Preparation method of special titanium dioxide for PEEK special plastic

Abstract

The invention belongs to the technical field of titanium dioxide, and particularly relates to a preparation method of special titanium dioxide for PEEK special plastics, the special titanium dioxide for PEEK special plastics is prepared through composite coating of cerium chloride and polydimethylsiloxane, and a cerium chloride modified and coated cerium oxide film layer can capture free radicals and inhibit high-temperature oxidation of PEEK; the dispersion performance of the titanium dioxide and the compatibility of the titanium dioxide and PEEK can be improved through modified coating of the polydimethylsiloxane; after a PEEK crude product is prepared by mixing and hot pressing the prepared special titanium dioxide for the PEEK special plastic and the PEEK, dopamine amide is used for surface modification, and the dopamine amide can be connected with the surfaces of the PEEK and the titanium dioxide, so that the surface defects are reduced, and the impact resistance of the PEEK special plastic is improved; the prepared PEEK special plastic has excellent antibacterial performance and impact resistance. The special titanium dioxide for the PEEK special plastic disclosed by the invention has excellent oxidation resistance, dispersibility and compatibility with PEEK.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of titanium dioxide, and particularly relates to a preparation method of titanium dioxide special for PEEK special plastic. BACKGROUND

[0002] Polyether ether ketone (PEEK) is a kind of special polymer engineering plastic prepared by condensation polymerization of 4,4-difluorobenzophenone and hydroquinone in the presence of alkali metal carbonate with diphenyl sulfone as a solvent. PEEK is often used in high-end fields such as aerospace, automobile and medical devices due to its excellent mechanical properties, high temperature resistance and chemical stability. Titanium dioxide as an important functional filler or colorant for PEEK, mainly plays a role in enhancing performance, improving appearance or improving biocompatibility. However, the chemical structure of titanium dioxide is quite different from that of PEEK, which easily leads to poor interface bonding, and the titanium dioxide is prone to agglomeration.

[0003] A kind of titanium dioxide for plastic and ink and its preparation method are disclosed in Chinese patent CN110669358B, which comprises the following steps: pretreatment of rutile titanium dioxide by beating, grinding and grading, then inorganic coating of zinc oxide and aluminum oxide, further treatment, and finally organic coating to obtain the product. The titanium dioxide for plastic and ink prepared by the method has good weather resistance and gloss, and can well meet the subsequent use. However, the prior art has the technical problem that the surface morphology of titanium dioxide for PEEK special plastic is not further modified to further improve the antioxidant property and dispersibility of titanium dioxide. SUMMARY

[0004] The purpose of the present application is to provide a preparation method of titanium dioxide special for PEEK special plastic, which solves the technical problem of further modifying the surface morphology of titanium dioxide for PEEK special plastic in the prior art to improve the antioxidant property and dispersibility of titanium dioxide.

[0005] In order to achieve the above-mentioned purpose, the present application adopts the following technical solutions:

[0006] A preparation method of titanium dioxide special for PEEK special plastic, comprising the following steps:

[0007] S1, according to mass fraction, 1000-1500 parts of titanium dioxide is added to deionized water, a dispersing agent is added, and grinding and beating is carried out for 1-2 hours, then sieving is carried out, deionized water is added to adjust the concentration of titanium dioxide to 300-400 g / L, and titanium dioxide slurry is prepared;

[0008] S2, according to mass fraction, 100-150 parts of titanium dioxide slurry is heated to 60-65℃, 30-50 g / L cerium chloride solution is added dropwise, while ammonia water is added to adjust pH to maintain between 9-10, stirring and aging, collecting the solid by filtration, drying and grinding to obtain inorganic coated titanium dioxide;

[0009] S3, according to mass fraction, 100-150 parts of inorganic coated titanium dioxide is added into polydimethylsiloxane ethanol solution, stirring and aging, collecting the solid by filtration, crushing by airflow crusher to obtain PEEK special plastic dedicated titanium dioxide.

[0010] As preferred, the titanium dioxide in S1 is rutile titanium dioxide.

[0011] As preferred, the dispersant in S1 is any one of sodium hexametaphosphate, sodium pyrophosphate, polycarboxylate, and the amount of dispersant added is 0.15-0.25% of the mass of titanium dioxide.

[0012] As preferred, the amount of cerium chloride added in S2 is 3-5% of the mass of titanium dioxide, and the cerium chloride solution is added dropwise within 1-2h, stirring and aging at 500-700 rpm for 1-2h.

[0013] As preferred, the amount of polydimethylsiloxane added in S3 is 3-5% of the mass of titanium dioxide, and the polydimethylsiloxane ethanol solution is added dropwise within 1-2h, heating to 50-60℃, stirring and aging at 500-700 rpm for 1-2h.

[0014] The PEEK special plastic dedicated titanium dioxide is used to prepare PEEK special plastic, and the preparation method comprises the following steps:

[0015] S11, according to mass fraction, 100 parts of PEEK granules and 3-8 parts of PEEK special plastic dedicated titanium dioxide are mixed uniformly, and then hot-pressed to obtain PEEK crude product;

[0016] S12, according to mass fraction, 80-100 parts of PEEK crude product is polished, washed with anhydrous ethanol, added into 100-200 parts of 1-1.2 g / L aqueous solution of tris-hydroxymethyl aminomethane, and 0.2-0.3 parts of dopamine amide surface modification is added, then the PEEK crude product is taken out, washed with deionized water, and dried to obtain PEEK special plastic.

[0017] As preferred, in S11, hot-pressing is performed at 370-400℃ under a pressure of 5-10 MPa for 0.5-1h.

[0018] As preferred, in S12, the pH of the system is adjusted to 7.5-8.5 by hydrochloric acid and sodium hydroxide solution, then 0.2-0.3 parts of dopamine amide is added, and the surface modification is performed at 40-50℃ for 20-24h.

[0019] As preferred, the preparation method of the dopamine amide comprises the following steps:

[0020] S21, according to mass fraction, 18-20 parts of sodium borate and 8-10 parts of sodium bicarbonate are added into 100-150 parts of deionized water, 10-12 parts of dopamine hydrochloride is added in a nitrogen atmosphere, 12-15 parts of allyl succinic anhydride is dissolved in tetrahydrofuran and then added into the system, sodium hydroxide solution is added dropwise to adjust the pH to 8.5-9, and the temperature is raised to 40-60 DEG C for 6-12 h;

[0021] S22, after the reaction, 100-150 parts of ethyl acetate is added for extraction, the lower water phase is separated, the pH is adjusted to 1.5-2 with concentrated hydrochloric acid, 100-150 parts of ethyl acetate is added for extraction, the upper organic phase is separated after water removal, and the dopamine amide is prepared by rotary evaporation.

[0022] As preferred, the synthesis principle is as follows:

[0023]

[0024] The mass spectrometry analysis results are as follows: m / z: 279.11 (100.0%), 280.11 (15.7%), 281.12 (1.1%), 281.11 (1.1%).

[0025] As preferred, the water removal step of the organic phase in S22 is stirring for 0.5-1 h after adding 5-10 parts of anhydrous magnesium sulfate, and then filtering to remove the solid.

[0026] As described above, by adopting the technical scheme, the application has the following beneficial effects:

[0027] 1. The PEEK special plastic special titanium white powder is prepared by cerium chloride and polydimethylsiloxane composite coating, the cerium oxide film layer modified by cerium chloride has oxygen vacancy defects, can capture free radicals, and inhibit PEEK high temperature oxidation; the polydimethylsiloxane modification coating can improve the dispersion performance of the titanium white powder and improve the compatibility of the titanium white powder with PEEK; the PEEK special plastic special titanium white powder prepared by the application has excellent oxidation resistance, dispersion and compatibility with PEEK.

[0028] 2. The PEEK special plastic special titanium white powder and PEEK are mixed and hot-pressed to prepare a PEEK crude product, and then the dopamine amide surface modification is carried out, the dopamine amide can connect the PEEK and the titanium white powder surface, reduce the surface defects, and improve the impact resistance of the PEEK special plastic; the prepared PEEK special plastic has excellent antibacterial performance and impact resistance.

[0029] 3. This invention prepares dopamine amide by reacting dopamine hydrochloride and allyl succinic anhydride. The introduction of amide bonds improves the thermal stability of dopamine amide, and the carboxyl group of succinylated dopamine enhances the surface polarity of PEEK and improves its antifouling performance. The prepared dopamine amide is applied to the surface modification of PEEK special plastics to improve the antifouling performance of PEEK special plastics. Detailed Implementation

[0030] 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 skilled in the art without creative effort are within the scope of protection of the present invention.

[0031] Example 1: A method for preparing titanium dioxide for PEEK special plastics, comprising the following steps:

[0032] S1. By mass, add 1000 parts of CY-T30 titanium dioxide to deionized water, add 2 parts of sodium hexametaphosphate and sodium pyrophosphate in a mass ratio of 1:1 to prepare a dispersant, grind and slurry for 1 hour, pass through a 350-mesh sieve, add deionized water to adjust the concentration of titanium dioxide to 300 g / L, and prepare titanium dioxide slurry.

[0033] S2. According to the mass fraction, heat 100 parts of titanium dioxide slurry with a concentration of 300 g / L to 60°C, add 30 parts of cerium chloride solution with a concentration of 30 g / L, and simultaneously add ammonia water to adjust the pH to maintain 9. The cerium chloride solution is added over 1 hour. Stir and age at 700 rpm for 2 hours, filter and collect the solid, dry and grind at 80°C to obtain inorganic coated titanium dioxide.

[0034] S3. Dissolve 3 parts of polydimethylsiloxane in 100 parts of ethanol by mass, then add 100 parts of inorganic coated titanium dioxide, add ammonia water to adjust the pH to 9, heat to 60℃ and stir at 700 rpm for 2 hours, filter to collect the solid, and pulverize it through an air jet mill to obtain PEEK special plastic titanium dioxide.

[0035] The titanium dioxide specifically for PEEK specialty plastics obtained in this embodiment is used to prepare PEEK specialty plastics. The preparation method includes the following steps:

[0036] S11. By weight, 100 parts of PEEK granules and 5 parts of PEEK special plastic titanium dioxide are mixed evenly and then hot-pressed at 380℃ and 8MPa for 0.5h to obtain PEEK crude product.

[0037] S12, by mass fraction, 100 parts of PEEK crude product is polished, washed with anhydrous ethanol, added into 200 parts of 1.2g / L aqueous solution of tris-hydroxymethyl aminomethane, the pH of the system is adjusted to 8.5 with hydrochloric acid and sodium hydroxide solution, then 0.3 parts of dopamine amide is added, the temperature is raised to 50℃, and the surface is modified for 20h, then the PEEK crude product is taken out, washed with deionized water, dried, and PEEK special plastic is prepared.

[0038] The preparation method of dopamine amide in this embodiment comprises the following steps:

[0039] S21, by mass fraction, 18.5 parts of sodium borate and 8 parts of sodium bicarbonate are added into 100 parts of deionized water, 10 parts of dopamine hydrochloride is added under nitrogen atmosphere, 12 parts of allyl succinic anhydride is dissolved in 30 parts of tetrahydrofuran and then added into the system, sodium hydroxide solution is added dropwise to adjust the pH to 8.5, and the temperature is raised to 40℃ for 12h;

[0040] S22, after the reaction is completed, 100 parts of ethyl acetate is added for extraction, the lower aqueous phase is separated, the pH is adjusted to 1.5 with concentrated hydrochloric acid, 100 parts of ethyl acetate is added for extraction, the upper organic phase is separated after water removal, and dopamine amide is prepared by rotary evaporation.

[0041] Example 2, the preparation method of a kind of PEEK special plastic special titanium dioxide powder in this embodiment comprises the following steps:

[0042] S1, by mass fraction, 1000 parts of CY-T25N titanium dioxide powder is added into deionized water, 2.5 parts of polycarboxylate dispersant is added, grinded and beaten for 2h, passed through 300 mesh sieve, deionized water is added to adjust the concentration of titanium dioxide to 320g / L, and titanium dioxide slurry is prepared;

[0043] S2, by mass fraction, 150 parts of titanium dioxide slurry with a concentration of 320g / L is raised to 65℃, 48 parts of 40g / L cerium chloride solution is added dropwise, ammonia water is added dropwise to adjust the pH to maintain between 9.5, the cerium chloride solution is dropped in 1.5h, stirred at a speed of 500rpm for 1h, the solid is collected by filtration, dried and ground to prepare inorganic coated titanium dioxide powder;

[0044] S3, by mass fraction, 3.5 parts of polydimethylsiloxane is dissolved in 100 parts of ethanol, then 110 parts of inorganic coated titanium dioxide powder is added, ammonia water is added dropwise to adjust the pH to maintain between 9.5, the temperature is raised to 60℃, and the stirring is carried out at a speed of 500rpm for 2h, the solid is collected by filtration, crushed by airflow crusher, and PEEK special plastic special titanium dioxide powder is prepared.

[0045] The PEEK special plastic special titanium dioxide powder prepared in this embodiment is used to prepare PEEK special plastic, and the preparation method comprises the following steps:

[0046] S11, 100 parts of PEEK granules and 3 parts of PEEK special plastic special titanium white powder are mixed uniformly, and then hot-pressed at 370 DEG C under a pressure of 5 MPa for 1 h to obtain a PEEK crude product;

[0047] S12, 80 parts of PEEK crude product are polished, washed with anhydrous ethanol, added into 120 parts of 1.1 g / L aqueous solution of tris-hydroxymethyl aminomethane, and then adjusted to pH 7.8 by using hydrochloric acid and sodium hydroxide solution, and then added with 0.2 parts of dopamine amide, and then heated to 40 DEG C for surface modification for 24 h, and then the PEEK crude product is taken out, washed with deionized water, and then dried to obtain a PEEK special plastic.

[0048] The dopamine amide of the present embodiment is prepared by the same method as that of Example 1.

[0049] Example 3, a method for preparing a PEEK special plastic special titanium white powder of the present embodiment, comprises the following steps:

[0050] S1, 1200 parts of NR-03 titanium white powder are added into deionized water, 2.5 parts of sodium hexametaphosphate dispersant are added, and then ground and beaten for 1 h, and then filtered through a 350 mesh sieve, and then deionized water is added to adjust the concentration of titanium dioxide to 340 g / L to obtain a titanium dioxide slurry;

[0051] S2, 150 parts of the titanium dioxide slurry with a concentration of 340 g / L are heated to 65 DEG C, 50 parts of 50 g / L cerium chloride solution are added dropwise, and ammonia water is added dropwise to adjust the pH to 10, the cerium chloride solution is added dropwise within 2 h, and then stirred and aged at 600 rpm for 2 h, and then the solid is collected by filtration, and then dried and ground to obtain an inorganic coated titanium white powder;

[0052] S3, 5 parts of polydimethylsiloxane are dissolved in 100 parts of ethanol, and then 150 parts of the inorganic coated titanium white powder are added, and then ammonia water is added dropwise to adjust the pH to 10, and then heated to 50 DEG C, and then stirred and aged at 600 rpm for 2 h, and then the solid is collected by filtration, and then crushed by an air flow crusher to obtain a PEEK special plastic special titanium white powder.

[0053] The PEEK special plastic special titanium white powder prepared in the present embodiment is used to prepare a PEEK special plastic, and the preparation method comprises the following steps:

[0054] S11, 100 parts of PEEK granules and 8 parts of PEEK special plastic special titanium white powder are mixed uniformly, and then hot-pressed at 390 DEG C under a pressure of 10 MPa for 0.5 h to obtain a PEEK crude product;

[0055] S12, by mass parts, 90 parts of PEEK crude product is polished, washed with anhydrous ethanol, added to 200 parts of 1.2g / L aqueous solution of tris-hydroxymethyl aminomethane, the system pH is adjusted to 8.5 with hydrochloric acid and sodium hydroxide solution, then 0.3 parts of dopamine amide is added, heated to 50℃ for surface modification for 24h, the PEEK crude product is taken out, washed with deionized water, dried to obtain PEEK special plastic.

[0056] The dopamine amide of the present embodiment is prepared by the same method as that of Example 1.

[0057] Example 4, a method for preparing a titanium dioxide powder for PEEK special plastic of the present embodiment, comprises the following steps:

[0058] S1, by mass parts, 1500 parts of CY-T30 titanium dioxide powder is added to deionized water, 3 parts of sodium hexametaphosphate dispersant is added, grinded and pulped for 1h, passed through a 400 mesh sieve, deionized water is added to adjust the concentration of titanium dioxide to 400g / L, to obtain titanium dioxide slurry;

[0059] S2, by mass parts, 150 parts of titanium dioxide slurry with a concentration of 400g / L is heated to 65℃, 40 parts of 45g / L cerium chloride solution is added dropwise, and ammonia water is added to adjust the pH to 10, the cerium chloride solution is added dropwise within 1h, stirred at a speed of 700rpm for 2h, the solid is collected by filtration, dried and grinded to obtain inorganic coated titanium dioxide powder;

[0060] S3, by mass parts, 4 parts of polydimethylsiloxane is dissolved in 100 parts of ethanol, then 120 parts of inorganic coated titanium dioxide powder is added, ammonia water is added to adjust the pH to 10, heated to 50℃, stirred at a speed of 700rpm for 1h, the solid is collected by filtration, grinded by airflow crusher to obtain titanium dioxide powder for PEEK special plastic.

[0061] The titanium dioxide powder for PEEK special plastic prepared in the present embodiment is used to prepare PEEK special plastic, and the preparation method comprises the following steps:

[0062] S11, by mass parts, 100 parts of PEEK granules and 8 parts of titanium dioxide powder for PEEK special plastic are mixed uniformly, then hot-pressed at 400℃ under a pressure of 8MPa for 0.5h to obtain PEEK crude product;

[0063] S12, by mass parts, 100 parts of PEEK crude product is polished, washed with anhydrous ethanol, added to 150 parts of 1.2g / L aqueous solution of tris-hydroxymethyl aminomethane, the system pH is adjusted to 8.5 with hydrochloric acid and sodium hydroxide solution, then 0.2 parts of dopamine amide is added, heated to 50℃ for surface modification for 24h, the PEEK crude product is taken out, washed with deionized water, dried to obtain PEEK special plastic.

[0064] The dopamine amide of the present embodiment is different from that of Example 1 in that the pH is adjusted to 9 by dropwise addition of a sodium hydroxide solution in step S21, and the reaction is carried out at 60°C for 6h.

[0065] Example 5, a preparation method of a PEEK special plastic dedicated titanium white powder of the present embodiment, comprises the following steps:

[0066] S1, according to mass fraction, 1500 parts of CY-T30 titanium white powder is added to deionized water, 3.5 parts of a dispersant prepared by adding sodium hexametaphosphate and sodium pyrophosphate in a mass ratio of 1:1 is added, and grinding and beating is carried out for 2h, then it is passed through a 300 mesh sieve, deionized water is added to adjust the concentration of titanium dioxide to 350g / L, and titanium dioxide slurry is prepared;

[0067] S2, according to mass fraction, 150 parts of titanium dioxide slurry with a concentration of 350g / L is heated to 60°C, 50 parts of a cerium chloride solution with a concentration of 35g / L is added dropwise, and ammonia water is added dropwise to adjust the pH to maintain 9.5, the cerium chloride solution is added dropwise within 1h, stirring is carried out at a speed of 500rpm, and aging is carried out for 1h, then the solid is collected by filtration, dried and ground to prepare inorganic coated titanium white powder;

[0068] S3, according to mass fraction, 5 parts of polydimethylsiloxane is dissolved in 100 parts of ethanol, then 150 parts of inorganic coated titanium white powder is added, ammonia water is added to adjust the pH to maintain 9.5, the temperature is raised to 50°C, stirring is carried out at a speed of 500rpm, and aging is carried out for 1h, then the solid is collected by filtration, crushed by an airflow crusher, and a PEEK special plastic dedicated titanium white powder is prepared.

[0069] The PEEK special plastic dedicated titanium white powder prepared in the present embodiment is used to prepare PEEK special plastic, and the preparation method comprises the following steps:

[0070] S11, according to mass fraction, 100 parts of PEEK granules and 7 parts of PEEK special plastic dedicated titanium white powder are uniformly mixed, then hot pressing is carried out at 370°C under a pressure of 6MPa for 1h to prepare PEEK crude product;

[0071] S12, according to mass fraction, 80 parts of PEEK crude product is polished, washed with anhydrous ethanol, added to 200 parts of a 1g / L aqueous solution of tris-hydroxymethyl aminomethane, the pH of the system is adjusted to 7.5 by using hydrochloric acid and sodium hydroxide solution, then 0.3 parts of dopamine amide is added, the temperature is raised to 40°C, surface modification is carried out for 24h, then the PEEK crude product is taken out, washed with deionized water, and dried to prepare PEEK special plastic.

[0072] The dopamine amide of the present embodiment is prepared by the same method as that of Example 4.

[0073] Example 6, a preparation method of a PEEK special plastic dedicated titanium white powder of the present embodiment, comprises the following steps:

[0074] S1, by mass, 1000 parts of NR-03 titanium dioxide is added to deionized water, 2 parts of a dispersant prepared from sodium hexametaphosphate and sodium pyrophosphate in a mass ratio of 1:1 is added, and grinding and beating is performed for 2 h, then a 300-mesh sieve is passed through, deionized water is added to adjust the concentration of titanium dioxide to 360 g / L, and a titanium dioxide slurry is prepared;

[0075] S2, by mass, 100 parts of the titanium dioxide slurry with a concentration of 360 g / L is heated to 60°C, 50 parts of a 30 g / L cerium chloride solution is added dropwise, ammonia water is added to adjust the pH to maintain 9.5, the cerium chloride solution is added dropwise within 2 h, stirring is performed at a speed of 700 rpm, and aging is performed for 2 h, then the solid is collected by filtration, dried and ground to prepare inorganic coated titanium dioxide;

[0076] S3, by mass, 5 parts of polydimethylsiloxane is dissolved in 100 parts of ethanol, then 100 parts of the inorganic coated titanium dioxide is added, ammonia water is added to adjust the pH to maintain 9-10, heating is performed to 50°C, stirring is performed at a speed of 700 rpm, and aging is performed for 2 h, then the solid is collected by filtration, crushed by an airflow crusher, and PEEK special plastic dedicated titanium dioxide is prepared.

[0077] The PEEK special plastic dedicated titanium dioxide prepared in the embodiment is used to prepare PEEK special plastic, and the preparation method comprises the following steps:

[0078] S11, by mass, 100 parts of PEEK granules and 6 parts of PEEK special plastic dedicated titanium dioxide are uniformly mixed, then hot pressing is performed at 370-400°C under a pressure of 5-10 MPa for 0.5-1 h to prepare PEEK crude products;

[0079] S12, by mass, 80-100 parts of the PEEK crude products are polished, washed with anhydrous ethanol, added to 100-200 parts of a 1-1.2 g / L aqueous solution of tris-hydroxymethyl aminomethane, the pH of the system is adjusted to 7.5-8.5 using hydrochloric acid and sodium hydroxide solution, then 0.2-0.3 parts of dopamine amide is added, heating is performed to 40-50°C, surface modification is performed for 20-24 h, then the PEEK crude products are taken out, washed with deionized water, and dried to prepare PEEK special plastic.

[0080] The dopamine amide in the embodiment is prepared by the same method as in Example 4.

[0081] Comparative Example 1, the difference between the comparative example and Example 1 is that the titanium dioxide is not coated with polydimethylsiloxane.

[0082] Comparative Example 2, the difference between the comparative example and Example 1 is that the PEEK special plastic is not surface modified with dopamine amide.

[0083] Comparative Example 3, the difference between this comparative example and Example 1 is that the titanium white powder is not coated with cerium chloride.

[0084] Performance test

[0085] The PEEK special plastic special titanium white powder prepared in each example and comparative example is subjected to technical index test, and the whiteness, titanium dioxide content and average particle size thereof are measured. The test results are shown in Table 1 below:

[0086] Table 1 Technical index test

[0087]

[0088] The tensile strength and elongation at break of the PEEK special plastic prepared in each example and comparative example are tested according to GB / T 1040.1-2018 “Determination of tensile properties of plastics Part 1: General principles”.

[0089] The impact strength of the PEEK special plastic prepared in each example and comparative example is tested according to GB / T 1843-2008 “Determination of Izod impact strength of plastics”.

[0090] The test results are shown in Table 2 below:

[0091] Table 2 Mechanical property test

[0092]

[0093] From the above table data, it can be seen that the whiteness of the PEEK special plastic special titanium white powder prepared in Examples 1-6 is between 98.30 and 98.32, the titanium dioxide content is between 91.54 and 91.61%, and the average particle size is between 350 and 359 nm. The titanium white powder of Comparative Example 1 is not coated with polydimethylsiloxane, which leads to an increase in the degree of agglomeration of the titanium white powder, resulting in a whiteness of 98.28 and an average particle size of 377 nm. It shows that the PEEK special plastic special titanium white powder prepared by the present application has excellent dispersibility and high purity; the tensile strength of the PEEK special plastic prepared in Examples 1-6 is between 105.71 and 107.04 MPa, the elongation at break is between 54.67 and 55.59%, and the impact strength is between 100.93 and 101.87 kJ / m 2 It shows that the PEEK special plastic special titanium white powder prepared by the present application applied to the PEEK special plastic makes the PEEK special plastic have excellent mechanical properties and impact resistance.

[0094] The above merely describes preferred embodiments of the present application, but the protection scope of the present application is not limited thereto, and any person skilled in the art, within the technical scope disclosed by the present application, can make equivalent replacements or changes according to the technical scheme and inventive concept of the present application, which should be covered within the protection scope of the present application.

[0095] The preferred embodiments of the application disclosed above are only used to help explain the application. The preferred embodiments do not describe all the details and do not limit the application to the specific embodiments. Obviously, many modifications and changes can be made according to the content of the present application. The present application selects and describes these embodiments in order to better explain the principles and practical applications of the present application, so that those skilled in the art can well understand and utilize the present application. The present application is limited only by the claims and their full scope and equivalents.

Claims

1. A method for preparing titanium dioxide special for PEEK specialty plastics, characterized in that, It comprises the following steps: S1, according to mass fraction, 1000-1500 parts of titanium dioxide is added to deionized water, adding dispersant, grinding and beating for 1-2h, sieving, adding deionized water to adjust the concentration of titanium dioxide to 300-400g / L, and preparing titanium dioxide slurry; S2, according to mass fraction, 100-150 parts of titanium dioxide slurry is heated to 60-65℃, 30-50g / L of cerium chloride solution is added dropwise, and ammonia water is added to adjust the pH to maintain between 9-10, stirring and aging, collecting the solid by filtration, drying and grinding to prepare inorganic coated titanium dioxide; S3, according to mass fraction, 100-150 parts of inorganic coated titanium dioxide is added to polydimethylsiloxane ethanol solution, stirring and aging, collecting the solid by filtration, and crushing by airflow crusher to prepare PEEK special plastic special titanium dioxide.

2. The method for preparing titanium dioxide special for PEEK special plastics according to claim 1, characterized in that, The titanium dioxide in S1 is rutile titanium dioxide, the dispersant is any one of sodium hexametaphosphate, sodium pyrophosphate and polycarboxylate, and the amount of dispersant added is 0.15-0.25% of the mass of titanium dioxide.

3. The method for preparing titanium dioxide special for PEEK plastics according to claim 1, characterized in that, The amount of cerium chloride added in S2 is 3-5% of the mass of titanium dioxide, and the cerium chloride solution is dropped within 1-2h, and the stirring and aging is carried out at a speed of 500-700rpm for 1-2h.

4. The method for preparing titanium dioxide special for PEEK plastics according to claim 1, characterized in that, The amount of polydimethylsiloxane added in S3 is 3-5% of the mass of titanium dioxide, and the polydimethylsiloxane ethanol solution is dropped within 1-2h, and the stirring and aging is carried out at a speed of 500-700rpm for 1-2h at a temperature of 50-60℃.

5. The method for preparing titanium dioxide special for PEEK plastics according to claim 1, characterized in that, The PEEK special plastic special titanium dioxide is used to prepare PEEK special plastic, and the preparation method comprises the following steps: S11, according to mass fraction, 100 parts of PEEK granules and 3-8 parts of PEEK special plastic special titanium dioxide are mixed uniformly, and hot pressing is carried out to prepare PEEK crude product; S12, according to mass fraction, 80-100 parts of PEEK crude product is polished, washed with anhydrous ethanol, added to 100-200 parts of 1-1.2g / L aqueous solution of tris-hydroxymethyl aminomethane, and 0.2-0.3 parts of dopamine amide is added for surface modification, the PEEK crude product is taken out, washed with deionized water, and dried to prepare PEEK special plastic.

6. The method for preparing titanium dioxide special for PEEK plastics according to claim 5, characterized in that, In S11, hot pressing is carried out at a temperature of 370-400℃ and a pressure of 5-10MPa for 0.5-1h; in S12, the pH of the system is adjusted to 7.5-8.5 with hydrochloric acid and sodium hydroxide solution, 0.2-0.3 parts of dopamine amide is added, and the surface modification is carried out at a temperature of 40-50℃ for 20-24h.

7. The method according to claim 5, wherein the method is characterized by, The preparation method of dopamine amide comprises the following steps: S21, according to mass fraction, 18-20 parts of sodium borate and 8-10 parts of sodium bicarbonate are added to 100-150 parts of deionized water, 10-12 parts of dopamine hydrochloride is added in a nitrogen atmosphere, 12-15 parts of allyl succinic anhydride is dissolved in tetrahydrofuran and added to the system, sodium hydroxide solution is added dropwise to adjust the pH to 8.5-9, and the reaction is carried out at a temperature of 40-60℃ for 6-12h. S22, after the reaction is finished, 100-150 parts of ethyl acetate is added for extraction, the lower water phase is separated, the pH is adjusted to 1.5-2 with concentrated hydrochloric acid, then 100-150 parts of ethyl acetate is added for extraction, the upper organic phase is separated, water is removed, and then rotary evaporation is performed to obtain dopamine amide.

8. The method according to claim 7, wherein the method is characterized by, The water removal step of the organic phase in S22 is stirring for 0.5-1 h after 5-10 parts of anhydrous magnesium sulfate is added, and then the solid is removed by filtration.

Images