CN110760186A - Regenerated silicon material and preparation method thereof - Google Patents
Regenerated silicon material and preparation method thereof Download PDFInfo
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- CN110760186A CN110760186A CN201910878596.8A CN201910878596A CN110760186A CN 110760186 A CN110760186 A CN 110760186A CN 201910878596 A CN201910878596 A CN 201910878596A CN 110760186 A CN110760186 A CN 110760186A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/20—Recycled plastic
Abstract
The invention discloses a regenerated silicon material and a preparation method thereof in the technical field of silicon materials, which comprises the following steps: s1: selecting materials, S2, cleaning, S3: crushing, S4, A, S5, B, S6, stirring, S7, reacting, S8, cooling, removing films and impurities on the waste silicon material square sheets in a cleaning mode to enable the loss rate of the waste silicon material square sheets to be within 5%, ensuring the quality of the square sheets, crushing the waste silicon material square sheets to form heat-conducting powder filler, mixing the prepared A component with the prepared B component to realize regeneration of the silicon material, combining an amine compound with a catalyst to enable the silicon material to have excellent flame retardant property, enabling the regenerated silicon material to have excellent heat conductivity, heat dissipation property and flame retardance, adding a small amount of high-temperature resistant auxiliary agent, improving the high-temperature resistance of the regenerated silicon material, ensuring the long-term heat dissipation stability under the high-temperature condition, and prolonging the service life.
Description
Technical Field
The invention relates to the technical field of silicon materials, in particular to a regenerated silicon material and a preparation method thereof.
Background
Silicon material is an important semiconductor material, the symbol of chemical element is Si, and silicon used in the electronic industry should have high purity and excellent electrical and mechanical properties. Silicon is the most productive and widely used semiconductor material, and its yield and usage mark the electronic industry level of a country,
however, the existing waste silicon material cannot be regenerated, the demand of the silicon material is large, and the capacity of the original silicon is insufficient and cannot meet the demand, for example, a waste silicon material square piece is a silicon material produced after a semiconductor is scrapped, has abundant quantity, and can be applied to other positions if being regenerated, so that the resource saving effect is realized.
Disclosure of Invention
The present invention is directed to a regenerated silicon material and a method for preparing the same, which solves the above-mentioned problems of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: a regenerated silicon material and a preparation method thereof comprise the following steps:
s1: selecting materials: the method comprises the following steps of weighing 45-65 parts by weight of waste silicon material square pieces, 2-3 parts by weight of Wang acid, 2-3 parts by weight of sodium hydroxide solution, 2-3 parts by weight of dilute acid, 1-3 parts by weight of high-temperature resistant auxiliary agent, 20-30 parts by weight of end group vinyl silicone oil, 0.2-3 parts by weight of adhesion promoter, 0.4-3 parts by weight of catalyst, 0.6-3 parts by weight of inhibitor and 0.2-3 parts by weight of amine compound;
s2, cleaning: soaking the waste silicon material square pieces in the S1 in the aqua regia, taking out the silicon material square pieces after soaking, washing the silicon material square pieces clean with water, carrying out alkali washing on the washed waste silicon material square pieces through a sodium hydroxide solution, taking out the silicon material square pieces after the alkali washing, washing the silicon material square pieces clean with water again, soaking the washed waste silicon material square pieces in dilute acid, washing the silicon material square pieces with high-purity water after soaking, and dehydrating and drying the washed waste silicon material square pieces;
s3: crushing: putting the silicon material square pieces treated in the step S2 into a crushing box for crushing for 3-5 hours;
s4, preparation of A part: putting the material obtained by crushing the S3 into a dispersion machine, sequentially adding the terminal vinyl silicone oil, the amine compound, the adhesion promoter and the catalyst, vacuumizing, and stirring at the speed of 200-1000 r/min for 40-70 min under the environment with the vacuum degree of-0.08-0.04 MPa and the temperature of 25-35 ℃;
s5, preparation of part B: putting the material obtained by crushing the S3 into a dispersion machine, sequentially adding the terminal vinyl silicone oil, the adhesion promoter and the inhibitor, and stirring for 30-60 min at the speed of 200-1000 r/min under the environment with the vacuum degree of-0.08-0.04 MPa and the temperature of 25-35 ℃;
s6, stirring: taking the parts A and B in S4 and S5 with equal mass, moderating and uniformly mixing at room temperature, adding a high-temperature-resistant auxiliary agent, and continuously stirring;
s7, reaction: heating to 100-115 ℃ under the vacuum protection condition, vacuumizing, stirring and dispersing for 40-80 min;
s8, cooling: after the reaction of S7 is finished, standing to cool the obtained material to room temperature to obtain a regenerated silicon material;
further, in the step S2, soaking in aqua regia for 34-50 h, washing with alkali for 2-3 h, and soaking in dilute acid for 12-32 h.
Further, the dilute acid in the S1 is hydrofluoric acid, and the high-temperature resistant auxiliary agent in the S1 is selected from one or more of an organic silicon copper complex, an organic silicon aluminum complex, an organic silicon iron complex and an organic silicon zirconium complex.
Further, the amine compound in S1 is one or more of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenetriamine, or tetramethylethylenediamine.
Further, the adhesion promoter in S1 is one or two selected from bis (diethyl citrate) dipropoxy zirconium chelate, distearoyl isopropoxy aluminate, diisobutyl bis (ethyl acetoacetate) titanate and isopropyl titanate; the catalyst in S1 is selected from one of chloroplatinic acid isopropanol solution, karstedt platinum catalyst and Willing platinum catalyst, and the inhibitor in S1 is selected from one or more of vinyl ring body, 1, 4-butynediol, ethynyl cyclohexanol, maleic acid monoester and maleic acid diisoallyl ester.
Further, in the step S2, after being washed with high-purity water, the water is firstly dewatered and dried by a centrifuge, and then dried.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, firstly, a cleaning mode is adopted to remove films and impurities on the waste silicon material square sheets, so that the loss rate of the waste silicon material square sheets is within 5%, the quality of the square sheets is ensured, then the waste silicon material square sheets are crushed into heat conduction powder fillers, the regeneration of the silicon material is realized by mixing the prepared component A and the prepared component B, and the amine compound is used together with the catalyst, so that the silicon material has excellent flame retardant property, the regenerated silicon material has excellent heat conductivity, heat dissipation and flame retardance, and a small amount of high-temperature resistant auxiliary agent is added, so that the high-temperature resistance of the regenerated silicon material is improved, the long-term heat dissipation stability under the high-temperature condition is ensured, and the service life is longer.
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.
Example 1
A regenerated silicon material and a preparation method thereof comprise the following steps:
s1: selecting materials: 45 parts of waste silicon material square slices, 2 parts of Wang acid, 2 parts of sodium hydroxide solution, 2 parts of dilute acid, 1 part of high-temperature resistant assistant, 20 parts of end group vinyl silicone oil, 0.2 part of adhesion promoter, 0.4 part of catalyst, 0.6 part of inhibitor and 0.2 part of amine compound are respectively weighed according to parts by weight;
s2, cleaning: soaking the waste silicon material square pieces in the S1 in the aqua regia, taking out the silicon material square pieces after soaking, washing the silicon material square pieces clean with water, carrying out alkali washing on the washed waste silicon material square pieces through a sodium hydroxide solution, taking out the silicon material square pieces after the alkali washing, washing the silicon material square pieces clean with water again, soaking the washed waste silicon material square pieces in dilute acid, washing the silicon material square pieces with high-purity water after soaking, and dehydrating and drying the washed waste silicon material square pieces;
s3: crushing: putting the silicon material square pieces treated in the step S2 into a crushing box for crushing for 3 hours;
s4, preparation of A part: putting the crushed material of S3 into a dispersion machine, sequentially adding terminal vinyl silicone oil, amine compound, adhesion promoter and catalyst, vacuumizing, and stirring at the speed of 200r/min for 40min under the environment of vacuum degree of-0.08 MPa and temperature of 25 ℃;
s5, preparation of part B: putting the crushed material of S3 into a dispersion machine, sequentially adding the terminal vinyl silicone oil, the adhesion promoter and the inhibitor, and stirring for 30min at the speed of 200r/min under the environment of vacuum degree of-0.08-MPa and temperature of 25 ℃;
s6, stirring: taking the parts A and B in S4 and S5 with equal mass, moderating and uniformly mixing at room temperature, adding a high-temperature-resistant auxiliary agent, and continuously stirring;
s7, reaction: heating to 100 ℃ under the vacuum protection condition, vacuumizing, stirring, and performing dispersion reaction for 40 min;
s8, cooling: after the reaction of S7 is finished, standing to cool the obtained material to room temperature to obtain a regenerated silicon material;
comprises soaking in aqua regia for 34h, washing with alkali for 2h, and soaking in dilute acid for 12h in S2.
The diluted acid in S1 is hydrofluoric acid, and the high-temperature resistant additive in S1 is one or more selected from organosilicon copper complex, organosilicon silicon aluminum complex, organosilicon silicon iron complex and organosilicon zirconium complex.
The amine compound in S1 is one or more of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenetriamine or tetramethylethylenediamine.
The adhesion promoter in S1 is one or two selected from bis (diethyl citrate) dipropoxy zirconium chelate, distearoyl isopropoxy aluminate, diisobutyl bis (ethyl acetoacetate) titanate and isopropyl titanate; the catalyst in S1 is selected from one of chloroplatinic acid isopropanol solution, karstedt platinum catalyst and Willing platinum catalyst, and the inhibitor in S1 is selected from one or more of vinyl ring body, 1, 4-butynediol, ethynyl cyclohexanol, maleic acid monoester and maleic acid diisoallyl ester.
And S2, washing with high-purity water, dewatering by using a centrifugal machine, spin-drying, and drying.
Example 2
A regenerated silicon material and a preparation method thereof comprise the following steps:
s1: selecting materials: the method comprises the following steps of weighing 50 parts by weight of waste silicon material square pieces, 2.5 parts by weight of Wang acid, 2.5 parts by weight of sodium hydroxide solution, 2.5 parts by weight of dilute acid, 2 parts by weight of high-temperature resistant auxiliary agent, 25 parts by weight of end group vinyl silicone oil, 1 part by weight of adhesion promoter, 2 parts by weight of catalyst, 2 parts by weight of inhibitor and 2 parts by weight of amine compound;
s2, cleaning: soaking the waste silicon material square pieces in the S1 in the aqua regia, taking out the silicon material square pieces after soaking, washing the silicon material square pieces clean with water, carrying out alkali washing on the washed waste silicon material square pieces through a sodium hydroxide solution, taking out the silicon material square pieces after the alkali washing, washing the silicon material square pieces clean with water again, soaking the washed waste silicon material square pieces in dilute acid, washing the silicon material square pieces with high-purity water after soaking, and dehydrating and drying the washed waste silicon material square pieces;
s3: crushing: putting the silicon material square pieces treated in the step S2 into a crushing box for crushing for 4 hours;
s4, preparation of A part: putting the crushed material of S3 into a dispersion machine, sequentially adding terminal vinyl silicone oil, amine compound, adhesion promoter and catalyst, vacuumizing, and stirring at 600r/min for 55min under the environment of vacuum degree of-0.06 MPa and temperature of 30 ℃;
s5, preparation of part B: putting the crushed material of S3 into a dispersion machine, sequentially adding the terminal vinyl silicone oil, the adhesion promoter and the inhibitor, and stirring for 45min at a speed of 600r/min under the environment of a vacuum degree of-0.06 MPa and a temperature of 30 ℃;
s6, stirring: taking the parts A and B in S4 and S5 with equal mass, moderating and uniformly mixing at room temperature, adding a high-temperature-resistant auxiliary agent, and continuously stirring;
s7, reaction: heating to 105 ℃ under the vacuum protection condition, vacuumizing, stirring, and dispersing for reaction for 60 min;
s8, cooling: after the reaction of S7 is finished, standing to cool the obtained material to room temperature to obtain a regenerated silicon material;
comprises soaking in S2 in aqua regia for 40h, washing with alkali for 2.5h, and soaking in dilute acid for 24 h.
The diluted acid in S1 is hydrofluoric acid, and the high-temperature resistant additive in S1 is one or more selected from organosilicon copper complex, organosilicon silicon aluminum complex, organosilicon silicon iron complex and organosilicon zirconium complex.
The amine compound in S1 is one or more of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenetriamine or tetramethylethylenediamine.
The adhesion promoter in S1 is one or two selected from bis (diethyl citrate) dipropoxy zirconium chelate, distearoyl isopropoxy aluminate, diisobutyl bis (ethyl acetoacetate) titanate and isopropyl titanate; the catalyst in S1 is selected from one of chloroplatinic acid isopropanol solution, karstedt platinum catalyst and Willing platinum catalyst, and the inhibitor in S1 is selected from one or more of vinyl ring body, 1, 4-butynediol, ethynyl cyclohexanol, maleic acid monoester and maleic acid diisoallyl ester.
And S2, washing with high-purity water, dewatering by using a centrifugal machine, spin-drying, and drying.
Example 3
A regenerated silicon material and a preparation method thereof comprise the following steps:
s1: selecting materials: the method comprises the following steps of weighing 65 parts of waste silicon material square pieces, 3 parts of Wang acid, 3 parts of sodium hydroxide solution, 3 parts of dilute acid, 3 parts of high-temperature resistant auxiliary agent, 30 parts of end group vinyl silicone oil, 3 parts of adhesion promoter, 3 parts of catalyst, 3 parts of inhibitor and 3 parts of amine compound in parts by weight;
s2, cleaning: soaking the waste silicon material square pieces in the S1 in the aqua regia, taking out the silicon material square pieces after soaking, washing the silicon material square pieces clean with water, carrying out alkali washing on the washed waste silicon material square pieces through a sodium hydroxide solution, taking out the silicon material square pieces after the alkali washing, washing the silicon material square pieces clean with water again, soaking the washed waste silicon material square pieces in dilute acid, washing the silicon material square pieces with high-purity water after soaking, and dehydrating and drying the washed waste silicon material square pieces;
s3: crushing: putting the silicon material square pieces treated in the step S2 into a crushing box for crushing for 5 hours;
s4, preparation of A part: putting the crushed material of S3 into a dispersion machine, sequentially adding terminal vinyl silicone oil, amine compound, adhesion promoter and catalyst, vacuumizing, and stirring at 1000r/min for 70min under the environment of vacuum degree of 0.04MPa and temperature of 35 ℃;
s5, preparation of part B: putting the crushed material of S3 into a dispersion machine, sequentially adding the terminal vinyl silicone oil, the adhesion promoter and the inhibitor, and stirring for 60min at the speed of 1000r/min under the environment of vacuum degree of-0.04 MPa and temperature of 35 ℃;
s6, stirring: taking the parts A and B in S4 and S5 with equal mass, moderating and uniformly mixing at room temperature, adding a high-temperature-resistant auxiliary agent, and continuously stirring;
s7, reaction: heating to 115 ℃ under the vacuum protection condition, vacuumizing, stirring, and performing dispersion reaction for 80 min;
s8, cooling: after the reaction of S7 is finished, standing to cool the obtained material to room temperature to obtain a regenerated silicon material;
comprises soaking in aqua regia for 50h, washing with alkali for 3h, and soaking in dilute acid for 32h in S2.
The diluted acid in S1 is hydrofluoric acid, and the high-temperature resistant additive in S1 is one or more selected from organosilicon copper complex, organosilicon silicon aluminum complex, organosilicon silicon iron complex and organosilicon zirconium complex.
The amine compound in S1 is one or more of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenetriamine or tetramethylethylenediamine.
The adhesion promoter in S1 is one or two selected from bis (diethyl citrate) dipropoxy zirconium chelate, distearoyl isopropoxy aluminate, diisobutyl bis (ethyl acetoacetate) titanate and isopropyl titanate; the catalyst in S1 is selected from one of chloroplatinic acid isopropanol solution, karstedt platinum catalyst and Willing platinum catalyst, and the inhibitor in S1 is selected from one or more of vinyl ring body, 1, 4-butynediol, ethynyl cyclohexanol, maleic acid monoester and maleic acid diisoallyl ester.
And S2, washing with high-purity water, dewatering by using a centrifugal machine, spin-drying, and drying.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A regenerated silicon material and a preparation method thereof are characterized in that: the method comprises the following steps:
s1: selecting materials: the method comprises the following steps of weighing 45-65 parts by weight of waste silicon material square pieces, 2-3 parts by weight of Wang acid, 2-3 parts by weight of sodium hydroxide solution, 2-3 parts by weight of dilute acid, 1-3 parts by weight of high-temperature resistant auxiliary agent, 20-30 parts by weight of end group vinyl silicone oil, 0.2-3 parts by weight of adhesion promoter, 0.4-3 parts by weight of catalyst, 0.6-3 parts by weight of inhibitor and 0.2-3 parts by weight of amine compound;
s2, cleaning: soaking the waste silicon material square pieces in the S1 in the aqua regia, taking out the silicon material square pieces after soaking, washing the silicon material square pieces clean with water, carrying out alkali washing on the washed waste silicon material square pieces through a sodium hydroxide solution, taking out the silicon material square pieces after the alkali washing, washing the silicon material square pieces clean with water again, soaking the washed waste silicon material square pieces in dilute acid, washing the silicon material square pieces with high-purity water after soaking, and dehydrating and drying the washed waste silicon material square pieces;
s3: crushing: putting the silicon material square pieces treated in the step S2 into a crushing box for crushing for 3-5 hours;
s4, preparation of A part: putting the material obtained by crushing the S3 into a dispersion machine, sequentially adding the terminal vinyl silicone oil, the amine compound, the adhesion promoter and the catalyst, vacuumizing, and stirring at the speed of 200-1000 r/min for 40-70 min under the environment with the vacuum degree of-0.08-0.04 MPa and the temperature of 25-35 ℃;
s5, preparation of part B: putting the material obtained by crushing the S3 into a dispersion machine, sequentially adding the terminal vinyl silicone oil, the adhesion promoter and the inhibitor, and stirring for 30-60 min at the speed of 200-1000 r/min under the environment with the vacuum degree of-0.08-0.04 MPa and the temperature of 25-35 ℃;
s6, stirring: taking the parts A and B in S4 and S5 with equal mass, moderating and uniformly mixing at room temperature, adding a high-temperature-resistant auxiliary agent, and continuously stirring;
s7, reaction: heating to 100-115 ℃ under the vacuum protection condition, vacuumizing, stirring and dispersing for 40-80 min;
s8, cooling: after the reaction of S7 is finished, standing to cool the obtained material to room temperature to obtain a regenerated silicon material;
the recycled silicon material and the preparation method thereof as claimed in claim 1, wherein: and in the S2, soaking in aqua regia for 34-50 h, washing with alkali for 2-3 h, and soaking in dilute acid for 12-32 h.
2. The recycled silicon material and the preparation method thereof as claimed in claim 1, wherein: the diluted acid in the S1 is hydrofluoric acid, and the high-temperature-resistant auxiliary agent in the S1 is selected from one or more of an organic silicon copper complex, an organic silicon aluminum complex, an organic silicon iron complex and an organic silicon zirconium complex.
3. The recycled silicon material and the preparation method thereof as claimed in claim 1, wherein: the amine compound in S1 is one or more of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, dipropylenetriamine or tetramethylethylenediamine.
4. The recycled silicon material and the preparation method thereof as claimed in claim 1, wherein: the adhesion promoter in S1 is one or two of bis (diethyl citrate) dipropoxy zirconium chelate, distearoyl isopropoxy aluminate, diisobutyl bis (ethyl acetoacetate) titanate and isopropyl titanate; the catalyst in S1 is selected from one of chloroplatinic acid isopropanol solution, karstedt platinum catalyst and Willing platinum catalyst, and the inhibitor in S1 is selected from one or more of vinyl ring body, 1, 4-butynediol, ethynyl cyclohexanol, maleic acid monoester and maleic acid diisoallyl ester.
5. The recycled silicon material and the preparation method thereof as claimed in claim 1, wherein: and in the S2, after being cleaned by high-purity water, the water is firstly dewatered and dried by a centrifugal machine, and then the water is dried.
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