CN101602837B - Method for preparing phenolic resin used for wire enamel - Google Patents
Method for preparing phenolic resin used for wire enamel Download PDFInfo
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- CN101602837B CN101602837B CN2009101817112A CN200910181711A CN101602837B CN 101602837 B CN101602837 B CN 101602837B CN 2009101817112 A CN2009101817112 A CN 2009101817112A CN 200910181711 A CN200910181711 A CN 200910181711A CN 101602837 B CN101602837 B CN 101602837B
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- wire enamel
- cresols
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Abstract
The invention discloses a method for preparing phenolic resin used for wire enamel, which comprises the following steps: dissolving cresol into distilled water at the temperature of between 70 and 80 DEG C, adding the cresol and weak base into the solution, stirring the mixture, heating the mixture to between 95 and 98 DEG C, then preserving the heat till emulsifying, adding weak acid into the mixture to neutralize the mixture after emulsifying the mixture for 1 to 3 hours, and stopping heating; and dehydrating the obtained solution in vacuum to lower the temperature along with the dehydration of water, heating the solution when the vacuum degree reaches the standard to continually dehydrate the solution so that the color of the solution becomes transparent from turbid, raising the temperature to certain temperature after the solution becomes clear, and stopping heating. The method has the advantage that the method can solve the problem of thermal impact resistance of the wire enamel, and improves the thermal impact resistance of a paint film; and the wire enamel has smooth appearance surface and good glossiness.
Description
Technical field
The present invention relates to the coating resin field, relate to especially and a kind ofly can improve wire enamel coating surface gloss, and also can improve the preparation method of the heat of enameled wire towards the resol of property
Background technology
Along with the enhancing of science and technology development and people's living safety consciousness, people require also more and more higher to employed enameled wire in electronics and the electric type product.Enameled wire is except requiring higher electrical property and stronger mechanical property, and its outward appearance also will be accomplished standards such as smooth surface, glossiness be good.In order to satisfy the requirement of market to enameled wire, wire enamel manufacturer all by test, strives for addressing this problem, after find can solve similar problem relatively by resol.But many manufacturers are that 2402 para-tert-butyl phenolic resins and the 2123 acidic phenol urea formaldehydes of purchasing on the market are used for wire enamel mostly at present, just on the purposes mainly be to make adhesive material to use, and or not the use that is well suited for wire enamel.When this two classes resol when consumption is bigger in wire enamel, can influence the sliding sense in surface of enameled wire, and reduce the resistance to cracking of paint film, so can only use on a small quantity, the too small heat that cannot improve the wire enamel paint film again of resol consumption causes wire enamel quality and outward appearance can not reach perfect unification towards property.
Summary of the invention
At the problems referred to above, the invention provides a kind of wire enamel quality that can make and reach a standard, heat-resisting good towards property, and the level and smooth glossiness preparation method who is used for the resol of wire enamel of outward appearance.
For realizing this purpose, the present invention adopts following technical scheme to realize:
The preparation method who is used for the resol of wire enamel, preparation as follows:
A, be the dissolvings of 70～80 ℃ of scopes with distilled water in temperature, add cresols and weak base and stir cresols, be warming up to 95～98 ℃ after, be incubated to emulsification, treat emulsification after 1～3 hour, add the weak acid neutralization, stop heating;
B, the solution that above-mentioned steps is obtained carry out vacuum hydro-extraction, and along with deviating from of moisture, temperature descends, treat to begin when vacuum tightness reaches standard heating, moisture is constantly deviate from, and solution colour is become transparent by muddiness, transparent back temperature is gone up to certain temperature again, stops heating; The standard of described vacuum tightness is: 〉=0.095Mpa; Described rise temperature is 5～10 ℃;
C, the resin solution that above-mentioned steps is obtained add phenol solvent, dissolve 2 hours, obtain required product;
Count in molar ratio, described cresols: formaldehyde is 1: 0.6～0.9;
By weight, described formaldehyde: distilled water is 1: 1.45～2.1;
By weight, described cresols: weak base is 100: 1～2;
Described formaldehyde is Paraformaldehyde 96;
Described cresols is M-and P-cresols, and wherein meta-cresol content is in 45～50% scopes;
Described weak base is selected from a kind of in trolamine or the ammoniacal liquor;
Described weak acid is selected from a kind of in phenylformic acid or the Whitfield's ointment;
Described phenol solvent is selected from least a with in phenol isomer or the ethyl phenol isomers of phenol, cresols isomers, xylenol.
Beneficial effect of the present invention is: can solve the heat-resisting problem towards property of wire enamel, improve the heat-resisting towards property of paint film, its appearance surfaces is smooth, glossiness good.
Embodiment
The present invention will be further described below by embodiment.
Embodiment 1:
In the there-necked flask of 1000ml, add 188 gram distilled water, start to stir and add 92 gram Paraformaldehyde 96s, be heated to 70 ℃ then, be incubated to material and dissolve fully, add 370 gram M-and P-cresols and 4 gram ammoniacal liquor.Be warmed up to 95 ℃, insulation is incubated 1 hour until " emulsification " after " emulsification " again.Add 3.5 gram phenylformic acid.Stop heating, go back to stream and be distillation.Carry out vacuum hydro-extraction, when vacuum tightness reaches the highest, begin to heat, constantly extract moisture out, resin changes transparent, and temperature is gone up 5 ℃ again, stops heating, adds 500 gram cresols, dissolves 2 hours, gets 35 seconds phenol resin solutions of solids content 38.6% viscosity.
Embodiment 2:
In the there-necked flask of 1000ml, add 188 gram distilled water, start to stir and add 92 gram Paraformaldehyde 96s, be heated to 80 ℃ then, be incubated to material and dissolve fully, add 370 gram M-and P-cresols and 5 gram trolamines.Be warmed up to 98 ℃, insulation is incubated 1 hour until " emulsification " after " emulsification " again.Add 4.5 gram phenylformic acid.Stop heating, go back to stream and be distillation.Carry out vacuum hydro-extraction, when vacuum tightness reaches the highest, begin to heat, constantly extract moisture out, resin changes transparent, and temperature is gone up 5 ℃ again, stops heating, adds 500 gram cresols, dissolves 2 hours, gets 42 seconds phenol resin solution of solids content 39.3% viscosity.
Embodiment 3:
In the there-necked flask of 1000ml, add 188 gram distilled water, start to stir and add 92 gram Paraformaldehyde 96s, be heated to 75 ℃ then, be incubated to material and dissolve fully, add 370 gram M-and P-cresols and 5 gram trolamines.Be warmed up to 96 ℃, insulation is incubated 2 hours until " emulsification " after " emulsification " again.Add 4 gram Whitfield's ointments.Stop heating, go back to stream and be distillation.Carry out vacuum hydro-extraction, when vacuum tightness reaches the highest, begin to heat, constantly extract moisture out, resin changes transparent, and temperature is gone up 5 ℃ again, stops heating, adds 500 gram cresols, dissolves 2 hours, gets 60 seconds phenol resin solution of 40.5% solids content viscosity.
Comparative example 1:
Add gram cresols in the there-necked flask of 1000ml, start and stir adding gram 2402 resol (going up marine products), be heated to 70 ℃ then, dissolved 4 hours, cooling obtains 2402 phenol resin solutions.
Comparative example 2:
Add gram cresols in the there-necked flask of 1000ml, start and stir adding gram 2123 resol (jiangsu wuxi product), be heated to 110 ℃ then, dissolved 4 hours, cooling obtains 2123 phenol resin solutions.Performance test
Mix with same polyesterimide wire enamel with the resol of embodiment and Comparative Examples gained and to obtain polyesterimide wire enamel, coat the enameled wire of same specification on same enamelling machine with identical technology, relatively paint film appearance, heat such as dash at performance (the results are shown in Table 1).
Table 1 paint film appearance and heat such as dash at performance comparison
Paint film property in the table 1 is by " GB 4074 enameled wire test methods " test.
By table 1 result as can be known, resol of the present invention all can improve the outward appearance and the hot punching performance of polyesterimide wire enamel paint film, can not influence the coiling of paint film.
Claims (5)
1. be used for the preparation method of the resol of wire enamel, it is characterized in that, as follows preparation:
A, be the dissolvings of 70～80 ℃ of scopes with distilled water in temperature, add M-and P-cresols and weak base and stir Paraformaldehyde 96, be warming up to 95～98 ℃ after, be incubated to emulsification, treat emulsification after 1～3 hour, add the weak acid neutralization, stop heating;
B, the solution that above-mentioned steps is obtained carry out vacuum hydro-extraction, and along with deviating from of moisture, temperature descends, and begin heating when treating vacuum tightness 〉=0.095Mpa, and moisture is constantly deviate from, and solution colour is become transparent by muddiness, and transparent back temperature is gone up 5～10 ℃ again, stops heating;
C, the resin solution that above-mentioned steps is obtained add phenol solvent, and dissolving obtains required product;
Meter in molar ratio, described to M-and P-cresols: Paraformaldehyde 96 is 1: 0.6～0.9;
By weight, described Paraformaldehyde 96: distilled water is 1: 1.45～2.1;
By weight, described M-and P-cresols: weak base is 100: 1～2.
2. the preparation method who is used for the resol of wire enamel according to claim 1 is characterized in that: described M-and P-cresols, wherein meta-cresol content is in 45～50% scopes.
3. the preparation method who is used for the resol of wire enamel according to claim 1 is characterized in that: described weak base is selected from a kind of in trolamine or the ammoniacal liquor.
4. the preparation method who is used for the resol of wire enamel according to claim 1 is characterized in that: described weak acid is selected from a kind of in phenylformic acid or the Whitfield's ointment.
5. the preparation method who is used for the resol of wire enamel according to claim 1 is characterized in that: described phenol solvent is selected from phenol, cresols isomers, xylenol isomers or the ethyl phenol isomers at least a kind of.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101817112A CN101602837B (en) | 2009-07-22 | 2009-07-22 | Method for preparing phenolic resin used for wire enamel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101817112A CN101602837B (en) | 2009-07-22 | 2009-07-22 | Method for preparing phenolic resin used for wire enamel |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101602837A CN101602837A (en) | 2009-12-16 |
| CN101602837B true CN101602837B (en) | 2011-05-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2009101817112A Expired - Fee Related CN101602837B (en) | 2009-07-22 | 2009-07-22 | Method for preparing phenolic resin used for wire enamel |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479539B (en) * | 2014-12-05 | 2017-07-11 | 四川东材科技集团股份有限公司 | A kind of high heat resistance impacts the preparation method of polyesterimide wire enamel |
| CN107177306A (en) * | 2017-07-26 | 2017-09-19 | 合肥铭佑高温技术有限公司 | A kind of heat resistance modified wire enamel and preparation method thereof |
| CN110698619A (en) * | 2019-11-26 | 2020-01-17 | 南通百川新材料有限公司 | Modified phenolic resin and preparation method thereof |
| CN115505083A (en) * | 2022-10-09 | 2022-12-23 | 南通百川新材料有限公司 | Nylon modified phenolic resin and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058627A (en) * | 2006-04-20 | 2007-10-24 | 西北工业大学 | Production technique for linear phenolic resin |
| CN101121772A (en) * | 2006-08-09 | 2008-02-13 | 中国石油化工集团公司 | Method for preparing line-type o-cresol novolac resin |
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2009
- 2009-07-22 CN CN2009101817112A patent/CN101602837B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101058627A (en) * | 2006-04-20 | 2007-10-24 | 西北工业大学 | Production technique for linear phenolic resin |
| CN101121772A (en) * | 2006-08-09 | 2008-02-13 | 中国石油化工集团公司 | Method for preparing line-type o-cresol novolac resin |
Non-Patent Citations (1)
| Title |
|---|
| JP昭56-049722A 1981.05.06 |
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| CN101602837A (en) | 2009-12-16 |
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Granted publication date: 20110518 Termination date: 20200722 |