CN113072742B - Preparation method of high-dispersity nano titanium dioxide/melamine resin for plastic products - Google Patents
Preparation method of high-dispersity nano titanium dioxide/melamine resin for plastic products Download PDFInfo
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08L61/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/2241—Titanium dioxide
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Abstract
The invention discloses a preparation method of high-dispersity nano titanium dioxide/melamine resin for plastic products, which takes glycerol-polyethylene glycol-isopropanol/hydrochloric acid solution as hydrolysis dispersion liquid of titanium tetrachloride; in the synthesis process of the titanium dioxide, the in-situ compounding of the titanium dioxide and the melamine methylol compound is realized through the polymerization reaction of melamine and formaldehyde; and the subsequent inorganic-organic coating treatment is carried out on the product to further improve the dispersibility of the material, and finally the titanium dioxide/melamine resin with high dispersibility is prepared, and has good performance in the application of plastics.
Description
Technical Field
The invention relates to the technical field of preparation of titanium dioxide and plastic additives, in particular to a preparation method of high-dispersity nano titanium dioxide/melamine resin for plastic products.
Background
Titanium dioxide is a substance with wide application prospects, and has the characteristics of optimal opacity, whiteness, stable chemical properties and ultraviolet shielding. In recent decades, titanium dioxide has been rapidly developed and widely used in various fields. Among them, the development of titanium dioxide in the plastic field is more prominent, and titanium dioxide is generally applied to plastic products such as building plastic steel windows, plastic automobile parts, plastic communication equipment, household electrical appliances and articles for daily use, which has become the second largest application field of titanium dioxide. In recent years, titanium dioxide modified resin is widely applied, and the advantages of inorganic matters, polymers and nano materials are perfectly combined with the advantages of nano inorganic particles and polymer composite materials. However, it has been found that in the master batch with high color density, the requirement of titanium dioxide dispersibility will be high due to the high content of titanium dioxide. CN106118140B discloses a preparation method of high-whiteness and high-temperature-resistance color master batch titanium dioxide, which adopts different composite salt calcination processes to regulate particle size and inorganic coating and organic coating treatment to finally prepare titanium dioxide for different color plastic products.
Disclosure of Invention
The invention mainly aims to solve the problems and provides a preparation method of high-dispersity nano titanium dioxide/melamine resin for plastic products, which specifically comprises the following steps:
(1) under magnetic stirring, uniformly mixing glycerol and melamine, adding polyethylene glycol, heating for 10-30min in a water-proof way, then adding isopropanol, uniformly stirring, then adding 0.1-2mol/L hydrochloric acid to adjust the pH value to 4-6, then stirring at a high rotating speed, dropwise adding titanium tetrachloride, and rapidly stirring for 5-20min until the test solution does not flow any more, so as to form a gelatinous titanium dioxide precursor;
(2) carrying out centrifugal separation on the titanium dioxide precursor prepared in the step (1), mixing and grinding the separated solid product with a proper amount of sodium stearate, adding formaldehyde, carrying out ultrasonic dispersion for 0.5-1h at 70-85 ℃, adding triethanolamine to adjust the pH value to 8-9 in the process, maintaining stable polymerization reaction, carrying out high-speed centrifugation on the product, separating the solid product, washing and filtering the solid product, and repeating the steps for 2-5 times to obtain a titanium dioxide/melamine hydroxymethyl compound;
(3) dispersing the product obtained in the step (2) in absolute ethyl alcohol to form slurry, adding aluminum silicate and sodium silicate to coat, carrying out ultrasonic treatment for 0.5-1h, transferring the product to a three-neck flask, carrying out oil bath heating under magnetic stirring, washing, filtering, drying, adding alkyl sodium sulfonate, and carrying out jet milling to obtain the high-dispersity nano titanium dioxide/melamine resin for plastic products.
Preferably, the volume ratio of the glycerol, the polyethylene glycol, the isopropanol and the titanium tetrachloride in the step (1) is (5-10): (1-5): (10-30): (1-5).
Preferably, the mass-to-volume ratio of the melamine, the formaldehyde and the titanium tetrachloride in the step (1) or the step (2) is (3.2-12.6) g, (5-20) mL and (3-5) mL.
Preferably, the sodium stearate in the step (2) accounts for 0.05-1% of the mass fraction of the titanium dioxide precursor.
Preferably, the high-speed centrifugation in step (2) is centrifugation at 9000-12000rpm/min for 6-10min each time.
Preferably, the oil bath heating in step (3) is heating reflux at 110-150 ℃ for 3-6 h.
Preferably, the molar ratio of the aluminum silicate to the sodium silicate in the step (3) is 1 (0.25-1), and the aluminum silicate and the sodium silicate account for 4-14% of the mass fraction of the titanium dioxide/melamine methylol compound in total.
Preferably, the sodium alkylsulfonate in the step (3) accounts for 0.1-1% of the mass fraction of the titanium dioxide/melamine methylol compound.
The invention also provides a method for preparing plastic based on the high-dispersity nano titanium dioxide/melamine resin, which specifically comprises the following steps: placing the prepared high-dispersity titanium dioxide/melamine resin, polypropylene powder, polyethylene wax, waterborne polyurethane and deionized water in a wet ball mill for fully mixing and grinding, and transferring the mixed slurry into a high-speed stirrer for further dispersing the friction force of the medium and refining the material; after washing and drying, the materials are discharged into a double-screw granulator to extrude plastic products.
Preferably, the mass ratio of the titanium dioxide/melamine resin to the polypropylene powder to the polyethylene wax to the waterborne polyurethane to the deionized water is (10-20): 3-8): 0.5-5): 2-6): 65-80.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) the method takes glycerol-polyethylene glycol-isopropanol/hydrochloric acid solution as hydrolysis dispersion liquid of titanium tetrachloride, and utilizes sodium stearate and polyethylene glycol to disperse and solubilize a system test solution so as to promote nucleation and growth of a titanium dioxide precursor.
(2) In the synthesis process of titanium dioxide, the in-situ compounding of the titanium dioxide and the melamine methylol compound is realized through the polymerization reaction of melamine and formaldehyde, and more hydrogen bonds are formed in the reaction liquid, so that the viscosity of the reaction liquid is enhanced; the modified titanium dioxide/melamine resin is modified by aluminum silicate, sodium silicate and sodium alkyl sulfonate subsequently, so that the dispersibility of the titanium dioxide/melamine resin is further improved, and the tensile property and the wear resistance of the plastic product are improved; and the addition of the aluminum silicate and the sodium silicate is also beneficial to increasing the whiteness of the material, and the production cost is saved.
Drawings
FIG. 1 is a graph showing the dispersion behavior of materials prepared in examples 1 to 3 of the present invention and comparative examples 1 to 3 in deionized water.
Detailed Description
Example 1
The high-dispersity nano titanium dioxide/melamine resin for plastic products prepared in embodiment 1 of the invention specifically comprises the following steps:
(1) under magnetic stirring, 5mL of glycerol and 6.3g of melamine are uniformly mixed, 5mL of polyethylene glycol is added, water is prevented for heating for 20min, then 20mL of isopropanol is added, stirring is uniformly carried out, 1mol/L of hydrochloric acid is added to adjust the pH value to 4, then 5mL of titanium tetrachloride is dropwise added at the rotating speed of 700rpm/min, stirring is carried out rapidly for 10min, until the test solution does not flow any more, and a gelatinous titanium dioxide precursor is formed;
(2) carrying out centrifugal separation on the titanium dioxide precursor prepared in the step (1), mixing and grinding the separated solid product and sodium stearate accounting for 0.6% of the mass fraction of the solid product, adding 10mL of formaldehyde, carrying out ultrasonic dispersion at 85 ℃ for 1h, adding triethanolamine to adjust the pH value to 9 in the process, maintaining stable polymerization reaction, centrifuging the product at 10000rpm/min for 10min, separating the solid product, washing and filtering the solid product, and repeating the steps for 3 times to obtain a titanium dioxide/melamine hydroxymethyl compound;
(3) dispersing the product obtained in the step (2) in absolute ethyl alcohol to form slurry, adding aluminum silicate accounting for 7% of the mass fraction of the slurry and sodium silicate accounting for 3% of the mass fraction of the slurry for coating, carrying out ultrasonic treatment for 0.5h, transferring the coated slurry to a three-neck flask, carrying out oil bath heating at 120 ℃ for 5h under the magnetic stirring, then carrying out washing, filtering and drying, finally adding sodium alkyl sulfonate accounting for 0.5% of the mass fraction of the coated slurry, and carrying out air flow crushing to obtain the high-dispersity nano titanium dioxide/melamine resin for plastic products.
A method for preparing plastic based on high-dispersity nano titanium dioxide comprises the following steps: placing 10kg of the prepared high-dispersity titanium dioxide/polypropylene resin, 4kg of polypropylene powder, 3kg of polyethylene wax, 3kg of waterborne polyurethane and 80kg of deionized water in a wet ball mill for fully mixing and grinding, and transferring the mixed slurry into a high-speed stirrer for further dispersing the friction force of a medium and refining materials; after washing and drying, the materials are discharged into a double-screw granulator to extrude plastic products.
Example 2
The high-dispersity nano titanium dioxide/melamine resin for plastic products prepared in embodiment 2 of the invention specifically comprises the following steps:
(1) under magnetic stirring, uniformly mixing 10mL of glycerol and 12.6.g of melamine, adding 5mL of polyethylene glycol, heating for 20min in a water-proof manner, then adding 20mL of isopropanol, uniformly stirring, adding 1mol/L of hydrochloric acid to adjust the pH value to 4, then dropwise adding 5mL of titanium tetrachloride at the rotating speed of 700rpm/min, rapidly stirring for 10min until the test solution does not flow any more, and forming a gelatinous titanium dioxide precursor;
(2) carrying out centrifugal separation on the titanium dioxide precursor prepared in the step (1), mixing and grinding the separated solid product and sodium stearate accounting for 0.3% of the mass fraction of the solid product, adding 20mL of formaldehyde, carrying out ultrasonic dispersion at 85 ℃ for 1h, adding triethanolamine to adjust the pH value to 9 in the process, maintaining stable polymerization reaction, centrifuging the product at 10000rpm/min for 10min, separating the solid product, washing and filtering the solid product, and repeating the steps for 3 times to obtain a titanium dioxide/melamine hydroxymethyl compound;
(3) dispersing the product obtained in the step (2) in absolute ethyl alcohol to form slurry, adding aluminum silicate accounting for 5% of the mass fraction of the slurry and sodium silicate accounting for 3% of the mass fraction of the slurry for coating, carrying out ultrasonic treatment for 0.5h, transferring the coated slurry to a three-neck flask, carrying out oil bath heating at 120 ℃ for 5h under the magnetic stirring, then carrying out washing, filtering and drying, finally adding sodium alkyl sulfonate accounting for 0.5% of the mass fraction of the coated slurry, and carrying out air flow crushing to obtain the high-dispersity nano titanium dioxide/melamine resin for plastic products.
A method for preparing plastic based on high-dispersity nano titanium dioxide comprises the following steps: placing 10kg of the prepared high-dispersity titanium dioxide/polypropylene resin, 4kg of polypropylene powder, 3kg of polyethylene wax, 3kg of waterborne polyurethane and 80kg of deionized water in a wet ball mill for fully mixing and grinding, and transferring the mixed slurry into a high-speed stirrer for further dispersing the friction force of a medium and refining materials; after washing and drying, the materials are discharged into a double-screw granulator to extrude plastic products.
Example 3
The high-dispersity nano titanium dioxide/melamine resin for plastic products prepared in embodiment 3 of the invention specifically comprises the following steps:
(1) under magnetic stirring, uniformly mixing 10mL of glycerol and 12.6.g of melamine, adding 5mL of polyethylene glycol, heating for 20min in a water-proof manner, then adding 20mL of isopropanol, uniformly stirring, adding 1mol/L of hydrochloric acid to adjust the pH value to 4, then dropwise adding 2mL of titanium tetrachloride at the rotating speed of 700rpm/min, rapidly stirring for 10min until the test solution does not flow any more, and forming a gelatinous titanium dioxide precursor;
(2) carrying out centrifugal separation on the titanium dioxide precursor prepared in the step (1), mixing and grinding the separated solid product and sodium stearate accounting for 0.2% of the mass fraction of the solid product, then adding 10mL of formaldehyde, carrying out ultrasonic dispersion at 85 ℃ for 1h, adding triethanolamine in the process to adjust the pH value to 9, maintaining stable polymerization reaction, then centrifuging the product at the rotating speed of 10000rpm/min for 10min, separating the solid product, washing and filtering, and repeating for 3 times to obtain a titanium dioxide/melamine hydroxymethyl compound;
(3) dispersing the product obtained in the step (2) in absolute ethyl alcohol to form slurry, adding aluminum silicate accounting for 3% of the mass fraction of the slurry and sodium silicate accounting for 2% of the mass fraction of the slurry for coating, carrying out ultrasonic treatment for 0.5h, transferring the coated slurry to a three-neck flask, carrying out oil bath heating at 120 ℃ for 5h under the magnetic stirring, then carrying out washing, filtering and drying, finally adding sodium alkyl sulfonate accounting for 0.5% of the mass fraction of the coated slurry, and carrying out air flow crushing to obtain the high-dispersity nano titanium dioxide/melamine resin for plastic products.
A method for preparing plastic based on high-dispersity nano titanium dioxide comprises the following steps: placing 10kg of the prepared high-dispersity titanium dioxide/polypropylene resin, 4kg of polypropylene powder, 3kg of polyethylene wax, 3kg of waterborne polyurethane and 80kg of deionized water in a wet ball mill for fully mixing and grinding, and transferring the mixed slurry into a high-speed stirrer for further dispersing the friction force of a medium and refining materials; after washing and drying, the materials are discharged into a double-screw granulator to extrude plastic products.
Comparative example 1
In comparative example 1 of the invention, the rest experimental conditions and test procedures of example 1 in the preparation method of the color master batch-grade titanium dioxide with high whiteness and high temperature resistance disclosed in CN106118140B are the same as those of example 1.
Comparative example 2
Comparative example 2 of the present invention differs from example 1 in that sodium stearate, aluminum polyethylene glycol silicate, sodium silicate and sodium alkyl sulfonate are not added and the remaining experimental conditions and test procedures are consistent with example 1.
Comparative example 3
Comparative example 3 of the present invention is different from example 1 in that titanium dioxide is not compounded, and the rest of experimental conditions and test procedures are the same as those of example 1.
(1) And (3) testing the dispersibility: the experiment adopts an ultraviolet absorption spectrophotometry to measure the absorbance change of the colloidal dispersion liquid of the titanium dioxide/melamine hydroxymethyl compound so as to research the dispersion effect of the titanium dioxide/melamine resin, the lower the absorbance value is, the better the dispersibility is shown as the lower the colloidal concentration of the dispersion system liquid is, and the specific test scheme is as follows: respectively weighing 10mg of the titanium dioxide/melamine methylol compounds prepared in the examples 1-3 and the comparative examples 1-3 by using a balance, respectively adding the 6 parts of materials into 100mL of deionized water under magnetic stirring, and uniformly stirring for 1h to uniformly disperse the materials; and then standing the mixture aside, and sampling to detect the absorbance value, (the detection instrument is an ultraviolet spectrophotometer, the sampling standard is that 1mL of test solution is taken every 2h, and the experiment is ended after the total sampling is carried out for 24 h), wherein the change curve of the absorbance value of the nano titanium dioxide dispersion system along with time is shown in figure 1.
It can be observed from fig. 1 that the titanium dioxide/melamine resins prepared in examples 1 to 3 of the present invention have the smallest absorbance values in the water dispersibility test for 24 hours as a whole, compared to the materials prepared in comparative examples 1 to 3. Its initial absorbance value was 0.71, and its absorbance changed with the lapse of the test time and finally became stable at 14 hours, and the absorbance value was 0.40, which indicates that the titanium dioxide/melamine resin prepared in example 1 had the best dispersibility and also laterally indicates the effects of sodium stearate, polyethylene glycol, aluminum silicate and sodium silicate on the titanium dioxide-modified melamine resin.
(2) And (3) performance testing: in the experiment, the plastic prepared in the embodiment 1 and the comparative examples 2-3 of the invention is tested by referring to the tensile property test of GB/T1040-2018 plastic and the rolling abrasion test of GB/T5478-2008 plastic, in the two test processes, the clamp is connected with the testing machine, and the testing speed of the testing machine is kept constant and does not change along with the change of the clamp. Wherein in the detection of the tensile property of the plastic, the unified test speed of the sample is 5 mm/min; in the wear performance test, the samples are unified into a 100mm circular mold, the thickness of the circular mold is 10mm, the mass of the circular mold is 20.8g, the test speed is 60r/min, the total test speed is 1000r, and the specific data are shown in the following table.
It can be observed from the data in the table that a plastic prepared based on a highly dispersible titanium dioxide/melamine resin as prepared in example 1 has the best tensile strength and the least wear loss, which is attributable to the good dispersibility of the material and, in turn, contributes to the improvement of the tensile and wear resistance properties of the material after preparation as a plastic.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. Such modifications and variations are considered to be within the scope of the invention.
Claims (3)
1. A preparation method of high-dispersity nano titanium dioxide/melamine resin for plastic products is characterized by comprising the following steps:
(1) under magnetic stirring, uniformly mixing glycerol and melamine, adding polyethylene glycol, heating for 10-30min in a water-proof way, then adding isopropanol, uniformly stirring, then adding 0.1-2mol/L hydrochloric acid to adjust the pH value to 4-6, then stirring at a high rotating speed, dropwise adding titanium tetrachloride, and rapidly stirring for 5-20min until the test solution does not flow any more, so as to form a gelatinous titanium dioxide precursor;
(2) carrying out centrifugal separation on the titanium dioxide precursor prepared in the step (1), mixing and grinding the separated solid product with a proper amount of sodium stearate, adding formaldehyde, carrying out ultrasonic dispersion for 0.5-1h at 70-85 ℃, adding triethanolamine to adjust the pH value to 8-9 in the process, maintaining stable polymerization reaction, carrying out high-speed centrifugation on the product, separating the solid product, washing and filtering the solid product, and repeating the steps for 2-5 times to obtain a titanium dioxide/melamine hydroxymethyl compound;
(3) dispersing the product obtained in the step (2) in absolute ethyl alcohol to form slurry, adding aluminum silicate and sodium silicate for coating, performing ultrasonic treatment for 0.5-1h, transferring the product to a three-neck flask, performing oil bath heating under magnetic stirring, washing, filtering, drying, adding sodium alkyl sulfonate, and performing jet milling to obtain the high-dispersity nano titanium dioxide/melamine resin for the plastic products;
wherein the volume ratio of the glycerol, the polyethylene glycol, the isopropanol and the titanium tetrachloride in the step (1) is (5-10): 1-5): 10-30): 1-5; the mass-to-volume ratio of the melamine, the formaldehyde and the titanium tetrachloride in the step (1) or the step (2) is (3.2-12.6) g, (5-20) mL, (3-5) mL; the sodium stearate in the step (2) accounts for 0.05-1% of the mass fraction of the titanium dioxide precursor; the high-speed centrifugation in the step (2) is centrifugation at the rotation speed of 12000rpm/min of 9000-; the oil bath heating in the step (3) is heating reflux for 3-6h at the temperature of 110-150 ℃; the molar ratio of the aluminum silicate to the sodium silicate in the step (3) is 1 (0.25-1), and the aluminum silicate to the sodium silicate account for 4-14% of the mass fraction of the titanium dioxide/melamine hydroxymethyl compound; the mass fraction of the sodium alkyl sulfonate in the step (3) is 0.1-1% of that of the titanium dioxide/melamine methylol compound.
2. A method for preparing plastics based on high-dispersity nano titanium dioxide/melamine resin is characterized by comprising the following steps: placing the high-dispersity titanium dioxide/melamine resin, polypropylene powder, polyethylene wax, waterborne polyurethane and deionized water prepared according to the method in a wet ball mill, fully mixing and grinding, and transferring the mixed slurry into a high-speed stirrer to further disperse the friction force of a medium and refine materials; after washing and drying, the materials are discharged into a double-screw granulator to extrude plastic products.
3. The method for preparing the plastic based on the high-dispersity nano titanium dioxide/melamine resin as claimed in claim 2, wherein the mass ratio of the titanium dioxide/melamine resin to the polypropylene powder to the polyethylene wax to the waterborne polyurethane to the deionized water is (10-20) to (3-8) to (0.5-5) to (2-6) to (65-80).
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