CN104086729B - A kind of dimethylbenzene phenol-formaldehyde resin modified and the method preparing water discharging board thereof - Google Patents
A kind of dimethylbenzene phenol-formaldehyde resin modified and the method preparing water discharging board thereof Download PDFInfo
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- CN104086729B CN104086729B CN201410353060.1A CN201410353060A CN104086729B CN 104086729 B CN104086729 B CN 104086729B CN 201410353060 A CN201410353060 A CN 201410353060A CN 104086729 B CN104086729 B CN 104086729B
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Abstract
The invention provides a kind of dimethylbenzene phenol-formaldehyde resin modified and the method preparing water discharging board thereof. This dimethylbenzene phenol-formaldehyde resin modified, by mass parts, comprises xylene formaldehyde resin 100 parts, phenol 50��100 parts, bisphenol-A 0��30 part, paraformaldehyde 10��50 parts, catalyst 0.1��2 part, deionized water 10��20 parts. The dimethylbenzene phenol-formaldehyde resin modified of the present invention has the advantage that solidification temperature is low, curing rate is fast and hardening time is short, water discharging board prepared by this dimethylbenzene phenol-formaldehyde resin modified is used to have high temperature resistant moist performance and the wear resistance of excellence, as finishing mill water discharging board, its service life increases significantly.
Description
Technical field
The present invention relates to phenolic resins field, particularly relate to a kind of dimethylbenzene phenol-formaldehyde resin modified and the method preparing water discharging board thereof.
Background technology
Owing to the phenolic hydroxyl group in phenolic resin is a highly polar group, hygroscopic, and cause that the goods mechanical strength when hot humid conditions uses greatly declines. It is difficult to meet modern industry to material instructions for use under hot humid conditions. Therefore phenolic resin is proposed and improve the requirement of high performance under thermostability and hot humid conditions.
In phenolic resin, generally introduce xylene formaldehyde resin construction unit (claim dimethylbenzene phenol-formaldehyde resin modified, or claim phenol modified xylene formaldehyde resin) to improve the high temperature resistant moist performance etc. of phenolic resin. Dimethylbenzene phenol-formaldehyde resin modified is by dimethylbenzene under acidic catalyst effect, synthesizes xylene formaldehyde resin with 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 phenolic resin, content of phenolic hydroxyl groups in phenolic resin is made to reduce on the one hand, the phenolic hydroxyl group in phenolic resin structure is made to be subject to segmentation and the encirclement of dimethylbenzene on the other hand, substantially increasing resistance to water and alkali resistance, mechanical strength also greatly improves simultaneously. Dimethylbenzene phenol-formaldehyde resin modified can prepare composite with compounds such as wood powder, cotton fiber, glass fibre, resurrection glass fibre, carbon fibers, can use under high hot moist environmental conditions. But the phenolic resin curing temperature height that dimethylbenzene is modified, curing rate is slow, and hardening time is long so that it is application is very limited; Therefore it is very necessary for preparing the fast dimethylbenzene phenol-formaldehyde resin modified of a kind of curing rate.
A kind of high-molecular-weight thermoplastic xylene formaldehyde resin preparation method and application thereof disclosed in prior art, this resin is oxygen-containing hardly, it is a kind of solid, composite can be prepared with wood powder, cotton fiber, glass fibre, carbon fiber and various auxiliary agent compound, but complicated process of preparation, harshness. Also disclosing the method that xylene formaldehyde resin, phenol, formaldehyde prepare the modified xylene formaldehyde resin of phenol when Catalyzed by Oxalic Acid in prior art, but the solidification temperature of the modified xylene formaldehyde resin of obtained phenol is high, hardening time is long, and its application is restricted. Up to the present, phenolic resin modified for dimethylbenzene and the composite prepared by fiber composite are not used as 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 phenol-formaldehyde resin modified, and this dimethylbenzene phenol-formaldehyde resin modified has the advantage that solidification temperature is low, curing rate is fast and hardening time is short.
For reaching this purpose, the present invention by the following technical solutions:
A kind of dimethylbenzene phenol-formaldehyde resin modified, by mass parts, including following components:
Such as, the mass parts of phenol can be 50 parts, 60 parts, 70 parts, 80 parts, 90 parts, 100 parts, the mass parts of bisphenol-A 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 catalyst 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 kind of dimethylbenzene phenol-formaldehyde resin modified dipping solution comprising above-mentioned dimethylbenzene phenol-formaldehyde resin modified, by mass parts, comprises following components:
Hexamethylenamine chemical name 1,3,5,7-tetra-aza-tricycle [3.3.1.1] decane, Chinese another name is hexamethylenetetramine, Urotropinum, hexamine, urotropinum, hexamethylenetetramine.
Preferably, solvent is a kind of in benzene, toluene, methanol, ethanol, butanone and methyl iso-butyl ketone (MIBK) or at least two mixture, and friction modifiers is a kind of in graphite, molybdenum bisuphide, aluminium sesquioxide, zirconium oxide, carborundum, magnesium oxide, calcium oxide or at least two mixture.
Preferably, solvent is the compositions of toluene and methyl iso-butyl ketone (MIBK).
Preferably, catalyst is hydrochloric acid, oxalic acid, p-methyl benzenesulfonic acid or a kind of or at least two mixture.
Another aspect of the present invention provides a kind of method using above-mentioned dimethylbenzene phenol-formaldehyde resin modified to prepare water discharging board, uses water discharging board prepared by this preparation method to have high temperature resistant moist performance and the wear resistance of excellence.
A kind of method using above-mentioned dimethylbenzene phenol-formaldehyde resin modified to prepare water discharging board, comprises the following steps:
(1) by mass parts, dimethylbenzene phenol-formaldehyde resin modified 100 parts, solvent 40��60 parts, hexamethylenamine 14 parts, friction modifiers 8��20 parts are sufficiently mixed and uniformly prepare dimethylbenzene phenol-formaldehyde resin modified dipping solution;
(2) by dimethylbenzene phenol-formaldehyde resin modified dipping solution pre-soaking fiber cloth, drying equipment dries to obtain prepreg;
(3) being arranged in after prepreg cutting between two block plates, heating between hot press two motor plate, pressurization make prepreg solidify, and then cooling, the demoulding, processing and heat treatment, machining obtain the modification phenolic resin-based composite water discharging board of dimethylbenzene.
Such as, 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, the method preparing dimethylbenzene phenol-formaldehyde resin modified is as follows:
A. by the xylene formaldehyde resin 100 parts of heating and melting, the phenol 50��100 parts of fusing, bisphenol-A 0��30 part and 10��20 parts of addition reactors of deionized water, add the half amount of catalyst 0.1��3 part, and it is slowly heated to boiling reflux, then keep 3��5 hours at 130��150 DEG C;
B. lower the temperature, add paraformaldehyde 10��50 parts, add the catalyst remaining second half amount, be warming up to 130��150 DEG C, be incubated 1��3 hour;
C. namely removed under reduced pressure unreacted reactant and water obtain dimethylbenzene phenol-formaldehyde resin modified.
Preferably, in step (2), fiber is a kind of in glass fibre, resurrection glass fibre, quartz fibre, ceramic fibre, cotton fiber and carbon fiber or at least two mixture, drying plant temperature is 110��130 DEG C, the volatile matter of prepreg is not more than 3%, and in prepreg, the content of fiber is 50��55%.
Preferably, in step (3), hot press heating-up temperature is 180��200 DEG C, moulding pressure 20��40MPa.
Compared with prior art, the invention have the benefit that dimethylbenzene phenol-formaldehyde resin modified provided by the invention, by mass parts, xylene formaldehyde resin 100 parts, phenol 50��100 parts, bisphenol-A 0��30 part, paraformaldehyde 10��50 parts, catalyst 0.1��2 part, deionized water 10��20 parts. The dimethylbenzene phenol-formaldehyde resin modified of the present invention has the advantage that solidification temperature is low, curing rate is fast and hardening time is short, water discharging board prepared by this dimethylbenzene phenol-formaldehyde resin modified is used to have high temperature resistant moist performance and the wear resistance of excellence, as finishing mill water discharging board, its service life increases significantly.
Detailed description of the invention
Further illustrate technical scheme separately below in conjunction with specific embodiments.
Raw material involved in following example is commercially available.
Embodiment 1: the dimethylbenzene phenol-formaldehyde resin modified of the present embodiment, by mass parts, comprises following components:
The preparation method of above-mentioned dimethylbenzene phenol-formaldehyde resin modified is as follows:
The hydrochloric acid that 100 grams of xylene formaldehyde resins, 100 grams of phenol, 20 grams of bisphenol-As, 10 grams of deionized waters, 0.5 gram of concentration are 36% is added in reactor, it is slowly heated to boiling reflux, keeping 180��300 minutes, be cooled to less than 90 DEG C, adding 40 grams of concentration is 36.5% paraformaldehyde, it is the hydrochloric acid of 36% that second time adds 0.5 gram of concentration, it is again heated to boiling reflux, reacts 60��100 minutes, decompression dehydration, dehydration finishing temperature is 150 DEG C, namely obtains solid dimethylbenzene phenol-formaldehyde resin modified.
In above-described embodiment, 0.5 gram of concentration be 36% hydrochloric acid to obtain hydrochloric acid actual through conversion be 0.18 gram, 40 grams of concentration be 36.5% paraformaldehyde actual be 14.6 grams.
The dimethylbenzene phenol-formaldehyde resin modified dipping solution of the present embodiment, by mass parts, comprises following components:
The preparation method of the dimethylbenzene phenol-formaldehyde resin modified-glass cloth composite water discharging board of the present embodiment is as follows:
Weigh the dimethylbenzene phenol-formaldehyde resin modified of 100 grams of above-mentioned preparations, namely 30 grams of toluene, 10 grams of methyl iso-butyl ketone (MIBK)s, 14 grams of hexamethylenamine, 10 grams of calcium oxide, 10 grams of magnesium oxide mix homogeneously obtain a kind of dimethylbenzene phenol-formaldehyde resin modified dipping solution;
Glass fabric is put in above-mentioned dimethylbenzene phenol-formaldehyde resin modified dipping solution and carry out preimpregnation, spread is 49.5%, dry subsequently into drying plant, drying plant temperature is 125 DEG C, drying time 10��20 minutes, the volatile matter of prepreg is not more than 3.0%, prepares dimethylbenzene phenol-formaldehyde resin modified-glass fabric prepreg;
By clipped for the prepreg of above-mentioned drying, overlap die-filling, be placed in two polishing corrosion resistant plates between, be placed on hot press temperature and be heat at 200 DEG C, pressurization under pressure 20��30MPa, and keep 1 hour with this understanding, through hot-press solidifying, then namely cooling and demolding, post processing obtain a kind of dimethylbenzene phenol-formaldehyde resin modified-glass fabric composite, thermally treated, machine to obtain dimethylbenzene phenol-formaldehyde resin modified-glass cloth composite water discharging board.
Embodiment 2: the present embodiment is different in that, dimethylbenzene phenol-formaldehyde resin modified, by mass parts, comprise following components:
The preparation method of above-mentioned dimethylbenzene phenol-formaldehyde resin modified 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, is slowly heated to boiling reflux, keeps 180��300 minutes, it is cooled to less than 90 DEG C, adding 40 gram of 36.5% paraformaldehyde, second time adds the hydrochloric acid of 0.5 gram 36%, is again heated to boiling reflux, react 60��100 minutes, add 20 grams of bisphenol-As, react 30min, decompression dehydration, dehydration finishing temperature is 150 DEG C, namely obtains solid dimethylbenzene phenol-formaldehyde resin modified.
In above-described embodiment, 0.5 gram of concentration be 36% hydrochloric acid to obtain hydrochloric acid actual through conversion be 0.18 gram, 40 grams of concentration be 36.5% paraformaldehyde actual be 14.6 grams.
Apart from the above, dimethylbenzene phenol-formaldehyde resin modified dipping solution and preparation method thereof is identical with embodiment 1.
Embodiment 3: the present embodiment is different in that, making hydrochloric acid 0.36 part into toluenesulfonic acid alcohol is 0.25 part, is the p-methyl benzenesulfonic acid alcoholic solution that 36% hydrochloric acid changes that 2.5 grams of concentration is 5% into by 0.5 gram of concentration, and in addition other is identical with embodiment 1.
In above-described embodiment, 2.5 grams of concentration be 5% p-methyl benzenesulfonic acid alcoholic solution actual through conversion p-methyl benzenesulfonic acid alcohol be 0.125g.
Embodiment 4: the dimethylbenzene phenol-formaldehyde resin modified of the present embodiment, by mass parts, comprises following components:
The preparation method of above-mentioned dimethylbenzene phenol-formaldehyde resin modified is as follows:
The p-methyl benzenesulfonic acid alcoholic solution that 100 grams of xylene formaldehyde resins, 100 grams of phenol, 10 grams of deionized waters, 2.5 grams of concentration are 5% is added in reactor, it is slowly heated to 135��150 DEG C, keep 180��300 minutes, it is cooled to less than 80 DEG C, adding 40 grams of concentration is the paraformaldehyde of 36.5%, it is 5% p-methyl benzenesulfonic acid alcohol that second time adds 2.5 grams of concentration, it is again heated to 100 DEG C, react 60��100 minutes under reflux, add 20 grams of bisphenol-As, decompression dehydration, dehydration temperaturre rises to 150 DEG C of blowings, namely obtains solid dimethylbenzene phenol-formaldehyde resin modified.
In above-described embodiment, 2.5 grams of concentration be 5% p-methyl benzenesulfonic acid alcoholic solution actual through conversion p-methyl benzenesulfonic acid alcohol be 0.125g, 40 grams of concentration be 36.5% paraformaldehyde actual through the paraformaldehyde that converts be 14.6 grams.
Apart from the above, other are identical with embodiment 1.
Modified to the dimethylbenzene phenol-formaldehyde resin modified that obtains in embodiment 1��4 and traditional phenol xylene formaldehyde resin (comparative example 1) measures solidification temperature, curing activation energy, hardening time at 120 DEG C, 135 DEG C, 150 DEG C, 165 DEG C, and result is following table such as:
Cross watch and can be seen that the dimethylbenzene phenol-formaldehyde resin modified of the present invention has, compared with the modified xylene formaldehyde resin of traditional phenol, the advantage that solidification temperature is low, curing rate is fast and hardening time is short,
Dimethylbenzene phenol-formaldehyde resin modified-glass cloth composite the water discharging board obtained in embodiment 1��4 and existing phenolic resin-cotton based composites water discharging board (comparative example 2) are carried out a time between overhauls(TBO) on probation, find that the water discharging board abrasion of embodiment 1��4 is less and uniform, heat resistance is excellent, without burned phenomenon, its service life is up to 2��March, and the water discharging board abrasion of comparative example 2 is relatively big, part is burned, and service life is 1��3 week.
The dimethylbenzene phenol-formaldehyde resin modified of the present invention has the advantage that solidification temperature is low, curing rate is fast and hardening time is short, using water discharging board prepared by this dimethylbenzene phenol-formaldehyde resin modified to have high temperature resistant moist performance and the wear resistance of excellence, its service life increases significantly.
It should be noted that and understand, when without departing from the spirit and scope of appended claims the present invention for required protection, it is possible to the present invention of foregoing detailed description is made various amendment and improvement. It is therefore desirable to the scope of the technical scheme of protection is not by the restriction of given any specific exemplary teachings.
Applicant states, the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment, but the invention is not limited in above-mentioned detailed process equipment and technological process, namely do not mean that the present invention has to rely on above-mentioned detailed process equipment and technological process could be implemented.The equivalence of each raw material of product of the present invention, it will be clearly understood that any improvement in the present invention, is replaced and the interpolation of auxiliary element, concrete way choice etc. by person of ordinary skill in the field, all falls within protection scope of the present invention and open scope.
Claims (4)
1. one kind uses the method that dimethylbenzene phenol-formaldehyde resin modified prepares water discharging board, it is characterised in that comprise the following steps:
(1) by mass parts, dimethylbenzene phenol-formaldehyde resin modified 100 parts, solvent 40��60 parts, hexamethylenamine 14 parts, friction modifiers 8��20 parts are sufficiently mixed and uniformly prepare dimethylbenzene phenol-formaldehyde resin modified dipping solution;
(2) by dimethylbenzene phenol-formaldehyde resin modified dipping solution pre-soaking fiber cloth, drying equipment dries to obtain prepreg;
(3) being arranged in after prepreg cutting between two block plates, heating between hot press two motor plate, pressurization make prepreg solidify, and then cooling, the demoulding, processing and heat treatment obtain the modification phenolic resin-based composite water discharging board of dimethylbenzene.
2. preparation method according to claim 1, it is characterized in that: in step (1), described solvent is a kind of in benzene, toluene, methanol, ethanol, butanone and methyl iso-butyl ketone (MIBK) or at least two mixture, and described friction modifiers is a kind of in graphite, molybdenum bisuphide, aluminium sesquioxide, zirconium oxide, carborundum, calcium oxide, magnesium oxide or at least two mixture.
3. preparation method according to claim 1, it is characterised in that in step (1), dimethylbenzene phenol-formaldehyde resin modified preparation method is as follows:
A. by mass parts, by the xylene formaldehyde resin 100 parts of heating and melting, the phenol 50��100 parts of fusing, bisphenol-A 0��30 part and 10��20 parts of addition reactors of deionized water, add the half amount of catalyst 0.1��2 part, and be slowly heated to boiling reflux;
B. lower the temperature, add paraformaldehyde 10��50 parts, add the catalyst remaining second half amount;
C. namely removed under reduced pressure unreacted reactant and water obtain dimethylbenzene phenol-formaldehyde resin modified.
4. preparation method according to claim 1, it is characterized in that, in step (2), fiber is a kind of in glass fibre, resurrection glass fibre, quartz fibre, ceramic fibre, cotton fiber and carbon fiber or at least two mixture, drying plant temperature is 110��130 DEG C, the volatile matter of prepreg is not more than 3%, and in prepreg, the content of fiber is 50��55%.
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CN107722555A (en) * | 2017-10-16 | 2018-02-23 | 吴义峰 | A kind of preparation method of Resisting fractre waterproof phenolic board |
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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 |
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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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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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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CN107722555A (en) * | 2017-10-16 | 2018-02-23 | 吴义峰 | A kind of preparation method of Resisting fractre waterproof phenolic board |
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