CN104086729A - Dimethyl benzene-modified phenolic resin and method thereof for preparing water cutting board - Google Patents
Dimethyl benzene-modified phenolic resin and method thereof for preparing water cutting board Download PDFInfo
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- CN104086729A CN104086729A CN201410353060.1A CN201410353060A CN104086729A CN 104086729 A CN104086729 A CN 104086729A CN 201410353060 A CN201410353060 A CN 201410353060A CN 104086729 A CN104086729 A CN 104086729A
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Abstract
The invention provides dimethyl benzene-modified phenolic resin and a method thereof for preparing a water cutting board. The dimethyl benzene-modified phenolic resin comprises the following components in parts by mass: 100 parts of dimethyl benzene formaldehyde resin, 50-100 parts of phenol, 0-30 parts of bisphenol A, 10-50 parts of paraformaldehyde, 0.1-2 parts of catalyst and 10-20 parts of deionized water. The dimethyl benzene-modified phenolic resin disclosed by the invention has the advantages of being low in curing temperature, quick in curing speed and short in curing time; the water cutting board prepared by using the dimethyl benzene-modified phenolic resin has excellent high temperature and humidity resistance and friction-abrasion resistance; and the water cutting board is used as the water cutting board for a finishing mill, service life of the water cutting board is greatly prolonged.
Description
Technical field
The present invention relates to phenolic resins field, relate in particular to a kind of dimethylbenzene modified phenolic resins and prepare the method for water discharging board.
Background technology
Because the phenolic hydroxyl group in resol is a strong polar group, easily water suction, and cause the physical strength of goods when high temperature wet condition is used greatly to decline.Be difficult to meet modern industry service requirements under high temperature wet condition to material.Therefore resol has been proposed to improve the requirement of high performance under thermotolerance and high temperature wet condition.
Conventionally in resol, introduce xylene formaldehyde resin structural unit (claim dimethylbenzene modified phenolic resins, or claim phenol modification xylene formaldehyde resin) to improve the high temperature resistant moist performance etc. of resol.Dimethylbenzene modified phenolic resins be by dimethylbenzene under an acidic catalyst effect, with the synthetic xylene formaldehyde resin of formaldehyde, then with phenol, formaldehyde reaction forms a kind of thermosetting resin.The hydrophobic structure of diformazan phenyl ring is introduced in the molecular structure of resol, make on the one hand content of phenolic hydroxyl groups in resol reduce, make on the other hand the phenolic hydroxyl group in resol structure be subject to cutting apart of dimethylbenzene and surround, greatly improved water tolerance and alkali resistance, physical strength also greatly improves simultaneously.Dimethylbenzene modified phenolic resins can with the compound matrix materials of preparing such as wood powder, cotton fibre, glass fibre, resurrection glass fibre, carbon fiber, can under high upsurge wet environment condition, use.But the phenolic resin curing temperature of dimethylbenzene modification is high, and curing speed is slow, and set time is long, its application is very limited; Therefore it is very necessary preparing the fast dimethylbenzene modified phenolic resins of a kind of curing speed.
A kind of high-molecular-weight thermoplastic xylene formaldehyde resin preparation method and application thereof are disclosed in prior art, this resin is almost oxygen-free, a kind of solid, can with the compound matrix material of preparing of wood powder, cotton fibre, glass fibre, carbon fiber and various auxiliary agent, but complicated process of preparation, harshness.In prior art, also disclose xylene formaldehyde resin, phenol, formaldehyde and under Catalyzed by Oxalic Acid condition, prepared the method for phenol modification xylene formaldehyde resin, but the solidification value of the phenol modification xylene formaldehyde resin that obtains is high, set time is long, and its application is restricted.Up to the present, the resol of dimethylbenzene modification and the prepared matrix material of fiber composite are not used as to the water discharging board of finishing mill.
Summary of the invention
In view of this, one aspect of the present invention provides a kind of dimethylbenzene modified phenolic resins, and this dimethylbenzene modified phenolic resins has advantages of that solidification value is low, curing speed is fast and set time is short.
For reaching this object, the present invention by the following technical solutions:
A dimethylbenzene modified phenolic resins, by mass parts, comprises following component:
For example, the mass parts of phenol can be 50 parts, 60 parts, 70 parts, 80 parts, 90 parts, 100 parts, the mass parts of dihydroxyphenyl propane can be 0 part, 5 parts, 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, the mass parts of paraformaldehyde can be 10 parts, 20 parts, 30 parts, 40 parts, 50 parts, the mass parts of catalyzer can be 0.1 part, 0.5 part, 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, and the mass parts of deionized water can be 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts.
A dimethylbenzene modified phenolic resins dipping solution that comprises above-mentioned dimethylbenzene modified phenolic resins, by mass parts, comprises following component:
Urotropine chemical name 1,3,5,7-tetra-aza-tricycles [3.3.1.1] decane, Chinese another name is for vulkacit H, Urotropinum, hexamine, amine are imitated, hexamethylenetetramine.
Preferably, solvent is mixtures a kind of in benzene, toluene, methyl alcohol, ethanol, butanone and methyl iso-butyl ketone (MIBK) or at least two kinds, and friction modifiers is mixtures a kind of in graphite, molybdenumdisulphide, aluminium sesquioxide, zirconium white, silicon carbide, magnesium oxide, calcium oxide or at least two kinds.
Preferably, solvent is the composition of toluene and methyl iso-butyl ketone (MIBK).
Preferably, catalyzer is hydrochloric acid, oxalic acid, tosic acid or mixture a kind of or at least two kinds.
The present invention provides on the other hand a kind of and uses above-mentioned dimethylbenzene modified phenolic resins to prepare the method for water discharging board, and the water discharging board that uses this preparation method to prepare has excellent high temperature resistant moist performance and wear resistance.
Use above-mentioned dimethylbenzene modified phenolic resins to prepare a method for water discharging board, comprise the following steps:
(1), by mass parts, 8～20 parts of 100 parts of dimethylbenzene modified phenolic resinss, 40～60 parts of solvents, 14 parts of urotropines, friction modifiers are fully mixed and make dimethylbenzene modified phenolic resins dipping solution;
(2) by dimethylbenzene modified phenolic resins dipping solution pre-soaking fiber cloth, drying equipment is dried to obtain prepreg;
(3) will after prepreg cutting, be arranged between two block plates, heating between thermocompressor two motor plates, pressurization are solidified prepreg, and then cooling, the demoulding, processing and heat treatment, machining obtain the modification phenolic resin-based matrix material water discharging board of dimethylbenzene.
For example, the mass parts of solvent can be 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, and friction modifiers can be 8 parts, 12 parts, 16 parts, 20 parts.
Preferably, prepare the method for dimethylbenzene modified phenolic resins as follows:
A. 0～30 part of 50～100 parts of phenol, dihydroxyphenyl propane and 10～20 parts of the deionized waters of 100 parts of the xylene formaldehyde resins of heating and melting, fusing are added in reactor, half amount that adds 0.1～3 part of catalyzer, and be slowly heated to boiling reflux, then at 130～150 ℃, keep 3～5 hours;
B. cooling, adds 10～50 parts of paraformaldehydes, then adds the catalyzer that remains second half amount, is warming up to 130～150 ℃, is incubated 1～3 hour;
C. decompression removes unreacted reactant and water obtain dimethylbenzene modified phenolic resins.
Preferably, in step (2), fiber is mixtures a kind of in glass fibre, resurrection glass fibre, silica fiber, ceramic fiber, cotton fibre and carbon fiber or at least two kinds, drying plant temperature is 110～130 ℃, the volatile matter of prepreg is not more than 3%, and in prepreg, the content of fiber is 50～55%.
Preferably, in step (3), thermocompressor Heating temperature is 180～200 ℃, moulding pressure 20～40MPa.
Compared with prior art, beneficial effect of the present invention is: dimethylbenzene modified phenolic resins provided by the invention, by mass parts, 100 parts of xylene formaldehyde resins, 50～100 parts of phenol, 0～30 part of dihydroxyphenyl propane, 10～50 parts of paraformaldehydes, 0.1～2 part of catalyzer, 10～20 parts of deionized waters.Dimethylbenzene modified phenolic resins of the present invention has advantages of that solidification value is low, curing speed is fast and set time is short, the water discharging board that uses this dimethylbenzene modified phenolic resins to prepare has excellent high temperature resistant moist performance and wear resistance, as finishing mill water discharging board, its work-ing life large leap ahead.
Embodiment
Further illustrate in conjunction with specific embodiments respectively technical scheme of the present invention below.
In following examples, related raw material is commercially available.
Embodiment 1: the dimethylbenzene modified phenolic resins of the present embodiment, by mass parts, comprises following component:
The preparation method of above-mentioned dimethylbenzene modified phenolic resins is as follows:
The hydrochloric acid that is 36% by 100 grams of xylene formaldehyde resins, 100 grams of phenol, 20 grams of dihydroxyphenyl propanes, 10 grams of deionized waters, 0.5 gram of concentration adds in reactor, slowly be heated to boiling reflux, keep 180～300 minutes, be cooled to below 90 ℃, adding 40 grams of concentration is 36.5% paraformaldehyde, add for the second time the hydrochloric acid that 0.5 gram of concentration is 36%, reheat to boiling reflux, react decompression dehydration 60～100 minutes, dehydration finishing temperature is 150 ℃, obtains solid dimethylbenzene modified phenolic resins.
In above-described embodiment, it is 0.18 gram that the hydrochloric acid that 0.5 gram of concentration is 36% obtains hydrochloric acid actual through converting, 40 grams of concentration be 36.5% paraformaldehyde actual be 14.6 grams.
The dimethylbenzene modified phenolic resins dipping solution of the present embodiment, by mass parts, comprises following component:
The preparation method of dimethylbenzene modified phenolic resins-glass cloth composite water discharging board of the present embodiment is as follows:
Taking the dimethylbenzene modified phenolic resins of 100 grams of above-mentioned preparations, 30 grams of toluene, 10 grams of methyl iso-butyl ketone (MIBK), 14 grams of urotropines, 10 grams of calcium oxide, 10 grams of magnesium oxide mixes and obtains a kind of dimethylbenzene modified phenolic resins dipping solution;
Glasscloth is put into above-mentioned dimethylbenzene modified phenolic resins dipping solution and carry out preimpregnation, spread is 49.5%, then entering drying plant dries, drying plant temperature is 125 ℃, drying time 10～20 minutes, the volatile matter of prepreg is not more than 3.0%, makes dimethylbenzene modified phenolic resins-glasscloth prepreg;
By the prepreg of above-mentioned oven dry through cutting, superimposed dress mould, be placed between the stainless steel plate of two polishings, being placed on temperature on thermocompressor is under heating, pressure 20～30MPa, to pressurize at 200 ℃, and keep with this understanding 1 hour, through hot-press solidifying, then cooling and demolding, aftertreatment obtain a kind of dimethylbenzene modified phenolic resins-glasscloth matrix material, through thermal treatment, machining, obtain dimethylbenzene modified phenolic resins-glass cloth composite water discharging board.
Embodiment 2: the difference of the present embodiment is, dimethylbenzene modified phenolic resins, by mass parts, comprises following component:
The preparation method of above-mentioned dimethylbenzene modified phenolic resins is as follows:
40 grams of xylene formaldehyde resins, 40 grams of phenol, 10 grams of deionized waters, the hydrochloric acid of 0.5 gram 36% are added in reactor, be slowly heated to boiling reflux, keep 180～300 minutes, be cooled to below 90 ℃, add 40 gram of 36.5% paraformaldehyde, add for the second time the hydrochloric acid of 0.5 gram 36%, reheat to boiling reflux, react 60～100 minutes, add 20 grams of dihydroxyphenyl propanes, reaction 30min, decompression dehydration, dehydration finishing temperature is 150 ℃, obtains solid dimethylbenzene modified phenolic resins.
In above-described embodiment, it is 0.18 gram that the hydrochloric acid that 0.5 gram of concentration is 36% obtains hydrochloric acid actual through converting, 40 grams of concentration be 36.5% paraformaldehyde actual be 14.6 grams.
Apart from the above, dimethylbenzene modified phenolic resins dipping solution and preparation method thereof is identical with embodiment 1.
Embodiment 3: the difference of the present embodiment is, making 0.36 part of hydrochloric acid into toluenesulphonic acids alcohol is 0.25 part, by 0.5 gram of concentration, is that 36% hydrochloric acid changes the tosic acid alcoholic solution that 2.5 grams of concentration are 5% into, and in addition other is identical with embodiment 1.
In above-described embodiment, the tosic acid alcoholic solution that 2.5 grams of concentration is 5% is actual through conversion tosic acid alcohol is 0.125g.
Embodiment 4: the dimethylbenzene modified phenolic resins of the present embodiment, by mass parts, comprises following component:
The preparation method of above-mentioned dimethylbenzene modified phenolic resins is as follows:
The tosic acid alcoholic solution that is 5% by 100 grams of xylene formaldehyde resins, 100 grams of phenol, 10 grams of deionized waters, 2.5 grams of concentration adds in reactor, slowly be heated to 135～150 ℃, keep 180～300 minutes, be cooled to below 80 ℃, add the paraformaldehyde that 40 grams of concentration are 36.5%, adding for the second time 2.5 grams of concentration is 5% tosic acid alcohol, reheat to 100 ℃, under refluxing, react 60～100 minutes, add 20 grams of dihydroxyphenyl propanes, decompression dehydration, dehydration temperaturre rises to 150 ℃ of blowings, obtains solid dimethylbenzene modified phenolic resins.
In above-described embodiment, the tosic acid alcoholic solution that 2.5 grams of concentration is 5% is actual through conversion tosic acid alcohol is 0.125g, and it is 14.6 grams that the paraformaldehyde that 40 grams of concentration is 36.5% passes through conversion paraformaldehyde actual.
Apart from the above, other are identical with embodiment 1.
The dimethylbenzene modified phenolic resins obtaining in embodiment 1～4 and traditional phenol modification xylene formaldehyde resin (comparative example 1) are measured to solidification value, curing activation energy, set time at 120 ℃, 135 ℃, 150 ℃, 165 ℃, and result is as following table:
Cross watch and can find out that dimethylbenzene modified phenolic resins of the present invention compares and have advantages of that solidification value is low, curing speed is fast and set time is short with traditional phenol modification xylene formaldehyde resin,
Dimethylbenzene modified phenolic resins-glass cloth composite the water discharging board obtaining in embodiment 1～4 and existing resol-cotton based composites water discharging board (comparative example 2) are tried out to a turnaround, the water discharging board wearing and tearing of finding embodiment 1～4 are less and even, heat resistance is good, without burned phenomenon, can reach for 2～March its work-ing life, and the wearing and tearing of the water discharging board of comparative example 2 are larger, part is burned, and be 1～3 week work-ing life.
Dimethylbenzene modified phenolic resins of the present invention has advantages of that solidification value is low, curing speed is fast and set time is short, the water discharging board that uses this dimethylbenzene modified phenolic resins to prepare has excellent high temperature resistant moist performance and wear resistance, its work-ing life large leap ahead.
Should be noted that and understand, in the situation that do not depart from the spirit and scope of accompanying claim the present invention for required protection, can make various modifications and improvement to the present invention of foregoing detailed description.Therefore, the scope of claimed technical scheme is not subject to the restriction of given any specific exemplary teachings.
Applicant's statement, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to the selection of the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (9)
1. a dimethylbenzene modified phenolic resins, is characterized in that: by mass parts, comprise following component:
2. dimethylbenzene modified phenolic resins according to claim 1, is characterized in that: described catalyzer is mixtures a kind of in hydrochloric acid, oxalic acid, tosic acid or at least two kinds.
3. the dimethylbenzene modified phenolic resins described in right to use requirement 1 is prepared a method for water discharging board, it is characterized in that, comprises the following steps:
(1), by mass parts, 8～20 parts of 100 parts of dimethylbenzene modified phenolic resinss, 40～60 parts of solvents, 14 parts of urotropines, friction modifiers are fully mixed and make dimethylbenzene modified phenolic resins dipping solution;
(2) by dimethylbenzene modified phenolic resins dipping solution pre-soaking fiber cloth, drying equipment is dried to obtain prepreg;
(3) will after prepreg cutting, be arranged between two block plates, heating between thermocompressor two motor plates, pressurization are solidified prepreg, and then cooling, the demoulding, processing and heat treatment obtain the modification phenolic resin-based matrix material water discharging board of dimethylbenzene.
4. preparation method according to claim 3, it is characterized in that: in step (1), described solvent is mixtures a kind of in benzene, toluene, methyl alcohol, ethanol, butanone and methyl iso-butyl ketone (MIBK) or at least two kinds, and described friction modifiers is mixtures a kind of in graphite, molybdenumdisulphide, aluminium sesquioxide, zirconium white, silicon carbide, calcium oxide, magnesium oxide or at least two kinds.
5. preparation method according to claim 3, is characterized in that, in step (1), dimethylbenzene modified phenolic resins preparation method is as follows:
A. by mass parts, 10～20 parts of 0～30 part of 50～100 parts of phenol, the dihydroxyphenyl propane of 100 parts of the xylene formaldehyde resins of heating and melting, fusing and deionized waters are added in reactor, add half amount of 0.1～2 part of catalyzer, and be slowly heated to boiling reflux;
B. cooling, adds 10～50 parts of paraformaldehydes, then adds the catalyzer that remains second half amount;
C. decompression removes unreacted reactant and water obtain dimethylbenzene modified phenolic resins.
6. preparation method according to claim 3, it is characterized in that, in step (2), fiber is mixtures a kind of in glass fibre, resurrection glass fibre, silica fiber, ceramic fiber, cotton fibre and carbon fiber or at least two kinds, drying plant temperature is 110～130 ℃, the volatile matter of prepreg is not more than 3%, and in prepreg, the content of fiber is 50～55%.
7. preparation method according to claim 3, is characterized in that, in step (3), thermocompressor Heating temperature is 180～200 ℃, moulding pressure 20～40MPa.
8. preparation method according to claim 5, is characterized in that, is heated at 130～150 ℃, keep 3～5 hours after boiling reflux in step a.
9. preparation method according to claim 5, is characterized in that, is warming up to 130～150 ℃ after adding the catalyzer of remaining second half amount in step b, is incubated 1～3 hour.
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| CN201410353060.1A CN104086729B (en) | 2014-07-22 | 2014-07-22 | A kind of dimethylbenzene phenol-formaldehyde resin modified and the method preparing water discharging board thereof |
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| CN201410353060.1A CN104086729B (en) | 2014-07-22 | 2014-07-22 | A kind of dimethylbenzene phenol-formaldehyde resin modified and the method preparing water discharging board thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104984998A (en) * | 2015-06-12 | 2015-10-21 | 靖江市高新窑炉材料有限公司 | Novel polymer scraper blade |
| CN107722555A (en) * | 2017-10-16 | 2018-02-23 | 吴义峰 | A kind of preparation method of Resisting fractre waterproof phenolic board |
| CN109553920A (en) * | 2017-09-27 | 2019-04-02 | 宝山钢铁股份有限公司 | A kind of heat resistant and wear resistant damage scratching rack macromolecule resin bridge crossing plate |
| CN110283423A (en) * | 2019-05-07 | 2019-09-27 | 太仓力达莱特精密工业有限公司 | A kind of friction block and preparation method thereof for brake clutch device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102276775A (en) * | 2011-07-21 | 2011-12-14 | 山东圣泉化工股份有限公司 | Modified phenolic resin and phenolic resin composition |
| CN103145939A (en) * | 2013-04-02 | 2013-06-12 | 开滦（集团）有限责任公司 | Modification method of xylene formaldehyde resin |
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2014
- 2014-07-22 CN CN201410353060.1A patent/CN104086729B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276775A (en) * | 2011-07-21 | 2011-12-14 | 山东圣泉化工股份有限公司 | Modified phenolic resin and phenolic resin composition |
| CN103145939A (en) * | 2013-04-02 | 2013-06-12 | 开滦（集团）有限责任公司 | Modification method of xylene formaldehyde resin |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104984998A (en) * | 2015-06-12 | 2015-10-21 | 靖江市高新窑炉材料有限公司 | Novel polymer scraper blade |
| CN104984998B (en) * | 2015-06-12 | 2017-08-29 | 靖江市高新窑炉材料有限公司 | A kind of novel high polymer Wiper blade |
| CN109553920A (en) * | 2017-09-27 | 2019-04-02 | 宝山钢铁股份有限公司 | A kind of heat resistant and wear resistant damage scratching rack macromolecule resin bridge crossing plate |
| CN107722555A (en) * | 2017-10-16 | 2018-02-23 | 吴义峰 | A kind of preparation method of Resisting fractre waterproof phenolic board |
| CN110283423A (en) * | 2019-05-07 | 2019-09-27 | 太仓力达莱特精密工业有限公司 | A kind of friction block and preparation method thereof for brake clutch device |
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| CN104086729B (en) | 2016-06-08 |
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