CN103965989B - A kind of method for modifying flame of flame retarding solid lubricant - Google Patents
A kind of method for modifying flame of flame retarding solid lubricant Download PDFInfo
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- 239000000314 lubricant Substances 0.000 title claims abstract description 75
- 230000000979 retarding effect Effects 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 79
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- 239000008098 formaldehyde solution Substances 0.000 claims abstract description 10
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 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
- 206010013786 Dry skin Diseases 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
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- 238000001035 drying Methods 0.000 claims description 9
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- 230000001050 lubricating effect Effects 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
- 238000007493 shaping process Methods 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
- 239000000463 material Substances 0.000 abstract description 18
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- 239000003063 flame retardant Substances 0.000 description 20
- 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 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
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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
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
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- 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
Abstract
The present invention relates to a kind of method for modifying flame of flame retarding solid lubricant, the method refers to a kind ofly is added in solid lubricant to by terpolycyantoamino-formaldehyde resin micro encapsulation ammonium polyphosphate powder the method obtaining flame retarding solid lubricant, comprise the steps: that (1) adopts trimeric cyanamide and formaldehyde solution to be obtained by reacting performed polymer, again performed polymer is distributed in the ethanolic soln containing ammonium polyphosphate, controls reaction conditions and form one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface; (2) by dried microcapsule ammonium polyphosphate and tetramethylolmethane, solid lubricant carries out melt blending, obtains solid mixture.(3) by hot-forming under the condition of solid mixture 140-150 DEG C.Present invention process is simple, and material source is extensive, and the material of gained has certain flame-retarding characteristic, may be used for the various power lubrication needing to safeguard.
Description
Technical field
The present invention relates to a kind of method for modifying flame of flame retarding solid lubricant, belong to the technical field of fire retardant material.
Background technology
Solid lubricant may be used for high/low temperature, high vacuum, severe radiation, and in the severe environment such as dust, humidity, seawater; Can use under the envrionment conditions that can not use lubricating oil; Lightweight, volume is little, unlike use lubricating oil, need sealing, hold-up vessel and liquid-supplying system; Alleviate workload and the expense of maintaining.Various macromolecular material such as tetrafluoroethylene, polyethylene, nylon, polyoxymethylene, polyphenylene sulfide etc. all can serve as solid lubricant, these macromolecular materials, except in powder form as except slip additive, have been 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, and in transport, use procedure, there is potential safety hazard, 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 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 usually: acid source, carbon source (or char-forming agent), source of the gas.Material as acid source is generally mineral acid, such as ammonium polyphosphate (APP); Char-forming agent is generally polyol, such as tetramethylolmethane (PER), starch; Source of the gas is the material that can produce gas in a heated condition, such as trimeric cyanamide (MEL), urea etc.But all there is the problem such as deliquescence and fire-retardant matrix poor compatibility in most Intumscent Flame Retardant System.Such as, the important component APP as Intumscent Flame Retardant System easily absorbs water deliquescence, matrix of moving out, and poor with the consistency of organism matrix.During flame-retardant additive especially as solid lubricant, APP and the poor consistency of solid lubricant certainly will affect the flame retardant properties of modified solid lubricant.Be applied in this Problems existing to solve APP, improve its water resisting property and with matrix phase capacitive, usually adopt and surface modification carried out to APP, such as, 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: join in 500ml there-necked flask by the formaldehyde solution of trimeric cyanamide and 37% according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=8-10, and heating in water bath is to 80 DEG C and be incubated 1h, and reaction process stirs all the time, and final obtained melamino-formaldehyde performed polymer, namely forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) microcapsule ammonium polyphosphate is prepared: be distributed to by 60g ammonium polyphosphate in 150ml ethanol, solution after dispersion terminates joins in there-necked flask, add melamino-formaldehyde prepolymer solution obtained in step (1) simultaneously, dilute sulphuric acid regulates the PH=4-5 of mixture, heating in water bath mixture temperature is 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, after 105 DEG C of dryings, obtains microcapsule ammonium polyphosphate powder;
(3) flame retarding solid lubricant is prepared
A, to choose in tetramethylolmethane, solid lubricant and step (2) obtained microcapsule ammonium polyphosphate, raw material is mixed, obtains blend; Wherein, shared by each component, mass percent 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, blend obtained in step a to be mixed in the molten state, obtain solid mixture; The processing condition of melting are: temperature 140 ~ 150 DEG C, and rotating speed is 70 ~ 90rpm, and the time is 10 ~ 30min;
C, molten mixture obtained in step b to be carried out pressure bonding shaping, and temperature is 140 ~ 150 DEG C, and pressure is 1 ~ 2MPa, and the time is 3 ~ 5min, namely obtains flame retarding 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, the natural poor compatibility of the solid lubricant more with organic constituent, add that ammonium polyphosphate powder itself is easily very easily reunited together between water-absorption particle, with solid lubricant mixing process in be not easy to disperse, the flame retarding solid lubricant transverse section obtained 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 not easily moisture absorption reunion between particle, the fire retardant material obtained after mixing with solid lubricant is inner without obvious ammonium polyphosphate agglomeration; The raising of microcapsule ammonium polyphosphate dispersity in solid lubricant, also improves the flame retardant properties of system to a certain extent; Therefore the present invention adopts trimeric cyanamide and formaldehyde coated ammonium polyphosphate to obtain microcapsule ammonium polyphosphate, then the technique of hot pressing composite molding after being mixed with solid lubricant by microcapsule ammonium polyphosphate, 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 its ammonium polyphosphate adopted and tetramethylolmethane are all environmentally friendly fire retardant, in use can not to environment.Present invention process is simple, and material source is extensive, and the material of gained has certain flame-retarding characteristic, may be used for the power lubrication between wheel rim of locomotive.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of microcapsule ammonium polyphosphate;
Fig. 2 is that product cross section obtained in original product solid lubricant, ammonium polyphosphate modified product and embodiment 1 amplifies comparison diagram;
Fig. 3 is product enlarged cross sectional views obtained in embodiment 2;
Fig. 4 is product enlarged cross sectional views obtained in embodiment 3;
Fig. 5 is product enlarged cross sectional views obtained in embodiment 4;
Fig. 6 is product enlarged cross sectional views obtained in embodiment 5;
Fig. 7 is product enlarged cross sectional views obtained in embodiment 6;
Fig. 8 is product enlarged cross sectional views obtained 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 flame retarding solid profit material of the present invention, 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 is to 80 DEG C and be incubated 1h, and reaction process stirs all the time, and final obtained melamino-formaldehyde performed polymer, namely forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) microcapsule ammonium polyphosphate is prepared: be distributed to by 60g ammonium polyphosphate in 150ml ethanol, solution after dispersion terminates joins in there-necked flask, add melamino-formaldehyde prepolymer solution obtained in step (1) simultaneously, dilute sulphuric acid regulates the PH=4 of mixture, heating in water bath mixture temperature is to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filter, with distilled water wash, after 105 DEG C of dryings, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0866g/100ml;
(3) flame retarding solid lubricant is prepared:
A, choose tetramethylolmethane 7.5%(Chemical Reagent Co., Ltd., Sinopharm Group by mass percent shared by each component, following examples are identical), solid lubricant 70%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory is made by oneself, following examples are identical) and step (2) in obtained microcapsule ammonium polyphosphate 22.5%, raw material is mixed, obtains blend;
B, mixed in the molten state by blend obtained in step a, the processing condition of melting are: temperature 140 DEG C, and rotating speed is 85rpm, and the time is 15min, obtains solid mixture;
C, solid mixture obtained in step b to be carried out pressure bonding shaping, and temperature is 140 DEG C, and pressure is 1.5MPa, and the time is 3min, namely obtains flame retarding solid lubricant after cooling.
The flame retarding solid lubricant product obtained in the present embodiment 1, according to GB T2046.2-2009, as specimen size 4 mm × 10 mm × 150mm, its gained oxygen index is 29%.
embodiment 2
The method for modifying flame of flame retarding solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: join in 500ml there-necked flask by the formaldehyde solution of trimeric cyanamide and 37% according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=9, and heating in water bath is to 80 DEG C and be incubated 1h, and reaction process stirs all the time, and final obtained melamino-formaldehyde performed polymer, namely forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) microcapsule ammonium polyphosphate is prepared: be distributed to by 60g ammonium polyphosphate in 150ml ethanol, solution after dispersion terminates joins in there-necked flask, add melamino-formaldehyde prepolymer solution obtained in step (1) simultaneously, dilute sulphuric acid regulates the PH=4.5 of mixture, heating in water bath mixture temperature is to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filter, with distilled water wash, after 105 DEG C of dryings, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0850g/100ml;
(3) flame retarding solid lubricant is prepared:
A, choose tetramethylolmethane 10% by mass percent shared by each component, solid lubricant 70%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory is made by oneself, following examples are identical) and step (2) in obtained microcapsule ammonium polyphosphate 20%, raw material is mixed, obtains blend;
B, mixed in the molten state by blend obtained in step a, the processing condition of melting are: temperature 145 DEG C, and rotating speed is 75rpm, and the time is 20min, obtains solid mixture;
C, solid mixture obtained in step b to be carried out pressure bonding shaping, and temperature is 145 DEG C, and pressure is 2MPa, and the time is 5min, namely obtains flame retarding solid lubricant after cooling.
The flame retarding solid lubricant product obtained in the present embodiment 2, according to GB T2046.2-2009, as specimen size 4 mm × 10 mm × 150mm, its gained oxygen index is 28.3%.
embodiment 3
The method for modifying flame of flame retarding solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: join in 500ml there-necked flask by the formaldehyde solution of trimeric cyanamide and 37% according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=10, and heating in water bath is to 80 DEG C and be incubated 1h, and reaction process stirs all the time, and final obtained melamino-formaldehyde performed polymer, namely forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) microcapsule ammonium polyphosphate is prepared: be distributed to by 60g ammonium polyphosphate in 150ml ethanol, solution after dispersion terminates joins in there-necked flask, add melamino-formaldehyde prepolymer solution obtained in step (1) simultaneously, dilute sulphuric acid regulates the PH=5 of mixture, heating in water bath mixture temperature is to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filter, with distilled water wash, after 105 DEG C of dryings, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0845g/100ml;
(3) flame retarding solid lubricant is prepared:
A, choose tetramethylolmethane 12% by mass percent shared by each component, solid lubricant 70%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory is made by oneself, following examples are identical) and step (2) in obtained microcapsule ammonium polyphosphate 18%, raw material is mixed, obtains blend;
B, mixed in the molten state by blend obtained in step a, the processing condition of melting are: temperature 150 DEG C, and rotating speed is 90rpm, and the time is 30min, obtains solid mixture;
C, solid mixture obtained in step b to be carried out pressure bonding shaping, and temperature is 150 DEG C, and pressure is 1.5MPa, and the time is 5min, namely obtains flame retarding solid lubricant after cooling.
The flame retarding solid lubricant product obtained in the present embodiment 3, according to GB T2046.2-2009, as specimen size 4mm × 10mm × 150mm, its gained oxygen index is 28.4.
embodiment 4
The method for modifying flame of flame retarding solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: join in 500ml there-necked flask by the formaldehyde solution of trimeric cyanamide and 37% according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=8.5, and heating in water bath is to 80 DEG C and be incubated 1h, and reaction process stirs all the time, and final obtained melamino-formaldehyde performed polymer, namely forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) microcapsule ammonium polyphosphate is prepared: be distributed to by 60g ammonium polyphosphate in 150ml ethanol, solution after dispersion terminates joins in there-necked flask, add melamino-formaldehyde prepolymer solution obtained in step (1) simultaneously, dilute sulphuric acid regulates the PH=4.2 of mixture, heating in water bath mixture temperature is to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filter, with distilled water wash, after 105 DEG C of dryings, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0830g/100ml;
(3) flame retarding solid lubricant is prepared:
A, choose tetramethylolmethane 15% by mass percent shared by each component, solid lubricant 67%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory is made by oneself, following examples are identical) and step (2) in obtained microcapsule ammonium polyphosphate 18%, raw material is mixed, obtains blend;
B, mixed in the molten state by blend obtained in step a, the processing condition of melting are: temperature 148 DEG C, and rotating speed is 85rpm, and the time is 15min, obtains solid mixture;
C, molten mixture obtained in step b to be carried out pressure bonding shaping, and temperature is 148 DEG C, and pressure is 2MPa, and the time is 5min, namely obtains flame retarding solid lubricant after cooling.
The flame retarding solid lubricant product obtained in the present embodiment 4, according to GB T2046.2-2009, as specimen size 4mm × 10 mm × 150mm, its gained oxygen index is 29%.
embodiment 5
The method for modifying flame of flame retarding solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: join in 500ml there-necked flask by the formaldehyde solution of trimeric cyanamide and 37% according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=9.5, and heating in water bath is to 80 DEG C and be incubated 1h, and reaction process stirs all the time, and final obtained melamino-formaldehyde performed polymer, namely forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) microcapsule ammonium polyphosphate is prepared: be distributed to by 60g ammonium polyphosphate in 150ml ethanol, solution after dispersion terminates joins in there-necked flask, add melamino-formaldehyde prepolymer solution obtained in step (1) simultaneously, dilute sulphuric acid regulates the PH=4.8 of mixture, heating in water bath mixture temperature is to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filter, with distilled water wash, after 105 DEG C of dryings, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0836g/100ml;
(3) flame retarding solid lubricant is prepared:
A, choose tetramethylolmethane 15% by mass percent shared by each component, solid lubricant 75%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory is made by oneself, following examples are identical) and step (2) in obtained microcapsule ammonium polyphosphate 10%, raw material is mixed, obtains blend;
B, mixed in the molten state by blend obtained in step a, the processing condition of melting are: temperature 142 DEG C, and rotating speed is 70rpm, and the time is 10min, obtains solid mixture;
C, solid mixture obtained in step b to be carried out pressure bonding shaping, and temperature is 142 DEG C, and pressure is 1MPa, and the time is 4min, namely obtains flame retarding solid lubricant after cooling.
The flame retarding solid lubricant product obtained in the present embodiment 5, according to GB T2046.2-2009, as specimen size 4mm × 10 mm × 150mm, its gained oxygen index is 28.5%.
embodiment 6
The method for modifying flame of flame retarding solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: join in 500ml there-necked flask by the formaldehyde solution of trimeric cyanamide and 37% according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=8.2, and heating in water bath is to 80 DEG C and be incubated 1h, and reaction process stirs all the time, and final obtained melamino-formaldehyde performed polymer, namely forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) microcapsule ammonium polyphosphate is prepared: be distributed to by 60g ammonium polyphosphate in 150ml ethanol, solution after dispersion terminates joins in there-necked flask, add melamino-formaldehyde prepolymer solution obtained in step (1) simultaneously, dilute sulphuric acid regulates the PH=4.5 of mixture, heating in water bath mixture temperature is to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filter, with distilled water wash, after 105 DEG C of dryings, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0870g/100ml;
(3) flame retarding solid lubricant is prepared:
A, choose tetramethylolmethane 5% by mass percent shared by each component, solid lubricant 70%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory is made by oneself, following examples are identical) and step (2) in obtained microcapsule ammonium polyphosphate 25%, raw material is mixed, obtains blend;
B, mixed in the molten state by blend obtained in step a, the processing condition of melting are: temperature 146 DEG C, and rotating speed is 73rpm, and the time is 25min, obtains solid mixture;
C, solid mixture obtained in step b to be carried out pressure bonding shaping, and temperature is 143 DEG C, and pressure is 1.2MPa, and the time is 3.5min, namely obtains flame retarding solid lubricant after cooling.
The flame retarding solid lubricant product obtained in the present embodiment 6, according to GB T2046.2-2009, as specimen size 4mm × 10 mm × 150mm, its gained oxygen index is 28%.
embodiment 7
The method for modifying flame of flame retarding solid lubricant of the present invention, comprises the steps:
(1) prepare melamino-formaldehyde performed polymer: join in 500ml there-necked flask by the formaldehyde solution of trimeric cyanamide and 37% according to mol ratio 1:3, use 10%Na
2cO
3solution regulates mixture PH=9.7, and heating in water bath is to 80 DEG C and be incubated 1h, and reaction process stirs all the time, and final obtained melamino-formaldehyde performed polymer, namely forms one deck terpolycyantoamino-formaldehyde resin on ammonium polyphosphate surface;
(2) microcapsule ammonium polyphosphate is prepared: be distributed to by 60g ammonium polyphosphate in 150ml ethanol, solution after dispersion terminates joins in there-necked flask, add melamino-formaldehyde prepolymer solution obtained in step (1) simultaneously, dilute sulphuric acid regulates the PH=5 of mixture, heating in water bath mixture temperature is to 70 DEG C, insulation 2h, reaction process stirs all the time; Sample cool to room temperature after reacting completely, filter, with distilled water wash, after 105 DEG C of dryings, obtain microcapsule ammonium polyphosphate powder, the solubleness of microcapsule ammonium polyphosphate is 0.0845g/100ml;
(3) flame retarding solid lubricant is prepared:
A, choose tetramethylolmethane 15% by mass percent shared by each component, solid lubricant 65%(solid lubricant comprises polyvinyl acetate (PVA), lubricating grease, graphite, rosin and stearic acid, laboratory is made by oneself, following examples are identical) and step (2) in obtained microcapsule ammonium polyphosphate 20%, raw material is mixed, obtains blend;
B, mixed in the molten state by blend obtained in step a, the processing condition of melting are: temperature 150 DEG C, and rotating speed is 90rpm, and the time is 25min, obtains solid mixture;
C, solid mixture obtained in step b to be carried out pressure bonding shaping, and temperature is 150 DEG C, and pressure is 2MPa, and the time is 5min, namely obtains flame retarding solid lubricant after cooling.
The flame retarding solid lubricant product obtained in the present embodiment 7, according to GB T2046.2-2009, as specimen size 4mm × 10 mm × 150mm, its gained oxygen index is 28.6%.
Each raw material cited by the present invention can realize the present invention, bound value and its interval value of each raw material can realize the present invention, bound value and its interval value of present invention process parameter (as temperature, time etc.) can realize the present invention, do not enumerate embodiment at this.
Above-described embodiment only illustrates inventive concept of the present invention for explaining, but not the restriction to rights protection of the present invention, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should fall into protection scope of the present invention.
Claims (2)
1. the method for modifying flame of a flame retarding solid lubricant, it 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 the Na of 10%
2cO
3solution regulates mixture pH=8-10, and heating in water bath is to 80 DEG C and be incubated 1h, and reaction process stirs all the time, final obtained melamino-formaldehyde performed polymer;
(2) microcapsule ammonium polyphosphate is prepared: be distributed to by 60g ammonium polyphosphate in 150mL ethanol, solution after dispersion terminates joins in there-necked flask, add melamino-formaldehyde prepolymer solution obtained in step (1) simultaneously, dilute sulphuric acid regulates the pH=4-5 of mixture, heating in water bath mixture temperature is 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, after 105 DEG C of dryings, obtains microcapsule ammonium polyphosphate powder;
(3) flame retarding solid lubricant is prepared:
A, to choose in tetramethylolmethane, solid lubricant and step (2) obtained microcapsule ammonium polyphosphate, raw material is mixed, obtains blend; Wherein, shared by each component, mass percent 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, blend obtained in step a to be mixed in the molten state, obtain solid mixture; The processing condition of melting are: temperature 140 ~ 150 DEG C, and rotating speed is 70 ~ 96rpm, and the time is 10 ~ 30min;
C, solid mixture obtained in step b to be carried out pressure bonding shaping, and temperature is 140 ~ 150 DEG C, and pressure is 1 ~ 2MPa, and the time is 3 ~ 5min, namely obtains flame retarding solid lubricant after cooling.
2. the method for modifying flame of flame retarding 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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| CN108582397A (en) * | 2018-05-25 | 2018-09-28 | 裴文韬 | A kind of preparation method of water proof fire retardant wheat straw board |
| CN109776861B (en) * | 2019-02-14 | 2021-03-09 | 青岛科技大学 | Intumescent flame retardant taking ethylene glycol modified melamine formaldehyde resin as char 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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| 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 |
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| 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 |
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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 |