A diatomaceous earth / chitosan composite modified asphalt paint and a preparation method thereof
By modifying asphalt paint with diatomaceous earth/chitosan composite material, the problems of poor adhesion and flexibility of existing asphalt paint are solved, achieving faster drying speed and better leveling performance, thus improving the anti-corrosion effect on metals.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- PANJIN NORTHERN ASPHALT CO LTD
- Filing Date
- 2024-08-27
- Publication Date
- 2026-08-04
AI Technical Summary
Existing asphalt paints have poor metal adhesion and flexibility, are prone to peeling after long-term use, lose their protective function, and have slow drying speed and poor leveling properties.
Asphalt paint modified with diatomaceous earth/chitosan composite material: Diatomaceous earth/chitosan composite material is prepared by ultrasonication and then combined with petroleum asphalt, organic solvents, vegetable oils, etc. to prepare modified asphalt paint. The porosity of diatomaceous earth and the chelating ability of chitosan are utilized to improve adhesion and leveling performance, and a drying agent is added to accelerate drying.
It significantly improves the metal adhesion, flexibility and drying speed of asphalt paint, reduces pinholes, and increases film thickness and viscosity.
Smart Images
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of metal anti-corrosion paint technology, and particularly relates to a diatomaceous earth / chitosan composite material modified asphalt paint and its preparation method. Background Technology
[0002] With the widespread application of metallic materials in various industries, corrosion problems have become increasingly prominent, causing huge economic losses. Metal anti-corrosion paint, by isolating metal from corrosive substances and effectively cutting off the corrosion cycle, is one of the most effective measures for protecting metal substrates from corrosion. Asphalt paint, as a type of metal anti-corrosion paint, has good water resistance, acid resistance, alkali resistance, and chemical resistance, and is mainly used for metal materials in indoor, underwater, underground, and equipment not exposed to sunlight. However, asphalt paint alone has poor metal adhesion and flexibility, and is prone to peeling after long-term use, losing its protective function and causing localized corrosion of the metal material, thus limiting its widespread application. Adding drying vegetable oils or alkyd resins to asphalt paint can improve adhesion and flexibility, but the drying speed will be affected and reduced. At the same time, the paint film formed by asphalt paint has pinholes, requiring the addition of leveling agents to improve the leveling properties of the asphalt paint. Summary of the Invention
[0003] In view of this, to solve this problem, the present invention provides a diatomaceous earth / chitosan composite material modified asphalt paint and its preparation method. The present invention utilizes ultrasound to prepare a diatomaceous earth / chitosan composite material (wherein ultrasound can rapidly and efficiently disperse solid materials such as diatomaceous earth and chitosan in solution, accelerating the reaction process of the composite material). The diatomaceous earth / chitosan composite material modified asphalt paint prepared by the invention not only significantly improves the adhesion, film thickness, and leveling performance of the asphalt paint on metal surfaces, but also exhibits good drying speed.
[0004] To achieve the above objectives, the present invention adopts the following technical solution:
[0005] The first technical objective of this invention is to provide a diatomaceous earth / chitosan composite material, made from the following raw materials in parts by weight:
[0006] Diatomaceous earth: 5-15 parts;
[0007] Silane coupling agent: 5-15 parts;
[0008] Ethanol aqueous solution: 150-200 parts;
[0009] Acetic acid: 0.5-2 parts;
[0010] Chitosan: 0.1-0.3 parts.
[0011] Furthermore, the silane coupling agent is γ-methacryloxypropyltrimethoxysilane, γ-aminopropyltriethoxysilane, or γ-glycidoxypropyltrimethoxysilane, preferably γ-methacryloxypropyltrimethoxysilane. Compared with the other two silane coupling agents, it has weaker polarity and is closer to the polarity of petroleum asphalt, making it more soluble in weakly polar organic solvents such as xylene and solvent oil, which can improve the dispersion stability of diatomaceous earth / chitosan composite materials in asphalt paint.
[0012] Furthermore, the ethanol solution has a mass fraction of 40-80%, preferably 45-55%.
[0013] Furthermore, the chitosan has a molecular weight of 30,000-100,000, preferably 30,000. Chitosan with a lower molecular weight is more soluble in acetic acid-containing solutions, which helps chitosan and diatomaceous earth to form non-covalent complexes on the surface.
[0014] Furthermore, the preparation method of the diatomaceous earth / chitosan composite material is as follows:
[0015] Step 1: Calcine diatomaceous earth in a muffle furnace at 450℃ for 3 hours, cool it to room temperature and add it to an ethanol aqueous solution, then add acetic acid and stir at 60℃ for 0.5-1 hours to obtain an acidified diatomaceous earth dispersion.
[0016] Step 2: Add silane coupling agent and chitosan to the acidified diatomaceous earth dispersion, sonicate at 80°C for 2 hours, then filter and dry to obtain diatomaceous earth / chitosan composite material.
[0017] It should be noted that the diatomaceous earth needs to be calcined at high temperature (450℃) to remove organic impurities, increase micropore permeability, and facilitate surface modification and composite with other materials.
[0018] The second technical objective of this invention is to provide a diatomaceous earth / chitosan composite material modified asphalt paint, made from the following raw materials in parts by weight:
[0019] Petroleum asphalt: 50-60 parts;
[0020] Organic solvent: 40-50 parts;
[0021] Vegetable oil: 5-10 parts;
[0022] Diatomaceous earth / chitosan composite material: 2-5 parts;
[0023] Drying agent: 0.3-1.5 parts;
[0024] Dispersant: 0.05-0.2 parts.
[0025] Furthermore, the petroleum asphalt is No. 10 building petroleum asphalt, preferably No. 10 building petroleum asphalt with a softening point of 110-130℃.
[0026] Furthermore, the organic solvent is selected from one or more combinations of No. 100 solvent oil, No. 200 solvent oil, toluene, and xylene, preferably a mixture of No. 200 solvent oil and xylene in a weight ratio of 1:(0.5-4), and more preferably a weight ratio of 1:(1-3).
[0027] Furthermore, the vegetable oil is selected from one or more combinations of soybean oil, castor oil, rapeseed oil, linseed oil, and tung oil, with tung oil being preferred.
[0028] Furthermore, the drying agent is composed of lead tar, cobalt tar and zinc tar in the following mass percentages: 20-30%, 20-30%, and 40-60%.
[0029] Furthermore, the dispersant is a phosphate ester type dispersant or a polyurethane dispersant, preferably a phosphate ester type dispersant, which has better compatibility with asphalt paint and is more conducive to the dispersion stability of diatomaceous earth / chitosan composite materials.
[0030] The third technical objective of this invention is to provide a method for preparing the modified asphalt paint, specifically including the following steps:
[0031] Step 1: Crush petroleum asphalt into granules and dissolve it in an organic solvent by stirring at room temperature for 2-3 hours to obtain unmodified asphalt paint mother liquor.
[0032] Step 2: Grind the diatomaceous earth / chitosan composite material into a fine powder, and add it together with tung oil, dispersant and drier to the unmodified asphalt paint mother liquor in that order. Stir at 80-100℃ for 2-3 hours to obtain the modified asphalt paint.
[0033] By adopting the above technical solution and selecting petroleum asphalt with a higher softening point, and crushing it into granules, the heat resistance of asphalt paint can be improved, and the solubility of petroleum asphalt in organic solvents can be enhanced, allowing petroleum asphalt to dissolve in organic solvents at room temperature. Chitosan itself possesses multiple hydroxyl and amino groups, exhibiting strong chelation and adsorption capabilities with metal surfaces. This allows the composite chitosan and diatomaceous earth to further improve the metal adhesion of asphalt paint. The porosity of diatomaceous earth can accelerate the evaporation of solvents in the paint film and the rate of oxidative drying reaction of vegetable oils, thereby accelerating the drying speed of the asphalt paint. Diatomaceous earth modified with a silane coupling agent can improve its wetting state, thereby enhancing the leveling performance of the asphalt paint. Dispersing the diatomaceous earth / chitosan composite material in asphalt paint can alter its rheological properties, increase viscosity, and increase film thickness.
[0034] Compared with the prior art, the beneficial effects of the present invention are:
[0035] By adding diatomaceous earth / chitosan composite material, the metal adhesion and flexibility of asphalt paint can be significantly improved, the drying speed of asphalt paint film can be accelerated, its leveling performance can be improved, and the formation of pinholes can be suppressed. In addition, the addition of composite material can increase the viscosity of asphalt paint and increase the film thickness. Detailed Implementation
[0036] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0037] The term "embodiment" used herein, as an example, is not necessarily to be construed as superior to or better than other embodiments. Performance testing in the embodiments of this application, unless otherwise specified, employs conventional testing methods in the art. It should be understood that the terminology used in this application is merely for describing particular implementations and is not intended to limit the scope of this disclosure.
[0038] Unless otherwise stated, the technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains; other experimental methods and technical means not specifically mentioned herein refer to experimental methods and technical means commonly used by one of ordinary skill in the art.
[0039] To better illustrate the content of this application, numerous specific details are provided in the following detailed embodiments. Those skilled in the art should understand that this application can be implemented even without certain specific details. In the embodiments, some methods, means, instruments, and devices well-known to those skilled in the art are not described in detail in order to highlight the main points of this application.
[0040] Without conflict, the technical features disclosed in the embodiments of this application can be combined arbitrarily, and the resulting technical solution belongs to the content disclosed in the embodiments of this application.
[0041] This invention discloses a diatomaceous earth / chitosan composite material and a method for preparing its modified asphalt paint.
[0042] To better understand the present invention, the following embodiments are provided for further detailed description of the present invention, but they should not be construed as limiting the present invention. Any non-essential improvements and adjustments made by those skilled in the art based on the above-described invention are also considered to fall within the protection scope of the present invention.
[0043] (I) Example of preparation of diatomaceous earth / chitosan composite material
[0044] The raw material composition and proportions for preparation examples 1-7 are shown in Table 1.
[0045] Preparation Examples 1-7: A method for preparing a diatomaceous earth / chitosan composite material is as follows:
[0046] Step 1: Calcine diatomaceous earth in a muffle furnace at 450°C for 3 hours, cool it to room temperature and add it to an ethanol-water solution, then add acetic acid and stir at 60°C for 0.5 hours to obtain an acidified diatomaceous earth dispersion.
[0047] Step 2: Add silane coupling agent γ-methacryloxypropyltrimethoxysilane (KH 570) and chitosan (MW=30000) to the acidified diatomaceous earth dispersion, sonicate at 80℃ for 2 hours, then filter and dry to obtain diatomaceous earth / chitosan composite material.
[0048] Table 1. Raw material composition and proportions for preparation examples 1-7
[0049]
[0050] (II) Examples of Preparation of Diatomaceous Earth / Chitosan Composite Material Modified Asphalt Paint
[0051] Example 1
[0052] This embodiment provides a diatomaceous earth / chitosan composite material modified asphalt paint, the preparation method of which is as follows:
[0053] Step 1: Crush 50g of No. 10 building petroleum asphalt into granules, and dissolve it in a mixture of 8g of No. 200 solvent oil and 25g of xylene by stirring at room temperature for 2 hours to obtain unmodified asphalt paint mother liquor.
[0054] Step 2: Grind 3g of the diatomaceous earth / chitosan composite material obtained in Preparation Example 1 into a fine powder, and add it to the unmodified asphalt paint mother liquor along with 10g of boiled tung oil, 0.05g of phosphate ester dispersant (Evonik TEGO DISPERS 655), 0.21g of cobalt tar, 0.21g of zinc tar, and 0.28g of lead tar in that order. Stir at 100°C for 3 hours to obtain modified asphalt paint.
[0055] Example 2
[0056] This embodiment provides a diatomaceous earth / chitosan composite material modified asphalt paint, the preparation method of which is as follows:
[0057] Step 1: Crush 50g of No. 10 building petroleum asphalt into granules, and dissolve it in a mixture of 8g of No. 200 solvent oil and 25g of xylene by stirring at room temperature for 2 hours to obtain unmodified asphalt paint mother liquor.
[0058] Step 2: Grind 5g of the diatomaceous earth / chitosan composite material obtained in Preparation Example 2 into a fine powder, and add it to the unmodified asphalt paint mother liquor along with 10g of boiled tung oil, 0.10g of phosphate ester dispersant (Evonik TEGO DISPERS 655), 0.09g of cobalt tar, 0.09g of zinc tar, and 0.12g of lead tar in sequence. Stir at 100°C for 3 hours to obtain modified asphalt paint.
[0059] Example 3
[0060] This embodiment provides a diatomaceous earth / chitosan composite material modified asphalt paint, the preparation method of which is as follows:
[0061] Step 1: Crush 50g of No. 10 building petroleum asphalt into granules, and dissolve it in a mixture of 8g of No. 200 solvent oil and 25g of xylene by stirring at room temperature for 2 hours to obtain unmodified asphalt paint mother liquor.
[0062] Step 2: Grind 3g of the diatomaceous earth / chitosan composite material obtained in Preparation Example 3 into a fine powder, and add it to the unmodified asphalt paint mother liquor along with 5g of boiled tung oil, 0.05g of phosphate ester dispersant (Evonik TEGO DISPERS 655), 0.09g of cobalt tar, 0.09g of zinc tar, and 0.12g of lead tar in sequence. Stir at 100°C for 3 hours to obtain modified asphalt paint.
[0063] Example 4
[0064] This embodiment provides a diatomaceous earth / chitosan composite material modified asphalt paint, the preparation method of which is as follows:
[0065] Step 1: Crush 50g of No. 10 building petroleum asphalt into granules, and dissolve it in a mixture of 8g of No. 200 solvent oil and 25g of xylene by stirring at room temperature for 2 hours to obtain unmodified asphalt paint mother liquor.
[0066] Step 2: Grind 5g of the diatomaceous earth / chitosan composite material obtained in Preparation Example 4 into a fine powder, and add it to the unmodified asphalt paint mother liquor along with 10g of boiled tung oil, 0.15g of phosphate ester dispersant (Evonik TEGO DISPERS 655), 0.3g of cobalt tar, 0.3g of zinc tar, and 0.4g of lead tar. Stir at 100°C for 3 hours to obtain modified asphalt paint.
[0067] Example 5
[0068] This embodiment provides a diatomaceous earth / chitosan composite material modified asphalt paint, the preparation method of which is as follows:
[0069] Step 1: Crush 50g of No. 10 building petroleum asphalt into granules, and dissolve it in a mixture of 8g of No. 200 solvent oil and 25g of xylene by stirring at room temperature for 2 hours to obtain unmodified asphalt paint mother liquor.
[0070] Step 2: Grind 5g of the diatomaceous earth / chitosan composite material obtained in Preparation Example 5 into a fine powder, and add it to the unmodified asphalt paint mother liquor along with 5g of boiled tung oil, 0.05g of phosphate ester type dispersant (Evonik TEGO DISPERS 655), 0.09g of cobalt tar, 0.09g of zinc tar, and 0.12g of lead tar in sequence. Stir at 100°C for 3 hours to obtain modified asphalt paint.
[0071] Example 6
[0072] This embodiment provides a diatomaceous earth / chitosan composite material modified asphalt paint, the preparation method of which is as follows:
[0073] Step 1: Crush 50g of No. 10 building petroleum asphalt into granules, and dissolve it in a mixture of 8g of No. 200 solvent oil and 25g of xylene by stirring at room temperature for 2 hours to obtain unmodified asphalt paint mother liquor.
[0074] Step 2: Grind 3g of the diatomaceous earth / chitosan composite material obtained in Preparation Example 6 into a fine powder, and add it to the unmodified asphalt paint mother liquor along with 5g of boiled tung oil, 0.10g of phosphate ester dispersant (Evonik TEGO DISPERS 655), 0.18g of cobalt tar, 0.18g of zinc tar, and 0.24g of lead tar. Stir at 100°C for 3 hours to obtain modified asphalt paint.
[0075] Example 7
[0076] This embodiment provides a diatomaceous earth / chitosan composite material modified asphalt paint, the preparation method of which is as follows:
[0077] Step 1: Crush 50g of No. 10 building petroleum asphalt into granules, and dissolve it in a mixture of 8g of No. 200 solvent oil and 25g of xylene by stirring at room temperature for 2 hours to obtain unmodified asphalt paint mother liquor.
[0078] Step 2: Grind 5g of the diatomaceous earth / chitosan composite material obtained in Preparation Example 7 into a fine powder, and add it to the unmodified asphalt paint mother liquor along with 10g of boiled tung oil, 0.05g of phosphate ester dispersant (Evonik TEGO DISPERS 655), 0.18g of cobalt tar, 0.18g of zinc tar, and 0.24g of lead tar in sequence. Stir at 100°C for 3 hours to obtain modified asphalt paint.
[0079] Comparative Example
[0080] 50g of No. 10 building petroleum asphalt was crushed into granules and dissolved in a mixture of 8g of No. 200 solvent oil and 25g of xylene by stirring at room temperature for 2 hours to obtain unmodified asphalt paint.
[0081] The viscosity (GB / T 1723), appearance, metal adhesion (GB / T 1720), flexibility (GB / T 1730), and actual drying time (GB / T 1728) of the asphalt paint in comparative examples and Examples 1-7 were measured. Generally, the higher the viscosity, the greater the film thickness. The appearance of the paint film was observed for pinholes; the more pinholes present, the worse the leveling. Metal adhesion was assessed by performing a circular scratch test on the paint film on a metal surface to observe the peeling. The results were graded from 1 to 7, with lower grades indicating stronger adhesion. Flexibility was assessed by subjecting the metal specimens to varying degrees of bending deformation using rods of different diameters. Smaller rod diameters resulted in greater bending deformation. The damage state of the paint film on the metal surface was observed. The test results showed the minimum rod diameter at which the paint film showed no cracks, peeling, or network patterns. A smaller minimum rod diameter indicated better flexibility. A shorter actual drying time indicated a faster drying speed. The test results for Examples 1-7 are shown in Table 2.
[0082] Table 2 shows the metal adhesion, flexibility, and actual drying time of the asphalt paint in Examples 1-7.
[0083]
[0084]
[0085] The results showed that adding diatomaceous earth / chitosan composite material to prepare modified asphalt paint significantly improved the film thickness, leveling properties, metal adhesion, and drying speed of the asphalt paint. Optimal performance could be achieved by controlling the preparation of the diatomaceous earth / chitosan composite material and the content of the diatomaceous earth / chitosan composite material, boiled tung oil, and drying agent in the asphalt paint.
[0086] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A diatomaceous earth / chitosan composite material modified asphalt paint, characterized in that, The diatomaceous earth / chitosan composite modified asphalt paint is made from the following raw materials in parts by weight: Petroleum asphalt: 50-60 parts; Organic solvent: 40-50 parts; Vegetable oil: 5-10 parts; Diatomaceous earth / chitosan composite material: 2-5 parts; Drying agent: 0.3-1.5 parts; Dispersant: 0.05-0.2 parts; The diatomaceous earth / chitosan composite material is made from the following raw materials in parts by weight: Diatomaceous earth: 5-15 parts; Silane coupling agent: 5-15 parts; Ethanol aqueous solution: 150-200 parts; Acetic acid: 0.5-2 parts; Chitosan: 0.1-0.3 parts; Furthermore, the preparation process of the diatomaceous earth / chitosan composite material is as follows: 1) Calcine diatomaceous earth in a muffle furnace at 430-460 ℃ for 2-4 h, cool to room temperature and add to an ethanol aqueous solution, then add acetic acid, and stir at 60-80 ℃ for 0.5-1 h to obtain an acidified diatomaceous earth dispersion. 2) Add silane coupling agent and chitosan to the acidified diatomaceous earth dispersion obtained in step 1), sonicate at 60-80 ℃ for 1.5-2.5 h, then filter and dry to obtain the diatomaceous earth / chitosan composite material.
2. The diatomaceous earth / chitosan composite modified asphalt paint according to claim 1, characterized in that, The petroleum asphalt is No. 10 building petroleum asphalt.
3. The diatomaceous earth / chitosan composite modified asphalt paint according to claim 1, characterized in that, The organic solvent is selected from one or more combinations of No. 100 solvent oil, No. 200 solvent oil, toluene, and xylene.
4. The diatomaceous earth / chitosan composite material modified asphalt paint according to claim 1, characterized in that, The vegetable oil is selected from one or more combinations of soybean oil, castor oil, rapeseed oil, linseed oil, and tung oil.
5. The diatomaceous earth / chitosan composite modified asphalt paint according to claim 1, characterized in that, The drying agent is composed of lead tar, cobalt tar and zinc tar in the following mass percentages: 20-30%, 20-30%, and 40-60%.
6. The diatomaceous earth / chitosan composite material modified bitumen paint according to claim 1, characterized in that, The dispersant is a phosphate ester type dispersant or a polyurethane dispersant.
7. The diatomaceous earth / chitosan composite material modified bitumen paint according to claim 6, characterized in that, The dispersant is a phosphate ester type dispersant.
8. The diatomaceous earth / chitosan composite material modified bitumen paint according to claim 7, characterized in that, The silane coupling agent is selected from one or more combinations of γ-methacryloxypropyltrimethoxysilane, γ-aminopropyltriethoxysilane, and γ-glycidoxypropyltrimethoxysilane.
9. The diatomaceous earth / chitosan composite material modified bitumen paint according to claim 7, characterized in that, The ethanol solution has a mass fraction of 40-80%, and the chitosan has a molecular weight of 30,000-100,000.
10. A method for preparing a diatomaceous earth / chitosan composite modified asphalt paint as described in claim 1, characterized in that, The method specifically includes the following steps: Step 1: Crush petroleum asphalt into granules and dissolve it in an organic solvent by stirring at room temperature for 2-3 hours to obtain unmodified asphalt paint mother liquor; Step 2: Grind the diatomaceous earth / chitosan composite material into a fine powder, and add it along with vegetable oil, dispersant and drier to the unmodified asphalt paint mother liquor obtained in Step 1. Stir at 80-100℃ for 2-3 h to obtain the modified asphalt paint.