CN1290888C - High-temp.-resisting and insulated phenolic resin without dirt-water discharge and its preparation method - Google Patents
High-temp.-resisting and insulated phenolic resin without dirt-water discharge and its preparation method Download PDFInfo
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- CN1290888C CN1290888C CN 200410025827 CN200410025827A CN1290888C CN 1290888 C CN1290888 C CN 1290888C CN 200410025827 CN200410025827 CN 200410025827 CN 200410025827 A CN200410025827 A CN 200410025827A CN 1290888 C CN1290888 C CN 1290888C
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Abstract
The present invention relates to high temperature resistance and phenolic insulation phenolic resin, and a preparation method thereof, particularly a preparation method of phenolic resin without sewage discharge. The present invention is characterized in that phenol, solid paraformaldehyde, polysulfone, catalysts and electrical property assistant are used as raw materials to prepare the phenolic resin through copolycondensation. The high temperature resistance and phenolic insulation phenolic resin and the preparation method thereof have the characteristics: (1) the vacuum pumping is not needed and the preparation process has no sewage discharge; (2) the solid content is high; the solid content of the phenolic resin prepared by the water solution method used at present is ordinarily between 45% and 55%, but the solid content of the phenolic resin without sewage discharge is between 75% and 85%; the resin content is high and the solidification at a forming temperature is rapid; (3) compared with those of the traditional phenolic resin, the heat resistance and the insulating property of the obtained phenolic resin are better; the present invention creates necessary conditions for developing phenolic plastic and composite materials with good combination properties.
Description
Affiliated technical field: the present invention relates to high temperature resistant, the resol and preparation method thereof that insulate of a kind of without sewage discharge, mainly adopting phenol, solid polyformaldehyde, polysulfones, electrical property auxiliary agent is raw material, prepares by copolycondensation.
Background technology: at present,, need to adopt resol in a lot of fields.It can be used for making moulding compound, stratified plastics, porous plastics, cellularpiston, various matrix material, tackiness agent, coating, ion exchange resin etc.Phenoplast are cheap, raw material is easy to get, and over-all properties is better.
But domestic and international conventional novolak resin all adopts aqueous solution formaldehyde, needs the vacuum hydro-extraction discharging behind the synthetic production resin, contains free phenol, aldehyde, alcohol in the water, and the sewage pollution rivers and lakes of discharging destroy environment and ecology.In addition, contain hydrophilic phenolic group in the resol that the aqua-solution method of Shi Yonging makes now, solids content is generally between 45~55%.Not only easy moisture absorption but also not ageing-resistant influences electrical property, thermotolerance.
Summary of the invention: for avoiding the defective of prior art, the present invention proposes high temperature resistant, the resol and preparation method thereof that insulate of a kind of without sewage discharge, major advantage is not vacuumize without sewage discharge in the preparation process.Resol solids content height provided by the invention is between 75~85%.Its resin content height solidifies fast under mold temperature, and preparation technology is easier; In polycondensation,, the thermotolerance of resol and insulativity are improved by changing formula for a product and preparation technology.
The invention is characterized in: the component of material prescription is that 100 parts of phenol, 40~45 parts of solid polyformaldehydes, 10~18 parts of polysulfones, catalyzer are that 2~6 parts of magnesium hydroxides, electrical property auxiliary agent are 4~10 parts of polyimide.
The preparation method of above-mentioned resol is characterized in that: make by following steps:
A: at device agitator is arranged, with the phenol heating and melting, Heating temperature is about 50~60 ℃ in the reactor of reflux exchanger, and carries out in stirring;
B: add catalyzer, polysulfone resin, solid polyformaldehyde, be warming up to 80~90 ℃ of temperature of reaction with the speed of 1~5 ℃/min;
C: under above-mentioned temperature of reaction, react, obtain yellowly during, add the electrical property auxiliary agent to beige transparent glue.
Reaction obtains yellow to the gelation time control of beige transparent glue with reactant, and the gelation time of control reactant is 60~110s on 50 ± 1 ℃ set plate.
The characteristics of the resol of the present invention's development are need not vacuumize without sewage discharge in (1) preparation process; (2) solids content height, the resol that makes of the aqua-solution method of Shi Yonging now, solids content is generally between 45~55%, and the solids content of without sewage discharge resol is between 75~85%, its resin content height, solidify fast under mold temperature, preparation technology is easier, is suitable for scale operation; (3) resol good (table 1) that the heat-resisting and insulating property of gained resol are more traditional is for phenoplast, the matrix material of development high comprehensive performance have been created prerequisite.
Description of drawings:
Fig. 1: embodiment synoptic diagram
Embodiment:
Now in conjunction with the accompanying drawings the present invention is further described:
Umber among the embodiment 1:(embodiment is weight part)
1, at device agitator is arranged, add 50 parts of phenol in the reactor of reflux exchanger, make phenol heating and fusion under agitation.
2, in aforesaid liquid, add 2 parts of catalyzer, 6 parts of polysulfone resins, 22 parts of solid polyformaldehydes, be warming up to 80~90 ℃ with the speed of 1~5 ℃/min;
3, reacted 3.5 hours under above-mentioned temperature of reaction, recording gelation time on 50 ± 1 ℃ set plate is 60~110s, obtains yellow extremely beige transparent glue, and adds 4 parts of electrical property auxiliary agents.
Embodiment 2:
1, at device agitator is arranged, add 50 parts of phenol in the reactor of reflux exchanger, make phenol heating and fusion under agitation.
2, in above-mentioned solution, add 2.5 parts of catalyzer, 9 parts of polysulfone resins, 20 parts of solid polyformaldehydes, be warming up to 80~90 ℃ with the speed of 1~5 ℃/min;
3, reacted 4 hours under above-mentioned temperature of reaction, recording gelation time on 50 ± 1 ℃ set plate is 60~110s, obtains yellow extremely beige transparent glue, and adds 5 parts of electrical property auxiliary agents.
Prepared resol solids content is 75~85%, the infrared spectra comparison of this resin and aqua-solution method resol can be found out, the structural similitude of without sewage discharge resol and aqua-solution method resol, just without sewage discharge resol is not at 1050cm
-1The charateristic avsorption band of dimethylene ehter bond appears in the place.Without sewage discharge is high temperature resistant, the performance of insulation phenoplast for directional glass fiber strengthens for table 1.
Table 1 directional glass fiber enhancing without sewage discharge is high temperature resistant, insulation phenoplast performance index
Type | 1 | 2 |
Shock strength/KJm 2 | 200.39 | 283.66. |
Flexural strength/MPa | 616.06 | 821.12 |
Tensile strength/MPa | 310.76 | 866 |
Compressive strength/MPa | 144.42 | 250 |
Surface resistivity/Ω | 6.8×10 11 | 6.08×10 14 |
Volume specific resistance/Ω cm | 4.7×10 11 | 7.83×10 14 |
10 6The Hz tangent of the dielectric loss angle | 0.0432 | 0.0279 |
The 106Hz specific inductivity | 7.08 | 5.7 |
50Hz voltage breakdown/KVmm -1 | 13.11 | 19.02 |
Martin heat resistance/℃ | >280 | >310 |
Remarks: 1---unmodified phenoplast; 2---without sewage discharge is high temperature resistant, the insulation phenoplast.
Claims (3)
1, high temperature resistant, the insulation resol of a kind of without sewage discharge, it is characterized in that: the component of material prescription is phenol 100 mass parts, solid polyformaldehyde 40~45 mass parts, polysulfones 10~18 mass parts, magnesium hydroxide 2~6 mass parts, polyimide 4~10 mass parts.
2, a kind of realize the described without sewage discharge of claim 1 high temperature resistant, the insulation resol the preparation method, it is characterized in that:
A: at device agitator is arranged, with the phenol heating and melting, Heating temperature is about 50~60 ℃ in the reactor of reflux exchanger, and carries out in stirring;
B: add catalyzer, polysulfone resin, solid polyformaldehyde, be warming up to 80~90 ℃ of temperature of reaction with the speed of 1~5 ℃/min;
C: under above-mentioned temperature of reaction, react, obtain yellowly during, add the electrical property auxiliary agent to beige transparent glue.
3, preparation method according to claim 4 is characterized in that: reaction obtains yellow to the gelation time control of beige transparent glue with reactant, and the gelation time of control reactant is 60~110s on 50 ± 1 ℃ set plate.
Priority Applications (1)
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CN 200410025827 CN1290888C (en) | 2004-01-16 | 2004-01-16 | High-temp.-resisting and insulated phenolic resin without dirt-water discharge and its preparation method |
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CN 200410025827 CN1290888C (en) | 2004-01-16 | 2004-01-16 | High-temp.-resisting and insulated phenolic resin without dirt-water discharge and its preparation method |
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CN1640905A CN1640905A (en) | 2005-07-20 |
CN1290888C true CN1290888C (en) | 2006-12-20 |
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CN1978479B (en) * | 2005-11-29 | 2010-10-06 | 西北工业大学 | Naphthol-modified phenolic resin, and its preparing method |
CN112079977A (en) * | 2020-09-24 | 2020-12-15 | 新乡市炬能耐材有限公司 | Modified high-temperature-resistant and high-strength phenolic resin binder for precoated sand and preparation method thereof |
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