CN105754062A - Low-hydroscopicity phenolic resin insulating gel and preparation method thereof - Google Patents
Low-hydroscopicity phenolic resin insulating gel and preparation method thereof Download PDFInfo
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- CN105754062A CN105754062A CN201610150193.8A CN201610150193A CN105754062A CN 105754062 A CN105754062 A CN 105754062A CN 201610150193 A CN201610150193 A CN 201610150193A CN 105754062 A CN105754062 A CN 105754062A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C09J161/04, C09J161/18 and C09J161/20
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Abstract
The invention relates to phenolic resin insulating gel and a preparation method thereof, in particular to low-hydroscopicity phenolic resin insulating gel and a preparation method thereof, and aims to solve the problem of insulativity lowering caused by high hydroscopicity and high water absorbing speed of existing phenolic resin.The low-hydroscopicity phenolic resin is composed of, by weight, 155-190 parts of phenol, 14-20 parts of NaOH solution of 40-50% in mass percentage, 270-345 parts of formaldehyde solution of 37-39% in mass percentage and 4.7-15 parts of gamma-aminopropyl triethoxysilane.In the synthesis process of the modified phenolic resin, a silane coupling agent KH550 is directly added into a reaction system for in-situ polymerization, so that reaction is more sufficient and the process is simple and easy to operate.
Description
Technical field
The present invention relates to a kind of phenolic resin insulating cement and preparation method thereof, particularly relate to a kind of low water absorbable phenolic resin
Insulating cement and preparation method thereof.
Background technology
Phenolic resin has excellent heat-resisting, acid and alkali-resistance, the characteristic of resistance to combustion and excellent electrical insulating property.But heat cured phenol
Yet suffering from the highest water imbibition after urea formaldehyde solidification, reason is to there is phenolic hydroxyl group and the methylol of polarity on it, according to phase
The principle that patibhaga-nimitta is molten, the hydroxyl of polarity runs into the water of polarity, it is easy to combines, causes phenolic resin to absorb water, thus make phenol
, there is safety in utilization problem in urea formaldehyde decreasing insulating in humid conditions.Therefore, phenolic resin to be stablized insulation
Property be necessary for limit hydroxyl effect, reduce phenolic resin water imbibition, frequently with following two method:
(l) block phenolic hydroxyl group.
(2) introduce other component to mix with phenolic resin generation chemical reaction or part, separate or surround phenolic hydroxyl group.
Generally researcher is often with dimethylbenzene phenol-formaldehyde resin modified, the most modified phenolic resin resistance to water, alkali resistance, toughness
All obtain a certain degree of raising with mechanical strength, but dimethylbenzene has severe toxicity, have impact on its popularization and application.
The method of modifying of current existing phenolic resin, it is preferred that emphasis is when improving its fragility, raising bonding strength, shortening solidification
Between, but the water imbibition of modified phenolic resin does not vary widely, and water absorption rate is the biggest, and partially modified method
Employ toxic agent, poor for applicability.Therefore, the most harmless a kind of method of modifying need to be found to reduce phenolic aldehyde
The water imbibition of resin, keeps its insulating properties.
Summary of the invention
By force and absorption speed is fast to the invention aims to solve existing phenolic resin water imbibition, causes decreasing insulating
Problem, and provide the preparation method of the excellent phenolic resin insulating cement of a kind of low water absorbable permanent insulation.
A kind of low water absorbable phenolic resin insulating cement is by weight by 155 parts～the phenol of 190 parts, 14 parts～20 parts
NaOH solution, 270 parts～the formalin of 345 parts and the gamma-aminopropyl-triethoxy-silane composition of 4.7 parts～15 parts；Institute
Stating the NaOH aqueous solution that NaOH solution is mass fraction 40%～50%, described formalin is mass fraction 37%
The formalin of 39%%.
The preparation method of a kind of low water absorbable phenolic resin insulating cement, sequentially includes the following steps:
One, weigh by weight 155 parts～the phenol of 190 parts, 14 parts～the NaOH solution of 20 parts, 270 parts～345
The formalin of part and the gamma-aminopropyl-triethoxy-silane (Silane coupling agent KH550) of 4.7 parts～15 parts；By weigh
Formalin is divided into two parts of A and B, and wherein the quality of A is the 70%～85% of formalin gross mass, and the quality of B is first
The 15%～30% of aldehyde solution gross mass；Described NaOH solution is the NaOH aqueous solution of mass fraction 40%～50%, institute
State the formalin that formalin is mass fraction 37% 39%；
Two, take in the phenol addition container that step one weighs, melt at a temperature of 40 DEG C～50 DEG C, be subsequently adding step one title
The NaOH solution taken, obtains mixed solution, reacts 8min～12min；
Three, in step 2 mixed liquor, add A, be warmed up to 70 DEG C～75 DEG C, be subsequently adding γ-aminopropyl that step one weighs
Triethoxysilane, then heat up, treat that temperature reaches 80 DEG C～85 DEG C, react 1h ± 5min；
Four, after reaction terminates, cooling, wait to cool to 70 DEG C～75 DEG C, add B, then heat up, treat that temperature reaches
80 DEG C～85 DEG C, react 200min ± 10min；
Five, after reaction terminates, it is cooled to less than 40 DEG C and the material in container is poured out, obtain phenolic resin.
The present invention has an advantage in that relative to prior art:
1. being possible not only to after KH550 modification reduces the water imbibition of thermosetting phenolic resin, improves insulating properties, and uses
Modified resinoid bond or the goods of dipping, Physical and mechanical properties also has some improvement.Prepared by the present invention
The water absorption test front volume resistance of KH550 modification low water absorbable insulating cement is 1.1 × 109—2.38×109Ω, and common not
Modified is only 0.27 × 109Ω；After water absorption test, the volume resistance of the low water absorbable insulating cement that KH550 is modified is 0.29
×109—0.58×109Ω, and common unmodified resin is only 0.068 × 109Ω, the low water absorbable of the present invention is modified absolutely
The resistivity of edge glue is higher than the phenolic resin that commonly insulate；The phenolic resin insulating cement bending resistance obtained by preparation method of the present invention is strong
Degree improves 3%～5% for prepared by 102.58MPa～149.89MPa, relatively commonsense method；Obtained by preparation method of the present invention
To phenolic resin insulating cement composite bending modulus be 5.46GPa～10.02GPa, relatively commonsense method prepare improve 4%～8%.
2. use nontoxic, degradable chemical reagent KH550 modification, environmental protection, and cost is obvious compared with other modifying agent
Reduce.
3., in phenol-formaldehyde resin modified building-up process, it is added directly in reaction system by Silane coupling agent KH550 first
Row in-situ polymerization, makes reaction more abundant, and technics comparing is simple, easily operates.
Detailed description of the invention
Technical solution of the present invention is not limited to act detailed description of the invention set forth below, also includes appointing between each detailed description of the invention
Meaning combination.
Detailed description of the invention one: a kind of low water absorbable phenolic resin insulating cement of present embodiment is by weight by 155 parts
～the γ of the phenol of 190 parts, 14 parts～the NaOH solution of 20 parts, 270 parts～the formalin of 345 parts and 4.7 parts～15 parts-
Aminopropyl triethoxysilane forms；Described NaOH solution is the NaOH aqueous solution of mass fraction 40%～50%, described
Formalin is the formalin of mass fraction 37% 39%.
Detailed description of the invention two: the preparation method of a kind of low water absorbable phenolic resin insulating cement of present embodiment, by following step
Suddenly carry out:
One, weigh by weight 155 parts～the phenol of 190 parts, 14 parts～the NaOH solution of 20 parts, 270 parts～345
The formalin of part and 4.7 parts～the gamma-aminopropyl-triethoxy-silane of 15 parts；The formalin weighed is divided into two parts of A and
B, wherein the quality of A is the 70%～85% of formalin gross mass, and the quality of B is formalin gross mass
15%～30%；Described NaOH solution is the NaOH aqueous solution of mass fraction 40%～50%, and described formalin is quality
The formalin of mark 37% 39%；
Two, take in the phenol addition container that step one weighs, melt at a temperature of 40 DEG C～50 DEG C, be subsequently adding step one title
The NaOH solution taken, obtains mixed solution, reacts 8min～12min；
Three, in step 2 mixed liquor, add A, be warmed up to 70 DEG C～75 DEG C, be subsequently adding γ-aminopropyl that step one weighs
Triethoxysilane, then heat up, treat that temperature reaches 80 DEG C～85 DEG C, react 1h ± 5min；
Four, after reaction terminates, cooling, wait to cool to 70 DEG C～75 DEG C, add B, then heat up, treat that temperature reaches
80 DEG C～85 DEG C, react 200min ± 10min；
Five, after reaction terminates, it is cooled to less than 40 DEG C and the material in container is poured out, obtain phenolic resin.
Detailed description of the invention three: present embodiment is unlike detailed description of the invention two, and step one weighs benzene by weight
172 parts of phenol.Other steps are identical with detailed description of the invention two with parameter.
Detailed description of the invention four: present embodiment is unlike detailed description of the invention two, and step one weighs by weight
NaOH solution 17 parts.Other steps are identical with detailed description of the invention two with parameter.
Detailed description of the invention five: present embodiment is unlike detailed description of the invention two, and step one weighs first by weight
Aldehyde solution 310 parts.Other steps are identical with detailed description of the invention two with parameter.
Detailed description of the invention six: present embodiment unlike detailed description of the invention two, step one weigh by weight γ-
Aminopropyl triethoxysilane 7.2 parts.Other steps are identical with detailed description of the invention two with parameter.
Detailed description of the invention seven: present embodiment unlike detailed description of the invention two, NaOH solution described in step one
The NaOH aqueous solution for mass fraction 40%.Other steps are identical with detailed description of the invention two with parameter.
Detailed description of the invention eight: present embodiment is unlike detailed description of the invention two, and the quality of step one A is formaldehyde
The 80% of solution gross mass.Other steps are identical with detailed description of the invention two with parameter.
Detailed description of the invention nine: present embodiment is unlike detailed description of the invention two, and the quality of step one B is formaldehyde
The 20% of solution gross mass.Other steps are identical with detailed description of the invention two with parameter.
Embodiment 1
The preparation method of a kind of low water absorbable phenolic resin insulating cement, sequentially includes the following steps:
One, taking 172.4g phenol and add in container, melt at a temperature of 40 DEG C, being subsequently adding 17.3g mass fraction is 40%
NaOH solution, obtain mixed solution, react 10min；
Two, adding the formaldehyde that mass fraction is 37% 39% in step one mixed liquor, its quality added is whole reaction
During formaldehyde total inventory 80%, be warmed up to 72 DEG C, treat that temperature reaches 82 DEG C, react 1h；
Three, after reaction terminates, cooling, wait to cool to 72 DEG C, add the formaldehyde that mass fraction is 37% 39%, add
The quality entered is the 20% of total inventory of formaldehyde in whole course of reaction, then heats up, and treats that temperature reaches 82 DEG C, reaction
200min；Total inventory of described formaldehyde is 310.4g；
Four, after reaction terminates, it is cooled to less than 40 DEG C and the material in container is poured out, obtain phenolic resin.
The resin drying prepared removes volatile matter, then according to the mensuration of GBT 1034-2008 plastic ink absorption processes
To water absorption rate.
Embodiment 2
The preparation method of a kind of low water absorbable phenolic resin insulating cement, sequentially includes the following steps:
One, taking 172.4g phenol and add in container, melt at a temperature of 40 DEG C, being subsequently adding 17.3g mass fraction is 40%
NaOH solution, obtain mixed solution, react 10min；
Two, adding the formaldehyde that mass fraction is 37% 39% in step one mixed liquor, its quality added is whole reaction
During formaldehyde total inventory 80%, be warmed up to 72 DEG C, add gamma-aminopropyl-triethoxy-silane 5.15g and (account for overall
The 3% of system), then heat up, treat that temperature reaches 82 DEG C, react 1h；
Three, after reaction terminates, cooling, wait to cool to 72 DEG C, add the formaldehyde that mass fraction is 37% 39%, add
The quality entered is the 20% of total inventory of formaldehyde in whole course of reaction, then heats up, and treats that temperature reaches 82 DEG C, reaction
200min；Total inventory of described formaldehyde is 310.4g；
Four, after reaction terminates, it is cooled to less than 40 DEG C and the material in container is poured out, obtain phenolic resin.
The resin drying prepared removes volatile matter, then according to the mensuration of GBT 1034-2008 plastic ink absorption processes
To water absorption rate.
Embodiment 3
The preparation method of a kind of low water absorbable phenolic resin insulating cement, sequentially includes the following steps:
One, taking 172.4g phenol and add in container, melt at a temperature of 40 DEG C, being subsequently adding 17.3g mass fraction is 40%
NaOH solution, obtain mixed solution, react 10min；
Two, adding the formaldehyde that mass fraction is 37% 39% in step one mixed liquor, its quality added is whole reaction
During formaldehyde total inventory 80%, be warmed up to 72 DEG C, add gamma-aminopropyl-triethoxy-silane 8.12g and (account for overall
The 5% of system), then heat up, treat that temperature reaches 82 DEG C, react 1h；
Three, after reaction terminates, cooling, wait to cool to 72 DEG C, add the formaldehyde that mass fraction is 37% 39%, add
The quality entered is the 20% of total inventory of formaldehyde in whole course of reaction, then heats up, and treats that temperature reaches 82 DEG C, reaction
200min；Total inventory of described formaldehyde is 310.4g；
Four, after reaction terminates, it is cooled to less than 40 DEG C and the material in container is poured out, obtain phenolic resin.
The resin drying prepared removes volatile matter, then according to the mensuration of GBT 1034-2008 plastic ink absorption processes
To water absorption rate.
Embodiment 4
The preparation method of a kind of low water absorbable phenolic resin insulating cement, sequentially includes the following steps:
One, taking 172.4g phenol and add in container, melt at a temperature of 40 DEG C, being subsequently adding 17.3g mass fraction is 40%
NaOH solution, obtain mixed solution, react 10min；
Two, adding the formaldehyde that mass fraction is 37% 39% in step one mixed liquor, its quality added is whole reaction
During formaldehyde total inventory 80%, be warmed up to 72 DEG C, add gamma-aminopropyl-triethoxy-silane 13.8g and (account for overall
The 8% of system), then heat up, treat that temperature reaches 82 DEG C, react 1h；
Three, after reaction terminates, cooling, wait to cool to 72 DEG C, add the formaldehyde that mass fraction is 37% 39%, add
The quality entered is the 20% of total inventory of formaldehyde in whole course of reaction, then heats up, and treats that temperature reaches 82 DEG C, reaction
200min；Total inventory of described formaldehyde is 310.4g
Four, after reaction terminates, it is cooled to less than 40 DEG C and the material in container is poured out, obtain phenolic resin.
The resin drying prepared removes volatile matter, then according to the mensuration of GBT 1034-2008 plastic ink absorption processes
To water absorption rate.
Process according to the mensuration of GBT 1034-2008 plastic ink absorption and specifically carry out by the following method: will be the most of the same race on request
The liquid phenolic resin of class is placed in molding jig, makes the disk of diameter about 100mm, thickness about 1mm), warp
(50 DEG C-some hours, 80 DEG C of-30min, 100 DEG C of-30min, 130 DEG C of-30min, until phenol to cross ladder-elevating temperature drying mode
Urea formaldehyde cure hard, completely disengages from from processing release paper.
1. above-mentioned pure resin glue sample is put into and the baking oven of 50 DEG C is dried at least more than 24h, then cool down in drier
To room temperature, weigh the quality of each sample, be accurate to 0.0001g (quality m1). repeat this step and no longer change to quality.
2. being put into by sample in the container filling distilled water, water temperature controls 23 DEG C or room temperature, after soaking 24h, takes out sample,
Wipe rapidly all of water of specimen surface with cleaning dry cloth or filter paper, again weigh each sample quality, be accurate to
0.0001g (quality m2).After sample is taken out from water, should complete to weigh in 1min.
The water suction mass fraction of c: sample
M1: the quality of dried sample, unit of gram (g) before soaking
M2: the quality of sample, unit of gram (g) after immersion
Table 1 is the resistance value before and after the water imbibition of all types of resin and water absorption test
Conclusion: the water imbibition being modified the thermosetting resin after process reduces.On the whole, Silane coupling agent KH550 is utilized
Modification, 3-8% consumption all plays a role, and the content of 5% is more quite a lot of compared with other resin.
Claims (9)
1. a low water absorbable phenolic resin insulating cement, it is characterised in that: described phenolic resin insulating cement is by weight by 155
Part～the phenol of 190 parts, 14 parts～the NaOH solution of 20 parts, 270 parts～the formalin of 345 parts and 4.7 parts～15 parts
Gamma-aminopropyl-triethoxy-silane forms；Described NaOH solution is the NaOH aqueous solution of mass fraction 40%～50%, described
Formalin is the formalin of mass fraction 37%～39%.
The preparation method of a kind of low water absorbable phenolic resin insulating cement the most as claimed in claim 1, it is characterised in that: the party
Method sequentially includes the following steps:
One, 155 parts～the phenol of 190 parts, 14 parts～the NaOH solution of 20 parts, 270 parts～345 parts are weighed by weight
Formalin and 4.7 parts～the gamma-aminopropyl-triethoxy-silane of 15 parts；The formalin weighed is divided into two parts of A and B,
Wherein the quality of A is the 70%～85% of formalin gross mass, and the quality of B is the 15%～30% of formalin gross mass；
Described NaOH solution is the NaOH aqueous solution of mass fraction 40%～50%, and described formalin is mass fraction 37%～39%
Formalin；
Two, take in the phenol addition container that step one weighs, melt at a temperature of 40 DEG C～50 DEG C, be subsequently adding step one title
The NaOH solution taken, obtains mixed solution, reacts 8min～12min；
Three, in step 2 mixed liquor, add A, be warmed up to 70 DEG C～75 DEG C, be subsequently adding γ-aminopropyl that step one weighs
Triethoxysilane, then heat up, treat that temperature reaches 80 DEG C～85 DEG C, react 1h ± 5min；
Four, after reaction terminates, cooling, wait to cool to 70 DEG C～75 DEG C, add B, then heat up, treat that temperature reaches
80 DEG C～85 DEG C, react 200min ± 10min；
Five, after reaction terminates, it is cooled to less than 40 DEG C and the material in container is poured out, obtain phenolic resin.
The preparation method of a kind of low water absorbable phenolic resin insulating cement the most according to claim 2, it is characterised in that: step
Rapid one weighs phenol 172 parts by weight.
The preparation method of a kind of low water absorbable phenolic resin insulating cement the most according to claim 2, it is characterised in that:
Step one weighs NaOH solution 17 parts by weight.
The preparation method of a kind of low water absorbable phenolic resin insulating cement the most according to claim 2, it is characterised in that step
One weighs formalin 310 parts by weight.
The preparation method of a kind of low water absorbable phenolic resin insulating cement the most according to claim 2, it is characterised in that: step
Rapid one weighs gamma-aminopropyl-triethoxy-silane 7.2 parts by weight.
The preparation method of a kind of low water absorbable phenolic resin insulating cement the most according to claim 2, it is characterised in that: step
NaOH solution described in rapid one is the NaOH aqueous solution of mass fraction 40%.
The preparation method of a kind of low water absorbable phenolic resin insulating cement the most according to claim 2, it is characterised in that: step
Quality is formalin gross mass the 80% of a rapid A.
The preparation method of a kind of low water absorbable phenolic resin insulating cement the most according to claim 2, it is characterised in that: step
Quality is formalin gross mass the 20% of a rapid B.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610150193.8A CN105754062B (en) | 2016-03-15 | 2016-03-15 | A kind of low water absorbable phenolic resin insulating cement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610150193.8A CN105754062B (en) | 2016-03-15 | 2016-03-15 | A kind of low water absorbable phenolic resin insulating cement |
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| CN105754062A true CN105754062A (en) | 2016-07-13 |
| CN105754062B CN105754062B (en) | 2018-01-23 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115418881A (en) * | 2022-09-16 | 2022-12-02 | 江苏亚振电力有限公司 | Preparation process of high-performance shielding insulating paper for high-voltage transformer |
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| CN105131877A (en) * | 2015-08-24 | 2015-12-09 | 江西省科学院应用化学研究所 | Silane modified phenolic resin adhesive |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190996A (en) * | 2010-03-08 | 2011-09-21 | 新沂市张氏磨具发展有限公司 | Quick-curing adhesive and preparation method thereof |
| CN102241804A (en) * | 2011-05-12 | 2011-11-16 | 四川上之登新材料有限公司 | Preparation method of coupling phenolic resin used for drilling fluid |
| CN102408681A (en) * | 2011-09-10 | 2012-04-11 | 广东东阳光铝业股份有限公司 | Composite material for packaging and preparation method thereof |
| CN102675572A (en) * | 2012-05-08 | 2012-09-19 | 浙江大学 | Application of organic silicon modifier in modified thermosetting phenolic resin |
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| CN115418881A (en) * | 2022-09-16 | 2022-12-02 | 江苏亚振电力有限公司 | Preparation process of high-performance shielding insulating paper for high-voltage transformer |
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| CN105754062B (en) | 2018-01-23 |
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