An inorganic silicon deep penetration crystallization waterproofing agent and its preparation process
By adding modified zinc oxide particles and nano-silicon dioxide to the inorganic silicone waterproofing agent, the problems of shallow penetration depth and poor durability of traditional inorganic silicone waterproofing agents are solved, and deeper penetration and better temperature and aging resistance are achieved.
Patent Information
- Application Number
- CN202411713926.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-27
- Publication Date
- 2025-07-01
- Estimated Expiration
- 2044-11-27
AI Technical Summary
The existing inorganic silicone waterproofing agent has a shallow penetration depth in concrete, and the waterproofing effect gradually weakens after long-term use, and its stability is poor under extreme environmental conditions, which affects the waterproofing effect.
The inorganic silicone deep penetration crystal waterproofing agent is used to form a composite structure of modified zinc oxide particles and nano-silica through the combination of active sodium silicate, nanocomposite particles, aluminate cement, coagulant, dispersant, thickener and preservative, thereby enhancing the penetration depth, temperature resistance and aging resistance of the waterproofing agent.
It significantly improves the penetration depth and durability of the waterproofing agent in concrete, ensures long-term waterproofing performance, adapts to various application environments, extends service life, and reduces the formation speed and adhesion of the surface hydration layer.
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Abstract
Description
Technical Field
[0001] This application relates to the field of concrete waterproof materials, and particularly to an inorganic silicon deep-penetrating crystallization waterproof agent and its preparation process. Background Art
[0002] In modern architecture, the waterproof performance of concrete structures is crucial for ensuring the durability and safety of buildings. As a porous material, concrete is prone to leakage when exposed to water or moisture for a long time, leading to problems such as internal steel bar corrosion and structural strength decline. Therefore, developing efficient, environmentally friendly, and durable waterproof materials is an important requirement in the construction industry.
[0003] Currently, common waterproof materials on the market include organic waterproof coatings, asphalt-based waterproof materials, and inorganic waterproof materials. Among them, inorganic silicon waterproof agents have attracted much attention due to their unique advantages. Inorganic silicon waterproof agents mainly react with free lime in concrete through silicate solutions to form insoluble calcium silicate crystals, which can fill the pores and micro-cracks inside the concrete, thereby improving the density and waterproof performance of the concrete.
[0004] However, there are still some problems with existing inorganic silicon waterproof agents in practical applications. For example, the penetration depth of traditional inorganic silicon waterproof agents in concrete is relatively shallow, usually only penetrating within a few millimeters of the surface. This results in a gradual weakening of the waterproof effect over time, especially in the case of long-term water immersion, the waterproof layer is prone to failure; and under extreme environmental conditions, such as high temperature, low temperature, strong acid and strong base environments, the stability of traditional inorganic silicon waterproof agents is poor, which may cause the waterproof layer to crack or peel off, affecting the waterproof effect.
[0005] Therefore, in order to effectively solve the above problems, this application provides an inorganic silicon deep-penetrating crystallization waterproof agent and its preparation process. The finally prepared waterproof agent not only has excellent waterproof and anti-corrosion properties, but also can further improve the penetration depth of the inorganic silicon waterproof agent in concrete and its temperature resistance and aging resistance, thereby ensuring that the waterproof agent has good long-term waterproof performance and can adapt to various application environments, having a very excellent application prospect. Summary of the Invention
[0006] To solve the above problems, in the first aspect of this application, an inorganic silicon deep-penetrating crystallization waterproof agent is provided. Calculated by mass, the raw materials are: 40 - 60 parts of active sodium silicate, 20 - 35 parts of nano composite particles, 10 - 15 parts of aluminate cement, 1 - 3 parts of coagulant, 5 - 15 parts of dispersant, 3 - 5 parts of thickener, 0.1 - 0.3 parts of preservative, and 40 - 65 parts of deionized water.
[0007] As a preferred embodiment, the mass ratio of the active sodium silicate, the nano composite particles and the aluminate cement is (45~55):(22~28):(12~15).
[0008] As a preferred embodiment, the mass ratio of the active sodium silicate, the nano composite particles and the aluminate cement is (48~52):(24~26):(14~15).
[0009] As a preferred embodiment, the modulus of the active sodium silicate is 2~4.
[0010] As a preferred embodiment, the modulus of the active sodium silicate is 2.5~3.5.
[0011] As a preferred embodiment, the nano composite particles are a composition of nano silicon dioxide and modified zinc oxide particles.
[0012] As a preferred embodiment, the mass ratio of the nano silicon dioxide and the modified zinc oxide particles is (2.8~3.5):(1.5~2.5).
[0013] As a preferred embodiment, the mass ratio of the nano silicon dioxide and the modified zinc oxide particles is (3~3.2):(1.9~2.3).
[0014] As a preferred embodiment, the average particle size of the nano silicon dioxide is 40~60nm.
[0015] As a preferred embodiment, the preparation method of the modified zinc oxide particles comprises the following steps: S1: Mix zinc oxide and zirconium chloride and add them to deionized water, add succinic anhydride and isopropyl tris(dodecylbenzenesulfonyl) titanate, heat up to 60~65°C and keep warm for 3~4h, after completion, centrifuge and filter the product, wash and dry to obtain pretreated particles; S2: Mix the pretreated particles with 1,4-phthalic acid and p-aminobenzoic acid and add them to DMF and stir completely, heat up to 120~130°C, keep warm and react for 20~22h, after completion, naturally cool the product to room temperature, wash 2~3 times alternately with DMF and absolute ethanol to obtain pre-modified particles; S3: Mix the pre-modified particles and ammonia water and add them to deionized water, dropwise add an aqueous solution of triethanolamine and tetraethyl orthosilicate in deionized water, the dropwise addition reaction temperature is 60~65°C, the dropwise addition time is 0.5~0.6h, after dropwise addition, keep warm at 70~75°C for 1~1.5h, after the reaction is completed, filter and wash to obtain the product.
[0016] As a preferred embodiment, the mass ratio of the zinc oxide, zirconium chloride, succinic anhydride and isopropyl tris(dodecylbenzenesulfonyl) titanate is (0.6~1):(4~5):(1.5~1.8):(0.2~0.25).
[0017] As a preferred embodiment, the average particle size of the zinc oxide is 5 to 10 nm.
[0018] As a preferred embodiment, the mass ratio of the pretreated particles, 1,4-benzenedicarboxylic acid, and p-aminobenzoic acid is (3.5 to 4):(2 to 2.5):(1 to 1.5).
[0019] As a preferred embodiment, the mass ratio of the pre-modified particles, ammonia water, triethanolamine, and tetraethyl orthosilicate is (5 to 5.5):(0.5 to 0.8):(0.1 to 0.15):(1.5 to 2).
[0020] As a preferred embodiment, the average particle size of the modified zinc oxide particles is 450 to 550 nm.
[0021] In the present application, by adding the above-mentioned compounding of modified zinc oxide particles and nano-silica, the waterproof and anti-corrosion properties of the waterproof agent can be greatly improved, and the temperature resistance, aging resistance, etc. of the waterproof agent in application environments such as high temperature and high humidity can also be greatly improved. The modified zinc oxide particles prepared in the present application can form a composite structure with framework particles as the internal core, zinc oxide as the external chimeric site, and finally coated with amorphous silica. The existence of this structure can not only form a guiding effect on water molecules through the hydroxyl groups of the particle sites on the surface, thereby assisting the water absorption effect of the central framework particles, but also form a rougher filled pore surface, and reduce the large particle pore diameter caused by the amplitude movement during the filling process of the microparticles, thereby reducing the pore size and increasing the resistance to water molecule penetration and the length of the penetration path. Therefore, while greatly improving the waterproof and anti-corrosion properties, it maintains an excellent service life and greatly reduces the formation rate and adhesion of the surface hydration layer.
[0022] On the other hand, through the co-action with the dispersant specifically selected and compounded in the present application, the fixing effect of the waterproof agent in the concrete can be greatly increased with the carrier multi-layer film structure of the compounded dispersant, enhancing the deep penetration effect. Furthermore, the crystallization filling of the waterproof agent can be realized deep inside, thereby improving the overall performance while improving the stability of the waterproof agent particles, avoiding the segregation and migration phenomena after the use of the waterproof agent, and thus having long-term aging resistance, waterproofness, heat resistance, etc.
[0023] As a preferred embodiment, the density of the aluminate cement is 2.5 to 3 g / cm 3 .
[0024] As a preferred embodiment, the coagulant is at least one of calcium chloride, calcium nitrate, sodium carbonate, polyphosphate, and aluminum sulfate.
[0025] As a preferred embodiment, the coagulant is aluminum sulfate.
[0026] As a preferred solution, the dispersant is a composition of C12 - C14 fatty alcohol polyoxyethylene ether, triphenylvinylphenol polyoxyethylene ether, and epoxy block polyether.
[0027] As a preferred solution, the mass ratio of C12 - C14 fatty alcohol polyoxyethylene ether, triphenylvinylphenol polyoxyethylene ether, and epoxy block polyether is (3 - 3.5):(1 - 2):(6 - 8).
[0028] As a preferred solution, the hydroxyl value of the C12 - C14 fatty alcohol polyoxyethylene ether is 70 - 90 mgKOH / g.
[0029] As a preferred solution, the C12 - C14 fatty alcohol polyoxyethylene ether is isomeric C13 fatty alcohol polyoxyethylene ether.
[0030] As a preferred solution, the weight - average molecular weight of the epoxy block polyether is 2000 - 4000 Da.
[0031] As a preferred solution, the ethylene oxide block content of the epoxy block polyether is 25 - 40 wt%.
[0032] As a preferred solution, the HLB value of the triphenylvinylphenol polyoxyethylene ether is 16 - 18.
[0033] As a preferred solution, the thickener is at least one of hydroxyethyl cellulose, hydroxypropyl methylcellulose, sodium polyacrylate, polyvinyl alcohol, and sodium carboxymethylcellulose.
[0034] As a preferred solution, the thickener is hydroxyethyl cellulose.
[0035] As a preferred solution, the preservative is at least one of sodium benzoate, potassium sorbate, methyl paraben, benzisothiazolinone, and pentanediol.
[0036] As a preferred solution, the preservative is sodium benzoate.
[0037] As a preferred solution, the mass ratio of the coagulant accelerator and the thickener is (1.5 - 2.2):(3.5 - 4.8).
[0038] As a preferred solution, the mass ratio of the coagulant accelerator and the thickener is (2 - 2.2):(4 - 4.3).
[0039] As a preferred solution, the mass ratio of the nano - composite particles and the dispersant is (22 - 28):(7 - 13).
[0040] As a preferred solution, the mass ratio of the nano composite particles to the dispersant is (24 - 26):(9 - 11).
[0041] The second aspect of the present application provides a preparation process of the above-mentioned inorganic silicon deep penetration crystallization waterproof agent, which specifically includes the following steps: S1: Mix the active sodium silicate with part of deionized water and stir until completely dissolved to form a uniform mixture. In another container, dry mix the nano composite particles, the dispersant and the aluminate cement evenly, and then add the remaining deionized water to make a paste to obtain a mixed paste; S2: Slowly add the mixed paste into the mixture, and stir with a high-speed stirrer at 800 - 1000 rpm for 30 - 40 min to ensure that the two components are fully mixed. Then, add the coagulant, thickener and preservative in sequence, and continue to stir for 5 - 10 min after adding each material until all components are evenly distributed in the mixture; S3: After the stirring is completely finished, sieve the product through a 400 - 600 mesh sieve to remove large particles and impurities, and then transfer the product to a clean container for sealed storage, avoiding direct sunlight, and keeping the temperature between 10°C and 30°C to obtain the product.
[0042] The beneficial effects of the present application are as follows:
[0043] 1. The inorganic silicon deep penetration crystallization waterproof agent provided in the present application not only has excellent waterproof and anti-corrosion properties, but also can further improve the penetration depth of the inorganic silicon waterproof agent in concrete and its temperature resistance and aging resistance, thereby ensuring that the waterproof agent has good long-term waterproof performance and can adapt to various application environments, and has a very excellent application prospect.
[0044] 2. The inorganic silicon deep penetration crystallization waterproof agent provided in the present application, the added modified zinc oxide particles can form a composite structure with the framework particles as the internal core, zinc oxide as the external chimeric site, and finally coated with amorphous silica. The existence of this structure can not only form a guiding effect on water molecules through the hydroxyl groups of the surface chimeric particle sites, thereby assisting the water absorption effect of the central framework particles, but also form a rougher pore surface for filling, and reduce the large particle pore diameter caused by the amplitude movement during the filling process of the microparticles, thereby reducing the pore size and increasing the resistance of water molecule penetration and the length of the penetration path. Furthermore, while significantly improving the waterproof and anti-corrosion properties, it maintains an excellent service life and significantly reduces the formation speed and adhesion of the surface hydration layer.
[0045] 3. In the inorganic silicon deep-penetrating crystallization waterproof agent provided in this application, the added modified zinc oxide particles can also, through the combined action with the dispersant specifically selected and compounded in this application, significantly increase the fixing effect of the waterproof agent in concrete in the form of a carrier multi-layer film structure of the compounded dispersant, enhance the deep penetration effect, and then enable the crystallization filling of the waterproof agent in the deep interior. Furthermore, while improving the overall performance, the stability of the waterproof agent particles is enhanced, avoiding the segregation and migration phenomena after the use of the waterproof agent, and thus having long-term anti-aging, waterproof, heat-resistant and other properties. Detailed implementation mode
[0046] The following will further illustrate and demonstrate the technical solutions in the above-mentioned inventive content of this application in the form of specific implementation schemes. And the following embodiments are only actual examples for explaining and interpreting the content of the technical solutions in the specification, and should not limit the scope of the claims to be protected by this application. All technical products based on the technical solutions described in the inventive content of this application should be covered within the scope to be protected by this application.
[0047] In the following embodiments, unless otherwise specified, the raw materials are commercially available products that can be obtained, or can be prepared by methods well-known to those skilled in the art.
[0048] Example 1
[0049] In the first aspect of Example 1, an inorganic silicon deep-penetrating crystallization waterproof agent is provided. In terms of parts by mass, the raw materials are: 50.5 parts of active sodium silicate, 24.8 parts of nano composite particles, 14.8 parts of aluminate cement, 2.1 parts of coagulant promoter, 10.8 parts of dispersant, 4.2 parts of thickener, 0.16 part of preservative, and 55 parts of deionized water.
[0050] The modulus of the active sodium silicate is 2.8, and it is purchased from the 2.6 - 3.5 modulus grade products sold by Tangshan Fengnan Anli Chemical Co., Ltd.
[0051] The nano composite particles are a composition of nano silicon dioxide and modified zinc oxide particles, and the mass ratio of the two is 3.2:2.
[0052] The average particle size of the nano silicon dioxide is 55 nm.
[0053] The preparation method of the modified zinc oxide particles comprises the following steps: S1: 0.8 parts of zinc oxide and 4.4 parts of zirconium chloride are mixed and added to 100 parts of deionized water, 1.6 parts of succinic anhydride and 0.24 parts of isopropyltri(dodecylbenzenesulfonyl) titanate are added, the temperature is raised to 65 °C and kept warm for 3 h. After completion, the product is centrifuged and filtered, washed and dried to obtain pretreated particles; S2: 3.8 parts of the pretreated particles, 2.2 parts of 1,4-benzenedicarboxylic acid and 1.4 parts of 4-aminobenzoic acid are mixed and added to 120 parts of DMF and stirred completely. The temperature is raised to 120 °C and kept warm for 22 h. After completion, the product is naturally cooled to room temperature and washed 3 times alternately with DMF and absolute ethanol to obtain pre-modified particles; S3: 5.2 parts of the pre-modified particles and 0.6 parts of ammonia water are mixed and added to 180 parts of deionized water, and an aqueous solution of deionized water containing 0.14 parts of triethanolamine and 1.8 parts of tetraethyl orthosilicate (40 parts in total) is added dropwise. The dropwise addition reaction temperature is 65 °C, the dropwise addition time is 0.5 h. After the dropwise addition is completed, it is kept warm at 70 °C for 1.5 h. After the reaction is completed, it is filtered and washed to obtain the product.
[0054] The average particle size of zinc oxide is 8 nm; the average particle size of the modified zinc oxide particles is 489 nm.
[0055] The density of the aluminate cement is 2.8 g / cm 3 , and the A700 model product sold by Zhengzhou Jinghua Special Cement Co., Ltd. is purchased.
[0056] The coagulant is aluminum sulfate; the thickener is hydroxyethyl cellulose; the preservative is sodium benzoate;
[0057] The dispersant is a composition of isomeric C13 fatty alcohol polyoxyethylene ether, triphenylvinylphenol polyoxyethylene ether and epoxy block polyether, and the mass ratio of the three is 3.5:1.5:7.
[0058] The hydroxyl value of isomeric C13 fatty alcohol polyoxyethylene ether is 75 mgKOH / g, and the E-1312 model product sold by Haining Guoyun Chemical Co., Ltd. is purchased.
[0059] The weight average molecular weight of the epoxy block polyether is 3000 Da, and the L64 model ethylene oxide-propylene oxide block polyether product sold by BASF in Germany is purchased, and the ethylene oxide block content is 38 wt%.
[0060] The HLB value of triphenylvinylphenol polyoxyethylene ether is 17.4.
[0061] In the second aspect of this embodiment, a preparation process of the above inorganic silicon deep-penetrating crystallization waterproof agent is provided, which specifically includes the following steps: S1: Mix the active sodium silicate with a part of deionized water and stir until completely dissolved to form a uniform mixture. In another container, dry-mix the nano composite particles, dispersant and aluminate cement evenly, and then add the remaining deionized water to make a slurry to obtain a mixed slurry; S2: Slowly add the mixed slurry to the mixture, and stir with a high-speed stirrer at 1000 rpm for 35 minutes to ensure that the two components are fully mixed. Then, add a coagulant, thickener and preservative in sequence, and continue to stir for 8 minutes after adding each material until all components are evenly distributed in the mixture; S3: After the stirring is completely finished, screen the product through a 450-mesh sieve to remove large particles and impurities. Then, transfer the product to a clean container and seal it for storage, avoiding direct sunlight, and keeping the temperature between 10°C and 30°C to obtain the product.
[0062] Example 2
[0063] The specific implementation manner of this embodiment is basically the same as that of Example 1, except that: for the inorganic silicon deep-penetrating crystallization waterproof agent, by mass, the raw materials are: 55 parts of active sodium silicate, 22.2 parts of nano composite particles, 12.4 parts of aluminate cement, 1.5 parts of coagulant, 7.8 parts of dispersant, 4.8 parts of thickener, 0.16 part of preservative, and 58 parts of deionized water.
[0064] Example 3
[0065] The specific implementation manner of this embodiment is basically the same as that of Example 1, except that: for the inorganic silicon deep-penetrating crystallization waterproof agent, by mass, the raw materials are: 45.5 parts of active sodium silicate, 27.5 parts of nano composite particles, 15 parts of aluminate cement, 2.2 parts of coagulant, 12.6 parts of dispersant, 3.5 parts of thickener, 0.16 part of preservative, and 60 parts of deionized water.
[0066] Comparative Example 1
[0067] The specific implementation manner of this comparative example is basically the same as that of Example 1, except that: for the inorganic silicon deep-penetrating crystallization waterproof agent, by mass, the raw materials are: 65.5 parts of active sodium silicate, 10.5 parts of nano composite particles, 20.5 parts of aluminate cement, 2.1 parts of coagulant, 10.8 parts of dispersant, 4.2 parts of thickener, 0.16 part of preservative, and 60 parts of deionized water.
[0068] Comparative Example 2
[0069] The specific implementation manner of this comparative example is basically the same as that of Example 1, except that: for the inorganic silicon deep penetration crystallization waterproof agent, by mass, the raw materials are: 50.5 parts of active sodium silicate, 33.8 parts of nano composite particles, 14.8 parts of aluminate cement, 2.1 parts of coagulant promoter, 4.1 parts of dispersant, 4.2 parts of thickener, 0.16 parts of preservative, and 60 parts of deionized water.
[0070] Comparative Example 3
[0071] The specific implementation manner of this comparative example is basically the same as that of Example 1, except that: the preparation method of the modified zinc oxide particles includes the following steps: S1: Mix 0.2 parts of zinc oxide and 6.8 parts of zirconium chloride and add them to 100 parts of deionized water. Add 1.8 parts of succinic anhydride and 0.35 parts of isopropyl tris(dodecylbenzenesulfonyl) titanate, heat up to 65 °C and keep warm for 3 h. After completion, centrifuge and filter the product, wash and dry it to obtain pretreated particles; S2: Mix 4.2 parts of pretreated particles, 2.9 parts of 1,4-benzenedicarboxylic acid and 0.8 parts of p-aminobenzoic acid and add them to 160 parts of DMF and stir completely. Heat up to 120 °C and keep warm and react for 22 h. After completion, naturally cool the product to room temperature, wash it 3 times alternately with DMF and absolute ethanol to obtain pre-modified particles; S3: Mix 5.2 parts of pre-modified particles and 0.6 parts of ammonia water and add them to 180 parts of deionized water. Dropwise add a deionized water solution containing 0.14 parts of triethanolamine and 1.8 parts of tetraethyl orthosilicate (a total of 40 parts). The dropping reaction temperature is 65 °C and the dropping time is 0.5 h. After dropping, keep warm at 70 °C for 1.5 h. After the reaction is completed, filter and wash to obtain the product.
[0072] The average particle size of the modified zinc oxide particles is 410 nm.
[0073] Comparative Example 4
[0074] The specific implementation of this comparative example is basically the same as that of Example 1, except that: the preparation method of the modified zinc oxide particles includes the following steps: S1: 2.5 parts of zinc oxide and 2.5 parts of zirconium chloride are mixed and added to 100 parts of deionized water, 1.1 parts of succinic anhydride and 0.18 parts of isopropyl tris(dodecylbenzenesulfonyl) titanate are added, the temperature is raised to 65 °C and kept warm for 3 h. After completion, the product is centrifuged and filtered, washed and dried to obtain pretreated particles; S2: 3.8 parts of the pretreated particles, 2.2 parts of 1,4-benzenedicarboxylic acid and 1.4 parts of p-aminobenzoic acid are mixed and added to 120 parts of DMF and stirred completely. The temperature is raised to 120 °C and kept warm for 22 h. After completion, the product is naturally cooled to room temperature and washed 3 times alternately with DMF and absolute ethanol to obtain pre-modified particles; S3: 4.2 parts of the pre-modified particles and 0.9 parts of ammonia water are mixed and added to 180 parts of deionized water, and an aqueous solution of deionized water containing 0.16 parts of triethanolamine and 3 parts of tetraethyl orthosilicate (40 parts in total) is added dropwise. The dropping reaction temperature is 65 °C, the dropping time is 0.5 h, and after dropping, it is kept warm at 70 °C for 1.5 h. After the reaction is completed, it is filtered and washed to obtain the product.
[0075] The average particle size of the modified zinc oxide particles is 604 nm.
[0076] Comparative Example 5
[0077] The specific implementation of this comparative example is basically the same as that of Example 1, except that: the average particle size of zinc oxide is 35 nm; the average particle size of the modified zinc oxide particles is 721 nm.
[0078] Comparative Example 6
[0079] The specific implementation of this comparative example is basically the same as that of Example 1, except that: the dispersant is a composition of isomeric C13 fatty alcohol polyoxyethylene ether, triphenylvinylphenol polyoxyethylene ether and epoxy block polyether, and the mass ratio of the three is 8:5:3.
[0080] Comparative Example 7
[0081] The specific implementation of this comparative example is basically the same as that of Example 1, except that: the hydroxyl value of isomeric C13 fatty alcohol polyoxyethylene ether is 150 mgKOH / g, and it is a product of model E-1304 sold by Haian Guoyun Chemical Co., Ltd.
[0082] The weight average molecular weight of the epoxy block polyether is 1500 Da, and it is an ethylene oxide-propylene oxide block polyether product of model L42 sold by BASF in Germany, and the ethylene oxide block content is 20 wt%.
[0083] Performance evaluation:
[0084] Mechanical tests: The flexural strength and compressive strength of the waterproofing agents prepared in the examples and comparative examples were tested with reference to the standard GB / T 18445-2012. The test values were the average of 10 tests and were recorded in Table 1.
[0085] Waterproof tests: The waterproofing agents prepared in the examples and comparative examples were tested for impermeability with reference to the standard GB / T 18445-2012. The impermeability pressure was measured. The test values were the average of 10 tests and were recorded in Table 1.
[0086] Corrosion and heat resistance tests: The waterproofing agents prepared in the examples and comparative examples were immersed in a 10 wt% NaCl solution for 28 days at a temperature maintained at 60 ± 2 °C. After the test was completed, they were taken out and observed for any obvious corrosion, damage, yellowing, and cracking. If not, it was recorded as qualified; otherwise, it was unqualified. 50 specimens were tested in each group, and the qualification rate of the specimens was recorded in Table 1.
[0087] Table 1 Performance test results
[0088]
[0089] From the data results of the examples, comparative examples, and Table 1 of this application, it can be seen that Examples 1-3 of this application have obvious advantages over Comparative Examples 1-6 in terms of mechanical properties, waterproof and corrosion resistance properties, heat resistance properties, and aging resistance properties. This is mainly because of the combined effect of the defined modified composite particles added in this application, the selection of specific dispersants, and other cooperative technical solutions. However, since Comparative Examples 1-7 did not adopt the technical solutions defined in this application, obvious disadvantages occurred in the above performance tests, which further proves the necessity of the defined technical solutions of this application for the technical effects and solving technical problems of this application.
Claims
1. An inorganic silicon deep penetrating crystalline waterproofing agent, characterized in that: The raw materials are, by weight: 40-60 parts of active sodium silicate, 20-35 parts of nanocomposite particles, 10-15 parts of aluminate cement, 1-3 parts of coagulant, 5-15 parts of dispersant, 3-5 parts of thickener, 0.1-0.3 parts of preservative, and 40-65 parts of deionized water; The modulus of the active sodium silicate is 2 to 4; The nanocomposite particles are a composition of nano silicon dioxide and modified zinc oxide particles; The mass ratio of the nano-silicon dioxide to the modified zinc oxide particles is (2.8-3.5): (1.5-2.5); The average particle size of the nano silicon dioxide is 40-60 nm; Preparation method of modified zinc oxide particles The following steps are involved: S1: Mix zinc oxide and zirconium chloride and add them to deionized water, add succinic anhydride and isopropyl tri(dodecylbenzenesulfonyl) titanate, heat to 60-65°C and keep warm for 3-4 hours, after completion, centrifuge and filter the product, wash and dry to obtain pretreated particles; S2: Mix the pretreated particles with 1,4-phthalic acid and p-aminobenzoic acid and add them to DMF, stir thoroughly, heat to 120-130°C, keep warm for 20-22 hours, after completion, naturally cool the product to room temperature, wash alternately with DMF and anhydrous ethanol 2-3 times to obtain pre-modified particles; S3: Mix the pre-modified particles and ammonia water and add them to deionized water, add triethanolamine and deionized water solution of ethyl orthosilicate dropwise, the dropwise reaction temperature is 60-65°C, the dropwise addition time is 0.5-0.6h, after the dropwise addition is completed, keep warm at 70-75°C for 1-1.5 hours, filter and wash after the reaction is completed, and obtain; The mass ratio of zinc oxide, zirconium chloride, succinic anhydride and isopropyl tri(dodecylbenzenesulfonyl) titanate is (0.6-1): (4-5): (1.5-1.8): (0.2-0.25); The mass ratio of 1,4-phthalic acid to p-aminobenzoic acid in the pretreated particles is (3.5-4): (2-2.5): (1-1.5); The average particle size of the modified zinc oxide particles is 450-550 nm; The dispersant is a composition of C12-C14 fatty alcohol polyoxyethylene ether, tristyrylphenol polyoxyethylene ether and epoxy block polyether, and the mass ratio of the three is (3-3.5): (1-2): (6-8); The hydroxyl value of the C12-C14 fatty alcohol polyoxyethylene ether is 70-90 mgKOH / g; the HLB value of the tristyrylphenol polyoxyethylene ether is 16-18; The weight average molecular weight of the epoxy block polyether is 2000-4000 Da; the ethylene oxide block content of the epoxy block polyether is 25-40 wt %.
2. The inorganic silicon deep penetrating crystalline waterproofing agent according to claim 1, characterized in that: The mass ratio of the active sodium silicate, the nanocomposite particles and the aluminate cement is (45-55): (22-28): (12-15).
3. The inorganic silicon deep penetrating crystalline waterproofing agent according to claim 2, characterized in that: The average particle size of the zinc oxide is 5-10 nm.
4. The inorganic silicon deep penetrating crystalline waterproofing agent according to claim 3, characterized in that: The density of the aluminate cement is 2.5-3 g / cm 3 .
5. The inorganic silicon deep penetrating crystalline waterproofing agent according to claim 4, characterized in that: The coagulant is at least one of calcium chloride, calcium nitrate, sodium carbonate, polyphosphate and aluminum sulfate.
6. A process for preparing the inorganic silicon deep penetrating crystalline waterproofing agent according to any one of claims 1 to 5, characterized in that: The specific steps include: S1: Mix active sodium silicate with part of deionized water, stir until completely dissolved to form a uniform mixed liquid. In another container, dry-mix the nanocomposite particles, dispersant and aluminate cement, and then add the remaining deionized water to make a slurry to obtain a mixed slurry. S2: Slowly add the mixed slurry to the mixed liquid, stir with a high-speed stirrer at 800-1000rpm for 30-40min to ensure that the two components are fully mixed, then add the coagulant, thickener and preservative in turn, and continue stirring for 5-10min after adding each material until all the ingredients are evenly distributed in the mixed liquid. S3: After the stirring is completely completed, pass the product through a 400-600 mesh sieve to remove large particles and impurities, then transfer the product to a clean container and seal it for storage, avoid direct sunlight, and keep the temperature between 10℃ and 30℃.
Citation Information
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