CN109535526A - A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment - Google Patents

A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment Download PDF

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CN109535526A
CN109535526A CN201811431291.4A CN201811431291A CN109535526A CN 109535526 A CN109535526 A CN 109535526A CN 201811431291 A CN201811431291 A CN 201811431291A CN 109535526 A CN109535526 A CN 109535526A
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季忠勋
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Xuzhou Emperor Yi Electronics Co Ltd
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Xuzhou Emperor Yi Electronics Co Ltd
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Abstract

A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment, it is as follows that raw material forms component by weight: 10~15 parts of sulfonate polystyrene resin, 2.5~4.5 parts of silicon nitride powder, 11~17 parts of silicon powder, 3~8 parts of polystyrene, 13~17 parts of carbon black, 22~25.5 parts of zinc oxide, 0.5~1.5 part of stearic acid, wear resistant polyvinyl plastic with filling material of nanometer silicon nitride: 6~13 parts of masterbatch, 4.5~7.5 parts of filler, 1~3 part of mother liquor, the present invention can not only significantly improve high molecular material performance, it can simplify procedure of processing simultaneously, reduce cost, substantially improve the cost performance of silicon powder material, absorption property is good, high temperature resistant, it does not burn, with excellent insulating properties, chemical purity is high, dispersion performance is good, it is widely used in electronics currently as new material Many industrial circles such as equipment, silicon rubber, medicine.

Description

A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment
Technical field
The present invention relates to a kind of preparation methods of Nano powder of silicon nitride for industrial electrical equipment, are related to a kind of inorganic The preparation method of nonmetallic materials.
Background technique
Since the 1980s, an emerging sciemtifec and technical sphere --- nano science and nanotechnology are able to be born and fluffy The exhibition of breaking out.So far, nanosecond science and technology oneself penetrated into the fields such as material, electronics, chemistry, biology, especially in the application of Material Field.
The industrial large-scale production of Nano powder of silicon nitride at present mainly uses silicon powder direct nitridation method, and there are following for the method Problem:
1) poor thermal conductivity of silicon powder causes silicon power raw material inside and the external temperature difference big, keeps reaction process unstable；
2) sintering of silicon powder hinders the infiltration of nitrogen, increases production process energy consumption, and purity is difficult to control.
Summary of the invention
The technical problem to be solved by the present invention is to, provide a kind of not only can greatly change in view of the deficiencies of the prior art Kind high molecular material performance, while can simplify procedure of processing, cost is reduced, the cost performance of silicon powder material, dosage are substantially improved Small, function is strong, meets the developing direction of safety and environmental friendliness, has great development potentiality, and absorption property is good, resistance to height Temperature is not burnt, and has excellent insulating properties, chemical purity is high, the good nano silicon nitride for industrial electrical equipment of dispersion performance The preparation method of silicon powder.
To achieve the goals above, the present invention provides a kind of preparation of Nano powder of silicon nitride for industrial electrical equipment Method, comprising the following steps:
A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment is made through the following steps, weighs chlorine Sulfonated polyethylene is dissolved in chloroform that produce mother liquor spare, chlorosulfonated polyethylene, silicon nitride powder, silicon powder, polystyrene, charcoal Black, zinc oxide, stearic acid, N, N '-diphenyl-para-phenylene diamine, diethylene glycol (DEG), sulphur, zinc diethyl dithiocarbamate are dissolved in three In chloromethanes, masterbatch is prepared through two-stage mixing in mixer and open mill；It weighs Nano powder of silicon nitride to be put into container, add Enter chloroform, ultrasonic disperse 25min prepares modified nano silicon nitride filler, masterbatch, mother liquor and modified nano silicon nitride are filled out Heating is uniformly mixed material in a high speed mixer, and injection molding is heated on injection molding machine；
Its technical characteristic is as follows: it is as follows that raw material forms component by weight: 10~15 parts of sulfonate polystyrene resin, silicon nitride powder 2.5~4.5 parts, 11~17 parts of silicon powder, 3~8 parts of polystyrene, 13~17 parts of carbon black, 22~25.5 parts of zinc oxide, stearic acid 0.5~1.5 part, N, 12~14 parts of N '-diphenyl-para-phenylene diamine, 14~17 parts of diethylene glycol (DEG), zinc diethyl dithiocarbamate 7.5~9.5 parts；
Mother liquor: 11~14 parts of chlorosulfonated polyethylene resin, 3.5~5.5 parts of chloroform；
Filler: 4~7 parts of Nano powder of silicon nitride, 3.5~6.5 parts of chloroform；
Wear resistant polyvinyl plastic with filling material of nanometer silicon nitride: 6~13 parts of masterbatch, 4.5~7.5 parts of filler, mother liquor 1~3 Part.
A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment, comprising the following steps:
(1) it prepares: 2.5~4.5 parts of silicon nitride powder, 11~17 parts of silicon powder, 3~8 parts of polystyrene is mixed with solvent, Be pressed into spherical shape under 15~20.5Mpa, in nitrogen atmosphere in 1800~2200 DEG C keep the temperature 18~for 24 hours, sintering generate silicon nitride； 10~15 parts and 3.5~5.5 parts of chloroform of sulfonate polystyrene resin are uniformly mixed, wait be completely dissolved, for use
(2) it produces: by 10~15 parts of sulfonate polystyrene resin, the nitrogen by melt index range between 25~35g/5min It is 2.5~4.5 parts of SiClx powder, 11~17 parts of silicon powder, 3~8 parts of polystyrene, 13~17 parts of carbon black, 22~25.5 parts of zinc oxide, hard 0.5~1.5 part of resin acid, N, 12~14 parts of N '-diphenyl-para-phenylene diamine, 14~17 parts of diethylene glycol (DEG), diethyl-dithio amino first 7.5~9.5 parts of sour zinc；It is uniformly mixed in high-speed mixer, two sections of mixings is carried out in mixer and open mill, one section is kneaded It is carried out in mixer, rotor speed 85rmin-1；Two-stage mixing carries out on a mill, and roller speed ratio is 1:1.55, preceding Roll temperature is 65 DEG C, and rear roll temperature is 50 DEG C, and dump temperature is 60 DEG C or so；Rubber compound vulcanizes on vulcanizing press, vulcanization Condition be 240 DEG C × 10min, product pass through water cooling, pelletizing, for use；
(3) prepared by filler: 4~7 parts of Nano powder of silicon nitride are put into container, and 3.5~6.5 parts of ultrasounds of chloroform are added Dispersion 25min obtains modified Nano powder of silicon nitride filler, spare；
(4) production of wear resistant polyvinyl plastic with filling material of nanometer silicon nitride: 6~13 parts of masterbatch, 4.5~7.5 parts of filler, 1~3 part of mother liquor, heating is uniformly mixed in a high speed mixer, and injection molding is heated on injection molding machine.
Preferably, in the step (1), silicon nitride powder include diameter 50 μm~80 μm of coarse fodder and diameter be 30 μm with Under fines；
It is 40 μm of fineves below that the silicon powder, which includes diameter in 50 μm~80 μm of coarse fodder and diameter,；
The partial size of the polystyrene-silica dioxide granule is 0.05~0.25mm；
The solvent is by water with ethyl alcohol according to volume ratio 1:(0.2~0.5) it mixes and forms.
A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment of the present invention not only can greatly change Kind high molecular material performance, while can simplify procedure of processing, cost is reduced, the cost performance of silicon powder material, dosage are substantially improved Small, function is strong, meets the developing direction of safety and environmental friendliness, has great development potentiality, and absorption property is good, resistance to height Temperature is not burnt, and has excellent insulating properties, chemical purity is high, and dispersion performance is good, is widely used in electricity currently as new material Many industrial circles such as sub- equipment, silicon rubber, medicine.
Specific embodiment
The present invention is described in further details below by embodiment.
Embodiment 1
A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment, comprising the following steps:
(1) it prepares: 2.5 parts of silicon nitride powder, 11 parts of silicon powder, 3 parts of polystyrene being mixed with solvent, are suppressed at 15Mpa At spherical shape, in 1800 DEG C of heat preservation 18h in nitrogen atmosphere, sintering generates silicon nitride；By 10 parts of sulfonate polystyrene resin and trichlorine 3.5 parts of methane are uniformly mixed, wait be completely dissolved, for use
(2) it produces: by 10 parts of sulfonate polystyrene resin, the silicon nitride powder 2.5 by melt index range between 25/5min Part, 11 parts of silicon powder, 3 parts of polystyrene, 13 parts of carbon black, 22 parts of zinc oxide, 0.5 part of stearic acid, N, N '-diphenyl-para-phenylene diamine 12 Part, 14 parts of diethylene glycol (DEG), 7.5 parts of zinc diethyl dithiocarbamate；It is uniformly mixed in high-speed mixer, in mixer and mill Two sections of mixings are carried out in machine, one section of mixing carries out in mixer, rotor speed 85rmin-1；Two-stage mixing is in open mill Upper progress, roller speed ratio are 1:1.55, and preceding roll temperature is 65 DEG C, and rear roll temperature is 50 DEG C, and dump temperature is 60 DEG C or so；It is kneaded Glue vulcanizes on vulcanizing press, conditions of vulcanization be 240 DEG C × 10min, product pass through water cooling, pelletizing, for use；
(3) prepared by filler: 4 parts of Nano powder of silicon nitride are put into container, and 3.5 parts of ultrasonic disperses of chloroform are added 25min obtains modified Nano powder of silicon nitride filler, spare；
(4) production of wear resistant polyvinyl plastic with filling material of nanometer silicon nitride: 6 parts of masterbatch, 4.5 parts of filler, 1 part of mother liquor, Heating is uniformly mixed in a high speed mixer, and injection molding is heated on injection molding machine.
Embodiment 2
A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment, comprising the following steps:
(1) it prepares: 4.5 parts of silicon nitride powder, 17 parts of silicon powder, 8 parts of polystyrene is mixed with solvent, pushed in 20.5Mpa Spherical shape is made, in nitrogen atmosphere for 24 hours in 2200 DEG C of heat preservations, sintering generates silicon nitride；By 15 parts of sulfonate polystyrene resin and three 5.5 parts of chloromethanes are uniformly mixed, wait be completely dissolved, for use
(2) it produces: by 15 parts of sulfonate polystyrene resin, the silicon nitride powder by melt index range between 35g/5min 4.5 parts, 17 parts of silicon powder, 8 parts of polystyrene, 17 parts of carbon black, 25.5 parts of zinc oxide, 1.5 parts of stearic acid, N, N '-diphenyl is to benzene 14 parts of diamines, 17 parts of diethylene glycol (DEG), 9.5 parts of zinc diethyl dithiocarbamate；It is uniformly mixed in high-speed mixer, in mixer It is kneaded with carrying out two sections in open mill, one section of mixing carries out in mixer, rotor speed 85rmin-1；Two-stage mixing exists It is carried out on open mill, roller speed ratio is 1:1.55, and preceding roll temperature is 65 DEG C, and rear roll temperature is 50 DEG C, and dump temperature is 60 DEG C of left sides It is right；Rubber compound vulcanizes on vulcanizing press, conditions of vulcanization be 240 DEG C × 10min, product pass through water cooling, pelletizing, for use；
(3) prepared by filler: 7 parts of Nano powder of silicon nitride are put into container, and 6.5 parts of ultrasonic disperses of chloroform are added 25min obtains modified Nano powder of silicon nitride filler, spare；
(4) production of wear resistant polyvinyl plastic with filling material of nanometer silicon nitride: 13 parts of masterbatch, 7.5 parts of filler, 3 parts of mother liquor, Heating is uniformly mixed in a high speed mixer, and injection molding is heated on injection molding machine.
Embodiment 3
A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment, comprising the following steps:
(1) it prepares: 3 parts of silicon nitride powder, 14 parts of silicon powder, 5 parts of polystyrene being mixed with solvent, are suppressed at 18.5Mpa At spherical shape, in 2000 DEG C of heat preservation 20h in nitrogen atmosphere, sintering generates silicon nitride；By 12.5 parts of sulfonate polystyrene resin and three 4 parts of chloromethanes are uniformly mixed, wait be completely dissolved, for use
(2) it produces: by 12.5 parts of sulfonate polystyrene resin, the silicon nitride powder by melt index range between 30g/5min 3 parts, 14 parts of silicon powder, 5 parts of polystyrene, 15 parts of carbon black, 23.5 parts of zinc oxide, 1.0 parts of stearic acid, N, N '-diphenyl is to benzene two 13 parts of amine, 15.5 parts of diethylene glycol (DEG), 8 parts of zinc diethyl dithiocarbamate；Be uniformly mixed in high-speed mixer, in mixer and Two sections of mixings are carried out in open mill, one section of mixing carries out in mixer, rotor speed 85rmin-1；Two-stage mixing is being opened It is carried out in mill, roller speed ratio is 1:1.55, and preceding roll temperature is 65 DEG C, and rear roll temperature is 50 DEG C, and dump temperature is 60 DEG C or so； Rubber compound vulcanizes on vulcanizing press, conditions of vulcanization be 240 DEG C × 10min, product pass through water cooling, pelletizing, for use；
(3) prepared by filler: 5.5 parts of Nano powder of silicon nitride are put into container, and 5 parts of ultrasonic disperses of chloroform are added 25min obtains modified Nano powder of silicon nitride filler, spare；
(4) production of wear resistant polyvinyl plastic with filling material of nanometer silicon nitride: 9.5 parts of masterbatch, 6 parts of filler, 2 parts of mother liquor, Heating is uniformly mixed in a high speed mixer, and injection molding is heated on injection molding machine.
Micron order, sub-meter grade, nanoscale are all detection classifications under the microscope.

Claims (3)

1. a kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment, which is characterized in that through the following steps system , it weighs chlorosulfonated polyethylene and is dissolved in chloroform that produce mother liquor spare, chlorosulfonated polyethylene, silicon nitride powder, silicon powder, gather Styrene, carbon black, zinc oxide, stearic acid, N, N '-diphenyl-para-phenylene diamine, diethylene glycol (DEG), sulphur, diethyl-dithio amino first Sour zinc is dissolved in chloroform, prepares masterbatch through two-stage mixing in mixer and open mill；Nano powder of silicon nitride is weighed to put Enter in container, chloroform is added, ultrasonic disperse 25min prepares modified nano silicon nitride filler, and masterbatch, mother liquor and modification are received Rice silicon nitride filler heats in a high speed mixer to be uniformly mixed, and injection molding is heated on injection molding machine；
Its technical characteristic is as follows: it is as follows that raw material forms component by weight: 10~15 parts of sulfonate polystyrene resin, silicon nitride powder 2.5 ~4.5 parts, 11~17 parts of silicon powder, 3~8 parts of polystyrene, 13~17 parts of carbon black, 22~25.5 parts of zinc oxide, stearic acid 0.5~ 1.5 parts, N, 12~14 parts of N '-diphenyl-para-phenylene diamine, 14~17 parts of diethylene glycol (DEG), zinc diethyl dithiocarbamate 7.5~ 9.5 part；
Mother liquor: 11~14 parts of chlorosulfonated polyethylene resin, 3.5~5.5 parts of chloroform；
Filler: 4~7 parts of Nano powder of silicon nitride, 3.5~6.5 parts of chloroform；
Wear resistant polyvinyl plastic with filling material of nanometer silicon nitride: 6~13 parts of masterbatch, 4.5~7.5 parts of filler, 1~3 part of mother liquor.
2. a kind of preparation method of Nano powder of silicon nitride for industrial electrical equipment according to claim 1, special Sign is, comprising the following steps:
(1) it prepares: 2.5~4.5 parts of silicon nitride powder, 11~17 parts of silicon powder, 3~8 parts of polystyrene is mixed with solvent, 15~ Be pressed into spherical shape under 20.5Mpa, in nitrogen atmosphere in 1800~2200 DEG C keep the temperature 18~for 24 hours, sintering generate silicon nitride；By sulphur Change 10~15 parts and 3.5~5.5 parts of chloroform of polyvinyl resin to be uniformly mixed, wait be completely dissolved, for use
(2) it produces: by 10~15 parts of sulfonate polystyrene resin, the silicon nitride by melt index range between 25~35g/5min 2.5~4.5 parts of powder, 11~17 parts of silicon powder, 3~8 parts of polystyrene, 13~17 parts of carbon black, 22~25.5 parts of zinc oxide, stearic acid 0.5~1.5 part, N, 12~14 parts of N '-diphenyl-para-phenylene diamine, 14~17 parts of diethylene glycol (DEG), zinc diethyl dithiocarbamate 7.5~9.5 parts；It is uniformly mixed in high-speed mixer, two sections of mixings is carried out in mixer and open mill, one section is kneaded in mixing It is carried out in machine, rotor speed 85rmin-1；Two-stage mixing carries out on a mill, and roller speed ratio is 1:1.55, preceding roller temperature Degree is 65 DEG C, and rear roll temperature is 50 DEG C, and dump temperature is 60 DEG C or so；Rubber compound vulcanizes on vulcanizing press, conditions of vulcanization For 240 DEG C × 10min, product passes through water cooling, pelletizing, for use；
(3) prepared by filler: 4~7 parts of Nano powder of silicon nitride are put into container, and 3.5~6.5 parts of ultrasonic disperses of chloroform are added 25min obtains modified Nano powder of silicon nitride filler, spare；
(4) production of wear resistant polyvinyl plastic with filling material of nanometer silicon nitride: 6~13 parts of masterbatch, 4.5~7.5 parts of filler, mother liquor 1~3 part, heating is uniformly mixed in a high speed mixer, and injection molding is heated on injection molding machine.
3. it is 30 μ that the silicon nitride powder of step (1), which includes diameter in 50 μm~80 μm of coarse fodder and diameter, according to claim 2 M fines below；
It is 40 μm of fineves below that the silicon powder, which includes diameter in 50 μm~80 μm of coarse fodder and diameter,；
The partial size of the polystyrene-silica dioxide granule is 0.05~0.25mm；
The solvent is by water with ethyl alcohol according to volume ratio 1:(0.2~0.5) it mixes and forms.
CN201811431291.4A 2018-11-26 2018-11-26 A kind of preparation method of the Nano powder of silicon nitride for industrial electrical equipment Pending CN109535526A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113416474A (en) * 2021-05-12 2021-09-21 宁波格莱美厨具有限公司 Uniform heat conduction non-stick pan coating and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113416474A (en) * 2021-05-12 2021-09-21 宁波格莱美厨具有限公司 Uniform heat conduction non-stick pan coating and preparation method thereof
CN113416474B (en) * 2021-05-12 2022-03-15 宁波格莱美厨具有限公司 Uniform heat conduction non-stick pan coating and preparation method thereof

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Application publication date: 20190329