CN113801374B - Rare earth stabilizer processing method based on green production - Google Patents
Rare earth stabilizer processing method based on green production Download PDFInfo
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- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
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Abstract
The invention discloses a rare earth stabilizer processing method based on green production, and relates to the technical field of stabilizers. According to the invention, electromagnetic heating is firstly utilized to assist lanthanum nitrate to react with arginine to generate lanthanum arginine, so that the reaction rate is improved, the use of additives is reduced, and then ultrasonic graded pressurization is utilized to dry, so that the drying efficiency is improved, and the surface agglomeration at the initial stage is effectively avoided; then under the triple actions of ultrasonic wave, electrostatic field and microwave, tri-n-butoxy phenyl triazine reacts with the arginine lanthanum to form arginine lanthanum particles with needle-shaped microsphere structures, so that the rare earth stabilizer has light stabilization effect; and finally, crosslinking the arginine lanthanum particles and the calcium carbonate whiskers under an alternating electric field, so that the thermal stability of the rare earth stabilizer is improved. The method for processing the rare earth stabilizer based on green production has the effects of high-efficiency thermal stability and light stability.
Description
Technical Field
The invention relates to the technical field of stabilizers, in particular to a rare earth stabilizer processing method based on green production.
Background
The polyvinyl chloride has excellent corrosion resistance and flame retardance, and products of the polyvinyl chloride are widely applied to various fields of industrial and agricultural production due to low price, rich raw materials and mature manufacturing process. However, polyvinyl chloride has a disadvantage of poor thermal stability, and in order to improve the thermal stability, a thermal stabilizer must be added during the processing. At present, lead salt stabilizers are mainly used in the market, and although the lead salt stabilizers are low in price and have good stabilizing effect, the released lead salt stabilizers can cause serious pollution to the environment after polyvinyl chloride products are abandoned, and the requirements of modern green environmental protection and sustainable development are not met, so that the rare earth stabilizers begin to appear to people.
The industrial production of rare earth stabilizers mostly adopts a double decomposition method and a direct method, the double decomposition method is mainly characterized in that stearic acid and caustic soda react to generate a sodium stearate soap solution, and then rare earth compounds are added to react to generate the sodium stearate soap solution, so that the prepared rare earth stabilizer has good color and luster and high purity, but the yield is low, and a large amount of additives are used, so that organic wastewater is easily generated; the direct method is mainly characterized in that stearic acid and rare earth compounds are subjected to direct melting reaction, although additives are not used, the direct melting reaction is usually carried out in a high-temperature environment, so that the rare earth stabilizer is easy to oxidize at high temperature, and the color and the purity of the product are influenced; in addition, most of the rare earth stabilizers in the market have single function and only have thermal stability effect. Therefore, the invention provides a green processing method, which can prepare the rare earth stabilizer with better color and purity without using additives under the high-temperature environment, and simultaneously meets the requirement that one stabilizer achieves multiple functional effects.
Disclosure of Invention
The invention aims to provide a rare earth stabilizer processing method based on green production, which aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: a processing method of a rare earth stabilizer based on green production is characterized by mainly comprising the following processing methods: the method comprises the steps of preparing arginine lanthanum by using electromagnetic heating to assist lanthanum nitrate to react with arginine, drying by using ultrasonic vacuum grading pressurization to obtain arginine lanthanum solid, reacting tri-n-butoxy phenyl triazine with the arginine lanthanum solid under triple actions of ultrasonic waves, electrostatic fields and microwaves to obtain arginine lanthanum particles, and finally reacting the arginine lanthanum particles with calcium carbonate whiskers under an alternating electric field to obtain the rare earth stabilizer.
Further, the processing method of the rare earth stabilizer comprises the following specific steps:
(1) Dispersing lanthanum nitrate and arginine with the mass 2-3 times of that of lanthanum nitrate into deionized water with the mass 25-30 times of that of lanthanum nitrate, stirring at 200rpm for 20-30 min, placing in an electromagnetic induction heater, heating to 60-70 ℃, and reacting for 40-50 min to obtain lanthanum arginine;
(2) Carrying out ultrasonic treatment on the arginine lanthanum for 10-15 min, and carrying out graded pressure drying to obtain an arginine lanthanum solid;
(3) Dispersing solid arginine lanthanum and tri-n-butoxy phenyl triazine with the mass of 0.7-0.9 time of that of the solid arginine lanthanum into absolute ethyl alcohol with the mass of 10-15 times of that of the solid arginine lanthanum, adding nitric acid with the mass fraction of 10% until the pH value of the solution is 3-4, stirring at the speed of 200-300 rpm for 30-40 min at room temperature, placing the solution in a microwave oven, reacting at 90 ℃ for 8-10 min, performing ultrasonic treatment for 15-20 min, placing the solution in an electrostatic field, standing for 20-30 min, filtering, washing with distilled water for 10-15 times, and drying in a constant-temperature drying oven at 60 ℃ for 4-6 h to obtain arginine lanthanum particles;
(4) Dispersing the arginine lanthanum particles in an ethanol water solution with the mass of 10-15 times of that of the arginine lanthanum particles, wherein the mass ratio of ethanol to water in the ethanol water solution is 1.
Further, the high-frequency current frequency in the electromagnetic induction heater in the step (1) is 25-30 kHz, and the power is 60kW.
Furthermore, the ultrasonic frequency in the step (2) is 100-120W and 40-50 kHz.
Further, the step (2) of drying by stage pressurization comprises the steps of adjusting the pressure to 60kPa, maintaining the pressure for 40-50 s, adjusting the pressure to 20kPa, maintaining the pressure for 60-80 s, adjusting the pressure to 4kPa, maintaining the pressure for 90-100 s, and releasing the pressure.
Further, the pressure relief rate in the pressure relief process is 10-15 kPa/min.
Further, the ultrasonic frequency in the step (3) is 300-400W and 40-50 kHz; the electrostatic field frequency is 70-80 kV/m; the microwave frequency is 800-900W.
Further, the external electric field in the step (4) is a sine alternating electric field, the frequency is 40-50 Hz, and the voltage is 100-150V.
Further, the frequency of the centrifugal drying in the step (4) is 1500-2000 rpm.
Compared with the prior art, the invention has the following beneficial effects:
the rare earth stabilizer is prepared by heating reaction, drying, micron structure synthesis, crosslinking reaction and other steps in sequence, so that the rare earth stabilizer has high-efficiency thermal stability and light stability.
Firstly, nitrate ions of lanthanum nitrate react with amino of arginine to generate thermal stabilizer arginine lanthanum under the assistance of electromagnetic heating, and water is used as a catalyst by utilizing the electric field effect of electromagnetic energy to participate in the formation of transition state of arginine lanthanum, so that the use of an additive is reduced, the dependence on reaction temperature is reduced, the whole reaction process is carried out in a medium-low temperature environment, the occurrence of side reactions such as high-temperature oxidation and the like is reduced, and the color and the purity of a product are improved; secondly, ultrasonic grading pressurization is used for drying the arginine lanthanum, so that the drying efficiency is improved, and the surface agglomeration at the initial stage is effectively avoided; then through triple actions of ultrasonic waves, electrostatic fields and microwaves, in the microwave curing process, the arginine lanthanum crystal nucleus expands and grows into a micron sphere, and the cavitation effect of the ultrasonic waves is utilized to accelerate the growth of the micron sphere; the ultrasonic oscillation is utilized to promote the collision of the ultraviolet absorbent tri-n-butoxy phenyl triazine and the arginine lanthanum, and a precipitate is formed on the surface of the arginine lanthanum, so that the rare earth stabilizer has a light stabilizing effect; under the guidance of an electrostatic field, the surface precipitate of the lanthanum arginine grows along the direction of the electrostatic field to form needle crystals, and the tri-n-butoxy phenyl triazine collides with the lanthanum arginine to generate a large amount of energy and heat to accelerate the crystal growth to form a needle micron spherical structure, so that the contact area with a matrix is increased, and the stabilizing effect of the rare earth stabilizer on the matrix is improved.
Secondly, after calcium carbonate grows out whiskers by utilizing the centrifugal force of a high-speed rotating bed, through an alternating electric field, when the calcium carbonate is in contact with the surfaces of the arginine lanthanum particles, stronger electric traction force in the alternating electric field promotes the calcium carbonate whiskers and the acicular structure of the arginine lanthanum particles to be wound and crosslinked, and the relaxation action of the positive electrode and the negative electrode of the electric field is fully utilized, so that the relative motion and collision among the calcium carbonate and the arginine lanthanum particle atoms are increased, the formation of atomic groups is facilitated, the reaction of the calcium carbonate and the arginine lanthanum particles is promoted, the crosslinking compactness is improved, and the thermal stability effect of the rare earth stabilizer is enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are used to illustrate the method of testing each index of the green-production-based rare earth stabilizer prepared in the following examples as follows:
preparation of polyvinyl chloride samples: and (3) uniformly mixing 50 parts of polyvinyl chloride resin powder, 50 parts of polyvinyl chloride resin paste and 3 parts of rare earth stabilizer, flatly paving to form a film, and plasticizing in a constant-temperature drying oven at 120 ℃ for 20-30 min to obtain a film product for testing various performances of polyvinyl chloride.
Light stability: polyvinyl chloride samples are prepared from the rare earth stabilizers in the embodiment and the comparative example with the same quality, and are subjected to a light stabilization effect test, and the tensile strength of the samples is measured according to the national standard GBT 16422.3.
Thermal stability: polyvinyl chloride samples are prepared from the rare earth stabilizers in the embodiment and the comparative example with the same quality, and are subjected to a thermal stability effect test, and the time required for complete blackening of the samples is measured according to GB/T9349.
Reaction time: the time taken for the preparation of lanthanum arginine solid in the preparation of rare earth stabilizers of examples and comparative examples was manually measured.
Example 1
The method for processing the rare earth stabilizer based on green production mainly comprises the following processing steps:
(1) Dispersing lanthanum nitrate and arginine with the mass 2 times of that of lanthanum nitrate in deionized water with the mass 25 times of that of lanthanum nitrate, stirring at 200rpm for 30min, placing in an electromagnetic induction heater, heating to 60 ℃, and reacting for 40min to obtain lanthanum arginine;
(2) Treating arginine lanthanum by ultrasonic wave for 10min, and performing graded pressure drying to obtain arginine lanthanum solid;
(3) Dispersing solid arginine lanthanum and tri-n-butoxy phenyl triazine with the mass of 0.7 time that of the solid arginine lanthanum into absolute ethyl alcohol with the mass of 10 times that of the solid arginine lanthanum, adding nitric acid with the mass fraction of 10% until the pH value of the solution is 3, stirring at the room temperature at the speed of 200rpm for 40min, placing the solution in a microwave oven, reacting at the temperature of 90 ℃ for 8min, performing ultrasonic treatment for 15min, placing the solution in an electrostatic field, standing for 20min, filtering, washing with distilled water for 10 times, and drying in a constant-temperature drying oven at the temperature of 60 ℃ for 4h to obtain arginine lanthanum particles;
(4) Dispersing the argininyl lanthanum particles in an ethanol aqueous solution with the mass ratio of ethanol to water being 1.2.5, adding calcium carbonate whiskers with the mass being 0.01 time of that of the argininyl lanthanum particles, connecting an external electric field, heating to 80 ℃ while stirring at the speed of 100rpm, keeping the temperature for 2 hours, filtering, washing for 13 times by using distilled water and absolute ethanol in sequence, and centrifuging and spin-drying for 2 hours to obtain the rare earth stabilizer based on green production.
Further, the high-frequency current frequency in the electromagnetic induction heater in the step (1) is 25kHz, and the power is 60kW.
Further, the ultrasonic frequency in the step (2) is 100W and 40kHz.
Further, the step (2) of the step of drying under pressure comprises the steps of adjusting the pressure to 60kPa, maintaining the pressure for 40s, adjusting the pressure to 20kPa, maintaining the pressure for 60s, adjusting the pressure to 4kPa, maintaining the pressure for 90s, and releasing the pressure.
Further, the pressure relief rate in the pressure relief process is 10kPa/min.
Further, the ultrasonic frequency in the step (3) is 300W and 40kHz; the electrostatic field frequency is 70kV/m; the microwave frequency is 800W.
Further, the external electric field in the step (4) is a sine alternating electric field, the frequency is 40Hz, and the voltage is 100V.
Further, the frequency of the centrifugal drying in the step (4) is 1500rpm.
Example 2
The method for processing the rare earth stabilizer based on green production mainly comprises the following processing steps:
(1) Dispersing lanthanum nitrate and arginine with the mass 3 times that of lanthanum nitrate into deionized water with the mass 30 times that of lanthanum nitrate, stirring at 300rpm for 20min, placing in an electromagnetic induction heater, heating to 70 ℃, and reacting for 50min to obtain lanthanum arginine;
(2) Treating arginine lanthanum by ultrasonic for 15min, and performing graded pressure drying to obtain arginine lanthanum solid;
(3) Dispersing solid arginine lanthanum and tri-n-butoxy phenyl triazine with the mass of 0.9 time that of the solid arginine lanthanum into absolute ethyl alcohol with the mass of 15 times that of the solid arginine lanthanum, adding nitric acid with the mass fraction of 10% until the pH value of the solution is 4, stirring at the speed of 300rpm for 30min at room temperature, placing the solution in a microwave oven, reacting at 90 ℃ for 10min, performing ultrasonic treatment for 20min, placing the solution in an electrostatic field, standing for 30min, filtering, washing with distilled water for 15 times, and drying in a constant-temperature drying oven at 60 ℃ for 6h to obtain arginine lanthanum particles;
(4) Dispersing argininyl lanthanum particles in an ethanol aqueous solution 15 times the mass of the argininyl lanthanum particles, wherein the mass ratio of ethanol to water in the ethanol aqueous solution is 1.
Further, the high-frequency current frequency in the electromagnetic induction heater in the step (1) is 30kHz, and the power is 60kW.
Further, the ultrasonic frequency in the step (2) is 120W and 50kHz.
Further, the step (2) of the step of drying under pressure comprises the steps of adjusting the pressure to 60kPa, maintaining the pressure for 50s, adjusting the pressure to 20kPa, maintaining the pressure for 80s, adjusting the pressure to 4kPa, maintaining the pressure for 100s, and releasing the pressure.
Further, the pressure relief rate in the pressure relief process is 15kPa/min.
Further, the ultrasonic frequency in the step (3) is 400W and 50kHz; the electrostatic field frequency is 80kV/m; the microwave frequency is 900W.
Further, the external electric field in the step (4) is a sine alternating electric field, the frequency is 50Hz, and the voltage is 150V.
Further, the frequency of the centrifugal drying in the step (4) is 2000rpm.
Comparative example 1
The green production-based rare earth stabilizer processing method mainly comprises the following processing steps:
(1) Dispersing lanthanum nitrate and arginine with the mass 2.3 times of that of lanthanum nitrate into deionized water with the mass 26.1 times of that of lanthanum nitrate, stirring at 200rpm for 24min, placing in an electromagnetic induction heater, heating to 66 ℃, and reacting for 43min to obtain lanthanum arginine;
(2) Treating arginine lanthanum by ultrasonic wave for 13min, and performing graded pressure drying to obtain arginine lanthanum solid;
(3) Dispersing arginine lanthanum solid and tri-n-butoxy phenyl triazine with the mass of 0.77 time of that of the arginine lanthanum solid into absolute ethyl alcohol with the mass of 13.5 times of that of the arginine lanthanum solid, adding nitric acid with the mass fraction of 10% until the pH value of the solution is 3.5, stirring at the room temperature at the speed of 220rpm for 36min, performing ultrasonic treatment for 18min, placing in an electrostatic field, standing for 26min, filtering, washing with distilled water for 13 times, and drying in a constant-temperature drying oven at the temperature of 60 ℃ for 4.5h to obtain arginine lanthanum particles;
(4) Dispersing the arginine lanthanum particles in an ethanol water solution with the mass 14.2 times that of the arginine lanthanum particles, wherein the mass ratio of ethanol to water in the ethanol water solution is 1.
Further, the high-frequency current frequency in the electromagnetic induction heater in the step (1) is 27kHz, and the power is 60kW.
Further, the ultrasonic frequency in the step (2) is 115W and 43kHz.
Further, the step (2) of the step of drying under pressure comprises the steps of adjusting the pressure to 60kPa, maintaining the pressure for 43s, adjusting the pressure to 20kPa, maintaining the pressure for 71s, adjusting the pressure to 4kPa, maintaining the pressure for 94s, and releasing the pressure.
Further, the pressure relief rate in the pressure relief process is 13kPa/min.
Further, the electrostatic field frequency in the step (3) is 72kV/m; the microwave frequency was 856W.
Further, the external electric field in the step (4) is a sine alternating electric field, the frequency is 47Hz, and the voltage is 130V.
Further, the frequency of the centrifugal drying in the step (4) is 1700rpm.
Comparative example 2
The method for processing the rare earth stabilizer based on green production mainly comprises the following processing steps:
(1) Dispersing lanthanum nitrate and arginine with the mass 2.3 times of that of lanthanum nitrate into deionized water with the mass 26.1 times of that of lanthanum nitrate, stirring at 200rpm for 24min, placing in an electromagnetic induction heater, heating to 66 ℃, and reacting for 43min to obtain lanthanum arginine;
(2) Treating arginine lanthanum by ultrasonic wave for 13min, and performing graded pressure drying to obtain arginine lanthanum solid;
(3) Dispersing solid arginine lanthanum and tri-n-butoxy phenyl triazine with the mass of 0.77 time that of the solid arginine lanthanum into absolute ethyl alcohol with the mass of 13.5 times that of the solid arginine lanthanum, adding nitric acid with the mass fraction of 10% until the pH of the solution is 3.5, stirring at the speed of 220rpm for 36min at room temperature, placing the solution in a microwave oven, reacting at the temperature of 90 ℃ for 9min, placing the solution in an electrostatic field, standing for 26min, filtering, washing with distilled water for 13 times, and drying in a constant-temperature drying oven at the temperature of 60 ℃ for 4.5h to obtain arginine lanthanum particles;
(4) Dispersing the lanthanum arginine particles in an ethanol aqueous solution with the mass ratio of ethanol to water being 1.
Further, the high-frequency current frequency in the electromagnetic induction heater in the step (1) is 27kHz, and the power is 60kW.
Further, the ultrasonic frequency in the step (2) is 115W and 43kHz.
Further, the step (2) of the step of drying under pressure comprises the steps of adjusting the pressure to 60kPa, maintaining the pressure for 43s, adjusting the pressure to 20kPa, maintaining the pressure for 71s, adjusting the pressure to 4kPa, maintaining the pressure for 94s, and releasing the pressure.
Further, the pressure relief rate in the pressure relief process is 13kPa/min.
Further, the electrostatic field frequency in the step (3) is 72kV/m; the microwave frequency was 856W.
Further, the external electric field in the step (4) is a sine alternating electric field, the frequency is 47Hz, and the voltage is 130V.
Further, the frequency of the centrifugal drying in the step (4) is 1700rpm.
Comparative example 3
The method for processing the rare earth stabilizer based on green production mainly comprises the following processing steps:
(1) Dispersing lanthanum nitrate and arginine with the mass 2.3 times of that of lanthanum nitrate into deionized water with the mass 26.1 times of that of lanthanum nitrate, stirring at 200rpm for 24min, placing in an electromagnetic induction heater, heating to 66 ℃, and reacting for 43min to obtain lanthanum arginine;
(2) Treating arginine lanthanum by ultrasonic wave for 13min, and performing graded pressure drying to obtain arginine lanthanum solid;
(3) Dispersing solid arginine lanthanum and tri-n-butoxy phenyl triazine with the mass of 0.77 time that of the solid arginine lanthanum into absolute ethyl alcohol with the mass of 13.5 times that of the solid arginine lanthanum, adding nitric acid with the mass fraction of 10% until the pH of the solution is 3.5, stirring at the speed of 220rpm for 36min at room temperature, placing the solution in a microwave oven, reacting at the temperature of 90 ℃ for 9min, performing ultrasonic treatment for 18min, filtering, washing with distilled water for 13 times, and drying in a constant-temperature drying oven at the temperature of 60 ℃ for 4.5h to obtain arginine lanthanum particles;
(4) Dispersing the lanthanum arginine particles in an ethanol aqueous solution with the mass ratio of ethanol to water being 1.
Further, the high-frequency current frequency in the electromagnetic induction heater in the step (1) is 27kHz, and the power is 60kW.
Further, the ultrasonic frequency in the step (2) is 115W and 43kHz.
Further, the step (2) of the staged pressure drying process comprises the steps of adjusting the pressure to 60kPa, maintaining the pressure for 43s, adjusting the pressure to 20kPa, maintaining the pressure for 71s, adjusting the pressure to 4kPa, maintaining the pressure for 94s, and releasing the pressure.
Further, the pressure relief rate in the pressure relief process is 13kPa/min.
Further, the ultrasonic frequency in the step (3) is 330W and 48kHz; the microwave frequency was 856W.
Further, the external electric field in the step (4) is a sine alternating electric field, the frequency is 47Hz, and the voltage is 130V.
Further, the frequency of the centrifugal drying in the step (4) is 1700rpm.
Comparative example 4
The method for processing the rare earth stabilizer based on green production mainly comprises the following processing steps:
(1) Dispersing lanthanum nitrate and arginine with the mass 2.3 times of that of lanthanum nitrate into deionized water with the mass 26.1 times of that of lanthanum nitrate, stirring at 200rpm for 24min, placing in an electromagnetic induction heater, heating to 66 ℃, and reacting for 43min to obtain lanthanum arginine;
(2) Treating arginine lanthanum by ultrasonic wave for 13min, and performing graded pressure drying to obtain arginine lanthanum solid;
(3) Dispersing solid arginine lanthanum and tri-n-butoxy phenyl triazine with the mass of 0.77 time that of the solid arginine lanthanum into absolute ethyl alcohol with the mass of 13.5 times that of the solid arginine lanthanum, adding nitric acid with the mass fraction of 10% until the pH of the solution is 3.5, stirring at the speed of 220rpm for 36min at room temperature, placing the solution in a microwave oven, reacting at the temperature of 90 ℃ for 9min, performing ultrasonic treatment for 18min, placing the solution in an electrostatic field, standing for 26min, filtering, washing with distilled water for 13 times, and drying in a constant-temperature drying oven at the temperature of 60 ℃ for 4.5h to obtain arginine lanthanum particles;
(4) Dispersing the arginine lanthanum particles in an ethanol water solution with the mass 14.2 times that of the arginine lanthanum particles, wherein the mass ratio of ethanol to water in the ethanol water solution is 1.
Further, the high-frequency current frequency in the electromagnetic induction heater in the step (1) is 27kHz, and the power is 60kW.
Further, the ultrasonic frequency in the step (2) is 115W and 43kHz.
Further, the step (2) of the step of drying under pressure comprises the steps of adjusting the pressure to 60kPa, maintaining the pressure for 43s, adjusting the pressure to 20kPa, maintaining the pressure for 71s, adjusting the pressure to 4kPa, maintaining the pressure for 94s, and releasing the pressure.
Further, the pressure relief rate in the pressure relief process is 13kPa/min.
Further, the ultrasonic frequency in the step (3) is 330W and 48kHz; the electrostatic field frequency is 72kV/m; the microwave frequency was 856W.
Comparative example 5
The green production-based rare earth stabilizer processing method mainly comprises the following processing steps:
(1) Dispersing lanthanum nitrate and arginine with the mass 2.3 times of that of lanthanum nitrate into deionized water with the mass 26.1 times of that of lanthanum nitrate, stirring at 200rpm for 24min, heating to 290 ℃, reacting for 190min, and drying at room temperature for 12h to obtain lanthanum arginine;
(2) Dispersing arginine lanthanum and tri-n-butoxy phenyl triazine with the mass of 0.77 time that of the arginine lanthanum into absolute ethyl alcohol with the mass of 13.5 times that of the arginine lanthanum, adding nitric acid with the mass fraction of 10% until the pH of the solution is 3.5, stirring at the room temperature at the speed of 220rpm for 15h, filtering, washing with distilled water for 13 times, and drying in a constant-temperature drying oven at 60 ℃ for 4.5h to obtain arginine lanthanum particles;
(3) Dispersing the lanthanum arginate particles in an ethanol water solution with the mass ratio of ethanol to water being 1.
Effects of the invention
The following table 1 shows the results of performance analysis of the green-produced rare earth stabilizers using examples 1 to 2 of the present invention and comparative examples 1 to 5.
TABLE 1
From the comparison of the experimental data of examples 1 and 2 and comparative example 5, it can be found that in the reaction process of lanthanum nitrate and arginine, the reaction rate is improved and the reaction time is shortened by using electromagnetic heating assistance and adopting ultrasonic vacuum fractional pressure drying; through triple actions of ultrasonic waves, electrostatic fields and microwaves, tri-n-butoxy phenyl triazine reacts with arginine lanthanum to generate an acicular microsphere structure, so that the light stabilization effect is achieved, and the stabilization effect of the rare earth stabilizer is enlarged; under the action of an alternating electric field, the surface needle-shaped structure of the lanthanum arginine particles is wound and reacts with the calcium carbonate whiskers to form a composite rare earth stabilizer, so that the thermal stability effect of the rare earth stabilizer is enhanced; from the comparison of experimental data of examples 1 and 2 and comparative example 1, it can be found that, in the reaction process of tri-n-butoxy phenyl triazine and lanthanum arginine, microwave curing is not used, the lanthanum arginine crystal nucleus can not expand into a micron sphere, the volume is too small, tri-n-butoxy phenyl triazine precipitate can not be loaded, and thus a needle-shaped structure can not be formed, the cross-linking with calcium carbonate whisker is influenced, and the heat stability and light stability of the rare earth stabilizer are reduced; from the comparison of the experimental data of examples 1 and 2 and comparative example 2, it can be found that the micron sphere grows slowly without using ultrasonic wave in the reaction process of tri-n-butoxy phenyl triazine and arginine lanthanum, and when the reaction is not completely cured, the supported precipitate stops the growth of the microsphere, the content of the precipitate is less, the light stabilization effect of the rare earth stabilizer is affected, meanwhile, the oscillation effect of the ultrasonic wave is not generated, the tri-n-butoxy phenyl triazine and arginine lanthanum cannot collide to form the precipitate, so that a needle-shaped structure cannot be generated, calcium carbonate whisker cannot be crosslinked, and the heat stabilization effect of the rare earth stabilizer is affected; from the comparison of the experimental data of examples 1 and 2 and comparative example 3, it can be found that, in the reaction process of tri-n-butoxy phenyl triazine and lanthanum arginine, no electrostatic field is used, the precipitate can not form needle crystals along the electrostatic field and only adheres to the surface of lanthanum arginine, so that the content of the ultraviolet absorbent is low, the light stabilization effect of the rare earth stabilizer is reduced, and the precipitate can not be crosslinked with calcium carbonate whiskers in the subsequent reaction, so that the thermal stability of the rare earth stabilizer is affected; from the comparison of the experimental data of the examples 1 and 2 and the comparative example 4, it can be found that the alternating electric field is not used when the lanthanum arginine particles and the calcium carbonate whiskers react, the electric traction force of the alternating electric field cannot be used for crosslinking the needle-shaped structures on the surfaces of the calcium carbonate whiskers and the lanthanum arginine particles, and only the weak hydrogen bonding action between the lanthanum arginine particles and the calcium carbonate whiskers leads to weak crosslinking action force between the lanthanum arginine particles and the calcium carbonate whiskers, so that the chain breakage is easy to occur in the actual use process, and the stabilizing effect of the rare earth stabilizer is influenced.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. A processing method of a rare earth stabilizer based on green production is characterized by mainly comprising the following processing methods:
(1) Dispersing lanthanum nitrate and arginine with the mass 2-3 times of that of lanthanum nitrate in deionized water with the mass 25-30 times of that of lanthanum nitrate, stirring at 200-300rpm for 20-30min, placing in an electromagnetic induction heater, heating to 60-70 ℃, and reacting for 40-50min to obtain lanthanum arginine;
(2) Treating arginine lanthanum by ultrasonic for 10 to 15min, and performing graded pressure drying to obtain an arginine lanthanum solid;
(3) Dispersing solid arginine lanthanum and tri-n-butoxy phenyl triazine with the mass of 0.7-0.9 times of that of the solid arginine lanthanum in absolute ethyl alcohol with the mass of 10-15 times of that of the solid arginine lanthanum, adding nitric acid with the mass fraction of 10% until the pH of the solution is 3-4, stirring at the room temperature at the speed of 200-300rpm for 30-40min, placing the solution in a microwave oven, reacting at 90 ℃ for 8-10min, performing ultrasonic treatment for 15-20min, placing the solution in an electrostatic field, standing for 20-30min, filtering, washing with distilled water for 10-15 times, and drying in a constant-temperature drying box at 60 ℃ for 4-6h to obtain arginine lanthanum particles;
(4) Dispersing arginine lanthanum particles in an ethanol water solution with the mass of 10-15 times of that of the arginine lanthanum particles, wherein the mass ratio of ethanol to water in the ethanol water solution is 1:2.5, adding calcium carbonate whiskers with the mass of 0.01-0.02 time of the arginine lanthanum particles, connecting an external electric field, stirring at 100rpm while heating to 80-100 ℃, keeping the temperature for 2-4 h, filtering, washing with distilled water and absolute ethanol for 13-16 times in sequence, and centrifuging and spin-drying for 1-2h to obtain the green production-based rare earth stabilizer.
2. The processing method of the rare earth stabilizer based on green production as claimed in claim 1, wherein the high-frequency current frequency in the electromagnetic induction heater in the step (1) is 25 to 30kHz, and the power is 60kW.
3. The processing method of the green production-based rare earth stabilizer as claimed in claim 1, wherein the ultrasonic frequency in step (2) is 100 to 120W and 40 to 50kHz.
4. The method for processing the rare earth stabilizer based on green production according to claim 1, wherein the step (2) of staged pressure drying is to adjust the pressure to 60kPa, maintain the pressure for 40 to 50s, adjust the pressure to 20kPa, maintain the pressure for 60 to 80s, adjust the pressure to 4kPa, maintain the pressure for 90 to 100s, and release the pressure.
5. The green production based rare earth stabilizer processing method according to claim 4, characterized in that the pressure relief rate in the pressure relief process is 10 to 15kPa/min.
6. The processing method of the rare earth stabilizer based on green production, as claimed in claim 1, wherein the ultrasonic frequency in step (3) is 300 to 400W and 40 to 50kHz; the frequency of the electrostatic field is 70 to 80kV/m; the microwave frequency is 800 to 900W.
7. The method for processing the rare earth stabilizer based on green production as claimed in claim 1, wherein the external electric field in the step (4) is a sinusoidal alternating electric field, the frequency is 40 to 50Hz, and the voltage is 100 to 150V.
8. The green production based rare earth stabilizer processing method according to claim 1, wherein the frequency of the centrifugal drying in the step (4) is 1500 to 2000rpm.
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Denomination of invention: A Processing Method for Rare Earth Stabilizers Based on Green Production Effective date of registration: 20230629 Granted publication date: 20221206 Pledgee: China Zheshang Bank Co.,Ltd. Changzhou Branch Pledgor: Liyang Dadi New Materials Co.,Ltd. Registration number: Y2023980046759 |