CN112680099A - Concrete ultraviolet-resistant protective agent - Google Patents
Concrete ultraviolet-resistant protective agent Download PDFInfo
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- CN112680099A CN112680099A CN202011500578.5A CN202011500578A CN112680099A CN 112680099 A CN112680099 A CN 112680099A CN 202011500578 A CN202011500578 A CN 202011500578A CN 112680099 A CN112680099 A CN 112680099A
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Abstract
The application relates to the field of concrete protective agents, and particularly discloses a concrete ultraviolet-resistant protective agent which is prepared from the following raw materials in parts by weight: 25-35 parts of polysiloxane, 20-30 parts of dimethyl silane, 3-8 parts of silane modifier, 2-5 parts of emulsifier, 8-10 parts of surfactant and 10-25 parts of anti-ultraviolet agent, wherein the anti-ultraviolet agent is prepared from yttrium chloride, chitosan, 3-chloromethyl-3-methyl oxetane, polyethylene glycol and hexamethylene diisocyanate serving as raw materials, and the preparation method of the anti-ultraviolet agent comprises the following steps: s1, dispersing chitosan in isopropanol solution, adding 3-chloromethyl-3-methyl oxetane, and mixing uniformly to obtain modified chitosan; s2, dispersing yttrium chloride and the modified chitosan prepared in the step S1 by dimethyl sulfoxide solution under the heating condition, mixing the dispersion with polyethylene glycol and hexamethylene diisocyanate, and reacting to obtain the uvioresistant agent. The ultraviolet-resistant coating has the effects of stronger ultraviolet resistance and longer ultraviolet-resistant aging.
Description
Technical Field
The application relates to the field of concrete protective agents, in particular to a concrete ultraviolet-resistant protective agent.
Background
Concrete, a widely used building material, is generally composed of granular coarse aggregate, fine aggregate and cement hydrate, and plays a great role in modern building engineering. In the use process of concrete, outdoor concrete is radiated by strong ultraviolet rays for a long time, and because the wavelength of the ultraviolet rays is shorter and the energy is higher, the high-energy ultraviolet rays can break hydrogen bonds in cement paste to destroy the frost resistance of the concrete.
In recent years, attention has been paid to the ultraviolet resistance of concrete protectors, and it is common to add a substance capable of reflecting ultraviolet rays, such as silica or titania, to the protectors so as to impart the ultraviolet resistance to the concrete protectors. However, when the concrete protective agent in the related art is actually used, the problems of poor ultraviolet resistance and short ultraviolet resistance aging sometimes occur.
For example, chinese patent publication No. CN104961424A proposes a high weather-resistant concrete protective agent for fresh water, which comprises a composite of sericite, calcium carbonate, kaolin, hydrophilic fumed silica and titanium dioxide, and when the protective agent is actually used, especially in areas with strong ultraviolet irradiation and large day-night temperature difference such as tibetan, the ultraviolet resistance of the protective agent is poor, and the freeze-thaw resistance is significantly reduced after only 20 days of ultraviolet irradiation.
Disclosure of Invention
In order to solve the problem of poor ultraviolet resistance of a concrete protective agent in the related art, the application provides a concrete ultraviolet-resistant protective agent.
The application provides a concrete ultraviolet resistance protective agent adopts following technical scheme:
the concrete ultraviolet-resistant protective agent is prepared from the following raw materials in parts by weight:
25-35 parts of polysiloxane
20-30 parts of dimethylsilane
3-8 parts of silane modifier
2-5 parts of emulsifier
8-10 parts of surfactant
10-25 parts of anti-ultraviolet agent
The uvioresistant agent is prepared by taking yttrium chloride, chitosan, 3-chloromethyl-3-methyl oxetane, polyethylene glycol, hexamethylene diisocyanate and dimethyl sulfoxide solution as main raw materials, and the preparation method of the uvioresistant agent comprises the following steps:
s1, dispersing chitosan in isopropanol solution, adding 3-chloromethyl-3-methyloxetane, uniformly mixing, heating and filtering to obtain the modified chitosan, wherein the weight ratio of the chitosan to the 3-chloromethyl-3-methyloxetane is 1: (0.03-0.05);
s2, dispersing the modified chitosan prepared in the step S1 and yttrium chloride in dimethyl sulfoxide solution to obtain dispersion liquid; mixing the dispersion liquid with polyethylene glycol and hexamethylene diisocyanate, and reacting to obtain the uvioresistant agent, wherein the weight ratio of yttrium chloride to polyethylene glycol to hexamethylene diisocyanate to dimethyl sulfoxide solution is 1: (30-50): (8-10): 3.
by adopting the technical scheme, silane and siloxane in the concrete protective agent can act with the anti-ultraviolet agent in a synergistic manner, so that a silane chain is overlapped with a polyurethane network, and illumination can be refracted, and therefore, the anti-ultraviolet capability of concrete is improved.
Preferably, after 3-chloromethyl-3-methyloxetane is added in step S1, the mixture is heated to 50-80 ℃.
By adopting the technical scheme, the prepared chitosan monomer embedded with the oxetane is relatively pure, so that the uvioresistant effect of the uvioresistant agent is relatively good.
Preferably, the yttrium chloride and the modified chitosan are dispersed in a dimethyl sulfoxide solution at 70-80 ℃ to obtain a dispersion liquid in the step of S2.
By adopting the technical scheme, the prepared anti-ultraviolet agent is purer, so that the anti-ultraviolet effect of the concrete protective agent is better.
Preferably, the weight ratio of chitosan to 3-chloromethyl-3-methyloxetane in the S1 step is 1: 0.04, the weight ratio of yttrium chloride, polyethylene glycol and hexamethylene diisocyanate in the step S2 is 1: (35-40): (8-10): 3.
by adopting the technical scheme, the obtained anti-ultraviolet agent has complete reaction, so that the concrete protective agent has better anti-ultraviolet property.
Preferably, the surfactant is one of higher fatty acid salt, sulfonate and sulfate.
By adopting the technical scheme, the higher fatty acid salt, the sulfonate and the sulfate are all suitable for being used as the surfactant of the concrete protective agent.
Preferably, the silane modifier is gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
By adopting the technical scheme, when the gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane is used as the silane modifier, the concrete protective agent has better ultraviolet resistance.
Preferably, the emulsifier is an anionic emulsifier.
By adopting the technical scheme, the anionic emulsifier has good thermal stability and better applicability.
Preferably, the feed is prepared from the following raw materials in parts by weight: 30 parts of polysiloxane, 25-30 parts of dimethylsilane, 5-6 parts of silane modifier, 3-4 parts of emulsifier, 9 parts of surfactant and 15-20 parts of uvioresistant agent.
By adopting the technical scheme, the concrete protective agent has better ultraviolet resistance effect.
In summary, the present application has the following beneficial effects:
1. because the anti-ultraviolet agent, the silane and the siloxane are used as main raw materials, the silane and the siloxane in the concrete protective agent can act with the anti-ultraviolet agent synergistically, so that a silane chain and a polyurethane network are overlapped, and illumination can be refracted, so that the anti-ultraviolet capability of concrete is improved, chitosan and the oxetane can be crosslinked again, a broken molecular chain in the protective agent is repaired, and the concrete protective agent has a continuous anti-ultraviolet effect;
2. the preferred use in this application is that the weight ratio of chitosan to 3-chloromethyl-3-methyloxetane in the S1 step is 1: 0.04, the weight ratio of yttrium chloride, polyethylene glycol and hexamethylene diisocyanate in the step S2 is 1: (35-40): (8-10): 3, the concrete protective agent obtains better anti-ultraviolet effect.
Detailed Description
The present application is described in further detail below with reference to preparation examples and examples.
The raw material sources used in the preparation examples and the examples are shown in the following table 1:
TABLE 1 sources of raw materials
Preparation example of anti-ultraviolet agent
Preparation example 1
An uvioresistant agent is prepared by using yttrium chloride, chitosan, 3-chloromethyl-3-methyl oxetane, polyethylene glycol with the polymerization degree of 242 and hexamethylene diisocyanate as main raw materials, and the preparation method comprises the following steps:
s1, dispersing 10g of the mixture into 40mL of isopropanol solution with the concentration of 87 wt%, continuing to add 0.3g of 3-chloromethyl-3-methyl oxetane, heating to 90 ℃, and keeping the temperature for 2h under the stirring condition until the reaction is complete; then, filtering, cleaning and drying to obtain modified chitosan;
and (3) adding S2, 10g of yttrium chloride and all modified chitosan prepared in S1 into 30g of 98 wt% dimethyl sulfoxide aqueous solution, heating to 60 ℃, keeping the temperature, stirring for 10 hours to obtain a dispersion, adding 300g of polyethylene glycol with the polymerization degree of 242 and 80g of hexamethylene diisocyanate into the dispersion, and uniformly mixing to obtain the anti-ultraviolet agent.
Preparation examples 2 to 3
Preparation examples 2 to 3 are based on preparation example 1 and differ from preparation example 1 only in that: the weight ratios of the raw materials used in the S1 step and the S2 step are different, and are specifically shown in Table 2.
TABLE 2 weight ratios of raw materials in preparation examples 1 to 3
Preparation examples 4 to 7
Preparation examples 4 to 7 are based on preparation example 1, differing from preparation example 1 only in that: 3-chloromethyl-3-methyloxetane was added in step S1, and the stirring temperature was varied, as shown in Table 3.
TABLE 3 stirring temperature of S1 step in production examples 1 to 5
Preparation examples 8 to 10
Preparation examples 8 to 10 are based on preparation example 1, differing from preparation example 1 only in that: in the step S2, polyethylene glycol having a polymerization degree of 242 and hexamethylene diisocyanate were added, and the stirring temperature was varied, as shown in table 4.
TABLE 4 stirring temperature of S2 step in preparation examples 8 to 10
Preparation example | Preparation example 1 | Preparation example 6 | Preparation example 7 | Preparation example 8 |
S1 stirring temperature (. degree.C.) | 60 | 80 | 75 | 70 |
Preparation examples 11 to 13
Preparation examples 11 to 13 are based on preparation example 1, differing from preparation example 1 only in that: the raw materials used in the S1 and S2 steps are different in weight ratio, and are specifically shown in Table 5.
TABLE 5 weight ratios of raw materials in production examples 11 to 13
Examples
Example 1
The concrete ultraviolet-resistant protective agent is prepared by mixing the following raw materials at the rotating speed of 200 r/min:
polysiloxane-1525 g
Dimethylsilane 20g
Vinyltris (2-methoxyethoxy) silane 7g
Polyoxyethylene ether TX-102 g
Sodium palmitate 9g
Anti-ultraviolet agent 13g
The anti-ultraviolet agent is derived from preparation example 1.
Examples 2 to 5
Examples 2 to 5 are based on example 1 and differ from example 1 only in that: the amounts of the raw materials are different, and are shown in Table 6.
TABLE 6 raw material amounts in examples 1-5
Examples 6 to 7
Examples 6 to 7 are based on example 1 and differ from example 1 only in that: the surfactant used was different and is shown in Table 7.
TABLE 7 surfactants of examples 6-7
Examples | Example 1 | Example 6 | Example 7 |
Surface active agent | Sodium palmitate | Methanesulfonic acid magnesium salt | AES fatty alcohol polyoxyethylene ether sodium sulfate (type 270N) |
Example 8
Example 8 is based on example 1 and differs from example 1 only in that: the silane modifier is gamma- (2, 3-epoxy propoxy) propyl trimethoxy silane.
Example 9
Example 9 is based on example 1 and differs from example 1 only in that: the emulsifier used was sodium lauryl sulfate.
Examples 10 to 12
Examples 10 to 12 are based on example 1 and differ from example 1 only in that: the amounts of the raw materials are different, and are shown in Table 8.
TABLE 8 raw material quantities in examples 10-12
Examples 13 to 24
Examples 13 to 24 are based on example 1 and differ from example 1 only in that: the source of the uvioresistant agent is different, and the uvioresistant agent is shown in table 9.
TABLE 9 source of anti-UV agent in examples 13-24
Comparative example
Comparative example 1
Comparative example 1 is based on example 1 and differs from example 1 only in that: the concrete protective agent is added with nano silicon dioxide which is equal to the uvioresistant agent and replaces the uvioresistant agent.
Comparative example 2
Comparative example 2 is based on example 1 and differs from example 1 only in that: the concrete protective agent is added with organosilicon emulsion which is equal to polysiloxane-15 and dimethyl silane instead of polysiloxane-15 and dimethyl silane.
Comparative example 3
The concrete protective material with the publication number of CN102030558A comprises the following concrete components in percentage by weight: 50 parts of 40% MP-15 resin liquid, 5 parts of DZ520 concrete protective agent, 10 parts of xylene, EFKA-40100.2 parts, 0.3 part of organic bentonite, 5 parts of titanium dioxide, 5 parts of mica powder, 10 parts of quartz powder and 68000.3 parts of a moderate DE, and the concrete preparation steps are as follows:
weighing 40% of MP-15 resin liquid, a concrete protective agent and a wetting dispersant in required amounts, adding the mixture into a dispersion tank, and dispersing at a low speed for 5-10 minutes to obtain a mixture I; then weighing a certain amount of pigment and filler, adding the pigment and filler into the mixture I, and dispersing at a high speed for 15-20 minutes to obtain a mixture II; and weighing a certain amount of thixotropic agent and defoaming agent, adding the thixotropic agent and the defoaming agent into the mixture II, dispersing for 20 minutes at a high speed, grinding the mixture in a sand mill until the fineness of the mixture is less than or equal to 40 microns after the dispersion is finished, adjusting the viscosity of the mixture to be qualified by using a solvent, filtering the mixture by using a 80-mesh screen to obtain the material, and subpackaging the material according to the packaging specification.
Performance test
(1) Manufacturing concrete samples according to the standard of the test procedure of hydraulic concrete (SL 352-2006): a, B groups of concrete test pieces are manufactured according to the water cement ratio of 0.4, each group of test pieces adopts a prism test piece with the uniform size of 100mm multiplied by 400mm, the curing time is 28 days, 4 days before the test age is reached, and the test pieces are taken out of the curing box.
(2) And (3) spraying a concrete protective agent on each test piece of the group A test pieces, wherein when the concrete protective agent is sprayed, a low-pressure spray gun is used for spraying construction twice, the time interval of the two construction is 1h, 36ml of the concrete protective agent is sprayed on each test piece, and the group B does not spray the concrete protective agent.
Detection test
Concrete ultraviolet radiation and freeze-thaw cycle test
(1) The model number of the SC/ZN-PA ultraviolet aging test box is adopted to simulate the ultraviolet irradiation environment, and the aging in the SC/ZN-PA ultraviolet aging test box for one day is equivalent to the aging in the outdoor for 24 days. A, B groups of test pieces are put into an ultraviolet aging test box for ultraviolet radiation test, and after the test is finished, the initial mass is measured by an electronic scale.
(2) Placing the tested test pieces of the test group into a test piece box of a freeze-thaw circulator, and performing freeze-thaw cycle test according to a quick freezing method mentioned in the test method standard of the long-term performance and the durability of common concrete (GB/T50082-2009) III 1, wherein the central temperature of the test piece when being frozen is (-18 +/-2) DEG C, the central temperature of the test piece when being melted is (5 +/-2) DEG C, the temperature difference between the inside and the outside of the test piece is not more than 28 ℃, the time for freezing the test piece is not less than 0.5 time of one freeze-thaw cycle time, the melting time is not less than 0.25 time of one freeze-thaw cycle time, and the interval time between the freezing stage and the melting stage is not more than 10 min. The data is measured every 25 cycles, and the test piece should be taken out when the data is measured, and the water and the dregs on the surface are wiped off and then the measurement is carried out. And after the data is measured, turning around the test piece and re-loading the test piece into the test piece box, starting the next cycle, and finishing the test when the number of freeze-thaw cycles of the test reaches 275.
in the formula, WnThe mass loss rate (%) of the test piece after n freeze-thaw cycles; g0Is the initial mass (kg) of the test piece before the test; gnThe mass (kg) of the test piece after n freeze-thaw cycles.
The test results of the freeze-thaw cycles after aging the group a and group B test pieces in the aging test chamber for one day are shown in table 10.
TABLE 10-1. examples 1 to 6 test pieces each have a mass loss ratio (%)
TABLE 10-2. examples 7-13 test pieces mass loss (%)
TABLE 10-3 quality loss ratio (%)
TABLE 10-4 test pieces of examples 21-25 and comparative examples 1-2 were found to have a mass loss ratio (%)
The test results of freeze-thaw cycling of the group a and group B test pieces after aging in the aging test chamber for 3 days are shown in table 11.
TABLE 11 quality loss rate (%)
The better the frost resistance of the concrete, the lower the mass loss rate after freeze-thaw cycling, and analysis of the above experimental data shows that:
data for comparative examples 1-5 and control: the concrete protective agent of example 1 has the lowest mass loss rate of concrete after use, so that example 1 is the best example of examples 1 to 5.
Compared with the test results of the group B test pieces, the test results of the group A test pieces do not use a concrete protective agent, the group A test pieces and the group B test pieces are subjected to freeze-thaw cycle tests after being aged in an aging test box, and the mass loss rate of the group A test pieces is far smaller than that of the group B test pieces.
Compared with the comparative examples 1 and 2, the concrete protective agent of the example 1 has the advantages that the ultraviolet resistant agent prepared according to the specific raw material ratio and the specific process is not added into the concrete protective agent of the comparative example 1, the nano silicon dioxide with the same amount as the ultraviolet resistant agent is added, the organic silicon emulsion with the same amount as the polysiloxane-15 and the dimethyl silane is added into the concrete protective agent of the comparative example 2 to replace the polysiloxane-15 and the dimethyl silane, the concrete using the concrete protective agent of the example 1 has the mass loss rate which is far lower than that of the concrete using the concrete protective agents of the comparative examples 1 and 2, and the ultraviolet resistant agent can act with the polysiloxane-15 and the dimethyl silane in a synergistic manner and cannot be used.
Example 5 is different from comparative example 3 only in that the concrete protectant of comparative example 3 is a commonly used concrete protectant with ultraviolet resistance, and the concrete using the concrete protectant of example 1 has a lower mass loss rate than the concrete using the concrete protectant of comparative example 3, indicating that the concrete protectant of the present application has excellent ultraviolet resistance.
Examples 6 to 7 are different from example 1 only in the surfactant used, and the concrete using the concrete protectant in examples 6 to 7 has a small difference in mass loss rate from that of the concrete using the concrete protectant in example 1, indicating that a higher fatty acid salt, a sulfonate salt, and a sulfate salt can be used as the surfactant of the protectant of the present application.
Example 8 is different from example 1 only in that the silane modifier used in example 8 is γ - (2, 3-glycidoxy) propyltrimethoxysilane, and the concrete using the concrete protectant of example 8 has a lower mass loss than the concrete of the concrete protectant of example 1, indicating that the concrete protectant has a better ultraviolet resistance when the silane modifier is γ - (2, 3-glycidoxy) propyltrimethoxysilane.
Example 9 is different from example 1 only in that the emulsifier used in example 9 is sodium lauryl sulfate, and the concrete using the concrete protectant in example 9 has a lower mass loss rate than the concrete using the concrete protectant in example 1, indicating that the concrete protectant has a better ultraviolet resistance when the emulsifier used is sodium lauryl sulfate.
Examples 10 to 12 are different from example 1 only in the amount of the respective raw materials used in examples 10 to 12, and the concrete using the concrete protectant in examples 10 to 12 has a lower mass loss than the concrete of the concrete protectant in example 1, which shows that the concrete protectant has a better ultraviolet resistance when the raw materials are, by weight, polysiloxane-1530 parts, dimethylsilane 25 to 30 parts, silane modifier 5 to 6 parts, emulsifier 3 to 4 parts, surfactant 9 parts, and ultraviolet resistant agent 15 to 20 parts.
Examples 15 to 18 are different from examples 13 to 14 only in the source of the preparation examples of examples 15 to 16, and the concrete using the concrete protectant of examples 15 to 18 has a lower mass loss rate than the concrete of the concrete protectant of examples 13 to 14, which shows that the concrete protectant has a better ultraviolet ray resistance effect when the heating temperature is 50 to 80 ℃ in the step S1.
Examples 19 to 21 are different from example 1 only in the source of the preparation examples of examples 19 to 21, and the concrete using the concrete protectant of examples 19 to 21 has a lower mass loss than the concrete of the concrete protectant of example 1, which shows that the concrete protectant has a better ultraviolet resistance when the heating temperature is 70 to 80 ℃ in the step S2.
Examples 22 to 24 were compared with example 22, differing only in the origin of the preparation examples of examples 23 to 25, and the concrete using the concrete protectant of examples 22 to 24 had a lower mass loss than the concrete of the concrete protectant of example 1, indicating that the weight ratio of chitosan to 3-chloromethyl-3-methyloxetane in the step S1 was 1: 0.04 and S2, wherein the weight ratio of yttrium chloride, polyethylene glycol with the polymerization degree of 242 and hexamethylene diisocyanate is 1: (35-40): (8-10): and 3, the concrete protective agent has better ultraviolet resistance effect.
After 3 days of the aging test box, compared with the test results of the comparative example 3, the mass loss of the concrete test piece of the comparative example 3 and the mass loss of the concrete test piece of the group B are increased sharply after the concrete test piece of the comparative example 3 and the group B test piece are irradiated by ultraviolet rays for a long time, and the mass loss rate of the concrete using the protective agent of the examples 1 to 25 is increased slightly, namely, the ultraviolet resistance effect of the concrete protective agent prepared by the application is almost unchanged after the concrete protective agent is used for a long time, which shows that the concrete protective agent prepared by the application has the effect of continuous ultraviolet resistance.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The concrete ultraviolet-resistant protective agent is characterized by being prepared from the following raw materials in parts by weight:
25-35 parts of polysiloxane
20-30 parts of dimethylsilane
3-8 parts of silane modifier
2-5 parts of emulsifier
8-10 parts of surfactant
10-25 parts of anti-ultraviolet agent
The uvioresistant agent is prepared by taking yttrium chloride, chitosan, 3-chloromethyl-3-methyl oxetane, polyethylene glycol, hexamethylene diisocyanate and dimethyl sulfoxide solution as main raw materials, and the preparation method of the uvioresistant agent comprises the following steps:
s1, dispersing chitosan in isopropanol solution, adding 3-chloromethyl-3-methyloxetane, uniformly mixing, heating and filtering to obtain the modified chitosan, wherein the weight ratio of the chitosan to the 3-chloromethyl-3-methyloxetane is 1: (0.03-0.05);
s2, dispersing the modified chitosan prepared in the step S1 and yttrium chloride in dimethyl sulfoxide solution to obtain dispersion liquid; mixing the dispersion liquid with polyethylene glycol and hexamethylene diisocyanate, and reacting to obtain the uvioresistant agent, wherein the weight ratio of yttrium chloride to polyethylene glycol to hexamethylene diisocyanate to dimethyl sulfoxide solution is 1: (30-50): (8-10): 3.
2. the concrete ultraviolet ray protection agent according to claim 1, characterized in that: after 3-chloromethyl-3-methyloxetane was added in step S1, the mixture was heated to 50-80 ℃.
3. The concrete ultraviolet ray protection agent according to claim 1, characterized in that: in the step S2, yttrium chloride and modified chitosan are dispersed in dimethyl sulfoxide solution at 70-80 ℃ to obtain dispersion liquid.
4. The ultraviolet ray protection agent for concrete as claimed in claim 1, wherein the weight ratio of chitosan to 3-chloromethyl-3-methyloxetane in the step of S1 is 1: 0.04, the weight ratio of yttrium chloride, polyethylene glycol and hexamethylene diisocyanate in the step S2 is 1: (35-40): (8-10): 3.
5. the concrete ultraviolet ray protection agent according to claim 1, characterized in that: the surfactant is one of higher fatty acid salt, sulfonate and sulfate.
6. The concrete ultraviolet ray protection agent according to claim 1, characterized in that: the silane modifier is gamma- (2, 3-epoxy propoxy) propyl trimethoxy silane.
7. The concrete ultraviolet ray protection agent according to claim 1, characterized in that: the emulsifier is an anionic emulsifier.
8. The concrete ultraviolet-resistant protective agent as claimed in claim 1, which is prepared from the following raw materials in parts by weight: 30 parts of polysiloxane, 25-30 parts of dimethylsilane, 5-6 parts of silane modifier, 3-4 parts of emulsifier, 9 parts of surfactant and 15-20 parts of uvioresistant agent.
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Application publication date: 20210420 |