JP2012062411A - Screw seizure-preventing grease - Google Patents
Screw seizure-preventing grease Download PDFInfo
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- JP2012062411A JP2012062411A JP2010208289A JP2010208289A JP2012062411A JP 2012062411 A JP2012062411 A JP 2012062411A JP 2010208289 A JP2010208289 A JP 2010208289A JP 2010208289 A JP2010208289 A JP 2010208289A JP 2012062411 A JP2012062411 A JP 2012062411A
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- grease
- phosphate
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- 239000004519 grease Substances 0.000 title claims abstract description 112
- 239000007770 graphite material Substances 0.000 claims abstract description 47
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 40
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 39
- 239000010452 phosphate Substances 0.000 claims abstract description 39
- 239000007787 solid Substances 0.000 claims abstract description 27
- 239000000314 lubricant Substances 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 17
- 230000002265 prevention Effects 0.000 claims description 35
- 239000002245 particle Substances 0.000 claims description 30
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 238000005554 pickling Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000000573 anti-seizure effect Effects 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 2
- 230000001050 lubricating effect Effects 0.000 abstract description 2
- 206010010904 Convulsion Diseases 0.000 description 70
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 40
- 235000021317 phosphate Nutrition 0.000 description 32
- 229910002804 graphite Inorganic materials 0.000 description 27
- 239000010439 graphite Substances 0.000 description 27
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical class O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 23
- 238000000034 method Methods 0.000 description 20
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 15
- 229910052744 lithium Inorganic materials 0.000 description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 14
- 239000011575 calcium Substances 0.000 description 13
- 239000000344 soap Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 11
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 10
- 229960005069 calcium Drugs 0.000 description 10
- 229910052791 calcium Inorganic materials 0.000 description 10
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 8
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 8
- 238000005461 lubrication Methods 0.000 description 7
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- QQFLQYOOQVLGTQ-UHFFFAOYSA-L magnesium;dihydrogen phosphate Chemical compound [Mg+2].OP(O)([O-])=O.OP(O)([O-])=O QQFLQYOOQVLGTQ-UHFFFAOYSA-L 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 5
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 5
- 235000019785 monomagnesium phosphate Nutrition 0.000 description 5
- 229910000401 monomagnesium phosphate Inorganic materials 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000007743 anodising Methods 0.000 description 4
- 239000010687 lubricating oil Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 235000011009 potassium phosphates Nutrition 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000002562 thickening agent Substances 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000001506 calcium phosphate Substances 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 238000009832 plasma treatment Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical class [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 3
- -1 zinc phosphate compound Chemical class 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910021383 artificial graphite Inorganic materials 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000002542 deteriorative effect Effects 0.000 description 2
- 235000019700 dicalcium phosphate Nutrition 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005098 hot rolling Methods 0.000 description 2
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical class [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 2
- 239000004137 magnesium phosphate Substances 0.000 description 2
- 235000010994 magnesium phosphates Nutrition 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910000160 potassium phosphate Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- 235000011008 sodium phosphates Nutrition 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical class [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000004641 Diallyl-phthalate Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229930182556 Polyacetal Natural products 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 description 1
- 229940062672 calcium dihydrogen phosphate Drugs 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- IQBJFLXHQFMQRP-UHFFFAOYSA-K calcium;zinc;phosphate Chemical compound [Ca+2].[Zn+2].[O-]P([O-])([O-])=O IQBJFLXHQFMQRP-UHFFFAOYSA-K 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- RPUZVWKKWXPKIP-UHFFFAOYSA-H dialuminum;hydrogen phosphate Chemical compound [Al+3].[Al+3].OP([O-])([O-])=O.OP([O-])([O-])=O.OP([O-])([O-])=O RPUZVWKKWXPKIP-UHFFFAOYSA-H 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229920000840 ethylene tetrafluoroethylene copolymer Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000019691 monocalcium phosphate Nutrition 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001230 polyarylate Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229940065287 selenium compound Drugs 0.000 description 1
- 150000003343 selenium compounds Chemical class 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- WYPBVHPKMJYUEO-NBTZWHCOSA-M sodium;(9z,12z)-octadeca-9,12-dienoate Chemical compound [Na+].CCCCC\C=C/C\C=C/CCCCCCCC([O-])=O WYPBVHPKMJYUEO-NBTZWHCOSA-M 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
- 229940078499 tricalcium phosphate Drugs 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical class [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- LKCUKVWRIAZXDU-UHFFFAOYSA-L zinc;hydron;phosphate Chemical compound [Zn+2].OP([O-])([O-])=O LKCUKVWRIAZXDU-UHFFFAOYSA-L 0.000 description 1
Landscapes
- Lubricants (AREA)
Abstract
Description
本発明は、ネジ焼付き防止グリースに関し、さらに詳しくは、高温域での潤滑性能の劣化が少なく、耐焼付き性を向上させることができ、高温環境で使用される装置等に有用なネジ焼付き防止グリースに関するものである。 The present invention relates to a screw seizure prevention grease. More specifically, the seizure resistance is less deteriorated in a high temperature range, the seizure resistance can be improved, and the seizure is useful for an apparatus used in a high temperature environment. It relates to prevention grease.
ネジは機械要素として幅広く使用される重要な部品であり、通常ネジ面における潤滑は低速・高面圧となる上、高温から極低温までの使用環境の多様化および機械の高速化、高精度化など技術の進歩に伴い、過酷な潤滑条件となることが多い。一般に、ネジ焼付き防止グリースとしては油やグリースが使用されているが、特殊環境下においては固体潤滑剤がさらに含有されている。例えば、高温炉、加熱炉等に用いられるネジは、高温・高面圧下に長時間置かれるために焼付きや破損等を起こしやすいことが知られ、二硫化モリブデン(MoS2)含有ペースト等の固体潤滑剤を含んだネジ焼付き防止グリースが潤滑とともに焼付きや破損を防ぐ目的で使用されている。 Screws are important parts that are widely used as machine elements. Normally, the lubrication on the thread surface is low speed and high surface pressure, and the working environment is diversified from high temperature to extremely low temperature, and the speed and accuracy of the machine are increased. As technology advances, severe lubrication conditions often occur. Generally, oil or grease is used as the screw seizure prevention grease, but in a special environment, a solid lubricant is further contained. For example, screws used in high-temperature furnaces, heating furnaces, etc. are known to be susceptible to seizure and damage because they are placed under high temperature and high surface pressure for a long time, such as molybdenum disulfide (MoS 2 ) -containing pastes. Screw seizure prevention grease containing solid lubricant is used for the purpose of preventing seizure and breakage as well as lubrication.
しかしながら、600℃以上の高温下において使用できる高温用ネジ焼付き防止グリースはなく、例えば固体潤滑剤として使用されるMoS2は、600℃以上では充分な潤滑特性を発揮できなかった。 However, there is no high-temperature screw seizure-preventing grease that can be used at a high temperature of 600 ° C. or higher. For example, MoS 2 used as a solid lubricant cannot exhibit sufficient lubricating characteristics at 600 ° C. or higher.
一方、特許文献1には、500℃以上の熱間圧延プロセスで使用される熱間圧延ロールの摩耗および焼付き抑制するために、耐焼付き性や耐摩耗性に優れた固体潤滑剤を含有するグリースが提案されているが、耐摩耗性の向上にはMoS2およびグラファイト、耐焼付き性の向上にはリン酸カリウムおよび高分子ポリマーと言う様に、用途別にそれぞれ機能が異なる材料を混合して成るグリースであり、配合する固体潤滑剤の種類が多く、高コストであった。 On the other hand, Patent Document 1 contains a solid lubricant excellent in seizure resistance and wear resistance in order to suppress wear and seizure of a hot rolling roll used in a hot rolling process at 500 ° C. or higher. Although grease has been proposed, materials with different functions can be mixed depending on the application, such as MoS 2 and graphite for improving wear resistance and potassium phosphate and polymer for improving seizure resistance. There are many types of solid lubricants to be blended and the cost is high.
本発明は、このような状況下になされたもので、数種類の固体潤滑剤を使用することなく、高温域での潤滑性能の劣化が少なく、耐焼付き性を向上させることができ、高温環境で使用される装置等に有用なネジ焼付き防止グリースを提供することを目的とするものである。 The present invention has been made under such circumstances, and without using several kinds of solid lubricants, there is little deterioration of the lubrication performance in a high temperature range, and seizure resistance can be improved. An object of the present invention is to provide a screw seizure-preventing grease useful for a device to be used.
本発明者らは、前記目的を達成するために鋭意研究を重ねた結果、下記の知見を得た。
リン酸塩で表面が被覆されてなる黒鉛材料を、グリース基材と共に、特定の割合で含有する潤滑剤が、ネジ焼付き防止グリースとしてその目的に適合し得ることを見出した。本発明は、かかる知見に基づいて完成したものである。
As a result of intensive studies to achieve the above object, the present inventors have obtained the following knowledge.
It has been found that a lubricant containing a graphite material whose surface is coated with a phosphate in a specific ratio together with a grease base material can meet the purpose as a screw seizure prevention grease. The present invention has been completed based on such findings.
すなわち、本発明は、
(1) グリース基材と、固体潤滑剤とを必須成分とするネジ焼付き防止グリースであって、該固体潤滑剤として、リン酸塩で被覆されてなる黒鉛材料を5〜60質量%含むことを特徴とするネジ焼付き防止グリース、
(2) リン酸塩で被覆される前の黒鉛材料の平均粒径が5〜40μmである、上記(1)項に記載のネジ焼付き防止グリース、
(3) リン酸塩で被覆される前の黒鉛材料が、予め酸洗処理が施されたものである、上記(1)または(2)項に記載のネジ焼付き防止グリース、
(4) リン酸塩で被覆されてなる黒鉛材料が、黒鉛材料を、濃度0.5〜10質量%のリン酸塩水溶液で処理したものである、上記(1)〜(3)項のいずれか1項に記載のネジ焼付き防止グリース、
(5) リン酸塩水溶液100質量部当たり、黒鉛材料40〜50質量部を用いる、上記(4)項に記載のネジ焼付き防止グリース、および
(6) グリース基材と、固体潤滑剤とを必須成分とするネジ焼付き防止グリースを製造する方法であって、該固体潤滑剤として、リン酸塩で被覆されてなる黒鉛材料を5〜60質量%含有させることを特徴とするネジ焼付き防止グリースの製造方法、
を提供するものである。
That is, the present invention
(1) Screw seizure prevention grease comprising a grease base material and a solid lubricant as essential components, and containing 5 to 60% by mass of a graphite material coated with phosphate as the solid lubricant. Screw seizure prevention grease, characterized by
(2) The screw seizure-preventing grease according to (1) above, wherein the average particle size of the graphite material before being coated with phosphate is 5 to 40 μm,
(3) The screw seizure-preventing grease according to (1) or (2) above, wherein the graphite material before being coated with the phosphate has been previously pickled.
(4) Any of the above items (1) to (3), wherein the graphite material coated with phosphate is obtained by treating the graphite material with a phosphate aqueous solution having a concentration of 0.5 to 10% by mass. Or the screw seizure prevention grease according to claim 1,
(5) The screw seizure-preventing grease according to (4) above, wherein 40 to 50 parts by mass of the graphite material is used per 100 parts by mass of the phosphate aqueous solution, and (6) the grease base material and the solid lubricant. A method for producing a screw seizure prevention grease as an essential component, comprising 5 to 60% by mass of a graphite material coated with phosphate as the solid lubricant, Grease manufacturing method,
Is to provide.
本発明によれば、高温域での潤滑性能の劣化が少なく、耐焼付き性を向上させることができ、高温環境で使用される装置等に有用なネジ焼付き防止グリース、およびその製造方法を提供することができる。 According to the present invention, there is provided a screw seizure-preventing grease that is less susceptible to deterioration of lubrication performance in a high temperature range, can improve seizure resistance, and is useful for an apparatus used in a high temperature environment, and a manufacturing method thereof. can do.
本発明のネジ焼付き防止グリースは、グリース基材と、固体潤滑剤とを必須成分とするネジ焼付き防止グリースであって、該固体潤滑剤として、リン酸塩で被覆されてなる黒鉛材料を5〜60質量%含むことを特徴とする。
[グリース基材]
本発明のネジ焼付き防止グリースに用いられるグリース基材は、耐摩耗性や耐焼付き性に優れるリン酸塩で被覆された黒鉛材料を運搬するものであって、グリース基剤自身に耐摩耗性や耐焼付き性等の特性を期待するものではない。
The screw seizure prevention grease of the present invention is a screw seizure prevention grease comprising a grease base material and a solid lubricant as essential components, and a graphite material coated with phosphate is used as the solid lubricant. 5-60 mass% is contained, It is characterized by the above-mentioned.
[Grease base]
The grease base material used in the screw seizure prevention grease of the present invention conveys a graphite material coated with a phosphate having excellent wear resistance and seizure resistance, and the grease base itself has wear resistance. It does not expect characteristics such as seizure resistance.
したがって、ここで使用できるグリース基剤は種類にとらわれない。グリース基剤としては、例えば潤滑油を増ちょう剤で増ちょう化させたグリースを用いることができ、具体的には、潤滑油をカルシウム石けん、リチウム石けん、ナトリウム石けん、アルミニウム石けん、バリウム石けん等で増ちょう化させたカルシウムグリース、リチウムグリース、ナトリウムグリース、アルミニウムグリース、バリウムグリース等又はそれらの混合グリースが挙げられるが、これらに限定されるものではない。上記、潤滑油としては、従来から公知の鉱物油、エステル系合成油、炭化水素系合成油等の普通に使用されている潤滑油又はそれらの混合油等が挙げられるが、これらに限定されるものではない。望ましくは、リチウムグリースおよびカルシウムグリースであるが、さらに望ましくは、リチウムグリースが良い。リチウムグリースとしては、リチウム石けんグリースおよびリチウムコンプレックスグリースがあり、リチウム石けんグリースはリチウム石けんを増ちょう剤として使用し、リチウムコンプレックスグリースは高級脂肪酸と二塩基酸やホウ酸などとの複合リチウム石けんを増ちょう剤として使用する。また、カルシウムグリースも同様に、カルシウム石けんグリースおよびカルシウムコンプレックスグリースがあり、カルシウム石けんグリースはカルシウム石けんを増ちょう剤として使用し、カルシウムコンプレックスグリースは高級脂肪酸と酢酸のような低級脂肪酸のカルシウム複合石けんを増ちょう剤として使用するが、これらに限定されるものではない。 Therefore, the grease base that can be used here is not limited by type. As the grease base, for example, a grease obtained by thickening a lubricating oil with a thickener can be used. Specifically, the lubricating oil may be a calcium soap, a lithium soap, a sodium soap, an aluminum soap, a barium soap, or the like. Examples include, but are not limited to, calcium grease, lithium grease, sodium grease, aluminum grease, barium grease and the like, or a mixed grease thereof. Examples of the lubricating oil include conventionally used lubricating oils such as mineral oils, ester-based synthetic oils, hydrocarbon-based synthetic oils, and mixed oils thereof, but are not limited thereto. It is not a thing. Lithium grease and calcium grease are desirable, but lithium grease is more desirable. Lithium grease includes lithium soap grease and lithium complex grease. Lithium soap grease uses lithium soap as a thickener, and lithium complex grease increases complex lithium soap composed of higher fatty acid and dibasic acid or boric acid. Used as a fungicide. Similarly, calcium grease includes calcium soap grease and calcium complex grease.Calcium soap grease uses calcium soap as a thickener, and calcium complex grease contains calcium complex soap of higher fatty acids and lower fatty acids such as acetic acid. Although used as a thickener, it is not limited to these.
これらのグリース基材は1種を単独で用いてもよく、2種以上を組み合わせて用いてもよい。 These grease base materials may be used individually by 1 type, and may be used in combination of 2 or more type.
[リン酸塩で被覆されてなる黒鉛材料]
本発明のネジ焼付き防止グリースにおいて、前述したグリース基材と共に用いられるリン酸塩で被覆された黒鉛材料としては、原料の黒鉛材料をリン酸塩水溶液で接触処理してなるものを使用することができる。
[Graphite material coated with phosphate]
In the screw seizure prevention grease of the present invention, as the graphite material coated with the phosphate used together with the above-mentioned grease base material, a material obtained by contact treatment of the raw graphite material with a phosphate aqueous solution should be used. Can do.
原料の黒鉛材料としては、リン酸塩で被覆された黒鉛材料の耐熱性や耐酸化性を向上させる観点から、予め前処理を施したものを用いることができる。 From the viewpoint of improving the heat resistance and oxidation resistance of the graphite material coated with phosphate, a raw material graphite material that has been pretreated can be used.
前記前処理法としては、装置や操作の簡便さの面から湿式法が好ましいが、乾式法を採用することもできる。 As the pretreatment method, a wet method is preferable from the viewpoint of simplicity of apparatus and operation, but a dry method can also be adopted.
(湿式法による黒鉛材料の前処理)
湿式法による黒鉛材料の前処理としては、例えば酸洗処理や陽極酸化処理などを用いることができる。酸洗処理の場合、具体的には、酸として濃度85質量%以上のリン酸を用い、黒鉛材料1質量部に対して1〜5質量部程度の上記リン酸を加え、40〜60℃程度の温度で1〜10分間程度酸洗処理を行う。酸洗処理後の黒鉛材料は、充分に水洗したのち、リン酸塩による表面処理に供する。
(Pretreatment of graphite material by wet method)
As the pretreatment of the graphite material by the wet method, for example, pickling treatment or anodizing treatment can be used. In the case of the pickling treatment, specifically, phosphoric acid having a concentration of 85% by mass or more is used as the acid, and about 1 to 5 parts by mass of the phosphoric acid is added to 1 part by mass of the graphite material. Pickling treatment is performed at a temperature of about 1 to 10 minutes. The graphite material after the pickling treatment is sufficiently washed with water and then subjected to a surface treatment with phosphate.
この酸洗処理に用いる酸としては、機能面や環境面から、リン酸が好ましいが、硫酸や硝酸なども用いることができる。 As the acid used for the pickling treatment, phosphoric acid is preferable from the viewpoint of function and environment, but sulfuric acid, nitric acid and the like can also be used.
一方、陽極酸化処理の場合、具体的には硫酸浴などを用い、電極に1〜8V程度の電圧を印加し、浴温0〜10℃程度にて20〜50秒間程度陽極酸化処理を行う。陽極酸化処理後の黒鉛材料は充分に水洗したのち、リン酸塩による表面処理に供する。 On the other hand, in the case of anodizing, specifically, a sulfuric acid bath or the like is used, a voltage of about 1 to 8 V is applied to the electrode, and the anodizing is performed at a bath temperature of about 0 to 10 ° C. for about 20 to 50 seconds. The graphite material after the anodizing treatment is sufficiently washed and then subjected to a surface treatment with phosphate.
本発明においては、湿式法の中では装置や操作の簡便さの面から、酸洗処理が好ましい。 In the present invention, pickling treatment is preferable in the wet method from the viewpoint of simplicity of apparatus and operation.
(乾式法による黒鉛材料の前処理)
乾式法による黒鉛材料の前処理としては、例えば大気圧プラズマ処理、加熱処理、マイクロ波照射処理などを用いることができる。大気圧プラズマ処理の場合は、大気圧プラズマ発生装置を用いて、黒鉛材料にプラズマを照射することにより行われる。
(Pretreatment of graphite material by dry method)
As the pretreatment of the graphite material by the dry method, for example, atmospheric pressure plasma treatment, heat treatment, microwave irradiation treatment or the like can be used. In the case of atmospheric pressure plasma treatment, the graphite material is irradiated with plasma using an atmospheric pressure plasma generator.
プラズマ処理方法としては、黒鉛粒子にプラズマを照射し得る方法であれば、特に限定されない。望ましくは大気圧又は大気圧近傍の圧力下で、高周波電圧を対向する電極間に印加することにより放電プラズマを発生させる大気圧プラズマ方法が簡便で有効である。プラズマ発生源と黒鉛粒子との距離は50〜100mmが好ましく、50〜80mmがより好ましい。処理時間は、30〜180秒が好ましく、60〜120秒がより好ましい。黒鉛粒子はプラズマ照射時にエアー圧力で吹飛ばされるため、容器はプラズマが照射する部分のみ孔が開いた容器を使用することが好ましい。また、容器内に液体を満たし、その中に黒鉛粒子を浸漬させ、プラズマを照射することもできる。 The plasma processing method is not particularly limited as long as it is a method capable of irradiating the graphite particles with plasma. Desirably, an atmospheric pressure plasma method of generating discharge plasma by applying a high-frequency voltage between opposing electrodes under an atmospheric pressure or a pressure near atmospheric pressure is simple and effective. The distance between the plasma generation source and the graphite particles is preferably 50 to 100 mm, and more preferably 50 to 80 mm. The treatment time is preferably 30 to 180 seconds, and more preferably 60 to 120 seconds. Since graphite particles are blown off by air pressure during plasma irradiation, it is preferable to use a container in which a hole is opened only in a portion irradiated with plasma. Alternatively, the container can be filled with a liquid, and graphite particles can be immersed in the container and irradiated with plasma.
加熱処理の場合、具体的には、大気雰囲気下に、500〜800℃程度の温度にて、1〜5時間程度加熱処理する。 In the case of heat treatment, specifically, heat treatment is performed at a temperature of about 500 to 800 ° C. for about 1 to 5 hours in an air atmosphere.
一方、マイクロ波照射処理の場合、電子レンジを用いることができ、電子レンジを使用する際には、例えば550Wの電圧を印加し、10〜60秒間程度照射処理を行う。 On the other hand, in the case of the microwave irradiation treatment, a microwave oven can be used. When using the microwave oven, for example, a voltage of 550 W is applied and the irradiation treatment is performed for about 10 to 60 seconds.
本発明においては、乾式法の中では効果の点から、大気圧プラズマ処理が好ましい。
本発明においては、リン酸塩で被覆される黒鉛材料の平均粒径は、5〜40μmであることが好ましく、10〜30μmであることがより好ましい。
In the present invention, atmospheric pressure plasma treatment is preferable in the dry method from the viewpoint of effects.
In this invention, it is preferable that the average particle diameter of the graphite material coat | covered with a phosphate is 5-40 micrometers, and it is more preferable that it is 10-30 micrometers.
この平均粒径が5μm未満であると高温下で充分な耐焼付き性を発揮できず、ガス化し潤滑性が損われる。一方、40μmを超えるとネジ締結部に均一に入り込まない、もしくは、入り込んだとしても締め付けにより潰されてしまい、黒鉛表面が露出し、充分な潤滑性、耐焼付き性を発揮できない。 When the average particle size is less than 5 μm, sufficient seizure resistance cannot be exhibited at high temperatures, and gasification causes a loss of lubricity. On the other hand, when it exceeds 40 μm, it does not enter the screw fastening portion uniformly, or even if it enters, it is crushed by fastening, the graphite surface is exposed, and sufficient lubricity and seizure resistance cannot be exhibited.
(リン酸塩による黒鉛材料の被覆)
本発明において、原料の黒鉛材料としては、黒鉛材料をそのまま用いてもよいし、前述したように湿式法や乾式法により、前処理を施してから用いてもよいが、得られるリン酸塩で被覆された黒鉛材料の性能の観点から、予め前処理を施してなる黒鉛材料を用いることが好ましい。
(Coating of graphite material with phosphate)
In the present invention, as the raw material graphite material, the graphite material may be used as it is, or may be used after pretreatment by a wet method or a dry method as described above. From the viewpoint of the performance of the coated graphite material, it is preferable to use a graphite material that has been pretreated in advance.
〈リン酸塩〉
本発明において、黒鉛材料に被覆されるリン酸塩としては、その塩を構成する金属が、周期表(長周期型)1族、2族、12族または13族に属する金属であることが好ましい。具体的には1族に属するNa、K;2族に属するMg;12族に属するZn;13族に属するAl;などを好ましく挙げることができる。黒鉛材料の被覆に用いるリン酸塩としては、例えばリン酸アルミニウム類、リン酸マグネシウム類、リン酸カルシウム類、リン酸カリウム類、リン酸ナトリウム類およびリン酸亜鉛類の中から選ばれる少なくとも1種を挙げることができる。これらのリン酸塩は、水溶性やpHなどの観点から、リン酸水素塩が好ましい。
<Phosphate>
In the present invention, as the phosphate coated on the graphite material, the metal constituting the salt is preferably a metal belonging to Group 1, Group 2, Group 12, or Group 13 of the periodic table (long period type). . Specifically, Na and K belonging to Group 1, Mg belonging to Group 2, Zn belonging to Group 12, Al belonging to Group 13, and the like can be preferably exemplified. Examples of the phosphate used for coating the graphite material include at least one selected from aluminum phosphates, magnesium phosphates, calcium phosphates, potassium phosphates, sodium phosphates, and zinc phosphates. be able to. These phosphates are preferably hydrogen phosphates from the viewpoint of water solubility and pH.
例えば、リン酸アルミニウム類としては、リン酸二水素アルミニウム[Al(H2PO4)3]、リン酸水素アルミニウム[Al2(HPO4)3]が、リン酸マグネシウム類としては、リン酸水素マグネシウム[MgHPO4]、リン酸二水素マグネシウム[Mg(H2PO4)2]が、リン酸カルシウム類としては、リン酸二水素カルシウム[Ca(H2PO4)2]、リン酸水素カルシウム[CaHPO4]、リン酸三カルシウム[Ca3(PO4)2]、リン酸亜鉛カルシウム[Zn2Ca(PO4)2]が、リン酸カリウム類としては、リン酸二水素カリウム[KH2PO4]が、リン酸水素二カリウム[K2HPO4]が、リン酸ナトリウム類としては、リン酸二水素ナトリウム[NaH2PO4]、リン酸水素二ナトリウム[Na2HPO4]が、リン酸亜鉛類としては、リン酸水素亜鉛[ZnHPO4]、リン酸二水素亜鉛[Zn(H2PO4)2]が挙げられる。 For example, aluminum phosphates include aluminum dihydrogen phosphate [Al (H 2 PO 4 ) 3 ] and aluminum hydrogen phosphate [Al 2 (HPO 4 ) 3 ], and magnesium phosphates include hydrogen phosphate. Magnesium [MgHPO 4 ], magnesium dihydrogen phosphate [Mg (H 2 PO 4 ) 2 ], and calcium phosphates include calcium dihydrogen phosphate [Ca (H 2 PO 4 ) 2 ], calcium hydrogen phosphate [CaHPO] 4 ], tricalcium phosphate [Ca 3 (PO 4 ) 2 ], zinc calcium phosphate [Zn 2 Ca (PO 4 ) 2 ], potassium phosphates include potassium dihydrogen phosphate [KH 2 PO 4 ] is, dipotassium hydrogenphosphate [K 2 HPO 4]. Examples of sodium phosphates, sodium dihydrogen phosphate [NaH 2 O 4], disodium hydrogen phosphate [Na 2 HPO 4]. Examples of the zinc phosphate compound, hydrogen phosphate zinc [ZnHPO 4], and phosphoric acid dihydrogen zinc [Zn (H 2 PO 4) 2] It is done.
これらのリン酸水素塩は、1種を単独で用いてもよく、2種以上を組み合わせて用いてもよいが、これらの中で、性能の観点から、リン酸二水素アルミニウムおよびリン酸二水素マグネシウムが好ましく、特にリン酸二水素アルミニウムが好適である。 These hydrogen phosphate salts may be used alone or in combination of two or more thereof. Among these, from the viewpoint of performance, aluminum dihydrogen phosphate and dihydrogen phosphate Magnesium is preferred, and aluminum dihydrogen phosphate is particularly preferred.
(リン酸塩による黒鉛材料の被覆方法)
リン酸塩としては、好ましくはリン酸水素塩、特に好ましくはリン酸二水素アルミニウムおよび/またはリン酸二水素マグネシウムが用いられる。
(Method of coating graphite material with phosphate)
As the phosphate, hydrogen phosphate, preferably aluminum dihydrogen phosphate and / or magnesium dihydrogen phosphate is preferably used.
従って、本発明においては、リン酸塩として、特に好ましい上記リン酸二水素アルミニウムおよび/またはリン酸二水素マグネシウムを用いる。 Accordingly, in the present invention, particularly preferable aluminum dihydrogen phosphate and / or magnesium dihydrogen phosphate are used as the phosphate.
具体的にはまず、リン酸二水素アルミニウムおよび/またはリン酸二水素マグネシウム0.5〜10質量%を含む水溶液を調製する。この水溶液の調製において、リン酸二水素アルミニウムを用いる場合には、該水溶液の濃度は、好ましくは0.5〜10質量%、より好ましくは1〜5質量%である。一方、リン酸二水素マグネシウムを用いる場合には、該水溶液の濃度は、好ましくは0.5〜10質量%、より好ましくは0.5〜5質量%、さらに好ましくは1〜5質量%である。 Specifically, first, an aqueous solution containing 0.5 to 10% by mass of aluminum dihydrogen phosphate and / or magnesium dihydrogen phosphate is prepared. In the preparation of this aqueous solution, when aluminum dihydrogen phosphate is used, the concentration of the aqueous solution is preferably 0.5 to 10% by mass, more preferably 1 to 5% by mass. On the other hand, when using magnesium dihydrogen phosphate, the concentration of the aqueous solution is preferably 0.5 to 10% by mass, more preferably 0.5 to 5% by mass, and still more preferably 1 to 5% by mass. .
次に、このようにして調製されたリン酸二水素塩水溶液100質量部に対して、前述した黒鉛材料を40〜50質量部程度の割合で加え、例えば遊星ボールミルや回転翼式攪拌機などの攪拌混合を行う。簡易プロセスとして回転翼式が好ましい。攪拌時の水溶液温度は、10〜80℃程度、好ましくは25〜60℃、より好ましくは40〜50℃である。次いで、この混合物を、通常大気中にて乾燥後、解砕したのち、500〜800℃程度の温度にて100〜500Pa程度の減圧下、1〜5時間程度熱処理することにより、粒子表面に厚さ5〜500nm程度、好ましくは20〜100nmのリン酸塩被覆層を有する、黒鉛材料を得ることができる。 Next, with respect to 100 parts by mass of the dihydrogen phosphate aqueous solution thus prepared, the above-mentioned graphite material is added at a ratio of about 40 to 50 parts by mass, for example, stirring with a planetary ball mill or a rotary blade agitator. Mix. A rotary blade type is preferable as a simple process. The aqueous solution temperature at the time of stirring is about 10-80 degreeC, Preferably it is 25-60 degreeC, More preferably, it is 40-50 degreeC. Next, this mixture is usually dried in the air, crushed, and then heat-treated at a temperature of about 500 to 800 ° C. under a reduced pressure of about 100 to 500 Pa for about 1 to 5 hours, thereby thickening the particle surface. A graphite material having a phosphate coating layer of about 5 to 500 nm, preferably 20 to 100 nm can be obtained.
[ネジ焼付き防止グリースの組成]
本発明のネジ焼付き防止グリースは、必須成分として、前述したグリース基材と共に、リン酸塩で被覆されてなる黒鉛材料を含み、かつ前記のリン酸塩被覆黒鉛材料の含有量が5〜60質量%であることを要する。この含有量が5質量%未満では、所望の性能を有するネジ焼付き防止グリースが得られず、一方60質量%を超えるとネジ焼付き防止グリースが固形状になりやすく、ネジ面に部分的にしか塗布されず、その結果部分的に焼付きが生じる場合がある。好ましい含有量は10〜55質量%、より好ましくは30〜50質量%である。
[Composition of screw seizure prevention grease]
The screw seizure-preventing grease of the present invention contains, as an essential component, a graphite material coated with phosphate together with the above-described grease base material, and the content of the phosphate-coated graphite material is 5 to 60. It needs to be mass%. If the content is less than 5% by mass, a screw seizure prevention grease having the desired performance cannot be obtained. On the other hand, if the content exceeds 60% by mass, the screw seizure prevention grease tends to be solid and partially on the screw surface. Only the coating is applied, and as a result, partial seizure may occur. The preferred content is 10 to 55% by mass, more preferably 30 to 50% by mass.
(任意成分)
本発明のネジ焼付き防止グリースにおいては、前記必須成分以外に、本発明の効果が損なわれない範囲で必要に応じ、黒鉛、雲母、窒化ホウ素、二硫化モリブデン、ベントナイト、リン酸カリウム、高分子ポリマーなどを適宜量含んでもよい。
(Optional component)
In the screw seizure-preventing grease of the present invention, in addition to the above essential components, graphite, mica, boron nitride, molybdenum disulfide, bentonite, potassium phosphate, polymer, as necessary as long as the effects of the present invention are not impaired An appropriate amount of polymer or the like may be included.
前記高分子ポリマーとしては、例えばポリエチレン、ポリプロピレン、ポリエステル、ポリアセタール、ポリカーボネート、ポリアミド、ポリフェニレンオキシド、ポリスルホン、ポリアリレート、ポリフェニレンスルフィド、ABS樹脂、エチレン−四フッ化エチレン共重合体、ジアリルフタレート樹脂、フェノール樹脂、キトサン、ポリエチレングリコールなどが挙げられる。 Examples of the polymer include polyethylene, polypropylene, polyester, polyacetal, polycarbonate, polyamide, polyphenylene oxide, polysulfone, polyarylate, polyphenylene sulfide, ABS resin, ethylene-tetrafluoroethylene copolymer, diallyl phthalate resin, and phenol resin. , Chitosan, polyethylene glycol and the like.
また、添加剤として、分散液(グリセリン)、酸化防止剤(硫黄およびセレン化合物)、極圧剤(硫黄、塩素、リン)、錆止め剤(アミン類)、構造安定剤(ブチレン重合体)等を適宜量含んでもよい。
これらの任意成分は1種を単独で含んでいてもよく、2種以上を組み合わせて含んでいてもよい。
Additives such as dispersions (glycerin), antioxidants (sulfur and selenium compounds), extreme pressure agents (sulfur, chlorine, phosphorus), rust inhibitors (amines), structural stabilizers (butylene polymers), etc. An appropriate amount may be included.
These optional components may contain one kind alone, or may contain two or more kinds in combination.
本発明のネジ焼付き防止グリースは、数種類の固体潤滑剤を使用することなく、リン酸塩を被覆させてなる黒鉛材料を配合することで、高温域での潤滑性能を劣化させずに耐焼付き性を向上することができ、高温環境で使用される装置等に有用である。 The screw seizure prevention grease of the present invention is seizure resistant without deteriorating the lubrication performance in a high temperature range by blending a graphite material coated with phosphate without using several kinds of solid lubricants. This is useful for devices used in high temperature environments.
本発明はまた、グリース基材と、固体潤滑剤とを必須成分とするネジ焼付き防止グリースを製造する方法であって、該固体潤滑剤として、リン酸塩で被覆されてなる黒鉛材料を5〜60質量%含有させることを特徴とするネジ焼付き防止グリースの製造方法をも提供する。 The present invention is also a method for producing a screw seizure-preventing grease comprising a grease base material and a solid lubricant as essential components, wherein a graphite material coated with phosphate is used as the solid lubricant. Also provided is a method for producing a screw seizure-preventing grease characterized by containing ˜60 mass%.
次に、本発明を実施例により、さらに詳細に説明するが、本発明は、これらの例によってなんら限定されるものではない。
なお、各例で使用する原料黒鉛粒子の平均粒径及び各例で得られたネジ焼付き防止グリースの性能は、以下に示す方法に従って求めた。
EXAMPLES Next, although an Example demonstrates this invention further in detail, this invention is not limited at all by these examples.
The average particle diameter of the raw graphite particles used in each example and the performance of the screw seizure prevention grease obtained in each example were determined according to the following method.
(1)原料黒鉛粒子の平均粒径
原料黒鉛粒子の平均粒径は、レーザー回折式粒度分布測定装置[島津製作所製、機種名「SALD−2000A」]を用いて測定した。測定方法は、分散媒、分散剤として選定した水、リノール酸ナトリウム、エチルアルコール水溶液中に黒鉛粒子を投入し、超音波洗浄器で5分間均一に分散させた後、屈折率パラメータとして標準屈折率2.00−0.20iを選択し測定した。
(1) Average Particle Size of Raw Material Graphite Particles The average particle size of the raw material graphite particles was measured using a laser diffraction particle size distribution measuring device [manufactured by Shimadzu Corporation, model name “SALD-2000A”]. The measurement method is as follows. Graphite particles are placed in water, sodium linoleate, and ethyl alcohol aqueous solution selected as a dispersion medium and a dispersant, and uniformly dispersed for 5 minutes with an ultrasonic cleaner, and then the standard refractive index as a refractive index parameter. 2.00-0.20i was selected and measured.
(2)ネジ焼付き防止グリースの性能評価
ネジ焼付き防止グリースの耐焼付き性を評価するため、JIS B 1084「ネジ部品の締め付け試験方法」に準拠し、耐焼付き試験を実施した。
(2) Performance evaluation of screw seizure prevention grease In order to evaluate the seizure resistance of the screw seizure prevention grease, a seizure resistance test was performed in accordance with JIS B 1084 “Tightening test method for screw parts”.
ステンレス製(SUS304)のボルト、ナット及びワッシャー(M20)のネジ締結部やワッシャー部全体に均一にサンプルのネジ焼付き防止グリースを合計0.2g塗布し、穴(22mm)の開いたステンレス製ブロックに挟み込む。次に、ボルト一式をボルト締め付け試験機を用いて、回転数0.5rpmで締め付けトルクが392N・mになるまで締め付ける。締め付けトルクが392N・mになったら、速やかに反転(回転数0.5rpm)させ軸力が0Tになるまで緩める。このときの最大トルク値を測定しておく。この操作を3回繰返し、4度目に締め付けトルクが392N・mになったときにボルト一式を締め付け試験機から外す。締め付けた状態で各温度(300℃および800℃)の電気炉内に5時間放置する。 A stainless steel block with a hole (22 mm) with a total of 0.2 g of the sample screw anti-seizure grease applied uniformly to the entire screw fastening part and washer part of stainless steel (SUS304) bolts, nuts and washers (M20). Sandwiched between. Next, the set of bolts is tightened using a bolt tightening tester until the tightening torque reaches 392 N · m at a rotation speed of 0.5 rpm. When the tightening torque reaches 392 N · m, it is quickly reversed (rotation speed 0.5 rpm) and loosened until the axial force becomes 0T. The maximum torque value at this time is measured. This operation is repeated three times, and when the tightening torque reaches 392 N · m for the fourth time, the set of bolts is removed from the tightening tester. In a clamped state, it is left in an electric furnace at each temperature (300 ° C. and 800 ° C.) for 5 hours.
次に、室温まで冷却し、締め付け試験機に再度セットし、ボルトを緩める。加熱前の緩めトルクと加熱後の緩めトルクから耐焼付き性を評価した。ネジ締結部において、熱によるネジ焼付き防止グリースの材質への悪影響があると、焼付きが生じやすく、加熱前のトルクより加熱後のトルクが著しく大きくなる。 Next, cool to room temperature, set it again on the tightening tester, and loosen the bolts. The seizure resistance was evaluated from the loosening torque before heating and the loosening torque after heating. If there is an adverse effect on the material of the screw seizure prevention grease due to heat at the screw fastening portion, seizure is likely to occur, and the torque after heating becomes significantly larger than the torque before heating.
実施例1
<リン酸アルミニウムを被覆した黒鉛を配合したグリースの作製>
(1)リン酸アルミニウム被覆黒鉛の作製
第一リン酸アルミニウム(純正化学製リン酸二水素アルミニウム(一級)形状:粉末)を蒸留水に混ぜて溶解した水溶液(リン酸二水素アルミニウム濃度は1質量%)を作製した。次に、新日本テクノカーボン製人造黒鉛(平均粒径75μm)を45μm以下に分級した微細黒鉛粒子(平均粒径20μm)を出発原料に用いた。
前記水溶液100質量部に対し、上記微細黒鉛粒子42質量部を加え、回転翼式攪拌機[アズワン社製、機種名「PM−203」]により、温度50℃にて1時間攪拌した。
得られた混合物を大気中、110℃、24時間乾燥後、解砕したのち、真空中で800℃にて3時間熱処理を行った。熱処理後、乳鉢にて解砕し、粒子表面がリン酸二水素アルミニウムで被覆された黒鉛粉末を得た。
Example 1
<Preparation of grease containing graphite coated with aluminum phosphate>
(1) Preparation of aluminum phosphate-coated graphite Aqueous solution (primary aluminum dihydrogen phosphate (primary) shape: powder) mixed with distilled water and dissolved in aluminum phosphate (the concentration of aluminum dihydrogen phosphate is 1 mass) %). Next, fine graphite particles (average particle size 20 μm) obtained by classifying artificial graphite (average particle size 75 μm) made by Nippon Nippon Techno Carbon into 45 μm or less were used as starting materials.
42 parts by mass of the fine graphite particles were added to 100 parts by mass of the aqueous solution, and the mixture was stirred at a temperature of 50 ° C. for 1 hour with a rotary blade stirrer [manufactured by ASONE, model name “PM-203”].
The obtained mixture was dried in the atmosphere at 110 ° C. for 24 hours, crushed, and then heat-treated at 800 ° C. in vacuum for 3 hours. After the heat treatment, the powder was crushed in a mortar to obtain graphite powder whose particle surface was coated with aluminum dihydrogen phosphate.
(2)リン酸アルミニウム被覆黒鉛を配合したネジ焼付き防止グリースの作製
上記作製したリン酸アルミニウム被覆黒鉛粉末を株式会社エーゼット製リチウムグリースと質量比率で10:90になるよう混合した。混合方法は回転翼式攪拌機「PM−203」(前出)で100rpmで10分間攪拌を行い、目的とするリン酸アルミニウム被覆黒鉛粉末を配合したネジ焼付き防止グリースを作製した。
(2) Preparation of screw seizure prevention grease blended with aluminum phosphate-coated graphite The above-prepared aluminum phosphate-coated graphite powder was mixed with lithium grease manufactured by Azette Co., Ltd. at a mass ratio of 10:90. The mixing method was stirring with a rotary blade type stirrer “PM-203” (supra) at 100 rpm for 10 minutes to prepare a screw seizure-preventing grease containing the target aluminum phosphate-coated graphite powder.
実施例2〜4
実施例1(2)において、リン酸アルミニウム被覆黒鉛粉末とリチウムグリースの質量比率を30:70(実施例2)、40:60(実施例3)および55:45(実施例4)に変更した以外は、実施例1と同様な操作を行い、各リン酸アルミニウム被覆黒鉛粉末を配合したネジ焼付き防止グリースを作製した。
Examples 2-4
In Example 1 (2), the mass ratio of the aluminum phosphate-coated graphite powder and lithium grease was changed to 30:70 (Example 2), 40:60 (Example 3), and 55:45 (Example 4). Except for the above, the same operation as in Example 1 was performed to produce a screw seizure prevention grease containing each aluminum phosphate-coated graphite powder.
実施例5〜7
実施例3において、リン酸アルミニウム被覆黒鉛粉末作製時のリン酸アルミニウム水溶液濃度を0.5(実施例5)、5.0(実施例6)および10.0(実施例7)質量%に変更した以外は、実施例3と同様な操作を行い、リン酸アルミニウム被覆黒鉛粉末を配合したネジ焼付き防止グリースを作製した。
Examples 5-7
In Example 3, the concentration of the aqueous aluminum phosphate solution during preparation of the aluminum phosphate-coated graphite powder was changed to 0.5 (Example 5), 5.0 (Example 6), and 10.0 (Example 7) mass%. Except for the above, the same operation as in Example 3 was performed to produce a screw seizure-preventing grease containing aluminum phosphate-coated graphite powder.
実施例8
実施例3において、リン酸アルミニウムを被覆する前に、予め湿式法前処理として黒鉛表面を活性化させるために酸洗処理を施した以外は、実施例3と同様な操作を行い、リン酸アルミニウム被覆黒鉛粉末を配合したネジ焼付き防止グリースを作製した。
なお、上記酸洗処理は、以下に示す方法により行った。
Example 8
In Example 3, before the aluminum phosphate coating, the same operation as in Example 3 was performed except that a pickling process was performed in advance to activate the graphite surface as a wet process pretreatment. An anti-seizure grease containing coated graphite powder was prepared.
In addition, the said pickling process was performed by the method shown below.
原料の微細黒鉛粒子(平均粒径20μm)を、50℃に加熱したリン酸(和光純薬製特級、濃度85.0質量%以上)で5分間酸洗処理(黒鉛とリン酸の混合比率は質量比で1:8.5)し、蒸留水で水洗を2回実施し吸引ろ過を行うことにより、湿式法前処理黒鉛を得た。 Fine graphite particles (average particle size 20 μm) as raw materials are pickled with phosphoric acid (special grade made by Wako Pure Chemicals, concentration of 85.0% by mass or more) heated to 50 ° C. for 5 minutes (mixing ratio of graphite and phosphoric acid is Wet-processed graphite was obtained by carrying out suction filtration by carrying out water washing twice with distilled water by mass ratio 1: 8.5).
比較例1
<未処理黒鉛を配合したグリースの作製>
新日本テクノカーボン製人造黒鉛(平均粒径75μm)を45μm以下に分級した平均粒径20μmの微細黒鉛粒子をリチウムグリースと質量比率で40:60になるよう混合してネジ焼付き防止グリースを作製した。
Comparative Example 1
<Preparation of grease containing untreated graphite>
Produced grease to prevent screw seizure by mixing fine graphite particles with an average particle size of 20μm, which is obtained by classifying Nippon Nippon Technocarbon artificial graphite (average particle size 75μm) to 45μm or less to a mass ratio of 40:60. did.
比較例2
<二硫化モリブデンを配合したグリースの作製>
比較例1において、黒鉛を純正化学製二硫化モリブデン(平均粒径4μm)に変更した以外は、比較例1と同様にしてネジ焼付き防止グリースを作製した。
Comparative Example 2
<Preparation of grease containing molybdenum disulfide>
A screw seizure prevention grease was prepared in the same manner as in Comparative Example 1 except that the graphite was changed to Pure Chemical Molybdenum Disulfide (average particle size 4 μm) in Comparative Example 1.
比較例3
<固体潤滑剤を配合していないグリース>
株式会社エーゼット製リチウムグリース100%を使用して、ネジ焼付き防止グリースとした。
Comparative Example 3
<Grease not containing solid lubricant>
Screw grease seizure prevention grease was used using 100% lithium grease from Azette Co., Ltd.
比較例4
<リン酸アルミニウムを被覆した黒鉛を配合したグリースの作製>
実施例1(2)において、リン酸アルミニウム被覆黒鉛粉末とリチウムグリースの質量比率を70:30に変更した以外は、実施例1と同様な操作を行い、リン酸アルミニウム被覆黒鉛粉末を配合したネジ焼付き防止グリースを作製した。
Comparative Example 4
<Preparation of grease containing graphite coated with aluminum phosphate>
In Example 1 (2), a screw in which aluminum phosphate-coated graphite powder was blended was carried out in the same manner as in Example 1 except that the mass ratio of the aluminum phosphate-coated graphite powder and lithium grease was changed to 70:30. An anti-seizure grease was prepared.
実施例1〜8および比較例1〜4で作製されたネジ焼付き防止グリースについて、耐焼付性の評価を行った。その結果をネジ焼付き防止グリースの仕様と共に表1に示す。 The anti-seizure grease produced in Examples 1 to 8 and Comparative Examples 1 to 4 was evaluated for seizure resistance. The results are shown in Table 1 together with the specifications of the screw seizure prevention grease.
表1から、以下に示すことが分かる。
実施例1〜8のネジ焼付き防止グリースは、いずれも800℃の熱処理においても焼付きせず、トルクレンチで緩めることができた。特に、黒鉛粒子を予め湿式法前処理として酸洗処理を施して得られた実施例8のネジ焼付き防止グリースは、他の実施例のものに比べて性能が優れている。
From Table 1, it can be seen that:
The screw seizure prevention greases of Examples 1 to 8 were not seized even in the heat treatment at 800 ° C. and could be loosened with a torque wrench. In particular, the screw seizure-preventing grease of Example 8 obtained by subjecting graphite particles to a pickling treatment as a wet-type pretreatment in advance is superior in performance to the other examples.
これらに対し、比較例1、比較例3および比較例4は焼付きを起こし、ネジが緩まなかった。以上より、黒鉛粒子をリン酸アルミニウムで被覆することで、耐摩耗性と耐焼付き性の機能を持たせることができた。ネジ焼付き防止グリースの固体潤滑剤として、リン酸塩被覆黒鉛は有効であることが分った。 On the other hand, Comparative Example 1, Comparative Example 3 and Comparative Example 4 caused seizure and the screws did not loosen. From the above, it was possible to provide wear resistance and seizure resistance functions by coating the graphite particles with aluminum phosphate. It has been found that phosphate-coated graphite is effective as a solid lubricant for screw seizure prevention grease.
比較例2はグリース基材と二硫化モリブデンを含むネジ焼付き防止グリースであり、800℃での加熱後、緩めトルクは実施例1〜8のものよりも数値が高い。これにより600℃を超える温度では充分な潤滑性が発揮されないことが分かる。 Comparative Example 2 is a screw seizure prevention grease containing a grease base material and molybdenum disulfide, and after heating at 800 ° C., the loosening torque is higher than those of Examples 1-8. Thus, it can be seen that sufficient lubricity is not exhibited at temperatures exceeding 600 ° C.
比較例4は、グリース基材と、リン酸アルミニウム被覆黒鉛粉末70質量%を含むネジ焼付き防止グリースであり、この場合、被覆黒鉛粉末の含有量が70質量%と、60質量%を超えており、ネジ焼付き防止グリースが固形状となり、ネジ面に部分的にしか塗布されず、その結果部分的に焼付きが生じ、緩めトルクの数値が高くなる。 Comparative Example 4 is a grease seizure prevention grease containing a grease base material and 70% by mass of aluminum phosphate-coated graphite powder. In this case, the content of the coated graphite powder is 70% by mass and exceeds 60% by mass. Thus, the screw seizure prevention grease becomes solid and is only partially applied to the screw surface. As a result, seizure occurs partially, and the numerical value of the loosening torque increases.
本発明のネジ焼付き防止グリースは、数種類の固体潤滑剤を使用することなく、リン酸塩を被覆させてなる黒鉛材料を配合することで、高温域での潤滑性能を劣化させずに耐焼付き性を向上することができ、高温環境で使用される装置等に有用である。 The screw seizure prevention grease of the present invention is seizure resistant without deteriorating the lubrication performance in a high temperature range by blending a graphite material coated with phosphate without using several kinds of solid lubricants. This is useful for devices used in high temperature environments.
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CN115710527A (en) * | 2022-11-14 | 2023-02-24 | 二重(德阳)重型装备有限公司 | Fastener anti-seizure agent and preparation method thereof |
CN115710527B (en) * | 2022-11-14 | 2023-07-18 | 二重(德阳)重型装备有限公司 | Anti-seizing agent for fastener and preparation method thereof |
CN116676122A (en) * | 2023-05-30 | 2023-09-01 | 广州保赐利化工有限公司 | Bolt loosening agent and preparation method thereof |
CN116676122B (en) * | 2023-05-30 | 2023-12-22 | 广州保赐利化工有限公司 | Bolt loosening agent and preparation method thereof |
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