CN117550885A - Ageing-resistant porcelain insulator used in low-temperature environment - Google Patents
Ageing-resistant porcelain insulator used in low-temperature environment Download PDFInfo
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- CN117550885A CN117550885A CN202311494789.6A CN202311494789A CN117550885A CN 117550885 A CN117550885 A CN 117550885A CN 202311494789 A CN202311494789 A CN 202311494789A CN 117550885 A CN117550885 A CN 117550885A
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- 239000012212 insulator Substances 0.000 title claims abstract description 62
- 229910052573 porcelain Inorganic materials 0.000 title claims abstract description 60
- 230000032683 aging Effects 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 262
- 239000002994 raw material Substances 0.000 claims abstract description 39
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 38
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 38
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 38
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 19
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 19
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims abstract description 19
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 19
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 19
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 135
- 238000003756 stirring Methods 0.000 claims description 124
- 239000000243 solution Substances 0.000 claims description 118
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 108
- 239000007864 aqueous solution Substances 0.000 claims description 92
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 86
- 239000007788 liquid Substances 0.000 claims description 81
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 80
- 239000000725 suspension Substances 0.000 claims description 74
- 239000008367 deionised water Substances 0.000 claims description 57
- 229910021641 deionized water Inorganic materials 0.000 claims description 57
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 54
- 239000002202 Polyethylene glycol Substances 0.000 claims description 54
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 54
- 229920001223 polyethylene glycol Polymers 0.000 claims description 54
- 238000004321 preservation Methods 0.000 claims description 54
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 48
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 45
- 239000004202 carbamide Substances 0.000 claims description 45
- 238000001816 cooling Methods 0.000 claims description 45
- 239000004408 titanium dioxide Substances 0.000 claims description 43
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 40
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 claims description 40
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 40
- 239000006185 dispersion Substances 0.000 claims description 40
- 239000007790 solid phase Substances 0.000 claims description 35
- 238000001035 drying Methods 0.000 claims description 33
- 238000000926 separation method Methods 0.000 claims description 33
- 239000007900 aqueous suspension Substances 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 30
- 239000007787 solid Substances 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 26
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 24
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 24
- 229960003638 dopamine Drugs 0.000 claims description 24
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 235000019766 L-Lysine Nutrition 0.000 claims description 16
- 239000004472 Lysine Substances 0.000 claims description 16
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 239000012298 atmosphere Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000005336 cracking Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 15
- 238000005245 sintering Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 12
- 239000011812 mixed powder Substances 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 238000003825 pressing Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
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- C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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Abstract
The invention discloses an aging-resistant porcelain insulator used in a low-temperature environment, which comprises a porcelain insulator body, wherein the porcelain insulator body comprises the following raw materials: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the porcelain insulator body prepared by the method has good strength and freeze-thaw aging resistance, so that the porcelain insulator can be used in occasions with large temperature change, low-temperature environments such as high-altitude and high-latitude areas and the like, low-temperature cracking and damage are not easy to occur, and the application range of the porcelain insulator is enlarged.
Description
Technical Field
The invention relates to the technical field of insulator materials, in particular to an aging-resistant porcelain insulator used in a low-temperature environment.
Background
The porcelain insulator has excellent electromechanical performance, so that the porcelain insulator is widely applied in the power industry and plays an important role in mechanical support and electrical insulation. The porcelain insulator has a severe running environment in the service process, is complex in stress and has a serious threat to the safe and stable running of the power system when a fracture accident happens, and statistics of years of fracture accidents show that the probability of the fracture accident of the porcelain insulator is maximum in a low-temperature environment in winter. Therefore, the characteristics of the porcelain insulator in a low-temperature environment are optimized, and the porcelain insulator has important significance for reliable operation and safety and stability of a system.
Disclosure of Invention
For this reason, the invention provides an aging-resistant porcelain insulator used in a low-temperature environment, which comprises a porcelain insulator body, wherein the porcelain insulator body comprises the following raw materials: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the preparation method of the modified titanium dioxide powder comprises the following steps:
(1) Preparing an aqueous solution of hexadecyl trimethyl ammonium bromide in a reaction kettle, and preparing an ethanol solution of n-butyl titanate and polyethylene glycol; stirring the aqueous solution of cetyl trimethyl ammonium bromide, adding the aqueous solution of urea into the solution in a stirring state, keeping the temperature in a water bath to 50+/-5 ℃ after the addition, continuing stirring the solution for 5-6 min after the addition is completed, adding the ethanol solution of n-butyl titanate and polyethylene glycol into the solution in a stirring state, continuing to keep the temperature at 50+/-5 ℃ for 5-6 min after the addition is completed, sealing the reaction kettle, heating to 120+/-3 ℃, keeping the temperature for more than 5h, and magnetically stirring in the heat preservation process; air cooling to normal temperature after heat preservation is finished, opening the reaction kettle, performing solid-liquid separation, washing a solid phase with deionized water for more than 3 times, drying for more than 30min at 60 ℃, and then placing in a muffle furnace at 550 ℃ for calcination for more than 6h to obtain titanium dioxide powder;
(2) Preparing an aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, dispersing the titanium dioxide powder in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to form a dispersion, keeping the temperature of the dispersion at 65+/-3 ℃ in a water bath, stirring the dispersion for 10-15 min, adding N-hydroxysuccinimide and L-lysine into the dispersion in a stirring state, keeping the temperature at 65+/-3 ℃ for more than 4h after the addition is finished, performing solid-liquid separation, washing the solid phase with deionized water for more than 3 times, and drying the solid phase at 60 ℃ for more than 30min to obtain pretreated powder;
(3) Dispersing the pretreated powder in deionized water to form suspension, keeping the suspension at a constant temperature of 35+/-3 ℃ in a water bath, stirring the suspension for more than 5min after the suspension is heated, then adding dopamine into the suspension in a stirring state, stirring the suspension for more than 10min at a constant temperature of 35+/-3 ℃ after the addition is finished, then adding tris (hydroxymethyl) aminomethane into the suspension in a stirring state, stirring the suspension for more than 30min at a constant temperature of 35+/-3 ℃ after the addition is finished, then carrying out solid-liquid separation, and drying for more than 8h in a solid-phase 50 ℃ environment to obtain coated powder;
(4) Adding the coated powder into deionized water in a nitrogen protection atmosphere, stirring to form an aqueous suspension, carrying out water bath constant temperature to 80+/-3 ℃, carrying out heat preservation, and condensing and refluxing; then adding 2-acrylamide-2-methylpropanesulfonic acid into the water suspension under the stirring state in the nitrogen atmosphere, continuing to keep the temperature at 80+/-3 ℃ for stirring for more than 10 minutes after the addition, then adding ammonium persulfate solution under the stirring state, keeping the temperature at 80+/-3 ℃ for stirring for more than 5 hours in the nitrogen atmosphere after the addition is finished, and condensing and refluxing in the heat preservation process; and after the heat preservation is finished, air cooling is carried out to normal temperature, solid-liquid separation is carried out, the solid phase is washed by deionized water for more than 3 times, and the modified titanium dioxide powder is obtained after drying at 60 ℃ for more than 30 min.
Further, the porcelain insulator comprises the following raw materials in parts by weight: 50 parts of mullite powder, 5-8 parts of potassium feldspar powder, 6-10 parts of zirconia powder, 2-4 parts of barium carbonate powder, 14-16 parts of modified titanium dioxide powder, 2-4 parts of zinc oxide powder, 3-10 parts of magnesia powder and 20-30 parts of kaolin; each raw material is fine powder which is sieved by a 500-mesh screen.
Further, in the step (1), in the aqueous solution of cetyltrimethylammonium bromide, the concentration of cetyltrimethylammonium bromide is 6-8 g/L, and the solvent is water; in the ethanol solution of the n-butyl titanate and the polyethylene glycol, the concentration of the n-butyl titanate is 20-25 g/L, the concentration of the polyethylene glycol is 10-12 g/L, and the solvent is ethanol; in the aqueous solution of urea, the concentration of the urea is 15-16 g/L; the volume ratio of the added volume of the aqueous solution of urea, the ethanol solution of the n-butyl titanate and the polyethylene glycol to the volume ratio of the aqueous solution of the cetyltrimethylammonium bromide is that of the aqueous solution of urea: ethanol solution of n-butyl titanate and polyethylene glycol: aqueous solution of cetyltrimethylammonium bromide=1-2:10-15:20.
Further, in the step (2), the concentration of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 4-6 g/200mL, and the solid-liquid mass ratio of the titanium dioxide powder dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is solid/liquid=1:100; the mass ratio of the added N-hydroxysuccinimide to the L-lysine to the titanium dioxide powder in the dispersion is N-hydroxysuccinimide: l-lysine: titanium dioxide powder = 2-3:4-7:1.
Further, in the step (3), the pretreated powder is dispersed in deionized water to form suspension, and the solid-liquid mass ratio is solid/liquid=1:100; the mass ratio of the added dopamine to the tris (hydroxymethyl) aminomethane to the pretreated powder in the suspension is dopamine: tris (hydroxymethyl) aminomethane: pretreatment powder=0.6 to 0.8:0.1 to 0.2:1.
Further, in the step (4), the solid-liquid mass ratio of the coating powder added into deionized water is solid/liquid=1:100; the ammonium persulfate solution contains 3 mass percent of ammonium persulfate and water as a solvent; the mass ratio of the added mass of the 2-acrylamide-2-methylpropanesulfonic acid and ammonium persulfate solution to the mass ratio of the coated powder in the aqueous suspension is 2-acrylamide-2-methylpropanesulfonic acid: ammonium persulfate solution: coated powder = 2-3:0.3-0.5:1.
The invention has the beneficial effects that: the porcelain insulator body prepared by the method has good strength and freeze-thaw aging resistance, so that the porcelain insulator can be used in occasions with large temperature change, low-temperature environments such as high-altitude and high-latitude areas and the like, low-temperature cracking and damage are not easy to occur, and the application range of the porcelain insulator is enlarged.
Detailed Description
The invention is further illustrated below with reference to examples.
Example 1
The utility model provides a low temperature environment uses ageing-resistant porcelain insulator, includes porcelain insulator body, porcelain insulator body's raw materials include: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the raw materials are as follows in parts by weight: 50 parts of mullite powder, 5 parts of potassium feldspar powder, 6 parts of zirconia powder, 2 parts of barium carbonate powder, 14 parts of modified titanium dioxide powder, 2 parts of zinc oxide powder, 3 parts of magnesia powder and 20 parts of kaolin; each raw material is fine powder which is sieved by a 500-mesh screen. The preparation method of the modified titanium dioxide powder comprises the following steps:
(1) Preparing an aqueous solution of hexadecyl trimethyl ammonium bromide in a reaction kettle, and preparing an ethanol solution of n-butyl titanate and polyethylene glycol; in the aqueous solution of the cetyl trimethyl ammonium bromide, the concentration of the cetyl trimethyl ammonium bromide is 6g/L, and the solvent is water; in the ethanol solution of the n-butyl titanate and the polyethylene glycol, the concentration of the n-butyl titanate is 20g/L, the concentration of the polyethylene glycol is 10g/L, and the solvent is ethanol; stirring the aqueous solution of the cetyl trimethyl ammonium bromide, and then adding the aqueous solution of urea into the solution in a stirring state, wherein the concentration of the urea in the aqueous solution of urea is 15g/L; after the addition, the water bath is kept at a constant temperature of 50+/-5 ℃ until the temperature is reached, stirring the solution for 5min, and then adding the ethanol solution of the n-butyl titanate and the polyethylene glycol into the solution under the stirring state, wherein the volume ratio of the added volume of the ethanol solution of the urea, the n-butyl titanate and the polyethylene glycol to the volume ratio of the water solution of the cetyl trimethyl ammonium bromide is the water solution of urea: ethanol solution of n-butyl titanate and polyethylene glycol: aqueous solution of cetyltrimethylammonium bromide = 1:10:20; continuing to stir at the constant temperature of 50+/-5 ℃ for 5min after the charging is finished, sealing the reaction kettle, heating to 120+/-3 ℃ and preserving heat for 5h, and magnetically stirring in the heat preservation process; air cooling to normal temperature after heat preservation is finished, opening the reaction kettle, performing solid-liquid separation, washing a solid phase with deionized water for 3 times, drying for 30min at 60 ℃, and then placing in a muffle furnace at 550 ℃ for calcination for 6h to obtain titanium dioxide powder;
(2) Preparing an aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, wherein the concentration of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 4g/200mL, and dispersing titanium dioxide powder in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to form a dispersion, wherein the mass ratio of solid to liquid in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is solid/liquid=1:100; the dispersion is subjected to water bath constant temperature to 65+/-3 ℃ and heat preservation, the dispersion is stirred for 10min, and then N-hydroxysuccinimide and L-lysine are added into the dispersion under the stirring state, wherein the mass ratio of the added N-hydroxysuccinimide to the L-lysine to the titanium dioxide powder in the dispersion is N-hydroxysuccinimide: l-lysine: titanium dioxide powder = 2:4:1; after the addition is finished, preserving the temperature for 4 hours at 65+/-3 ℃, then carrying out solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30 minutes to obtain pretreated powder;
(3) Dispersing the pretreatment powder in deionized water to form suspension, wherein the solid-liquid mass ratio of the pretreatment powder dispersed in the deionized water to form suspension is solid/liquid=1:100; the suspension is subjected to water bath constant temperature to 35+/-3 ℃ and heat preservation, the suspension is stirred for 5min after the suspension is heated, then dopamine is added into the suspension in a stirring state, the suspension is stirred for 10min at the constant temperature of 35+/-3 ℃ after the addition is finished, then tris (hydroxymethyl) aminomethane is added into the suspension in the stirring state, and the mass ratio of the addition mass of the dopamine and the tris (hydroxymethyl) aminomethane to the mass ratio of the pretreated powder in the suspension is dopamine: tris (hydroxymethyl) aminomethane: pretreatment powder = 0.6:0.1:1; stirring at constant temperature of 35+/-3 ℃ for 30min after the addition is completed, then carrying out solid-liquid separation, and drying for 8h at the solid phase of 50 ℃ to obtain coated powder;
(4) In a nitrogen protection atmosphere, adding the coated powder into deionized water, and stirring to form an aqueous suspension, wherein the solid-liquid mass ratio of the coated powder added into the deionized water is solid/liquid=1:100; the water suspension is subjected to water bath constant temperature to 80+/-3 ℃ for heat preservation, and condensation and reflux are carried out; then adding 2-acrylamide-2-methylpropanesulfonic acid into the water suspension in a stirring state in a nitrogen atmosphere, keeping the temperature at 80+/-3 ℃ and stirring for 10min after the addition, and then adding an ammonium persulfate solution in the stirring state, wherein the mass percent of the ammonium persulfate in the ammonium persulfate solution is 3 percent, and the solvent is water; the mass ratio of the added mass of the 2-acrylamide-2-methylpropanesulfonic acid and ammonium persulfate solution to the mass ratio of the coated powder in the aqueous suspension is 2-acrylamide-2-methylpropanesulfonic acid: ammonium persulfate solution: coated powder = 2:0.3:1; after the charging is completed, the mixture is stirred for 5 hours at 80+/-3 ℃ in a nitrogen atmosphere, and the mixture is condensed and reflowed in the heat preservation process; and (3) after the heat preservation is finished, air cooling to normal temperature, solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30min to obtain the modified titanium dioxide powder.
Weighing the raw materials according to the parts by weight, uniformly mixing the raw materials to form mixed powder, adding water to adjust the water content to 25wt%, pressing into a blank, heating to 420 ℃ for presintering for 30min, heating to 650 ℃ at 15 ℃/min, preserving heat for 30min, heating to 1180 ℃ at 5 ℃/min, and sintering for 3h; cooling to 800 ℃ at 5 ℃/min after sintering is completed, preserving heat for 10min, cooling to 500 ℃ at 10 ℃/min, preserving heat for 10min, cooling to 150 ℃ at 15 ℃/min, taking out, and cooling to normal temperature to obtain the porcelain insulator and the test sample.
Example 2
The utility model provides a low temperature environment uses ageing-resistant porcelain insulator, includes porcelain insulator body, porcelain insulator body's raw materials include: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the raw materials are as follows in parts by weight: 50 parts of mullite powder, 6 parts of potassium feldspar powder, 8 parts of zirconia powder, 3 parts of barium carbonate powder, 15 parts of modified titanium dioxide powder, 3 parts of zinc oxide powder, 5 parts of magnesia powder and 24 parts of kaolin; each raw material is fine powder which is sieved by a 500-mesh screen. The preparation method of the modified titanium dioxide powder comprises the following steps:
(1) Preparing an aqueous solution of hexadecyl trimethyl ammonium bromide in a reaction kettle, and preparing an ethanol solution of n-butyl titanate and polyethylene glycol; in the aqueous solution of the cetyl trimethyl ammonium bromide, the concentration of the cetyl trimethyl ammonium bromide is 7g/L, and the solvent is water; in the ethanol solution of the n-butyl titanate and the polyethylene glycol, the concentration of the n-butyl titanate is 22g/L, the concentration of the polyethylene glycol is 11g/L, and the solvent is ethanol; stirring the aqueous solution of the cetyl trimethyl ammonium bromide, and then adding the aqueous solution of urea into the solution in a stirring state, wherein the concentration of the urea in the aqueous solution of urea is 15g/L; after the addition, the water bath is kept at a constant temperature of 50+/-5 ℃ until the temperature is reached, stirring the solution for 5min, and then adding the ethanol solution of the n-butyl titanate and the polyethylene glycol into the solution under the stirring state, wherein the volume ratio of the added volume of the ethanol solution of the urea, the n-butyl titanate and the polyethylene glycol to the volume ratio of the water solution of the cetyl trimethyl ammonium bromide is the water solution of urea: ethanol solution of n-butyl titanate and polyethylene glycol: aqueous solution of cetyltrimethylammonium bromide = 1:12:20; continuing to stir at the constant temperature of 50+/-5 ℃ for 5min after the charging is finished, sealing the reaction kettle, heating to 120+/-3 ℃ and preserving heat for 5h, and magnetically stirring in the heat preservation process; air cooling to normal temperature after heat preservation is finished, opening the reaction kettle, performing solid-liquid separation, washing a solid phase with deionized water for 3 times, drying for 30min at 60 ℃, and then placing in a muffle furnace at 550 ℃ for calcination for 6h to obtain titanium dioxide powder;
(2) Preparing an aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, wherein in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, the concentration of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 5g/200mL, and the titanium dioxide powder is dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to form a dispersion, and the solid-liquid mass ratio of the titanium dioxide powder dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is solid/liquid=1:100; the dispersion is subjected to water bath constant temperature to 65+/-3 ℃ and heat preservation, the dispersion is stirred for 10min, and then N-hydroxysuccinimide and L-lysine are added into the dispersion under the stirring state, wherein the mass ratio of the added N-hydroxysuccinimide to the L-lysine to the titanium dioxide powder in the dispersion is N-hydroxysuccinimide: l-lysine: titanium dioxide powder = 2:5:1; after the addition is finished, preserving the temperature for 4 hours at 65+/-3 ℃, then carrying out solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30 minutes to obtain pretreated powder;
(3) Dispersing the pretreatment powder in deionized water to form suspension, wherein the solid-liquid mass ratio of the pretreatment powder dispersed in the deionized water to form suspension is solid/liquid=1:100; the suspension is subjected to water bath constant temperature to 35+/-3 ℃ and heat preservation, the suspension is stirred for 5min after the suspension is heated, then dopamine is added into the suspension in a stirring state, the suspension is stirred for 10min at the constant temperature of 35+/-3 ℃ after the addition is finished, then tris (hydroxymethyl) aminomethane is added into the suspension in the stirring state, and the mass ratio of the addition mass of the dopamine and the tris (hydroxymethyl) aminomethane to the mass ratio of the pretreated powder in the suspension is dopamine: tris (hydroxymethyl) aminomethane: pretreatment powder = 0.7:0.1:1; stirring at constant temperature of 35+/-3 ℃ for 30min after the addition is completed, then carrying out solid-liquid separation, and drying for 8h at the solid phase of 50 ℃ to obtain coated powder;
(4) In a nitrogen protection atmosphere, adding the coated powder into deionized water, and stirring to form an aqueous suspension, wherein the solid-liquid mass ratio of the coated powder added into the deionized water is solid/liquid=1:100; the water suspension is subjected to water bath constant temperature to 80+/-3 ℃ for heat preservation, and condensation and reflux are carried out; then adding 2-acrylamide-2-methylpropanesulfonic acid into the water suspension in a stirring state in a nitrogen atmosphere, keeping the temperature at 80+/-3 ℃ and stirring for 10min after the addition, and then adding an ammonium persulfate solution in the stirring state, wherein the mass percent of the ammonium persulfate in the ammonium persulfate solution is 3 percent, and the solvent is water; the mass ratio of the added mass of the 2-acrylamide-2-methylpropanesulfonic acid and ammonium persulfate solution to the mass ratio of the coated powder in the aqueous suspension is 2-acrylamide-2-methylpropanesulfonic acid: ammonium persulfate solution: coated powder = 2:0.4:1; after the charging is completed, the mixture is stirred for 5 hours at 80+/-3 ℃ in a nitrogen atmosphere, and the mixture is condensed and reflowed in the heat preservation process; and (3) after the heat preservation is finished, air cooling to normal temperature, solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30min to obtain the modified titanium dioxide powder.
Weighing the raw materials according to the parts by weight, uniformly mixing the raw materials to form mixed powder, adding water to adjust the water content to 25wt%, pressing into a blank, heating to 420 ℃ for presintering for 30min, heating to 650 ℃ at 15 ℃/min, preserving heat for 30min, heating to 1180 ℃ at 5 ℃/min, and sintering for 3h; cooling to 800 ℃ at 5 ℃/min after sintering is completed, preserving heat for 10min, cooling to 500 ℃ at 10 ℃/min, preserving heat for 10min, cooling to 150 ℃ at 15 ℃/min, taking out, and cooling to normal temperature to obtain the porcelain insulator and the test sample.
Example 3
The utility model provides a low temperature environment uses ageing-resistant porcelain insulator, includes porcelain insulator body, porcelain insulator body's raw materials include: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the raw materials are as follows in parts by weight: 50 parts of mullite powder, 7 parts of potassium feldspar powder, 8 parts of zirconia powder, 3 parts of barium carbonate powder, 15 parts of modified titanium dioxide powder, 3 parts of zinc oxide powder, 7 parts of magnesia powder and 26 parts of kaolin; each raw material is fine powder which is sieved by a 500-mesh screen. The preparation method of the modified titanium dioxide powder comprises the following steps:
(1) Preparing an aqueous solution of hexadecyl trimethyl ammonium bromide in a reaction kettle, and preparing an ethanol solution of n-butyl titanate and polyethylene glycol; in the aqueous solution of the cetyl trimethyl ammonium bromide, the concentration of the cetyl trimethyl ammonium bromide is 7g/L, and the solvent is water; in the ethanol solution of the n-butyl titanate and the polyethylene glycol, the concentration of the n-butyl titanate is 24g/L, the concentration of the polyethylene glycol is 11g/L, and the solvent is ethanol; stirring the aqueous solution of the cetyl trimethyl ammonium bromide, and then adding the aqueous solution of urea into the solution in a stirring state, wherein the concentration of the urea in the aqueous solution of urea is 16g/L; after the addition, the water bath is kept at a constant temperature of 50+/-5 ℃ until the temperature is reached, stirring the solution for 5min, and then adding the ethanol solution of the n-butyl titanate and the polyethylene glycol into the solution under the stirring state, wherein the volume ratio of the added volume of the ethanol solution of the urea, the n-butyl titanate and the polyethylene glycol to the volume ratio of the water solution of the cetyl trimethyl ammonium bromide is the water solution of urea: ethanol solution of n-butyl titanate and polyethylene glycol: aqueous solution of cetyltrimethylammonium bromide = 2:14:20; continuing to stir at the constant temperature of 50+/-5 ℃ for 5min after the charging is finished, sealing the reaction kettle, heating to 120+/-3 ℃ and preserving heat for 5h, and magnetically stirring in the heat preservation process; air cooling to normal temperature after heat preservation is finished, opening the reaction kettle, performing solid-liquid separation, washing a solid phase with deionized water for 3 times, drying for 30min at 60 ℃, and then placing in a muffle furnace at 550 ℃ for calcination for 6h to obtain titanium dioxide powder;
(2) Preparing an aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, wherein in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, the concentration of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 5g/200mL, and the titanium dioxide powder is dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to form a dispersion, and the solid-liquid mass ratio of the titanium dioxide powder dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is solid/liquid=1:100; the dispersion is subjected to water bath constant temperature to 65+/-3 ℃ and heat preservation, the dispersion is stirred for 10min, and then N-hydroxysuccinimide and L-lysine are added into the dispersion under the stirring state, wherein the mass ratio of the added N-hydroxysuccinimide to the L-lysine to the titanium dioxide powder in the dispersion is N-hydroxysuccinimide: l-lysine: titanium dioxide powder = 3:6:1; after the addition is finished, preserving the temperature for 4 hours at 65+/-3 ℃, then carrying out solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30 minutes to obtain pretreated powder;
(3) Dispersing the pretreatment powder in deionized water to form suspension, wherein the solid-liquid mass ratio of the pretreatment powder dispersed in the deionized water to form suspension is solid/liquid=1:100; the suspension is subjected to water bath constant temperature to 35+/-3 ℃ and heat preservation, the suspension is stirred for 5min after the suspension is heated, then dopamine is added into the suspension in a stirring state, the suspension is stirred for 10min at the constant temperature of 35+/-3 ℃ after the addition is finished, then tris (hydroxymethyl) aminomethane is added into the suspension in the stirring state, and the mass ratio of the addition mass of the dopamine and the tris (hydroxymethyl) aminomethane to the mass ratio of the pretreated powder in the suspension is dopamine: tris (hydroxymethyl) aminomethane: pretreatment powder = 0.7:0.2:1; stirring at constant temperature of 35+/-3 ℃ for 30min after the addition is completed, then carrying out solid-liquid separation, and drying for 8h at the solid phase of 50 ℃ to obtain coated powder;
(4) In a nitrogen protection atmosphere, adding the coated powder into deionized water, and stirring to form an aqueous suspension, wherein the solid-liquid mass ratio of the coated powder added into the deionized water is solid/liquid=1:100; the water suspension is subjected to water bath constant temperature to 80+/-3 ℃ for heat preservation, and condensation and reflux are carried out; then adding 2-acrylamide-2-methylpropanesulfonic acid into the water suspension in a stirring state in a nitrogen atmosphere, keeping the temperature at 80+/-3 ℃ and stirring for 10min after the addition, and then adding an ammonium persulfate solution in the stirring state, wherein the mass percent of the ammonium persulfate in the ammonium persulfate solution is 3 percent, and the solvent is water; the mass ratio of the added mass of the 2-acrylamide-2-methylpropanesulfonic acid and ammonium persulfate solution to the mass ratio of the coated powder in the aqueous suspension is 2-acrylamide-2-methylpropanesulfonic acid: ammonium persulfate solution: coated powder = 3:0.4:1; after the charging is completed, the mixture is stirred for 5 hours at 80+/-3 ℃ in a nitrogen atmosphere, and the mixture is condensed and reflowed in the heat preservation process; and (3) after the heat preservation is finished, air cooling to normal temperature, solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30min to obtain the modified titanium dioxide powder.
Weighing the raw materials according to the parts by weight, uniformly mixing the raw materials to form mixed powder, adding water to adjust the water content to 25wt%, pressing into a blank, heating to 420 ℃ for presintering for 30min, heating to 650 ℃ at 15 ℃/min, preserving heat for 30min, heating to 1180 ℃ at 5 ℃/min, and sintering for 3h; cooling to 800 ℃ at 5 ℃/min after sintering is completed, preserving heat for 10min, cooling to 500 ℃ at 10 ℃/min, preserving heat for 10min, cooling to 150 ℃ at 15 ℃/min, taking out, and cooling to normal temperature to obtain the porcelain insulator and the test sample.
Example 4
The utility model provides a low temperature environment uses ageing-resistant porcelain insulator, includes porcelain insulator body, porcelain insulator body's raw materials include: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the raw materials are as follows in parts by weight: 50 parts of mullite powder, 8 parts of potassium feldspar powder, 10 parts of zirconia powder, 4 parts of barium carbonate powder, 16 parts of modified titanium dioxide powder, 4 parts of zinc oxide powder, 10 parts of magnesia powder and 30 parts of kaolin; each raw material is fine powder which is sieved by a 500-mesh screen. The preparation method of the modified titanium dioxide powder comprises the following steps:
(1) Preparing an aqueous solution of hexadecyl trimethyl ammonium bromide in a reaction kettle, and preparing an ethanol solution of n-butyl titanate and polyethylene glycol; in the aqueous solution of the cetyl trimethyl ammonium bromide, the concentration of the cetyl trimethyl ammonium bromide is 8g/L, and the solvent is water; in the ethanol solution of the n-butyl titanate and the polyethylene glycol, the concentration of the n-butyl titanate is 25g/L, the concentration of the polyethylene glycol is 12g/L, and the solvent is ethanol; stirring the aqueous solution of the cetyl trimethyl ammonium bromide, and then adding the aqueous solution of urea into the solution in a stirring state, wherein the concentration of the urea in the aqueous solution of urea is 16g/L; after the addition, the water bath is kept at a constant temperature of 50+/-5 ℃ until the temperature is reached, stirring the solution for 5min, and then adding the ethanol solution of the n-butyl titanate and the polyethylene glycol into the solution under the stirring state, wherein the volume ratio of the added volume of the ethanol solution of the urea, the n-butyl titanate and the polyethylene glycol to the volume ratio of the water solution of the cetyl trimethyl ammonium bromide is the water solution of urea: ethanol solution of n-butyl titanate and polyethylene glycol: aqueous solution of cetyltrimethylammonium bromide = 2:15:20; continuing to stir at the constant temperature of 50+/-5 ℃ for 5min after the charging is finished, sealing the reaction kettle, heating to 120+/-3 ℃ and preserving heat for 5h, and magnetically stirring in the heat preservation process; air cooling to normal temperature after heat preservation is finished, opening the reaction kettle, performing solid-liquid separation, washing a solid phase with deionized water for 3 times, drying for 30min at 60 ℃, and then placing in a muffle furnace at 550 ℃ for calcination for 6h to obtain titanium dioxide powder;
(2) Preparing an aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, wherein the concentration of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 6g/200mL, and dispersing titanium dioxide powder in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to form a dispersion, wherein the mass ratio of solid to liquid in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is solid/liquid=1:100; the dispersion is subjected to water bath constant temperature to 65+/-3 ℃ and heat preservation, the dispersion is stirred for 10min, and then N-hydroxysuccinimide and L-lysine are added into the dispersion under the stirring state, wherein the mass ratio of the added N-hydroxysuccinimide to the L-lysine to the titanium dioxide powder in the dispersion is N-hydroxysuccinimide: l-lysine: titanium dioxide powder = 3:7:1; after the addition is finished, preserving the temperature for 4 hours at 65+/-3 ℃, then carrying out solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30 minutes to obtain pretreated powder;
(3) Dispersing the pretreatment powder in deionized water to form suspension, wherein the solid-liquid mass ratio of the pretreatment powder dispersed in the deionized water to form suspension is solid/liquid=1:100; the suspension is subjected to water bath constant temperature to 35+/-3 ℃ and heat preservation, the suspension is stirred for 5min after the suspension is heated, then dopamine is added into the suspension in a stirring state, the suspension is stirred for 10min at the constant temperature of 35+/-3 ℃ after the addition is finished, then tris (hydroxymethyl) aminomethane is added into the suspension in the stirring state, and the mass ratio of the addition mass of the dopamine and the tris (hydroxymethyl) aminomethane to the mass ratio of the pretreated powder in the suspension is dopamine: tris (hydroxymethyl) aminomethane: pretreatment powder = 0.8:0.2:1; stirring at constant temperature of 35+/-3 ℃ for 30min after the addition is completed, then carrying out solid-liquid separation, and drying for 8h at the solid phase of 50 ℃ to obtain coated powder;
(4) In a nitrogen protection atmosphere, adding the coated powder into deionized water, and stirring to form an aqueous suspension, wherein the solid-liquid mass ratio of the coated powder added into the deionized water is solid/liquid=1:100; the water suspension is subjected to water bath constant temperature to 80+/-3 ℃ for heat preservation, and condensation and reflux are carried out; then adding 2-acrylamide-2-methylpropanesulfonic acid into the water suspension in a stirring state in a nitrogen atmosphere, keeping the temperature at 80+/-3 ℃ and stirring for 10min after the addition, and then adding an ammonium persulfate solution in the stirring state, wherein the mass percent of the ammonium persulfate in the ammonium persulfate solution is 3 percent, and the solvent is water; the mass ratio of the added mass of the 2-acrylamide-2-methylpropanesulfonic acid and ammonium persulfate solution to the mass ratio of the coated powder in the aqueous suspension is 2-acrylamide-2-methylpropanesulfonic acid: ammonium persulfate solution: coated powder = 3:0.5:1; after the charging is completed, the mixture is stirred for 5 hours at 80+/-3 ℃ in a nitrogen atmosphere, and the mixture is condensed and reflowed in the heat preservation process; and (3) after the heat preservation is finished, air cooling to normal temperature, solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30min to obtain the modified titanium dioxide powder.
Weighing the raw materials according to the parts by weight, uniformly mixing the raw materials to form mixed powder, adding water to adjust the water content to 25wt%, pressing into a blank, heating to 420 ℃ for presintering for 30min, heating to 650 ℃ at 15 ℃/min, preserving heat for 30min, heating to 1180 ℃ at 5 ℃/min, and sintering for 3h; cooling to 800 ℃ at 5 ℃/min after sintering is completed, preserving heat for 10min, cooling to 500 ℃ at 10 ℃/min, preserving heat for 10min, cooling to 150 ℃ at 15 ℃/min, taking out, and cooling to normal temperature to obtain the porcelain insulator and the test sample.
Comparative example 1
A porcelain insulator for comparison, the porcelain insulator comprising: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the raw materials are as follows in parts by weight: 50 parts of mullite powder, 6 parts of potassium feldspar powder, 8 parts of zirconia powder, 3 parts of barium carbonate powder, 15 parts of modified titanium dioxide powder, 3 parts of zinc oxide powder, 5 parts of magnesia powder and 24 parts of kaolin; each raw material is fine powder which is sieved by a 500-mesh screen. The preparation method of the modified titanium dioxide powder comprises the following steps:
(1) Preparing an aqueous solution of hexadecyl trimethyl ammonium bromide in a reaction kettle, and preparing an ethanol solution of n-butyl titanate and polyethylene glycol; in the aqueous solution of the cetyl trimethyl ammonium bromide, the concentration of the cetyl trimethyl ammonium bromide is 7g/L, and the solvent is water; in the ethanol solution of the n-butyl titanate and the polyethylene glycol, the concentration of the n-butyl titanate is 22g/L, the concentration of the polyethylene glycol is 11g/L, and the solvent is ethanol; stirring the aqueous solution of the cetyl trimethyl ammonium bromide, and then adding the aqueous solution of urea into the solution in a stirring state, wherein the concentration of the urea in the aqueous solution of urea is 15g/L; after the addition, the water bath is kept at a constant temperature of 50+/-5 ℃ until the temperature is reached, stirring the solution for 5min, and then adding the ethanol solution of the n-butyl titanate and the polyethylene glycol into the solution under the stirring state, wherein the volume ratio of the added volume of the ethanol solution of the urea, the n-butyl titanate and the polyethylene glycol to the volume ratio of the water solution of the cetyl trimethyl ammonium bromide is the water solution of urea: ethanol solution of n-butyl titanate and polyethylene glycol: aqueous solution of cetyltrimethylammonium bromide = 1:12:20; continuing to stir at the constant temperature of 50+/-5 ℃ for 5min after the charging is finished, sealing the reaction kettle, heating to 120+/-3 ℃ and preserving heat for 5h, and magnetically stirring in the heat preservation process; air cooling to normal temperature after heat preservation is finished, opening the reaction kettle, performing solid-liquid separation, washing a solid phase with deionized water for 3 times, drying for 30min at 60 ℃, and then placing in a muffle furnace at 550 ℃ for calcination for 6h to obtain titanium dioxide powder;
(2) Dispersing the titanium dioxide powder in deionized water to form suspension, wherein the mass ratio of solid to liquid of the suspension formed by dispersing the titanium dioxide powder in the deionized water is (solid/liquid=1:100); the suspension is subjected to water bath constant temperature to 35+/-3 ℃ and heat preservation, the suspension is stirred for 5min after the suspension is heated, then dopamine is added into the suspension in a stirring state, the suspension is stirred for 10min at the constant temperature of 35+/-3 ℃ after the addition is finished, then tris (hydroxymethyl) aminomethane is added into the suspension in the stirring state, and the mass ratio of the added mass of the dopamine to the tris (hydroxymethyl) aminomethane to the mass ratio of titanium dioxide powder in the suspension is dopamine: tris (hydroxymethyl) aminomethane: titanium dioxide powder = 0.7:0.1:1; stirring at constant temperature of 35+/-3 ℃ for 30min after the addition is completed, then carrying out solid-liquid separation, and drying for 8h at the solid phase of 50 ℃ to obtain coated powder;
(3) In a nitrogen protection atmosphere, adding the coated powder into deionized water, and stirring to form an aqueous suspension, wherein the solid-liquid mass ratio of the coated powder added into the deionized water is solid/liquid=1:100; the water suspension is subjected to water bath constant temperature to 80+/-3 ℃ for heat preservation, and condensation and reflux are carried out; then adding 2-acrylamide-2-methylpropanesulfonic acid into the water suspension in a stirring state in a nitrogen atmosphere, keeping the temperature at 80+/-3 ℃ and stirring for 10min after the addition, and then adding an ammonium persulfate solution in the stirring state, wherein the mass percent of the ammonium persulfate in the ammonium persulfate solution is 3 percent, and the solvent is water; the mass ratio of the added mass of the 2-acrylamide-2-methylpropanesulfonic acid and ammonium persulfate solution to the mass ratio of the coated powder in the aqueous suspension is 2-acrylamide-2-methylpropanesulfonic acid: ammonium persulfate solution: coated powder = 2:0.4:1; after the charging is completed, the mixture is stirred for 5 hours at 80+/-3 ℃ in a nitrogen atmosphere, and the mixture is condensed and reflowed in the heat preservation process; and (3) after the heat preservation is finished, air cooling to normal temperature, solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30min to obtain the modified titanium dioxide powder of the comparative example.
Weighing the raw materials according to the parts by weight, uniformly mixing the raw materials to form mixed powder, adding water to adjust the water content to 25wt%, pressing into a blank, heating to 420 ℃ for presintering for 30min, heating to 650 ℃ at 15 ℃/min, preserving heat for 30min, heating to 1180 ℃ at 5 ℃/min, and sintering for 3h; cooling to 800 ℃ at 5 ℃/min after sintering is completed, preserving heat for 10min, cooling to 500 ℃ at 10 ℃/min, preserving heat for 10min, cooling to 150 ℃ at 15 ℃/min, taking out and air cooling to normal temperature, and obtaining the porcelain insulator and the test sample of the comparative example.
Comparative example 2
A porcelain insulator for comparison, the porcelain insulator comprising: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the raw materials are as follows in parts by weight: 50 parts of mullite powder, 6 parts of potassium feldspar powder, 8 parts of zirconia powder, 3 parts of barium carbonate powder, 15 parts of modified titanium dioxide powder, 3 parts of zinc oxide powder, 5 parts of magnesia powder and 24 parts of kaolin; each raw material is fine powder which is sieved by a 500-mesh screen. The preparation method of the modified titanium dioxide powder comprises the following steps:
(1) Preparing an aqueous solution of hexadecyl trimethyl ammonium bromide in a reaction kettle, and preparing an ethanol solution of n-butyl titanate and polyethylene glycol; in the aqueous solution of the cetyl trimethyl ammonium bromide, the concentration of the cetyl trimethyl ammonium bromide is 7g/L, and the solvent is water; in the ethanol solution of the n-butyl titanate and the polyethylene glycol, the concentration of the n-butyl titanate is 22g/L, the concentration of the polyethylene glycol is 11g/L, and the solvent is ethanol; stirring the aqueous solution of the cetyl trimethyl ammonium bromide, and then adding the aqueous solution of urea into the solution in a stirring state, wherein the concentration of the urea in the aqueous solution of urea is 15g/L; after the addition, the water bath is kept at a constant temperature of 50+/-5 ℃ until the temperature is reached, stirring the solution for 5min, and then adding the ethanol solution of the n-butyl titanate and the polyethylene glycol into the solution under the stirring state, wherein the volume ratio of the added volume of the ethanol solution of the urea, the n-butyl titanate and the polyethylene glycol to the volume ratio of the water solution of the cetyl trimethyl ammonium bromide is the water solution of urea: ethanol solution of n-butyl titanate and polyethylene glycol: aqueous solution of cetyltrimethylammonium bromide = 1:12:20; continuing to stir at the constant temperature of 50+/-5 ℃ for 5min after the charging is finished, sealing the reaction kettle, heating to 120+/-3 ℃ and preserving heat for 5h, and magnetically stirring in the heat preservation process; air cooling to normal temperature after heat preservation is finished, opening the reaction kettle, performing solid-liquid separation, washing a solid phase with deionized water for 3 times, drying for 30min at 60 ℃, and then placing in a muffle furnace at 550 ℃ for calcination for 6h to obtain titanium dioxide powder;
(2) Preparing an aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, wherein in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, the concentration of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 5g/200mL, and the titanium dioxide powder is dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to form a dispersion, and the solid-liquid mass ratio of the titanium dioxide powder dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is solid/liquid=1:100; the dispersion is subjected to water bath constant temperature to 65+/-3 ℃ and heat preservation, the dispersion is stirred for 10min, and then N-hydroxysuccinimide and L-lysine are added into the dispersion under the stirring state, wherein the mass ratio of the added N-hydroxysuccinimide to the L-lysine to the titanium dioxide powder in the dispersion is N-hydroxysuccinimide: l-lysine: titanium dioxide powder = 2:5:1; after the addition is finished, preserving the temperature for 4 hours at 65+/-3 ℃, then carrying out solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30 minutes to obtain pretreated powder;
(3) Adding the pretreatment powder into deionized water in a nitrogen protection atmosphere, and stirring to form an aqueous suspension, wherein the solid-liquid mass ratio of the pretreatment powder added into the deionized water is solid/liquid=1:100; the water suspension is subjected to water bath constant temperature to 80+/-3 ℃ for heat preservation, and condensation and reflux are carried out; then adding 2-acrylamide-2-methylpropanesulfonic acid into the water suspension in a stirring state in a nitrogen atmosphere, keeping the temperature at 80+/-3 ℃ and stirring for 10min after the addition, and then adding an ammonium persulfate solution in the stirring state, wherein the mass percent of the ammonium persulfate in the ammonium persulfate solution is 3 percent, and the solvent is water; the mass ratio of the added mass of the 2-acrylamide-2-methylpropanesulfonic acid and ammonium persulfate solution to the mass ratio of the pretreated powder in the aqueous suspension is 2-acrylamide-2-methylpropanesulfonic acid: ammonium persulfate solution: pretreatment powder = 2:0.4:1; after the charging is completed, the mixture is stirred for 5 hours at 80+/-3 ℃ in a nitrogen atmosphere, and the mixture is condensed and reflowed in the heat preservation process; and (3) after the heat preservation is finished, air cooling to normal temperature, solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30min to obtain the modified titanium dioxide powder of the comparative example.
Weighing the raw materials according to the parts by weight, uniformly mixing the raw materials to form mixed powder, adding water to adjust the water content to 25wt%, pressing into a blank, heating to 420 ℃ for presintering for 30min, heating to 650 ℃ at 15 ℃/min, preserving heat for 30min, heating to 1180 ℃ at 5 ℃/min, and sintering for 3h; cooling to 800 ℃ at 5 ℃/min after sintering is completed, preserving heat for 10min, cooling to 500 ℃ at 10 ℃/min, preserving heat for 10min, cooling to 150 ℃ at 15 ℃/min, taking out and air cooling to normal temperature, and obtaining the porcelain insulator and the test sample of the comparative example.
Comparative example 3
A porcelain insulator for comparison, the porcelain insulator comprising: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the raw materials are as follows in parts by weight: 50 parts of mullite powder, 6 parts of potassium feldspar powder, 8 parts of zirconia powder, 3 parts of barium carbonate powder, 15 parts of modified titanium dioxide powder, 3 parts of zinc oxide powder, 5 parts of magnesia powder and 24 parts of kaolin; each raw material is fine powder which is sieved by a 500-mesh screen. The preparation method of the modified titanium dioxide powder comprises the following steps:
(1) Preparing an aqueous solution of hexadecyl trimethyl ammonium bromide in a reaction kettle, and preparing an ethanol solution of n-butyl titanate and polyethylene glycol; in the aqueous solution of the cetyl trimethyl ammonium bromide, the concentration of the cetyl trimethyl ammonium bromide is 7g/L, and the solvent is water; in the ethanol solution of the n-butyl titanate and the polyethylene glycol, the concentration of the n-butyl titanate is 22g/L, the concentration of the polyethylene glycol is 11g/L, and the solvent is ethanol; stirring the aqueous solution of the cetyl trimethyl ammonium bromide, and then adding the aqueous solution of urea into the solution in a stirring state, wherein the concentration of the urea in the aqueous solution of urea is 15g/L; after the addition, the water bath is kept at a constant temperature of 50+/-5 ℃ until the temperature is reached, stirring the solution for 5min, and then adding the ethanol solution of the n-butyl titanate and the polyethylene glycol into the solution under the stirring state, wherein the volume ratio of the added volume of the ethanol solution of the urea, the n-butyl titanate and the polyethylene glycol to the volume ratio of the water solution of the cetyl trimethyl ammonium bromide is the water solution of urea: ethanol solution of n-butyl titanate and polyethylene glycol: aqueous solution of cetyltrimethylammonium bromide = 1:12:20; continuing to stir at the constant temperature of 50+/-5 ℃ for 5min after the charging is finished, sealing the reaction kettle, heating to 120+/-3 ℃ and preserving heat for 5h, and magnetically stirring in the heat preservation process; air cooling to normal temperature after heat preservation is finished, opening the reaction kettle, performing solid-liquid separation, washing a solid phase with deionized water for 3 times, drying for 30min at 60 ℃, and then placing in a muffle furnace at 550 ℃ for calcination for 6h to obtain titanium dioxide powder;
(2) Preparing an aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, wherein in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, the concentration of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 5g/200mL, and the titanium dioxide powder is dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to form a dispersion, and the solid-liquid mass ratio of the titanium dioxide powder dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is solid/liquid=1:100; the dispersion is subjected to water bath constant temperature to 65+/-3 ℃ and heat preservation, the dispersion is stirred for 10min, and then N-hydroxysuccinimide and L-lysine are added into the dispersion under the stirring state, wherein the mass ratio of the added N-hydroxysuccinimide to the L-lysine to the titanium dioxide powder in the dispersion is N-hydroxysuccinimide: l-lysine: titanium dioxide powder = 2:5:1; after the addition is finished, preserving the temperature for 4 hours at 65+/-3 ℃, then carrying out solid-liquid separation, washing the solid phase with deionized water for 3 times, and drying at 60 ℃ for 30 minutes to obtain pretreated powder;
(3) Dispersing the pretreatment powder in deionized water to form suspension, wherein the solid-liquid mass ratio of the pretreatment powder dispersed in the deionized water to form suspension is solid/liquid=1:100; the suspension is subjected to water bath constant temperature to 35+/-3 ℃ and heat preservation, the suspension is stirred for 5min after the suspension is heated, then dopamine is added into the suspension in a stirring state, the suspension is stirred for 10min at the constant temperature of 35+/-3 ℃ after the addition is finished, then tris (hydroxymethyl) aminomethane is added into the suspension in the stirring state, and the mass ratio of the addition mass of the dopamine and the tris (hydroxymethyl) aminomethane to the mass ratio of the pretreated powder in the suspension is dopamine: tris (hydroxymethyl) aminomethane: pretreatment powder = 0.7:0.1:1; stirring for 30min at the constant temperature of 35+/-3 ℃ after the addition is finished, then carrying out solid-liquid separation, and drying for 8h at the solid phase of 50 ℃ to obtain coated powder which is used as the modified titanium dioxide powder in the comparative example.
Weighing the raw materials according to the parts by weight, uniformly mixing the raw materials to form mixed powder, adding water to adjust the water content to 25wt%, pressing into a blank, heating to 420 ℃ for presintering for 30min, heating to 650 ℃ at 15 ℃/min, preserving heat for 30min, heating to 1180 ℃ at 5 ℃/min, and sintering for 3h; cooling to 800 ℃ at 5 ℃/min after sintering is completed, preserving heat for 10min, cooling to 500 ℃ at 10 ℃/min, preserving heat for 10min, cooling to 150 ℃ at 15 ℃/min, taking out and air cooling to normal temperature, and obtaining the porcelain insulator and the test sample of the comparative example.
Example 5
The test specimens prepared in the above examples and comparative examples were tested for tensile strength and freeze-thaw aging resistance, in which the tensile strength was conducted on a stretcher, the test parameters of each specimen were identical, the freeze-thaw aging resistance was obtained by repeating freeze-thawing of the specimen at-50 to 40℃for 60 times, and whether cracks were generated on the surface of the specimen was observed, and the results are shown in Table 1.
TABLE 1
| Test group | Tensile Strength/MPa | Freeze thawing resistance |
| Example 1 | 279 | No surface crack |
| Example 2 | 291 | No surface crack |
| Example 3 | 286 | No surface crack |
| Example 4 | 281 | No surface crack |
| Comparative example 1 | 232 | Small amount of cracks on the surface |
| Comparative example 2 | 218 | Small amount of cracks on the surface |
| Comparative example 3 | 224 | Small amount of cracks on the surface |
As shown in Table 1, the porcelain insulator body prepared by the method has good strength and freeze-thaw aging resistance, so that the porcelain insulator can be used in occasions with large temperature variation, low-temperature environments such as high-altitude and high-latitude areas and the like, low-temperature cracking and damage are not easy to occur, and the application range of the porcelain insulator is enlarged. As can be seen from comparative example 2 and each comparative example, the mechanical properties of the resulting insulator are significantly improved when compared with the incompletely modified powder by adding the powder treated by the modification process according to the present invention, and it is seen that the modification process has a great influence on the properties of the porcelain insulator, which is probably mainly due to the influence of the modification process on the particle distribution dispersibility and the inter-particle bonding strength.
The foregoing detailed description of the embodiments of the present invention will be provided to those skilled in the art, and the detailed description and the examples should not be construed as limiting the invention.
Claims (6)
1. The ageing-resistant porcelain insulator used in the low-temperature environment is characterized by comprising a porcelain insulator body, wherein the porcelain insulator body comprises the following raw materials: mullite powder, potassium feldspar powder, zirconia powder, barium carbonate powder, modified titanium dioxide powder, zinc oxide powder, magnesia powder and kaolin; the preparation method of the modified titanium dioxide powder comprises the following steps:
(1) Preparing an aqueous solution of hexadecyl trimethyl ammonium bromide in a reaction kettle, and preparing an ethanol solution of n-butyl titanate and polyethylene glycol; stirring the aqueous solution of cetyl trimethyl ammonium bromide, adding the aqueous solution of urea into the solution in a stirring state, keeping the temperature in a water bath to 50+/-5 ℃ after the addition, continuing stirring the solution for 5-6 min after the addition is completed, adding the ethanol solution of n-butyl titanate and polyethylene glycol into the solution in a stirring state, continuing to keep the temperature at 50+/-5 ℃ for 5-6 min after the addition is completed, sealing the reaction kettle, heating to 120+/-3 ℃, keeping the temperature for more than 5h, and magnetically stirring in the heat preservation process; air cooling to normal temperature after heat preservation is finished, opening the reaction kettle, performing solid-liquid separation, washing a solid phase with deionized water for more than 3 times, drying for more than 30min at 60 ℃, and then placing in a muffle furnace at 550 ℃ for calcination for more than 6h to obtain titanium dioxide powder;
(2) Preparing an aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, dispersing the titanium dioxide powder in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to form a dispersion, keeping the temperature of the dispersion at 65+/-3 ℃ in a water bath, stirring the dispersion for 10-15 min, adding N-hydroxysuccinimide and L-lysine into the dispersion in a stirring state, keeping the temperature at 65+/-3 ℃ for more than 4h after the addition is finished, performing solid-liquid separation, washing the solid phase with deionized water for more than 3 times, and drying the solid phase at 60 ℃ for more than 30min to obtain pretreated powder;
(3) Dispersing the pretreated powder in deionized water to form suspension, keeping the suspension at a constant temperature of 35+/-3 ℃ in a water bath, stirring the suspension for more than 5min after the suspension is heated, then adding dopamine into the suspension in a stirring state, stirring the suspension for more than 10min at a constant temperature of 35+/-3 ℃ after the addition is finished, then adding tris (hydroxymethyl) aminomethane into the suspension in a stirring state, stirring the suspension for more than 30min at a constant temperature of 35+/-3 ℃ after the addition is finished, then carrying out solid-liquid separation, and drying for more than 8h in a solid-phase 50 ℃ environment to obtain coated powder;
(4) Adding the coated powder into deionized water in a nitrogen protection atmosphere, stirring to form an aqueous suspension, carrying out water bath constant temperature to 80+/-3 ℃, carrying out heat preservation, and condensing and refluxing; then adding 2-acrylamide-2-methylpropanesulfonic acid into the water suspension under the stirring state in the nitrogen atmosphere, continuing to keep the temperature at 80+/-3 ℃ for stirring for more than 10 minutes after the addition, then adding ammonium persulfate solution under the stirring state, keeping the temperature at 80+/-3 ℃ for stirring for more than 5 hours in the nitrogen atmosphere after the addition is finished, and condensing and refluxing in the heat preservation process; and after the heat preservation is finished, air cooling is carried out to normal temperature, solid-liquid separation is carried out, the solid phase is washed by deionized water for more than 3 times, and the modified titanium dioxide powder is obtained after drying at 60 ℃ for more than 30 min.
2. The aging-resistant porcelain insulator used in a low-temperature environment according to claim 1, wherein the porcelain insulator body comprises the following raw materials in parts by weight: 50 parts of mullite powder, 5-8 parts of potassium feldspar powder, 6-10 parts of zirconia powder, 2-4 parts of barium carbonate powder, 14-16 parts of modified titanium dioxide powder, 2-4 parts of zinc oxide powder, 3-10 parts of magnesia powder and 20-30 parts of kaolin; each raw material is fine powder which is sieved by a 500-mesh screen.
3. The low-temperature environment-used aging-resistant porcelain insulator according to claim 1, wherein in the step (1), the concentration of the cetyltrimethylammonium bromide in the aqueous solution of the cetyltrimethylammonium bromide is 6-8 g/L, and the solvent is water; in the ethanol solution of the n-butyl titanate and the polyethylene glycol, the concentration of the n-butyl titanate is 20-25 g/L, the concentration of the polyethylene glycol is 10-12 g/L, and the solvent is ethanol; in the aqueous solution of urea, the concentration of the urea is 15-16 g/L; the volume ratio of the added volume of the aqueous solution of urea, the ethanol solution of the n-butyl titanate and the polyethylene glycol to the volume ratio of the aqueous solution of the cetyltrimethylammonium bromide is that of the aqueous solution of urea: ethanol solution of n-butyl titanate and polyethylene glycol: aqueous solution of cetyltrimethylammonium bromide=1-2:10-15:20.
4. The low temperature environment use aging-resistant porcelain insulator according to claim 1, wherein in the step (2), the concentration of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 4-6 g/200mL, and the solid-liquid mass ratio of the titanium dioxide powder dispersed in the aqueous solution of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is solid/liquid=1:100; the mass ratio of the added N-hydroxysuccinimide to the L-lysine to the titanium dioxide powder in the dispersion is N-hydroxysuccinimide: l-lysine: titanium dioxide powder = 2-3:4-7:1.
5. The low temperature environment-friendly aging-resistant porcelain insulator according to claim 1, wherein in the step (3), the pretreatment powder is dispersed in deionized water to form suspension, and the solid-liquid mass ratio is solid/liquid=1:100; the mass ratio of the added dopamine to the tris (hydroxymethyl) aminomethane to the pretreated powder in the suspension is dopamine: tris (hydroxymethyl) aminomethane: pretreatment powder=0.6 to 0.8:0.1 to 0.2:1.
6. The low temperature environment-friendly aging-resistant porcelain insulator according to claim 1, wherein in the step (4), the solid-liquid mass ratio of the coating powder added into deionized water is solid/liquid=1:100; the ammonium persulfate solution contains 3 mass percent of ammonium persulfate and water as a solvent; the mass ratio of the added mass of the 2-acrylamide-2-methylpropanesulfonic acid and ammonium persulfate solution to the mass ratio of the coated powder in the aqueous suspension is 2-acrylamide-2-methylpropanesulfonic acid: ammonium persulfate solution: coated powder = 2-3:0.3-0.5:1.
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