An organic phosphonic acid treating agent, a high-temperature-resistant titanium dioxide, and a preparation method and application thereof

Abstract

The application provides an organic phosphonic acid treating agent, a high-temperature-resistant titanium white powder and a preparation method and application thereof, and relates to the technical field of titanium white powder modification. The organic phosphonic acid treating agent comprises an organic phosphonic acid compound, alcohol, phosphoric acid and water, and the mass ratio of the organic phosphonic acid compound, alcohol, phosphoric acid and water is 100: (5-10): (0.01-0.25): (0.75-0.99). The organic phosphonic acid treating agent is used for preparing the high-temperature-resistant titanium white powder. The stable coating layer formed by the organic phosphonic acid molecules on the surface of the titanium white powder, and the addition of phosphoric acid promotes more chemical adsorption on the surface, so that the modified titanium white powder can still maintain the structure and performance integrity in a high-temperature system, the temperature resistance of the powder is significantly improved, the interface compatibility of the titanium white powder and a water-based resin system is improved, and the powder is endowed with excellent dispersibility and stability.

Description

Technical Field

[0001] This application relates to the field of titanium dioxide modification technology, and in particular to an organophosphonic acid treatment agent, high-temperature resistant titanium dioxide, its preparation method and application. Background Technology

[0002] Driven by strong environmental policies, the global water-based ink market is gradually replacing traditional solvent-based inks. The rise of the water-based ink industry has become a new trend in the printing industry, but many problems exist in the transition to water-based inks. In particular, the high-temperature resistance characteristic is a significant challenge; most water-based inks only need to withstand temperatures up to 120 degrees Celsius. o C~150 o Short-term steaming or hot air treatment is acceptable for C, but in special printing fields such as glass and ceramics, it needs to withstand 500°C. o C~700 o C undergoes high-temperature sintering. Therefore, for titanium dioxide used in water-based inks, in addition to conventional properties, its chemical stability and temperature resistance are equally crucial.

[0003] To achieve the aforementioned properties, the surface modification of titanium dioxide must involve inorganic coating treatment, i.e., forming a dense oxide protective film on the surface of the titanium dioxide particles, such as single aluminum coating, silicon-aluminum composite coating, or zirconium-aluminum composite coating. This inorganic coating layer not only provides the powder with basic chemical stability and weather resistance, but also provides abundant surface active sites for subsequent organic processing. Based on this, high-temperature resistant organic processing agents can be selected to perform secondary surface modification on titanium dioxide, enabling the modified powder to have a thermal decomposition temperature exceeding 300°C. o C, and at 270 o It exhibits no color change within a certain temperature range and demonstrates good dispersibility in water-based inks. Compared to organosilicon, organophosphonic acid exhibits superior temperature resistance. This is primarily due to the relatively stable PC and POC bonds in its structure, low sensitivity to moisture, and the fact that its P-OH bonds are not prone to self-polymerization, while the POC bonds are not easily hydrolyzed and broken, only condensing to form POP bonds at higher temperatures. Secondly, treatment agents containing hydroxyl groups can bond with metal atoms on the powder surface, forming M(metal)-OP or M(metal)-O-Si bonds. However, phosphorus has stronger non-metallic properties than silicon. During the surface modification of metal oxide powders, organophosphonic acid can form both M(metal)-OPC and M(metal)-OPOC bonds, exhibiting greater diversity and stronger bonding than organosilicon, thus imparting better high-temperature resistance, compatibility, and dispersibility to titanium dioxide. Summary of the Invention

[0004] In view of this, this application provides an organophosphonic acid treatment agent, high-temperature resistant titanium dioxide, its preparation method and application, and the titanium dioxide prepared by this method has excellent high-temperature resistance, compatibility and dispersibility.

[0005] This application provides an organophosphonic acid treatment agent, comprising an organophosphonic acid compound, an alcohol, phosphoric acid, and water; The mass ratio of the organophosphonic acid compound, alcohol, phosphoric acid and water is 100:(5~10):(0.01~0.25):(0.75~0.99).

[0006] In some specific implementations, the organophosphonic acid compound is selected from C3~C4. 20 One or more of the alkylphosphonic acids; The alcohol is selected from C1-C8 monohydric alcohols and C2-C6 monohydric alcohols. 12 One or more of the diols.

[0007] In some specific implementations, the organophosphonic acid compound is selected from one or more of n-butylphosphonic acid, isopropylphosphonic acid, n-pentylphosphonic acid, n-hexylphosphonic acid, n-octylphosphonic acid, n-decylphosphonic acid, and n-dodecylphosphonic acid; The alcohol is one or more of methanol, ethanol, isopropanol, n-butanol, and ethylene glycol.

[0008] This application also provides a method for preparing high-temperature resistant titanium dioxide, comprising the following steps: (1) The titanium dioxide filter cake treated with inorganic coating is mixed with deionized water to obtain titanium dioxide slurry; (2) The titanium dioxide slurry is reacted with an organophosphonic acid treatment agent to obtain a slurry; (3) The slurry is post-treated to obtain high-temperature resistant titanium dioxide; The organophosphonic acid treatment agent is any one of the organophosphonic acid treatment agents described in the above technical solutions.

[0009] In some specific implementations, in step (1), the mass ratio of the titanium dioxide filter cake to deionized water is 1:(1~4).

[0010] In some specific implementations, in step (1), the inorganic coating process is a single aluminum coating.

[0011] In some specific implementations, in step (2), the mass of the organophosphonic acid treatment agent is 0.3% to 1.0% of the mass of the titanium dioxide filter cake in step (1); The reaction time is 10 min to 50 min, and the reaction temperature is 40 °C. o C~60 o C.

[0012] In some specific implementations, in step (3), the post-processing includes one or more of drying, crushing, and air jet milling; The drying temperature is 100. o C~160 o C. This application also provides a high-temperature resistant titanium dioxide, obtained according to the preparation method described in any of the above technical solutions.

[0013] This application also provides a high-temperature resistant water-based ink, comprising high-temperature resistant titanium dioxide prepared according to any one of the above technical solutions or the high-temperature resistant titanium dioxide described in the above technical solutions.

[0014] This application provides an organophosphonic acid treatment agent, high-temperature resistant titanium dioxide, and their preparation method and application. The organophosphonic acid treatment agent includes an organophosphonic acid compound, an alcohol, a phosphate, and water, wherein the mass ratio of the organophosphonic acid compound, alcohol, phosphate, and water is 100:(5~10):(0.01~0.25):(0.75~0.99). The method for preparing high-temperature resistant titanium dioxide includes the following steps: (1) mixing titanium dioxide filter cake treated with inorganic coating with deionized water to obtain titanium dioxide slurry; (2) reacting the titanium dioxide slurry with the organophosphonic acid treatment agent to obtain a slurry; and (3) post-treating the slurry to obtain high-temperature resistant titanium dioxide. This application utilizes an organophosphonic acid molecule to form a stable coating layer on the surface of inorganically coated titanium dioxide, and adds phosphoric acid to promote greater chemical adsorption on the surface. This allows the modified titanium dioxide to maintain its structural and performance integrity in high-temperature systems, significantly improving the powder's temperature resistance. This effectively overcomes the defects of traditional organosilicon-treated titanium dioxide, such as yellowing and failure at high temperatures. Simultaneously, this coating layer improves the interfacial compatibility between titanium dioxide and water-based resin systems, endowing the powder with excellent dispersibility and stability. The technical solution of this application can efficiently modify titanium dioxide for water-based inks, significantly improving the temperature resistance, dispersibility, compatibility, and stability of water-based inks. This application provides a new approach for preparing highly dispersed, highly stable, and high-temperature resistant titanium dioxide, possessing significant industrial application and promotion value. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the sample from the dispersion test of Comparative Example 2 in Experimental Example 3; Figure 2 This is a schematic diagram of the sample from the dispersion test in Example 1 of Experiment 3. Detailed Implementation

[0016] It should be understood that the expression “one or more of…” individually includes each of the objects described after the expression, as well as various different combinations of two or more of the described objects, unless otherwise understood from the context and usage. The expression “and / or” combined with three or more described objects should be understood to have the same meaning, unless otherwise understood from the context.

[0017] The terms “including,” “having,” or “containing,” including the use of their grammatical synonyms, should generally be understood as open-ended and non-restrictive, for example, not excluding other unstated elements or steps, unless otherwise specifically stated or understood from the context.

[0018] It should be understood that the order of steps or the sequence of actions is not important as long as this application remains operational. Furthermore, two or more steps or actions can be performed simultaneously.

[0019] The use of any and all instances or exemplary language such as “e.g.” or “including” herein is merely intended to better illustrate the application and does not constitute a limitation on the scope of the application unless the claims are made. No language in this specification should be construed as indicating that any unclaimed element is essential to the practice of this application.

[0020] Furthermore, the numerical ranges and parameters used to define this application are approximate values, and the relevant values ​​in the specific embodiments have been presented as precisely as possible. However, any numerical value inevitably contains standard deviations due to individual test methods. Therefore, unless otherwise explicitly stated, it should be understood that all ranges, quantities, values, and percentages used in this disclosure are modified with the word "approximately." Here, "approximately" generally means that the actual value is within plus or minus 10%, 5%, 1%, or 0.5% of a specific value or range.

[0021] This application provides an organophosphonic acid treatment agent, comprising an organophosphonic acid compound, an alcohol, a phosphoric acid, and water, wherein the mass ratio of the organophosphonic acid compound, alcohol, phosphoric acid, and water is 100:(5~10):(0.01~0.25):(0.75~0.99).

[0022] In some specific implementations, the phosphoric acid is provided in the form of an aqueous phosphoric acid solution, wherein the aqueous phosphoric acid solution has a mass fraction of 0.5% to 10% and a pH value of 1 to 2, more preferably a mass fraction of 1% to 5% and a pH value of 1 to 2. In some specific implementations, the organophosphonic acid compound is selected from C3 to C4. 20 One or more of the alkylphosphonic acids, preferably one or more of n-butylphosphonic acid, isopropylphosphonic acid, n-pentylphosphonic acid, n-hexylphosphonic acid, n-octylphosphonic acid, n-decylphosphonic acid, and n-dodecylphosphonic acid. In some specific implementations, the alcohol is selected from C1-C8 monohydric alcohols and C2-C6 monohydric alcohols. 12 One or more of the diols, wherein the alcohol is one or more of methanol, ethanol, isopropanol, n-butanol and ethylene glycol.

[0023] This application also provides a method for preparing high-temperature resistant titanium dioxide, comprising the following steps: (1) The titanium dioxide filter cake treated with inorganic coating is mixed with deionized water to obtain titanium dioxide slurry; (2) The titanium dioxide slurry is reacted with an organophosphonic acid treatment agent to obtain a slurry; (3) The slurry is post-treated to obtain high-temperature resistant titanium dioxide; The organophosphonic acid treatment agent is any one of the organophosphonic acid treatment agents described in the above technical solutions. In this application, titanium dioxide filter cake that has undergone inorganic coating treatment is first mixed with deionized water to obtain a titanium dioxide slurry.

[0024] Specifically, this application adds the inorganic coated titanium dioxide filter cake from the same batch that has not undergone organic treatment to deionized water and stirs it with a high-speed stirrer to obtain a uniform titanium dioxide slurry. The uniformly stirred titanium dioxide slurry is then transferred to a mechanical stirrer for continuous stirring.

[0025] In some specific implementations, the mass ratio of titanium dioxide filter cake to deionized water is 1:(1~4), preferably 1:(1~4), and more preferably 1:1.5. The mass of deionized water added is such that the titanium dioxide filter cake can be well dispersed. In some specific implementations, the rotation speed of the high-speed stirrer is 800 r / min~1200 r / min, preferably 1000 r / min. In some specific implementations, the rotation speed of the mechanical stirrer is 150 r / min~450 r / min, preferably 300 r / min. In some specific implementations, the inorganic coating treatment is a single aluminum coating, preferably alumina.

[0026] After obtaining the titanium dioxide slurry, the titanium dioxide slurry is reacted with an organophosphonic acid treatment agent to obtain a slurry.

[0027] Specifically, the organophosphonic acid treatment agent described in any of the above technical solutions is added to the titanium dioxide slurry in the mechanical stirrer to carry out the reaction. The organophosphonic acid treatment agent is prepared by mixing an alcohol and a phosphoric acid aqueous solution evenly, and then slowly adding the organophosphonic acid compound at room temperature, preparing and using immediately.

[0028] This application does not impose any particular restrictions on the sources of the alcohol, phosphoric acid, and organophosphonic acid compound, nor on the preparation of the phosphoric acid aqueous solution. In some specific implementations, the mass ratio of the organophosphonic acid compound, alcohol, and phosphoric acid aqueous solution is 100:(1~15):(1~10), preferably 100:(5~10):(1~5). In some specific implementations, the organophosphonic acid compound is selected from C3~C4. 20One or more of the alkylphosphonic acids, preferably one or more of n-butylphosphonic acid, isopropylphosphonic acid, n-pentylphosphonic acid, n-hexylphosphonic acid, n-octylphosphonic acid, n-decylphosphonic acid, and n-dodecylphosphonic acid, more preferably isopropylphosphonic acid, n-butylphosphonic acid, n-hexylphosphonic acid, or n-octylphosphonic acid. In some specific implementations, the alcohol is selected from C1-C8 monohydric alcohols and C2-C6 monohydric alcohols. 12 The phosphoric acid solution contains one or more of the following diols, preferably one or more of methanol, ethanol, isopropanol, n-butanol, and ethylene glycol, more preferably ethanol. In some specific implementations, the mass fraction of the phosphoric acid aqueous solution is 0.5% to 10%, preferably 1% to 5%. In some specific implementations, the pH value of the phosphoric acid aqueous solution is 1 to 2, preferably 1 to 2. In some specific implementations, the phosphoric acid aqueous solution is prepared by diluting an 85% phosphoric acid aqueous solution with deionized water. In some specific implementations, the organophosphonic acid treatment is preferably carried out under stirring conditions, and the stirring time is 20 min to 50 min, preferably 30 min. In some specific implementations, the mass of the organophosphonic acid aqueous solution in the step is 0.3% to 1.0% of the mass of the titanium dioxide composite material, preferably 0.3% to 0.5%. In some specific implementations, the reaction time is 10 min to 50 min, preferably 30 min. In some specific implementations, the reaction temperature is 40°C. o C~60 o C, preferably 50 o C.

[0029] After obtaining the slurry, the slurry is post-processed to obtain high-temperature resistant titanium dioxide.

[0030] This application does not impose any special limitations on the post-processing. In some specific implementations, the post-processing includes one or more of drying, crushing, and air jet milling. In some specific implementations, the drying temperature is 100°C. o C~160 o C, preferably 100 o C~140 o C.

[0031] This application provides a method for preparing high-temperature resistant titanium dioxide. The preparation method is simple, avoids significant solvent loss, and has advantages such as environmental friendliness and economy. In the prior art, the treatment effect of organosilicon-based treatment agents largely depends on the water content of the powder and the system. Too little water will not form an effective coating layer, while too much water will result in an excessively thick coating layer. However, the organophosphonic acid provided in this application is not sensitive to water, and the amount of water does not affect the coating effect. In addition, the addition of alcohol in this application can increase the solubility of organophosphonic acid compounds, which can prevent the formation of insoluble metal phosphonate precipitates during organic treatment, thus avoiding the impact on the organic treatment effect. The addition of phosphoric acid solution in this application can better stimulate its reactivity, promote more chemical adsorption on the surface, and after heat treatment, form an orderly film layer that is tightly connected to the inner layer, is not easily washed away by solvent, and is not easily detached by simple mechanical peeling.

[0032] This application also provides a high-temperature resistant titanium dioxide, which is obtained according to the preparation method described in any of the above technical solutions.

[0033] This application also provides a high-temperature resistant water-based ink, comprising high-temperature resistant titanium dioxide prepared according to any one of the above technical solutions or the high-temperature resistant titanium dioxide described in the above technical solutions.

[0034] This application provides an organophosphonic acid treatment agent, high-temperature resistant titanium dioxide, and their preparation method and application. The organophosphonic acid treatment agent includes an organophosphonic acid compound, an alcohol, a phosphate, and water, wherein the mass ratio of the organophosphonic acid compound, alcohol, phosphate, and water is 100:(5~10):(0.01~0.25):(0.75~0.99). The method for preparing high-temperature resistant titanium dioxide includes the following steps: (1) mixing titanium dioxide filter cake treated with inorganic coating with deionized water to obtain titanium dioxide slurry; (2) reacting the titanium dioxide slurry with the organophosphonic acid treatment agent to obtain a slurry; and (3) post-treating the slurry to obtain high-temperature resistant titanium dioxide. This application utilizes an organophosphonic acid molecule to form a stable coating layer on the surface of inorganically coated titanium dioxide, and adds phosphoric acid to promote greater chemical adsorption on the surface. This allows the modified titanium dioxide to maintain its structural and performance integrity in high-temperature systems, significantly improving the powder's temperature resistance. This effectively overcomes the defects of traditional organosilicon-treated titanium dioxide, such as yellowing and failure at high temperatures. Simultaneously, this coating layer improves the interfacial compatibility between titanium dioxide and water-based resin systems, endowing the powder with excellent dispersibility and stability. The technical solution of this application can efficiently modify titanium dioxide for water-based inks, significantly improving the temperature resistance, dispersibility, compatibility, and stability of water-based inks. This application provides a new approach for preparing highly dispersed, highly stable, and high-temperature resistant titanium dioxide, possessing significant industrial application and promotion value.

[0035] The present application is further illustrated below with reference to embodiments. The scope of protection of the present application is not limited to the following embodiments.

[0036] Example 1

[0037] Mix 5 g of ethanol with 10 g of 1% phosphoric acid aqueous solution until homogeneous. Slowly add 80 g of isopropylphosphonic acid solid under room temperature and magnetic stirring conditions. Stir for 30 min to form a homogeneous and transparent organophosphonic acid treatment agent 1#. Prepare and use immediately.

[0038] 300 g of filter cake (solid content 66.6%) from the same batch after inorganic treatment with single aluminum was added to 180 mL of deionized water and stirred evenly using a high-speed stirrer at 1000 r / min to obtain titanium dioxide slurry. The titanium dioxide slurry was then transferred to a mechanical stirrer at 300 r / min and stirred further. While stirring, 0.7 g of organophosphonic acid treatment agent #1 was added to the titanium dioxide slurry, and the reaction was carried out at room temperature for 30 min. The organically treated slurry was then subjected to a 120°C test. o Dry under C conditions for 24 h; break the dried solid into powder, and then pulverize it with airflow to obtain product A.

[0039] Example 2

[0040] Mix 5 g of ethanol with 10 g of 1% phosphoric acid aqueous solution until homogeneous. Slowly add 80 g of n-butylphosphonic acid solid under room temperature and magnetic stirring conditions. Stir for 30 min to form a homogeneous and transparent organophosphonic acid treatment agent 2#. Prepare and use immediately.

[0041] 300 g of filter cake (solid content 66.6%) from the same batch after inorganic treatment with single aluminum was added to 180 mL of deionized water and stirred evenly using a high-speed stirrer at 1000 r / min to obtain titanium dioxide slurry. The titanium dioxide slurry was then transferred to a mechanical stirrer at 300 r / min and stirred further. While stirring, 0.7 g of organophosphonic acid treatment agent #2 was added to the titanium dioxide slurry, and the reaction was carried out at room temperature for 30 min. The organically treated slurry was then subjected to a 120°C test. o Dry under condition C for 24 h; break the dried solid into powder, and then pulverize it with airflow to obtain product B.

[0042] Example 3

[0043] Mix 5 g of methanol with 10 g of 2% phosphoric acid aqueous solution until homogeneous. Slowly add 80 g of n-hexylphosphonic acid solid under room temperature and magnetic stirring. Stir for 30 min to form a homogeneous and transparent organophosphonic acid treatment agent 3#. Prepare and use immediately.

[0044] 300 g of filter cake (solid content 66.6%) from the same batch after inorganic treatment with single aluminum was added to 180 mL of deionized water and stirred evenly using a high-speed stirrer at 1000 r / min to obtain titanium dioxide slurry. The titanium dioxide slurry was then transferred to a mechanical stirrer at 300 r / min and stirred further. While stirring, 0.7 g of organophosphonic acid treatment agent #3 was added to the titanium dioxide slurry, and the reaction was carried out at room temperature for 30 min. The organically treated slurry was then subjected to a 120°C test. o Dry under C conditions for 24 h; break the dried solid into powder, and then pulverize it with airflow to obtain the finished product C.

[0045] Example 4

[0046] Mix 10 g of methanol with 10 g of 3% phosphoric acid aqueous solution until homogeneous. Slowly add 80 g of n-octylphosphonic acid solid under room temperature and magnetic stirring. Stir for 30 min to form a homogeneous and transparent organophosphonic acid treatment agent #4. Prepare and use immediately.

[0047] 300 g of filter cake (solid content 66.6%) from the same batch after inorganic treatment with single aluminum was added to 180 mL of deionized water and stirred evenly using a high-speed stirrer at 1000 r / min to obtain titanium dioxide slurry. The titanium dioxide slurry was then transferred to a mechanical stirrer at 300 r / min and stirred further. While stirring, 0.7 g of organophosphonic acid treatment agent #4 was added to the titanium dioxide slurry, and the reaction was carried out at room temperature for 30 min. The organically treated slurry was then subjected to a 120°C test. o Dry under C conditions for 24 h; break the dried solid into powder, and then pulverize it with airflow to obtain the finished product D.

[0048] Comparative Example 1

[0049] 300 g of filter cake (66.6% solid content) from the same batch after inorganic treatment with single aluminum was added to 180 mL of deionized water and stirred evenly using a high-speed stirrer at 1000 r / min to obtain a titanium dioxide slurry. The titanium dioxide slurry was then transferred to a mechanical stirrer at 300 r / min and stirred further. While stirring, 0.6 g of alkyl polysiloxane was added to the titanium dioxide slurry, and the reaction was carried out at room temperature for 30 min. The organically treated slurry was then subjected to further treatment at 120 °C. o Dry under C conditions for 24 h; break the dried solid into powder, and then pulverize it with airflow to obtain the finished product E.

[0050] Comparative Example 2

[0051] Mix 10 g of methanol and 10 g of deionized water thoroughly. Slowly add 80 g of n-octylphosphonic acid solid at room temperature with magnetic stirring. Stir for 30 min to form a homogeneous and transparent solution (No. 5). Prepare and use immediately.

[0052] 300 g of filter cake (solid content 66.6%) from the same batch after inorganic treatment with single aluminum was added to 180 mL of deionized water and stirred evenly using a high-speed stirrer at 1000 r / min to obtain titanium dioxide slurry. The titanium dioxide slurry was then transferred to a mechanical stirrer at 300 r / min and stirred further. While stirring, 0.7 g of solution 5# was added to the titanium dioxide slurry, and the reaction was carried out at room temperature for 30 min. The organically treated slurry was then subjected to further treatment at 120°C. o Dry under C conditions for 24 h; break the dried solid into powder, and then pulverize it with airflow to obtain the finished product F.

[0053] However, the powder was too sticky during the air jet milling process of this sample. After running for 3 to 5 minutes, the powder would block the air jet pipeline and needed to be cleared before air jet milling could continue. Increasing the air jet pressure could not solve the problem.

[0054] Test Example 1: Temperature Resistance Test

[0055] The temperature resistance was evaluated based on the change in whiteness before and after baking: 10 g of each of the following products were weighed into containers: product A prepared in Example 1, product B prepared in Example 2, product C prepared in Example 3, product D prepared in Example 4, product E prepared in Comparative Example 1, and product F prepared in Comparative Example 2. The powders were pressed and shaped using a tablet press to obtain a smooth powder layer. Each product was placed independently in a muffle furnace at 150℃ and 300℃ for 30 min, and the pigment whiteness was tested. The test results are shown in Table 1.

[0056] Table 1 shows that the whiteness change of titanium dioxide treated with organophosphonic acid (Examples 1-4) at 300℃ was all <0.7; the whiteness change of titanium dioxide not treated with organophosphonic acid (Comparative Example 1) at 300℃ was >1; the titanium dioxide not treated with organophosphonic acid (Comparative Example 2) showed slight yellowing of the powder visible to the naked eye, indicating that the alkylphosphonic acid did not form a uniform and dense film on the powder surface. This demonstrates that titanium dioxide treated with organophosphonic acid has excellent temperature resistance.

[0057] Table 1

[0058] Experimental Example 2: Compatibility Test

[0059] Weigh 90 g of each of the following products: Product A prepared in Example 1, Product B prepared in Example 2, Product C prepared in Example 3, Product D prepared in Example 4, Product E prepared in Comparative Example 1, and Product F prepared in Comparative Example 2, into beakers. Add 40 g of polyurethane resin, 1 g of wax powder, 1 g of aqueous dispersant, and 36 g of ethanol to each beaker independently. Disperse the mixture in a high-speed stirrer at 2000 r / min for 30 min, then grind it again using a sand mill. Take 84 g of the color paste and place it in a glass beaker for subsequent operations. Transfer the remaining color paste to a sealed glass jar and place it in a fume hood at room temperature to observe for any layering, floating patterns, etc. The experimental results are shown in Table 2.

[0060] Table 2 shows that the titanium dioxide treated with organophosphonic acid (Examples 1-3) did not exhibit stratification within 10 days. Although stratification occurred in Example 4, it was still superior to Comparative Example 1. In Comparative Example 2, the lack of phosphoric acid prevented the activation of the alkylphosphonic acid, thus hindering its chemical bonding with the titanium dioxide surface. This resulted in the alkylphosphonic acid desorbing from the powder surface, causing severe powder agglomeration and poor compatibility with the resin. This demonstrates that the titanium dioxide treated with organophosphonic acid exhibits excellent compatibility.

[0061] Table 2

[0062] Experimental Example 3: Dispersion Test

[0063] 12 g of acrylic resin was added to a glass containing 84 g of pigment (Example 2), and dispersed in a high-speed stirrer at 1000 r / min for 50 min. The product was obtained after filtration through a 325-mesh filter cloth. Its dispersibility was tested using an automatic fineness meter, and the experimental results are shown in Table 3.

[0064] Table 3 shows that the titanium dioxide treated with organophosphonic acid (Examples 1-4) has a higher fineness and fewer particles. Comparative Example 1 has a lower fineness and a higher particle count. When the powder from Comparative Example 2 was used to prepare water-based inks, a large amount of foam appeared after high-speed stirring in the color paste stage, and polyurethane resin floated out (yellow oil droplets). The powder could not be uniformly dispersed in the color paste, making subsequent testing impossible. (See [reference needed]). Figure 1 , Figure 1 This is a schematic diagram of the samples used in the dispersion test for Comparative Example 2. It can be seen that these are abnormal samples, meaning they have poor dispersibility; while the normal samples can be compared. Figure 2 A schematic diagram of the sample used in the dispersion test of Example 1. This demonstrates that titanium dioxide treated with organophosphonic acid exhibits excellent dispersibility.

[0065] Table 3

[0066] The above description is merely a preferred embodiment of this application, but the scope of protection of this application is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in this application, based on the technical solution and inventive concept of this application, should be included within the scope of protection of this application.

Claims

1. An organophosphonic acid treatment agent, characterized in that, Including organophosphonic acid compounds, alcohols, phosphoric acid, and water; The mass ratio of the organophosphonic acid compound, alcohol, phosphoric acid and water is 100:(5~10):(0.01~0.25):(0.75~0.99).

2. The organophosphonic acid treatment agent according to claim 1, characterized in that, The organophosphonic acid compound is selected from C3~C4. 20 One or more of the alkylphosphonic acids; The alcohol is selected from C1-C8 monohydric alcohols and C2-C6 monohydric alcohols. 12 One or more of the diols.

3. The organophosphonic acid treatment agent according to claim 2, characterized in that, The organophosphonic acid compound is selected from one or more of n-butylphosphonic acid, isopropylphosphonic acid, n-pentylphosphonic acid, n-hexylphosphonic acid, n-octylphosphonic acid, n-decylphosphonic acid, and n-dodecylphosphonic acid; The alcohol is one or more of methanol, ethanol, isopropanol, n-butanol, and ethylene glycol.

4. A method for preparing high-temperature resistant titanium dioxide, characterized in that, Includes the following steps: (1) The titanium dioxide filter cake treated with inorganic coating is mixed with deionized water to obtain titanium dioxide slurry; (2) The titanium dioxide slurry is reacted with an organophosphonic acid treatment agent to obtain a slurry; (3) The slurry is post-treated to obtain high-temperature resistant titanium dioxide; The organophosphonic acid treatment agent is the organophosphonic acid treatment agent according to any one of claims 1 to 3.

5. The preparation method according to claim 4, characterized in that, In step (1), the mass ratio of the titanium dioxide filter cake to deionized water is 1:(1~4).

6. The preparation method according to claim 4, characterized in that, In step (1), the inorganic coating process is a single aluminum coating.

7. The preparation method according to claim 4, characterized in that, In step (2), the mass of the organophosphonic acid treatment agent is 0.3% to 1.0% of the mass of the titanium dioxide filter cake in step (1); The reaction time is 10 min to 50 min, and the reaction temperature is 40 °C. o C~60 o C.

8. The preparation method according to claim 4, characterized in that, In step (3), the post-processing includes one or more of drying, crushing, and air jet milling; The drying temperature is 100. o C~160 o C.

9. A high-temperature resistant titanium dioxide, characterized in that, It is prepared by the preparation method according to any one of claims 4 to 8.

10. A high-temperature resistant water-based ink, characterized in that, This includes the high-temperature resistant titanium dioxide prepared by the preparation method according to any one of claims 4 to 8, or the high-temperature resistant titanium dioxide according to claim 9.

Images