CN103965989A - Flame-retarded modifying method for flame-retarded solid lubricating material - Google Patents
Flame-retarded modifying method for flame-retarded solid lubricating material Download PDFInfo
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- CN103965989A CN103965989A CN201410186154.4A CN201410186154A CN103965989A CN 103965989 A CN103965989 A CN 103965989A CN 201410186154 A CN201410186154 A CN 201410186154A CN 103965989 A CN103965989 A CN 103965989A
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- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 80
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 80
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 80
- 239000003063 flame retardant Substances 0.000 claims abstract description 58
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000003094 microcapsule Substances 0.000 claims abstract description 46
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
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- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000008098 formaldehyde solution Substances 0.000 claims abstract description 10
- 239000000314 lubricant Substances 0.000 claims description 70
- 239000000203 mixture Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 229920000642 polymer Polymers 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000003756 stirring Methods 0.000 claims description 18
- 229940059574 pentaerithrityl Drugs 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- 229920005989 resin Polymers 0.000 claims description 10
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 9
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 9
- 235000021355 Stearic acid Nutrition 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 239000004519 grease Substances 0.000 claims description 9
- 238000009413 insulation Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 9
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 9
- 239000011118 polyvinyl acetate Substances 0.000 claims description 9
- 239000008117 stearic acid Substances 0.000 claims description 9
- 239000001117 sulphuric acid Substances 0.000 claims description 9
- 235000011149 sulphuric acid Nutrition 0.000 claims description 9
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 9
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 13
- 238000005461 lubrication Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 229920000877 Melamine resin Polymers 0.000 abstract 3
- 238000012423 maintenance Methods 0.000 abstract 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000011159 matrix material Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- -1 humidity Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
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- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
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- 230000005540 biological transmission Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- 239000000470 constituent Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000003137 locomotive effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
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- 230000008569 process Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
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- 235000019698 starch Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
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- Lubricants (AREA)
Abstract
The invention relates to a flame-retarded modifying method for a flame-retarded solid lubricating material. The method adds melamine formaldehyde resin microcapsule ammonium polyphosphate powder to a solid lubricating material to obtain the flame-retarded solid lubricating material. The method comprises the following steps: (1) adopting melamine to react with a formaldehyde solution to obtain a prepolymer, then dispersing the prepolymer into an ethanol solution containing ammonium polyphosphate, and controlling a reaction condition to form a layer of melamine formaldehyde resin on the surface of ammonium polyphosphate; (2) carrying out melt blending for dried microcapsule ammonium polyphosphate and pentaerythritol and the solid lubricating material to obtain a solid mixture; (3) carrying out hot-press forming on the solid mixture at the temperature of 140-150 DEG C. The method is simple in technology and is wide in source of materials, and the obtain material has a certain flame retardant characteristic and can be used for various mechanical lubrication needing maintenance.
Description
Technical field
The present invention relates to a kind of method for modifying flame of fire-retardant solid lubricant, belong to the technical field of fire retardant material.
Background technology
Solid lubricant can be for height temperature, high vacuum, severe radiation, and in the severe environment such as dust, humidity, seawater; Can under the envrionment conditions that can not use lubricating oil, use; Lightweight, volume is little, need sealing, hold-up vessel and liquid-supplying system unlike using lubricating oil; Workload and the expense of maintaining are alleviated.Various macromolecular materials all can serve as solid lubricant as tetrafluoroethylene, polyethylene, nylon, polyoxymethylene, polyphenylene sulfide etc., these macromolecular materials except using powder type as slip additive, be made into polymer-based composite lubricated material after generally all adding other solid lubrication auxiliary agents (as molybdenumdisulphide, graphite, metal-powder etc.) as base material.General polymer base material is all inflammable, in transport, use procedure, has potential safety hazard, and use range is also limited, and seldom reports through the polymer-based solid lubricant of novel flame-retardant of modification.Allowing macromolecular material have fire retardancy usual method is toward wherein adding flame-retardant additive.
In recent years, halogen-free flame retardants flame-retardant high-molecular had caused very large concern.Surging with global environmental protection cry, fire retardant environmental requirement day by day improves, and expansion type flame retardant belongs to the one of halogen-free flame retardants, has good application prospect.Expansion type flame retardant composition includes three kinds of components conventionally: acid source, carbon source (or char-forming agent), source of the gas.Material as acid source is generally mineral acid, for example ammonium polyphosphate (APP); Char-forming agent is generally polyol, for example tetramethylolmethane (PER), starch; Source of the gas is the material that can produce gas under heating condition, for example trimeric cyanamide (MEL), urea etc.The problem such as but most Intumscent Flame Retardant System all exists deliquescence and fire-retardant matrix phase capacitive is poor.For example, as the important component APP of the Intumscent Flame Retardant System deliquescence that easily absorbs water, the matrix of moving out, and poor with the consistency of organism matrix.Especially, during as the flame-retardant additive of solid lubricant, the poor consistency of APP and solid lubricant certainly will affect the flame retardant properties of solid lubricant after modification.Be applied in the problem of this existence in order to solve APP, improve its water resisting property and with matrix phase capacitive, conventionally adopt APP carried out to surface modification, for example adopt coupling agent and microencapsulation technology.Terpolycyantoamino-formaldehyde resin is widely used microcapsule capsule wall material.
Summary of the invention
For above-mentioned technical problem, the object of this invention is to provide a kind of method for modifying flame of solid lubricant, the method technique is simple.Compared with ammonium polyphosphate, microcapsule ammonium polyphosphate can improve the consistency of this and material significantly as fire-retardant filler, also can improve its flame retardant properties simultaneously.
For achieving the above object, the present invention is achieved by the following technical solutions:
The method for modifying flame of solid lubrication bar material, comprises the following steps:
(1) prepare melamino-formaldehyde performed polymer: the formaldehyde solution of trimeric cyanamide and 37% is joined in 500ml there-necked flask according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=8-10, and heating in water bath to 80 DEG C is also incubated 1h, and reaction process stirs all the time, finally makes melamino-formaldehyde performed polymer, forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) prepare microcapsule ammonium polyphosphate: 60g ammonium polyphosphate is distributed in 150ml ethanol, disperse the solution after finishing to join in there-necked flask, add the melamino-formaldehyde prepolymer solution making in step (1) simultaneously, dilute sulphuric acid regulates the PH=4-5 of mixture, heating in water bath mixture temperature to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filters, with distilled water wash, 105 DEG C dry after, obtain microcapsule ammonium polyphosphate powder;
(3) prepare fire-retardant solid lubricant
A, choose the microcapsule ammonium polyphosphate making in tetramethylolmethane, solid lubricant and step (2), raw material is mixed, obtain blend; Wherein, the shared mass percent of each component is: microcapsule ammonium polyphosphate 15～25%, solid lubricant 65～75% and tetramethylolmethane 5～10%; Described solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid;
B, the blend making in step a is mixed under molten state, obtain solid mixture; The processing condition of melting are: 140～150 DEG C of temperature, and rotating speed is 70～90rpm, the time is 10～30min;
C, the molten mixture making in step b is carried out to pressure bonding moulding, temperature is 140～150 DEG C, and pressure is 1～2MPa, and the time is 3～5min, obtains fire-retardant solid lubricant after cooling.
In described step (2), the solubleness of microcapsule ammonium polyphosphate is 0.0866g/100ml.
Beneficial effect of the present invention is as follows:
Uncoated ammonium polyphosphate is a kind of inorganic substance, poor with the natural consistency of solid lubricant that organic constituent is more, add between the easy water-absorption particle of ammonium polyphosphate powder itself and very easily reunite together, with solid lubricant mixing process in be not easy disperse, the fire-retardant solid lubricant transverse section obtaining can observe ammonium polyphosphate agglomeration produce white dot; In the present invention, coated by the organic outer rigid housing of one deck through coated ammonium polyphosphate surface, cause being difficult for the moisture absorption between particle and reunite, the significantly ammonium polyphosphate agglomeration of the inner nothing of fire retardant material obtaining after mixing with solid lubricant; The raising of microcapsule ammonium polyphosphate dispersity in solid lubricant, has also improved the flame retardant properties of system to a certain extent; Therefore the present invention adopts trimeric cyanamide and formaldehyde coated ammonium polyphosphate to make microcapsule ammonium polyphosphate, then the technique of hot pressing composite molding after microcapsule ammonium polyphosphate is mixed with solid lubricant, has environmental protection, simple, quick, the efficient feature of technique.
The flame retardant processing method of the solid lubricant that the present invention obtains is simple, and the ammonium polyphosphate that it adopts and tetramethylolmethane are all environmentally friendly fire retardant, in use can be to environment.Technique of the present invention is simple, and material source is extensive, and the material of gained has certain flame-retarding characteristic, can be for the power lubrication between wheel rim of locomotive.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of microcapsule ammonium polyphosphate;
Fig. 2 is that the product cross section making in original product solid lubricant, ammonium polyphosphate modified product and embodiment 1 amplifies comparison diagram;
Fig. 3 is the product cross section enlarged view making in embodiment 2;
Fig. 4 is the product cross section enlarged view making in embodiment 3;
Fig. 5 is the product cross section enlarged view making in embodiment 4;
Fig. 6 is the product cross section enlarged view making in embodiment 5;
Fig. 7 is the product cross section enlarged view making in embodiment 6;
Fig. 8 is the product cross section enlarged view making in embodiment 7.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
embodiment 1
The method for modifying flame of the fire-retardant solid profit of the present invention material, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: trimeric cyanamide and 37% formaldehyde solution join in 500ml there-necked flask according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=8, and heating in water bath to 80 DEG C is also incubated 1h, and reaction process stirs all the time, finally makes melamino-formaldehyde performed polymer, forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) prepare microcapsule ammonium polyphosphate: 60g ammonium polyphosphate is distributed in 150ml ethanol, disperse the solution after finishing to join in there-necked flask, add the melamino-formaldehyde prepolymer solution making in step (1) simultaneously, dilute sulphuric acid regulates the PH=4 of mixture, heating in water bath mixture temperature to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filters, with distilled water wash, 105 DEG C dry after, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0866g/100ml;
(3) prepare fire-retardant solid lubricant:
A, choose tetramethylolmethane 7.5%(Chemical Reagent Co., Ltd., Sinopharm Group by the shared mass percent of each component, following examples are identical), solid lubricant 70%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory self-control, following examples are identical) and step (2) in the microcapsule ammonium polyphosphate 22.5% that makes, raw material is mixed, obtain blend;
B, the blend making in step a is mixed under molten state, the processing condition of melting are: 140 DEG C of temperature, and rotating speed is 85rpm, the time is 15min, obtains solid mixture;
C, the solid mixture making in step b is carried out to pressure bonding moulding, temperature is 140 DEG C, and pressure is 1.5MPa, and the time is 3min, obtains fire-retardant solid lubricant after cooling.
The fire-retardant solid lubricant product obtaining in the present embodiment 1, according to GB T2046.2-2009, in the time of specimen size 4 mm × 10 mm × 150mm, its gained oxygen index is 29%.
embodiment 2
The method for modifying flame of the fire-retardant solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: the formaldehyde solution of trimeric cyanamide and 37% is joined in 500ml there-necked flask according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=9, and heating in water bath to 80 DEG C is also incubated 1h, and reaction process stirs all the time, finally makes melamino-formaldehyde performed polymer, forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) prepare microcapsule ammonium polyphosphate: 60g ammonium polyphosphate is distributed in 150ml ethanol, disperse the solution after finishing to join in there-necked flask, add the melamino-formaldehyde prepolymer solution making in step (1) simultaneously, dilute sulphuric acid regulates the PH=4.5 of mixture, heating in water bath mixture temperature to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filters, with distilled water wash, 105 DEG C dry after, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0850g/100ml;
(3) prepare fire-retardant solid lubricant:
A, by the shared mass percent of each component choose tetramethylolmethane 10%, solid lubricant 70%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory self-control, following examples are identical) and step (2) in the microcapsule ammonium polyphosphate 20% that makes, raw material is mixed, obtain blend;
B, the blend making in step a is mixed under molten state, the processing condition of melting are: 145 DEG C of temperature, and rotating speed is 75rpm, the time is 20min, obtains solid mixture;
C, the solid mixture making in step b is carried out to pressure bonding moulding, temperature is 145 DEG C, and pressure is 2MPa, and the time is 5min, obtains fire-retardant solid lubricant after cooling.
The fire-retardant solid lubricant product obtaining in the present embodiment 2, according to GB T2046.2-2009, in the time of specimen size 4 mm × 10 mm × 150mm, its gained oxygen index is 28.3%.
embodiment 3
The method for modifying flame of the fire-retardant solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: the formaldehyde solution of trimeric cyanamide and 37% is joined in 500ml there-necked flask according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=10, and heating in water bath to 80 DEG C is also incubated 1h, and reaction process stirs all the time, finally makes melamino-formaldehyde performed polymer, forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) prepare microcapsule ammonium polyphosphate: 60g ammonium polyphosphate is distributed in 150ml ethanol, disperse the solution after finishing to join in there-necked flask, add the melamino-formaldehyde prepolymer solution making in step (1) simultaneously, dilute sulphuric acid regulates the PH=5 of mixture, heating in water bath mixture temperature to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filters, with distilled water wash, 105 DEG C dry after, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0845g/100ml;
(3) prepare fire-retardant solid lubricant:
A, by the shared mass percent of each component choose tetramethylolmethane 12%, solid lubricant 70%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory self-control, following examples are identical) and step (2) in the microcapsule ammonium polyphosphate 18% that makes, raw material is mixed, obtain blend;
B, the blend making in step a is mixed under molten state, the processing condition of melting are: 150 DEG C of temperature, and rotating speed is 90rpm, the time is 30min, obtains solid mixture;
C, the solid mixture making in step b is carried out to pressure bonding moulding, temperature is 150 DEG C, and pressure is 1.5MPa, and the time is 5min, obtains fire-retardant solid lubricant after cooling.
The fire-retardant solid lubricant product obtaining in the present embodiment 3, according to GB T2046.2-2009, in the time of specimen size 4mm × 10mm × 150mm, its gained oxygen index is 28.4.
embodiment 4
The method for modifying flame of the fire-retardant solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: the formaldehyde solution of trimeric cyanamide and 37% is joined in 500ml there-necked flask according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=8.5, and heating in water bath to 80 DEG C is also incubated 1h, and reaction process stirs all the time, finally makes melamino-formaldehyde performed polymer, forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) prepare microcapsule ammonium polyphosphate: 60g ammonium polyphosphate is distributed in 150ml ethanol, disperse the solution after finishing to join in there-necked flask, add the melamino-formaldehyde prepolymer solution making in step (1) simultaneously, dilute sulphuric acid regulates the PH=4.2 of mixture, heating in water bath mixture temperature to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filters, with distilled water wash, 105 DEG C dry after, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0830g/100ml;
(3) prepare fire-retardant solid lubricant:
A, by the shared mass percent of each component choose tetramethylolmethane 15%, solid lubricant 67%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory self-control, following examples are identical) and step (2) in the microcapsule ammonium polyphosphate 18% that makes, raw material is mixed, obtain blend;
B, the blend making in step a is mixed under molten state, the processing condition of melting are: 148 DEG C of temperature, and rotating speed is 85rpm, the time is 15min, obtains solid mixture;
C, the molten mixture making in step b is carried out to pressure bonding moulding, temperature is 148 DEG C, and pressure is 2MPa, and the time is 5min, obtains fire-retardant solid lubricant after cooling.
The fire-retardant solid lubricant product obtaining in the present embodiment 4, according to GB T2046.2-2009, in the time of the mm × 150mm of specimen size 4mm × 10, its gained oxygen index is 29%.
embodiment 5
The method for modifying flame of the fire-retardant solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: the formaldehyde solution of trimeric cyanamide and 37% is joined in 500ml there-necked flask according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=9.5, and heating in water bath to 80 DEG C is also incubated 1h, and reaction process stirs all the time, finally makes melamino-formaldehyde performed polymer, forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) prepare microcapsule ammonium polyphosphate: 60g ammonium polyphosphate is distributed in 150ml ethanol, disperse the solution after finishing to join in there-necked flask, add the melamino-formaldehyde prepolymer solution making in step (1) simultaneously, dilute sulphuric acid regulates the PH=4.8 of mixture, heating in water bath mixture temperature to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filters, with distilled water wash, 105 DEG C dry after, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0836g/100ml;
(3) prepare fire-retardant solid lubricant:
A, by the shared mass percent of each component choose tetramethylolmethane 15%, solid lubricant 75%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory self-control, following examples are identical) and step (2) in the microcapsule ammonium polyphosphate 10% that makes, raw material is mixed, obtain blend;
B, the blend making in step a is mixed under molten state, the processing condition of melting are: 142 DEG C of temperature, and rotating speed is 70rpm, the time is 10min, obtains solid mixture;
C, the solid mixture making in step b is carried out to pressure bonding moulding, temperature is 142 DEG C, and pressure is 1MPa, and the time is 4min, obtains fire-retardant solid lubricant after cooling.
The fire-retardant solid lubricant product obtaining in the present embodiment 5, according to GB T2046.2-2009, in the time of the mm × 150mm of specimen size 4mm × 10, its gained oxygen index is 28.5%.
embodiment 6
The method for modifying flame of the fire-retardant solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: the formaldehyde solution of trimeric cyanamide and 37% is joined in 500ml there-necked flask according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=8.2, and heating in water bath to 80 DEG C is also incubated 1h, and reaction process stirs all the time, finally makes melamino-formaldehyde performed polymer, forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) prepare microcapsule ammonium polyphosphate: 60g ammonium polyphosphate is distributed in 150ml ethanol, disperse the solution after finishing to join in there-necked flask, add the melamino-formaldehyde prepolymer solution making in step (1) simultaneously, dilute sulphuric acid regulates the PH=4.5 of mixture, heating in water bath mixture temperature to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filters, with distilled water wash, 105 DEG C dry after, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0870g/100ml;
(3) prepare fire-retardant solid lubricant:
A, by the shared mass percent of each component choose tetramethylolmethane 5%, solid lubricant 70%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory self-control, following examples are identical) and step (2) in the microcapsule ammonium polyphosphate 25% that makes, raw material is mixed, obtain blend;
B, the blend making in step a is mixed under molten state, the processing condition of melting are: 146 DEG C of temperature, and rotating speed is 73rpm, the time is 25min, obtains solid mixture;
C, the solid mixture making in step b is carried out to pressure bonding moulding, temperature is 143 DEG C, and pressure is 1.2MPa, and the time is 3.5min, obtains fire-retardant solid lubricant after cooling.
The fire-retardant solid lubricant product obtaining in the present embodiment 6, according to GB T2046.2-2009, in the time of the mm × 150mm of specimen size 4mm × 10, its gained oxygen index is 28%.
embodiment 7
The method for modifying flame of the fire-retardant solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: the formaldehyde solution of trimeric cyanamide and 37% is joined in 500ml there-necked flask according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=9.7, and heating in water bath to 80 DEG C is also incubated 1h, and reaction process stirs all the time, finally makes melamino-formaldehyde performed polymer, forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) prepare microcapsule ammonium polyphosphate: 60g ammonium polyphosphate is distributed in 150ml ethanol, disperse the solution after finishing to join in there-necked flask, add the melamino-formaldehyde prepolymer solution making in step (1) simultaneously, dilute sulphuric acid regulates the PH=5 of mixture, heating in water bath mixture temperature to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filters, with distilled water wash, 105 DEG C dry after, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0845g/100ml;
(3) prepare fire-retardant solid lubricant:
A, by the shared mass percent of each component choose tetramethylolmethane 15%, solid lubricant 65%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory self-control, following examples are identical) and step (2) in the microcapsule ammonium polyphosphate 20% that makes, raw material is mixed, obtain blend;
B, the blend making in step a is mixed under molten state, the processing condition of melting are: 150 DEG C of temperature, and rotating speed is 90rpm, the time is 25min, obtains solid mixture;
C, the solid mixture making in step b is carried out to pressure bonding moulding, temperature is 150 DEG C, and pressure is 2MPa, and the time is 5min, obtains fire-retardant solid lubricant after cooling.
The fire-retardant solid lubricant product obtaining in the present embodiment 7, according to GB T2046.2-2009, in the time of the mm × 150mm of specimen size 4mm × 10, its gained oxygen index is 28.6%.
The cited each raw material of the present invention can be realized the present invention, the bound value of each raw material with and interval value can realize the present invention, the bound value of processing parameter of the present invention (as temperature, time etc.) with and interval value can realize the present invention, do not enumerate embodiment at this.
Above-described embodiment is only for the inventive concept of the present invention of explaining, but not restriction to rights protection of the present invention, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should fall into protection scope of the present invention.
Claims (2)
1. a method for modifying flame for fire-retardant solid lubricant, is characterized in that comprising the following steps: (1) prepares melamino-formaldehyde performed polymer: the formaldehyde solution of trimeric cyanamide and 37% is joined in 500ml there-necked flask according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=8-10, and heating in water bath to 80 DEG C is also incubated 1h, and reaction process stirs all the time, finally makes melamino-formaldehyde performed polymer, forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) prepare microcapsule ammonium polyphosphate: 60g ammonium polyphosphate is distributed in 150ml ethanol, disperse the solution after finishing to join in there-necked flask, add the melamino-formaldehyde prepolymer solution making in step (1) simultaneously, dilute sulphuric acid regulates the PH=4-5 of mixture, heating in water bath mixture temperature to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filters, with distilled water wash, 105 DEG C dry after, obtain microcapsule ammonium polyphosphate powder;
(3) prepare fire-retardant solid lubricant:
A, choose the microcapsule ammonium polyphosphate making in tetramethylolmethane, solid lubricant and step (2), raw material is mixed, obtain blend; Wherein, the shared mass percent of each component is: microcapsule ammonium polyphosphate 15～25%, solid lubricant 65～75% and tetramethylolmethane 5～15%; Described solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid;
B, the blend making in step a is mixed under molten state, obtain solid mixture; The processing condition of melting are: 140～150 DEG C of temperature, and rotating speed is 70～96rpm, the time is 10～30min;
C, the solid mixture making in step b is carried out to pressure bonding moulding, temperature is 140～150 DEG C, and pressure is 1～2MPa, and the time is 3～5min, obtains fire-retardant solid lubricant after cooling.
2. the method for modifying flame of fire-retardant solid lubricant as claimed in claim 1, is characterized in that: in described step (2), the solubleness of microcapsule ammonium polyphosphate is 0.0866g/100ml.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927060A (en) * | 2015-02-07 | 2015-09-23 | 南阳理工学院 | Intumescent flame retardant and preparation method thereof |
| CN108582397A (en) * | 2018-05-25 | 2018-09-28 | 裴文韬 | A kind of preparation method of water proof fire retardant wheat straw board |
| CN109776861A (en) * | 2019-02-14 | 2019-05-21 | 青岛科技大学 | It is a kind of using glycol-modified melamine resin as the expansion type flame retardant of carbon forming agent |
| CN112376123A (en) * | 2020-11-04 | 2021-02-19 | 湖南中泰特种装备有限责任公司 | Microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010174204A (en) * | 2009-02-02 | 2010-08-12 | Yuko Shoji Co | Lubricant composition for plunger |
| CN103483873A (en) * | 2013-09-27 | 2014-01-01 | 清远市普塞呋磷化学有限公司 | Preparation method of low-viscosity microcapsule-wrapped APP (ammonium polyphosphate) |
| CN103710116A (en) * | 2013-12-27 | 2014-04-09 | 杨毅 | Coating material for preventing engine crankshaft from being locked, and preparation method and application method of coating material |
-
2014
- 2014-05-06 CN CN201410186154.4A patent/CN103965989B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010174204A (en) * | 2009-02-02 | 2010-08-12 | Yuko Shoji Co | Lubricant composition for plunger |
| CN103483873A (en) * | 2013-09-27 | 2014-01-01 | 清远市普塞呋磷化学有限公司 | Preparation method of low-viscosity microcapsule-wrapped APP (ammonium polyphosphate) |
| CN103710116A (en) * | 2013-12-27 | 2014-04-09 | 杨毅 | Coating material for preventing engine crankshaft from being locked, and preparation method and application method of coating material |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927060A (en) * | 2015-02-07 | 2015-09-23 | 南阳理工学院 | Intumescent flame retardant and preparation method thereof |
| CN104927060B (en) * | 2015-02-07 | 2017-10-24 | 南阳理工学院 | A kind of expansion type flame retardant and preparation method thereof |
| CN108582397A (en) * | 2018-05-25 | 2018-09-28 | 裴文韬 | A kind of preparation method of water proof fire retardant wheat straw board |
| CN109776861A (en) * | 2019-02-14 | 2019-05-21 | 青岛科技大学 | It is a kind of using glycol-modified melamine resin as the expansion type flame retardant of carbon forming agent |
| CN112376123A (en) * | 2020-11-04 | 2021-02-19 | 湖南中泰特种装备有限责任公司 | Microencapsulated ammonium polyphosphate flame-retardant ultra-high molecular weight polyethylene fiber and preparation method thereof |
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Denomination of invention: Flame retardant modification method of a flame-retardant solid lubricating material Granted publication date: 20151028 Pledgee: Zhejiang Tailong Commercial Bank Co.,Ltd. Shaoxing Shengzhou Small and Micro Enterprise Sub branch Pledgor: ZHEJIANG BAOSHENG RAILWAY NEW MATERIALS TECHNOLOGY CO.,LTD. Registration number: Y2024980006250 |