 2-3 parts of thickener, 5-8 parts of auxiliary enhancer, 200.5-1 parts of tween-200.5 and 60-80 parts of water. The stone protective agent provided by the invention belongs to fluorine-silicon protective agents, can directly permeate into stone in the using process, and cannot generate any influence on the surface of the stone, and the stone protective agent provided by the invention can achieve the effects of efficient sterilization, water prevention, moisture prevention, ageing resistance, microbial corrosion prevention and the like.
Description
Technical Field
The invention belongs to the technical field of stone protection, and particularly relates to a novel stone protective agent and a preparation method thereof.
Background
The stone protective agent is prepared by brushing, spraying, coating, rolling, spraying, soaking and the like, so that the stone protective agent is uniformly distributed on the surface of the stone or permeates into the stone to form protection, and the stone has the functions of water resistance, pollution resistance, acid and alkali resistance, ageing resistance, freeze thawing resistance, biological corrosion resistance and the like, thereby achieving the effects of prolonging the service life of the stone and improving the decorative performance of the stone. At present, the known stone protective agents have various classification modes, but generally have the effects of water resistance, soil resistance and oil resistance.
The novel oil-stain-resistant nanometer perfluorinated stone protective agent disclosed in the Chinese patent application CN110437734A comprises inorganic nanometer materials, silane coupling agents, perfluorinated organic matters, modified silicone oil and other components, and solves the problems that the surface of a stone product is easily damaged by oil stains and the service life of stone is shortened in the prior art, but the stone protective agent is easy to increase the toxicity of the protective agent due to the addition of a large amount of organic components, and the protective agent is also easily polluted by bacteria in the spraying process.
Most of the existing silicon-fluorine protective agents are insoluble in water, have poor antibacterial performance, are easily corroded by bacteria to prolong the penetration time of the protective agents, and along with the wider application range of the protective agents, the problems become a problem to be solved urgently in the field.
Disclosure of Invention
Aiming at the defects generally existing in the prior art, the invention provides a novel stone protective agent which can directly permeate into stone, does not have any influence on the surface of the stone, and can achieve the effects of efficient degerming, water prevention, moisture prevention, ageing resistance, microbial corrosion prevention and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
a novel stone protective agent comprises the following components in parts by weight: 30-35 parts of silicone oil, 15-20 parts of sodium monofluorophosphate, 1-2 parts of tripterygium wilfordii extract, 4-6 parts of curing agent, 1-3 parts of tea polyphenol, 1-3 parts of emulsifier, 2-3 parts of thickener, 5-8 parts of auxiliary reinforcing agent, 200.5-1 parts of tween-200.5 and 60-80 parts of water.
Preferably, the composition comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water.
Preferably, the preparation process of the silicone oil is as follows: adding 3-5 times of purified water into dimethyldichlorosilane at the temperature of 30-40 ℃, reacting for 1-2h to obtain a primary condensed ring body, and cracking and rectifying the ring body to obtain a low ring body; and then adding an MDM end sealing agent and active carbon as a catalyst, and mixing for 2 hours to obtain the catalyst.
Preferably, the curing agent is prepared from 3-dimethylaminopropylamine and 2-methylimidazole according to the weight ratio of 7-11: 2-5; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 15-20: 1 to 2.
Preferably, the curing agent is prepared by mixing 3-dimethylamino propylamine and 2-methylimidazole in a weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4.
Preferably, the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 5-7: 9-12; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate in a weight ratio of 1-2: 10-13: 4 to 7.
Preferably, the thickening agent is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate according to the weight ratio of 1.6: 11: 5.
The invention also provides a preparation method of the novel stone protective agent, which comprises the following steps:
s1, mixing the emulsifier with the silicone oil, and reacting at 40-50 ℃ for 40-50 min to obtain emulsified silicone oil;
s2, heating water to 50-60 ℃, adding the emulsified silicone oil prepared in the step S1 into the water, continuously adding sodium monofluorophosphate, tripterygium wilfordii extract and tea polyphenol into the water, and mixing and stirring uniformly to prepare a mixture I;
s3, cooling the mixture I prepared in the step S2 to 20-30 ℃, adding the thickening agent, the auxiliary reinforcing agent and the Tween-20, and uniformly mixing and stirring to prepare a mixture II;
s4, adding a curing agent into the mixture II prepared in the step S3, heating to 60-65 ℃, treating for 1-1.5 hours, and continuously heating to 120-130 ℃ for treating for 3-4 hours to obtain the modified epoxy resin.
Preferably, the mixing and stirring condition in the step S2 is stirring at a rotation speed of 800-1000 rpm for 20-30 min.
Preferably, the mixing and stirring condition in step S3 is stirring at 500-600 rpm for 30-40 min.
The fluorosilicone type stone protective agent provided by the invention belongs to a water-soluble protective agent, is different from a common fluorosilicone type protective agent, does not need to add an organic solvent, avoids the harm to the environment caused by the addition of a large amount of organic solvent, and can effectively reduce the toxic action brought by fluorine substances because the content of added silicone oil is greater than that of sodium monofluorophosphate in the process of preparing the protective agent.
In the further research and development process, the inventor discovers that the sterilization function of the protective agent can be effectively improved by adding a trace amount of tripterygium wilfordii extract into the protective agent, the anti-aging effect of the protective agent can be effectively improved by tea polyphenol, a small amount of tripterygium wilfordii extract and the tea polyphenol are added simultaneously, the time for the protective agent to permeate into stone is shortened, and the waste of the protective agent is effectively reduced.
Compared with the prior art, the novel stone protective agent provided by the invention has the following advantages:
(1) according to the novel stone protective agent provided by the invention, water-soluble silicone oil and sodium monofluorophosphate are added, so that the harm to the environment is effectively reduced;
(2) according to the novel stone protective agent provided by the invention, a small amount of tripterygium wilfordii extract and tea polyphenol are added, so that the sterilization function and the anti-aging effect of the protective agent are improved, the waterproof and moistureproof performances are improved by the aid of the reinforcing agent, and the erosion of microorganisms is effectively reduced;
(3) the novel stone protective agent provided by the invention has the advantages that the temperature is strictly controlled in the preparation process, the finally prepared protective agent has quick stone penetration time, and the waste of the protective agent is reduced.
Detailed Description
The present invention is further explained with reference to the following specific examples, but it should be noted that the following examples are only illustrative of the present invention and should not be construed as limiting the present invention, and all technical solutions similar or equivalent to the present invention are within the scope of the present invention. The method and the device are operated according to the conventional technical method and the content of the instrument instruction, wherein the specific technology or condition is not indicated in the embodiment; the reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
The sodium monofluorophosphate can be purchased from Hubei Yunw science and technology Limited, and has the CAS number of 10163-15-2; the Tripterygium wilfordii hook F extract can be purchased from Xianfu Zhengyuan biotechnology limited; the tea polyphenols can be purchased from Nanjing Songguan Biotech limited; the MDM capping agent is available from shanghai hao Chong chemical ltd; the polysorbate 80 is available from hebeipengyu biotechnology limited; the saponin is available from pharmaceutical chemical industry Co., Ltd, CAS number 11006-75-0.
Example 1A novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 30 parts of silicone oil, 15 parts of sodium monofluorophosphate, 1 part of tripterygium wilfordii extract, 4 parts of curing agent, 1 part of tea polyphenol, 1 part of emulsifier, 2 parts of thickener, 5 parts of auxiliary reinforcing agent, 200.5 parts of tween-and 60 parts of water; the preparation process of the silicone oil comprises the following steps: adding 3 times of purified water into dimethyldichlorosilane at the temperature of 30 ℃, reacting for 1h to obtain a primary condensed ring body, and cracking and rectifying the ring body to obtain a low ring body; then adding an MDM end sealing agent and active carbon as a catalyst, and mixing for 2 hours to obtain the catalyst; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to a weight ratio of 7: 2, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin according to a weight ratio of 15: 1, preparing a composition; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 5: 9 is prepared; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate in a weight ratio of 1: 10: 4.
The preparation method of the novel stone protective agent comprises the following steps:
s1, mixing the emulsifier with the silicone oil, and reacting at 40 ℃ for 40min to obtain emulsified silicone oil;
s2, heating water to 50 ℃, adding the emulsified silicone oil prepared in the step S1 into the water, continuously adding sodium monofluorophosphate, tripterygium wilfordii hook F extract and tea polyphenol into the water, stirring at the rotating speed of 800rpm for 20min, and uniformly mixing to obtain a mixture I;
s3, cooling the mixture I prepared in the step S2 to 20 ℃, adding the thickening agent, the auxiliary reinforcing agent and the Tween-20, stirring at the rotating speed of 500rpm for 30min until the mixture is uniformly mixed and stirred to prepare a mixture II;
s4, adding a curing agent into the mixture II prepared in the step S3, heating to 60 ℃, treating for 1h, and continuously heating to 120 ℃ for treating for 3h to obtain the modified epoxy resin.
Example 2A novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 35 parts of silicone oil, 20 parts of sodium monofluorophosphate, 2 parts of tripterygium wilfordii extract, 6 parts of curing agent, 3 parts of tea polyphenol, 3 parts of emulsifier, 3 parts of thickener, 8 parts of auxiliary reinforcing agent, 201 parts of tween-and 80 parts of water; the preparation process of the silicone oil comprises the following steps: adding 5 times of purified water into dimethyldichlorosilane at 40 ℃, reacting for 2h to obtain a primary condensed ring body, and cracking and rectifying the ring body to obtain a low ring body; then adding an MDM end sealing agent and active carbon as a catalyst, and mixing for 2 hours to obtain the catalyst; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 11: 5, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 20: 2, preparing a composition; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 7: 12; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate in a weight ratio of 2: 13: 7.
The preparation method of the novel stone protective agent comprises the following steps:
s1, mixing the emulsifier with the silicone oil, and reacting for 50min at 50 ℃ to obtain emulsified silicone oil;
s2, heating water to 60 ℃, adding the emulsified silicone oil prepared in the step S1 into the water, continuously adding sodium monofluorophosphate, tripterygium wilfordii hook F extract and tea polyphenol into the water, stirring for 30min at the rotating speed of 1000rpm until the mixture is uniformly stirred, and preparing a mixture I;
s3, cooling the mixture I prepared in the step S2 to 30 ℃, adding the thickening agent, the auxiliary reinforcing agent and the Tween-20, stirring at the rotating speed of 600rpm for 40min until the mixture is uniformly mixed, and preparing a mixture II;
s4, adding a curing agent into the mixture II prepared in the step S3, heating to 65 ℃, treating for 1.5h, and continuously heating to 130 ℃ for treating for 4h to obtain the modified epoxy resin.
Example 3A novel stone protectant
The novel stone protective agent comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water; the preparation process of the silicone oil comprises the following steps: adding 4 times of purified water into dimethyldichlorosilane at 35 ℃, reacting for 1.5h to obtain a primary condensed ring body, and cracking and rectifying the ring body to obtain a low ring body; then adding an MDM end sealing agent and active carbon as a catalyst, and mixing for 2 hours to obtain the catalyst; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate according to the weight ratio of 1.6: 11: 5.
The preparation method of the novel stone protective agent comprises the following steps:
s1, mixing the emulsifier with the silicone oil, and reacting for 45min at 45 ℃ to obtain emulsified silicone oil;
s2, heating water to 55 ℃, adding the emulsified silicone oil prepared in the step S1 into the water, continuously adding sodium monofluorophosphate, tripterygium wilfordii hook F extract and tea polyphenol into the water, stirring at 850rpm for 25min, and uniformly mixing to obtain a mixture I;
s3, cooling the mixture I prepared in the step S2 to 25 ℃, adding the thickening agent, the auxiliary reinforcing agent and the Tween-20 into the mixture I, stirring the mixture I at the rotation speed of 550rpm for 35min, and uniformly mixing and stirring the mixture I to prepare a mixture II;
s4, adding a curing agent into the mixture II prepared in the step S3, heating to 63 ℃ for processing for 1.2h, and continuously heating to 125 ℃ for processing for 3.5h to obtain the modified epoxy resin.
Comparative example 1 novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 5 parts of a curing agent, 2 parts of tea polyphenol, 2 parts of an emulsifier, 2.5 parts of a thickening agent, 6 parts of an auxiliary reinforcing agent, 200.8 parts of tween-tween and 70 parts of water; the preparation process of the silicone oil is the same as that of example 3; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate according to the weight ratio of 1.6: 11: 5.
The preparation method of the novel stone protective agent is similar to that of the embodiment 3;
the difference from example 3 is that comparative example 1 does not contain the extract of tripterygium wilfordii.
Comparative example 2 novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water; the silicone oil is purchased from Dongguan local textile auxiliary company Limited; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate according to the weight ratio of 1.6: 11: 5.
The preparation method of the novel stone protective agent is similar to that of the embodiment 3;
the difference from example 3 is that the silicone oil in comparative example 2 is selected from commercially available hydrophilic silicone oils.
Comparative example 3 novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water; the preparation process of the silicone oil is the same as that of example 3; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 1: 1, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate according to the weight ratio of 1.6: 11: 5.
The preparation method of the novel stone protective agent is similar to that of the embodiment 3;
the difference from example 3 is that the curing agent in comparative example 3 is prepared from 3-dimethylaminopropylamine and 2-methylimidazole in a weight ratio of 1: 1.
Comparative example 4 novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water; the preparation process of the silicone oil is the same as that of example 3; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 1: 1, preparing a composition; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate according to the weight ratio of 1.6: 11: 5.
The preparation process of the novel stone protective agent is similar to that of the embodiment 3;
the difference from example 3 is that the emulsifier in comparative example 4 is prepared from polysorbate 80 and saponin in a weight ratio of 1: 1.
Comparative example 5 novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water; the preparation process of the silicone oil comprises the following steps: adding 4 times of purified water into dimethyldichlorosilane at 35 ℃, reacting for 1.5h to obtain a primary condensed ring body, and cracking and rectifying the ring body to obtain a low ring body; then adding an MDM end sealing agent and active carbon as a catalyst, and mixing for 2 hours to obtain the catalyst; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 1: 1, preparing a composition; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate according to the weight ratio of 1.6: 11: 5.
The preparation method of the novel stone protective agent is similar to that of the embodiment 3;
the difference from example 3 is that the thickener in comparative example 5 is prepared from hydroxypropyl methylcellulose and sodium polyacrylate in a weight ratio of 1: 1.
Comparative example 6 novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water; the preparation process of the silicone oil is similar to that of example 3; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate in a weight ratio of 1: 1: 1.
The preparation method of the novel stone protective agent is similar to that of the embodiment 3;
the difference from example 3 is that the auxiliary enhancer in comparative example 6 is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate in a weight ratio of 1: 1: 1.
Comparative example 7 novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water; the preparation process of the silicone oil comprises the following steps: adding 4 times of purified water into dimethyldichlorosilane at 35 ℃, reacting for 1.5h to obtain a primary condensed ring body, and cracking and rectifying the ring body to obtain a low ring body; then adding an MDM end sealing agent and active carbon as a catalyst, and mixing for 2 hours to obtain the catalyst; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from nisin and sodium hexametaphosphate according to the weight ratio of 11: 5.
The preparation method of the novel stone protective agent is similar to that of the embodiment 3;
the difference from example 3 is that the auxiliary enhancer in comparative example 7 is prepared from nisin and sodium hexametaphosphate in a weight ratio of 11: 5.
Comparative example 8 novel stone protective agent
The novel stone protective agent comprises the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water; the preparation process of the silicone oil comprises the following steps: adding 4 times of purified water into dimethyldichlorosilane at 35 ℃, reacting for 1.5h to obtain a primary condensed ring body, and cracking and rectifying the ring body to obtain a low ring body; then adding an MDM end sealing agent and active carbon as a catalyst, and mixing for 2 hours to obtain the catalyst; the curing agent is prepared from 3-dimethylamino propylamine and 2-methylimidazole according to the weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4; the thickener is prepared from hydroxypropyl methyl cellulose and sodium polyacrylate according to a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate according to the weight ratio of 1.6: 11: 5.
The preparation method of the novel stone protective agent comprises the step of mixing and stirring the components uniformly at 25 ℃ to obtain the novel stone protective agent.
Test example 1 Performance test
1. Test samples: the novel stone protective agent prepared in the embodiments 1-3 and the comparative examples 1-8 of the invention;
2. the test method comprises the following steps: the novel stone protective agents prepared in the examples 1-3 and the comparative examples 1-8 are respectively coated on marble, the performance indexes are detected according to JC/T973-.
3. And (3) test results: the specific test results are shown in table 1 below:
TABLE 1 results of testing the properties of examples 1-3
TABLE 2 results of performance measurements of comparative examples 1 to 8
As can be seen from table 1, the performances of the novel stone protective agent prepared in the embodiments 1 to 3 of the present invention all meet the standards of the superior products, the inventors further continue to select other stones (such as granite, travertine, etc.) for performance tests, and the indexes of the superior products can be achieved as well, and when the inventors dilute the novel stone protective agent prepared in the present invention by 3 to 5 times, the performance indexes of the novel stone protective agent can still reach the performance indexes of the superior products, so that the addition amount of the novel stone protective agent is effectively reduced.
While table 2, which corresponds to table 1, gives the performance index for each group of comparative examples, it can be seen from table 2 that each performance of the groups of comparative examples 1-8 is degraded to different degrees, which just demonstrates the interaction of the components in the present invention.
Test example 2 penetration time comparison
1. Test samples: the novel stone protective agents prepared in examples 1 to 3 and comparative examples 1 to 8;
2. the test process comprises the following steps: taking 5mL of the stone protective agent respectively, and then taking 7 multiplied by 4 multiplied by 5cm3Pouring the stone protective agent on 11 marble blocks simultaneously and slowly, and recording the disappearance time of the stone protective agent on the marble;
3. and (3) test results: see table 3 for specific test results.
TABLE 3 comparison of the penetration times of the different test samples
As can be seen from the above Table 2, the penetration time of the novel stone protective agent prepared in the examples 1-3 of the present invention is significantly shorter than that of the comparative example, which prevents the solution loss caused by evaporation, sprinkling, etc. during the addition of the stone protective agent, especially, the penetration time of the novel stone protective agent prepared in the comparative example 1 and the novel stone protective agent prepared in the comparative examples 6-8 is 4.6min shorter than that of the best example 3, which further embodies the mutual promotion effect among the components of the present invention.
Finally, it should be noted that the above-described embodiments are described to facilitate understanding and use of the invention by those of ordinary skill in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. The novel stone protective agent is characterized by comprising the following components in parts by weight: 30-35 parts of silicone oil, 15-20 parts of sodium monofluorophosphate, 1-2 parts of tripterygium wilfordii extract, 4-6 parts of curing agent, 1-3 parts of tea polyphenol, 1-3 parts of emulsifier, 2-3 parts of thickener, 5-8 parts of auxiliary reinforcing agent, 200.5-1 parts of tween-200.5 and 60-80 parts of water.
2. The novel stone protective agent as claimed in claim 1, characterized by comprising the following components in parts by weight: 32 parts of silicone oil, 18 parts of sodium monofluorophosphate, 1.5 parts of tripterygium wilfordii extract, 5 parts of curing agent, 2 parts of tea polyphenol, 2 parts of emulsifier, 2.5 parts of thickening agent, 6 parts of auxiliary reinforcing agent, 200.8 parts of tween-and 70 parts of water.
3. A novel stone protective agent as claimed in claim 1 or 2, characterized in that the silicone oil is prepared by the following steps: adding 3-5 times of purified water into dimethyldichlorosilane at the temperature of 30-40 ℃, reacting for 1-2h to obtain a primary condensed ring body, and cracking and rectifying the ring body to obtain a low ring body; and then adding an MDM end sealing agent and active carbon as a catalyst, and mixing for 2 hours to obtain the catalyst.
4. The novel stone protective agent as claimed in claim 1 or 2, wherein the curing agent is prepared from 3-dimethylaminopropylamine and 2-methylimidazole in a weight ratio of 7-11: 2-5; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 15-20: 1 to 2.
5. The new stone protective agent as claimed in claim 4, wherein said curing agent is prepared from 3-dimethylaminopropylamine and 2-methylimidazole in a weight ratio of 9: 4, preparing a composition; the emulsifier is prepared from polysorbate 80 and saponin in a weight ratio of 17: 1.4.
6. A novel stone protective agent as claimed in claim 1 or 2, wherein said thickener is a mixture of hydroxypropyl methylcellulose and sodium polyacrylate in a weight ratio of 5-7: 9-12; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate in a weight ratio of 1-2: 10-13: 4 to 7.
7. The novel stone protective agent as claimed in claim 6, wherein the thickener is a mixture of hydroxypropyl methylcellulose and sodium polyacrylate in a weight ratio of 8: 11; the auxiliary reinforcing agent is prepared from sodium methylene dinaphthalene sulfonate, nisin and sodium hexametaphosphate according to the weight ratio of 1.6: 11: 5.
8. A method for preparing a novel stone protectant according to any of claims 1-7, comprising the steps of:
s1, mixing the emulsifier with the silicone oil, and reacting at 40-50 ℃ for 40-50 min to obtain emulsified silicone oil;
s2, heating water to 50-60 ℃, adding the emulsified silicone oil prepared in the step S1 into the water, continuously adding sodium monofluorophosphate, tripterygium wilfordii extract and tea polyphenol into the water, and mixing and stirring uniformly to prepare a mixture I;
s3, cooling the mixture I prepared in the step S2 to 20-30 ℃, adding the thickening agent, the auxiliary reinforcing agent and the Tween-20, and uniformly mixing and stirring to prepare a mixture II;
s4, adding a curing agent into the mixture II prepared in the step S3, heating to 60-65 ℃, treating for 1-1.5 hours, and continuously heating to 120-130 ℃ for treating for 3-4 hours to obtain the modified epoxy resin.
9. The method according to claim 8, wherein the mixing and stirring conditions in step S2 are stirring at 800-1000 rpm for 20-30 min.
10. The method according to claim 8, wherein the mixing and stirring conditions in step S3 are stirring at 500-600 rpm for 30-40 min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110552228.1A CN113233919A (en) | 2021-05-20 | 2021-05-20 | Novel stone protective agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110552228.1A CN113233919A (en) | 2021-05-20 | 2021-05-20 | Novel stone protective agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115925446A (en) * | 2022-04-07 | 2023-04-07 | 东莞市立信环保科技有限公司 | Universal stone protective agent |
-
2021
- 2021-05-20 CN CN202110552228.1A patent/CN113233919A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115925446A (en) * | 2022-04-07 | 2023-04-07 | 东莞市立信环保科技有限公司 | Universal stone protective agent |
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Application publication date: 20210810 |