CN105754062B - A kind of low water absorbable phenolic resin insulating cement - Google Patents
A kind of low water absorbable phenolic resin insulating cement Download PDFInfo
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- CN105754062B CN105754062B CN201610150193.8A CN201610150193A CN105754062B CN 105754062 B CN105754062 B CN 105754062B CN 201610150193 A CN201610150193 A CN 201610150193A CN 105754062 B CN105754062 B CN 105754062B
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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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- Phenolic Resins Or Amino Resins (AREA)
Abstract
A kind of low water absorbable phenolic resin insulating cement, the present invention relates to a kind of phenolic resin insulating cement and preparation method thereof, more particularly to a kind of low water absorbable phenolic resin insulating cement and preparation method thereof.The invention aims to solve the problem of existing phenolic resin water imbibition is strong and absorption speed is fast, causes decreasing insulating.The present invention low water absorbable phenolic resin insulating cement be by weight percentage 40%~50% by 155 parts~190 parts of phenol, 14 parts~20 parts mass fractions NaOH solution, 270 parts~345 parts mass fractions be 37%~39% formalin and 4.7 parts~15 parts of γ aminopropyl triethoxysilanes form；In phenol-formaldehyde resin modified building-up process of the present invention, Silane coupling agent KH550 is added directly into reaction system carries out in-situ polymerization first, make reaction more abundant, technics comparing is simple, easy to operate.
Description
Technical field
The present invention relates to a kind of phenolic resin insulating cement and preparation method thereof, more particularly to a kind of low water absorbable phenolic aldehyde tree
Fat 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.It is but heat cured
Very high water imbibition is still had after phenolic resin curing, reason is that there is the phenolic hydroxyl group of polarity and methylol, foundation thereon
The similar principle to mix, the hydroxyl of polarity run into the water of polarity, it is easy to reference to causing phenolic resin to absorb water, thus make phenol
, sex chromosome mosaicism safe to use be present in the decreasing insulating of urea formaldehyde in humid conditions.Therefore, phenolic resin insulating properties is stablized
The effect of hydroxyl must be just limited, reduces the water imbibition of phenolic resin, frequently with following two methods:
(l) phenolic hydroxyl group is blocked.
(2) other components are introduced chemical reaction occurs with phenolic resin or partly mixes, separates or surround phenolic hydroxyl group.
Usual researcher is often with dimethylbenzene phenol-formaldehyde resin modified, thus modified phenolic resin water resistance, alkali resistance, tough
Property and mechanical strength all obtain a certain degree of raising, 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 improve its fragility, improve bonding strength, shorten solidification
Time, but the water imbibition of modified phenolic resin does not vary widely, water absorption rate is still larger, and partially modified method
Toxic agent has been used, it is poor for applicability.Therefore, a kind of suitable harmless method of modifying need to be found to reduce phenolic aldehyde tree
The water imbibition of fat, keep its insulating properties.
The content of the invention
Existing phenolic resin water imbibition is strong and absorption speed is fast the invention aims to solving, and causes insulating properties
The problem of decline, and provide a kind of preparation method of the excellent phenolic resin insulating cement of low water absorbable permanent insulation.
A kind of low water absorbable phenolic resin insulating cement in parts by weight by 155 parts~190 parts of phenol, 14 parts~20 parts
NaOH solution, 270 parts~345 parts of formalin and 4.7 parts~15 parts of gamma-aminopropyl-triethoxy-silane composition；It is described
NaOH solution is the NaOH aqueous solution of mass fraction 40%~50%, and the formalin is mass fraction 37% -39%%
Formalin.
A kind of preparation method of low water absorbable phenolic resin insulating cement, is carried out according to the following steps：
First, weigh in parts by weight 155 parts~190 parts phenol, 14 parts~20 parts of NaOH solution, 270 parts~345 parts
Formalin and 4.7 parts~15 parts of gamma-aminopropyl-triethoxy-silane (Silane coupling agent KH550)；The formaldehyde that will be weighed
Solution is divided into two parts of A and B, and wherein A quality is that 70%~85%, B of formalin gross mass quality is that formalin is total
The 15%~30% of quality；The NaOH solution is the NaOH aqueous solution of mass fraction 40%~50%, and the formalin is
The formalin of mass fraction 37% -39%；
2nd, the phenol for taking step 1 to weigh is added in container, is melted at a temperature of 40 DEG C~50 DEG C, is then added step 1
The NaOH solution weighed, mixed solution is obtained, react 8min~12min；
3rd, A is added into step 2 mixed liquor, is warming up to 70 DEG C~75 DEG C, then add γ-ammonia third that step 1 weighs
Ethyl triethoxy silicane alkane, then heat up, treat that temperature reaches 80 DEG C~85 DEG C, react 1h ± 5min；
4th, 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；
5th, after reaction terminates, less than 40 DEG C is cooled to and pours out the material in container, obtains phenolic resin.
The present invention the advantage is that relative to prior art：
1. the water imbibition that can not only reduce thermosetting phenolic resin after KH550 modifications, improving insulating properties, and use
Modified resinoid bond or the product of dipping, Physical and mechanical properties also have some improvement.Prepared by the present invention
The water absorption test front volume resistance that KH550 is modified low water absorbable insulating cement is 1.1 × 109—2.38×109Ω, and commonly not
Modified is only 0.27 × 109Ω；After water absorption test, the volume resistance for 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, low water absorbable of the invention are modified exhausted
The resistivity of edge glue is higher than common insulation phenolic resin；The phenolic resin insulating cement bending resistance obtained by preparation method of the present invention is strong
Spend for 102.58MPa~149.89MPa, 3%~5% is improved compared with prepared by commonsense method；Obtained by preparation method of the present invention
The phenolic resin insulating cement composite bending modulus arrived is 5.46GPa~10.02GPa, and 4%~8% is improved compared with prepared by commonsense method.
2. it is modified using nontoxic, degradable chemical reagent KH550, environmental protection, and cost is obvious compared with other modifying agent
Reduce.
3. in phenol-formaldehyde resin modified building-up process, Silane coupling agent KH550 is added directly into reaction system first
In-situ polymerization is carried out, makes reaction more abundant, technics comparing is simple, easy to operate.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition between each embodiment
Any combination.
Embodiment one：A kind of low water absorbable phenolic resin insulating cement of present embodiment is in parts by weight by 155
Part~190 parts of phenol, 14 parts~20 parts of NaOH solution, 270 parts~345 parts of formalin and 4.7 parts~15 parts of γ-
Aminopropyl triethoxysilane forms；The NaOH solution be mass fraction 40%~50% the NaOH aqueous solution, the formaldehyde
Solution is the formalin of mass fraction 37% -39%.
Embodiment two：A kind of preparation method of low water absorbable phenolic resin insulating cement of present embodiment, by with
Lower step is carried out：
First, weigh in parts by weight 155 parts~190 parts phenol, 14 parts~20 parts of NaOH solution, 270 parts~345 parts
Formalin and 4.7 parts~15 parts of gamma-aminopropyl-triethoxy-silane；The formalin weighed is divided into two parts of A and B,
Wherein A quality is that 70%~85%, B of formalin gross mass quality is the 15%~30% of formalin gross mass；
The NaOH solution is the NaOH aqueous solution of mass fraction 40%~50%, and the formalin is mass fraction 37% -39%
Formalin；
2nd, the phenol for taking step 1 to weigh is added in container, is melted at a temperature of 40 DEG C~50 DEG C, is then added step 1
The NaOH solution weighed, mixed solution is obtained, react 8min~12min；
3rd, A is added into step 2 mixed liquor, is warming up to 70 DEG C~75 DEG C, then add γ-ammonia third that step 1 weighs
Ethyl triethoxy silicane alkane, then heat up, treat that temperature reaches 80 DEG C~85 DEG C, react 1h ± 5min；
4th, 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；
5th, after reaction terminates, less than 40 DEG C is cooled to and pours out the material in container, obtains phenolic resin.
Embodiment three：Unlike embodiment two, step 1 claims present embodiment in parts by weight
Take 172 parts of phenol.Other steps are identical with embodiment two with parameter.
Embodiment four：Unlike embodiment two, step 1 claims present embodiment in parts by weight
Take 17 parts of NaOH solution.Other steps are identical with embodiment two with parameter.
Embodiment five：Unlike embodiment two, step 1 claims present embodiment in parts by weight
Take 310 parts of formalin.Other steps are identical with embodiment two with parameter.
Embodiment six：Unlike embodiment two, step 1 claims present embodiment in parts by weight
Take 7.2 parts of gamma-aminopropyl-triethoxy-silane.Other steps are identical with embodiment two with parameter.
Embodiment seven：Present embodiment is unlike embodiment two, NaOH solution described in step 1
For the NaOH aqueous solution of mass fraction 40%.Other steps are identical with embodiment two with parameter.
Embodiment eight：For present embodiment unlike embodiment two, step 1 A quality is formaldehyde
The 80% of solution gross mass.Other steps are identical with embodiment two with parameter.
Embodiment nine：For present embodiment unlike embodiment two, step 1 B quality is formaldehyde
The 20% of solution gross mass.Other steps are identical with embodiment two with parameter.
Embodiment 1
A kind of preparation method of low water absorbable phenolic resin insulating cement, is carried out according to the following steps：
First, take 172.4g phenol to add in container, melted at a temperature of 40 DEG C, then adding 17.3g mass fractions is
40% NaOH solution, mixed solution is obtained, react 10min；
2nd, the formaldehyde that mass fraction is 37% -39% is added into step 1 mixed liquor, its quality added is whole
The 80% of the total amount of feeding of formaldehyde in course of reaction, is warming up to 72 DEG C, treats that temperature reaches 82 DEG C, reacts 1h；
3rd, after reaction terminates, cooling, wait to cool to 72 DEG C, add the formaldehyde that mass fraction is 37% -39%, add
Quality be 20% of the total amount of feeding of formaldehyde in whole course of reaction, then heat up, treat that temperature reaches 82 DEG C, reaction
200min；The total amount of feeding of the formaldehyde is 310.4g；
4th, after reaction terminates, less than 40 DEG C is cooled to and pours out the material in container, obtains phenolic resin.
Obtained resin removes volatile matter through drying, and is then handled according to the measure of GBT 1034-2008 plastic ink absorptions
Obtain water absorption rate.
Embodiment 2
A kind of preparation method of low water absorbable phenolic resin insulating cement, is carried out according to the following steps：
First, take 172.4g phenol to add in container, melted at a temperature of 40 DEG C, then adding 17.3g mass fractions is
40% NaOH solution, mixed solution is obtained, react 10min；
2nd, the formaldehyde that mass fraction is 37% -39% is added into step 1 mixed liquor, its quality added is whole
The 80% of the total amount of feeding of formaldehyde in course of reaction, 72 DEG C are warming up to, add gamma-aminopropyl-triethoxy-silane 5.15g and (account for total
System 3%), then heat up, treat that temperature reaches 82 DEG C, react 1h；
3rd, after reaction terminates, cooling, wait to cool to 72 DEG C, add the formaldehyde that mass fraction is 37% -39%, add
Quality be 20% of the total amount of feeding of formaldehyde in whole course of reaction, then heat up, treat that temperature reaches 82 DEG C, reaction
200min；The total amount of feeding of the formaldehyde is 310.4g；
4th, after reaction terminates, less than 40 DEG C is cooled to and pours out the material in container, obtains phenolic resin.
Obtained resin removes volatile matter through drying, and is then handled according to the measure of GBT 1034-2008 plastic ink absorptions
Obtain water absorption rate.
Embodiment 3
A kind of preparation method of low water absorbable phenolic resin insulating cement, is carried out according to the following steps：
First, take 172.4g phenol to add in container, melted at a temperature of 40 DEG C, then adding 17.3g mass fractions is
40% NaOH solution, mixed solution is obtained, react 10min；
2nd, the formaldehyde that mass fraction is 37% -39% is added into step 1 mixed liquor, its quality added is whole
The 80% of the total amount of feeding of formaldehyde in course of reaction, 72 DEG C are warming up to, add gamma-aminopropyl-triethoxy-silane 8.12g and (account for total
System 5%), then heat up, treat that temperature reaches 82 DEG C, react 1h；
3rd, after reaction terminates, cooling, wait to cool to 72 DEG C, add the formaldehyde that mass fraction is 37% -39%, add
Quality be 20% of the total amount of feeding of formaldehyde in whole course of reaction, then heat up, treat that temperature reaches 82 DEG C, reaction
200min；The total amount of feeding of the formaldehyde is 310.4g；
4th, after reaction terminates, less than 40 DEG C is cooled to and pours out the material in container, obtains phenolic resin.
Obtained resin removes volatile matter through drying, and is then handled according to the measure of GBT 1034-2008 plastic ink absorptions
Obtain water absorption rate.
Embodiment 4
A kind of preparation method of low water absorbable phenolic resin insulating cement, is carried out according to the following steps：
First, take 172.4g phenol to add in container, melted at a temperature of 40 DEG C, then adding 17.3g mass fractions is
40% NaOH solution, mixed solution is obtained, react 10min；
2nd, the formaldehyde that mass fraction is 37% -39% is added into step 1 mixed liquor, its quality added is whole
The 80% of the total amount of feeding of formaldehyde in course of reaction, 72 DEG C are warming up to, add gamma-aminopropyl-triethoxy-silane 13.8g and (account for total
System 8%), then heat up, treat that temperature reaches 82 DEG C, react 1h；
3rd, after reaction terminates, cooling, wait to cool to 72 DEG C, add the formaldehyde that mass fraction is 37% -39%, add
Quality be 20% of the total amount of feeding of formaldehyde in whole course of reaction, then heat up, treat that temperature reaches 82 DEG C, reaction
200min；The total amount of feeding of the formaldehyde is 310.4g
4th, after reaction terminates, less than 40 DEG C is cooled to and pours out the material in container, obtains phenolic resin.
Obtained resin removes volatile matter through drying, and is then handled according to the measure of GBT 1034-2008 plastic ink absorptions
Obtain water absorption rate.
Specifically carried out by the following method according to the measure processing of GBT 1034-2008 plastic ink absorptions：On request by difference
The liquid phenolic resin of species is placed on from molding jig, and diameter 100mm or so disk, thickness 1mm or so is made), by rank
Ladder heating drying mode (50 DEG C-some hours, 80 DEG C of -30min, 100 DEG C of -30min, 130 DEG C of -30min, until phenolic resin
Cure hard, completely disengage from processing release paper.
1. above-mentioned pure resin glue sample is put into 50 DEG C of baking oven and dries at least more than 24h, it is then cold in drier
But room temperature is arrived, weighs the quality of each sample, 0.0001g (quality m1) is accurate to and repeats this step and no longer change to quality.
2. sample is put into the container for filling distilled water, water temperature control is in 23 DEG C or room temperature, after soaking 24h, taking-up examination
Sample, all water of specimen surface is wiped rapidly with dry cloth or filter paper is cleaned, the quality of each sample is weighed again, is accurate to
0.0001g (quality m2).After sample is taken out from water, it should complete to weigh in 1min.
c：The water suction mass fraction of sample
m1：The quality of sample, unit of gram (g) after being dried before immersion
m2：The quality of sample, unit of gram (g) after immersion
Table 1 is the resistance value before and after the water imbibition and water absorption test of all types of resins
Conclusion：The water imbibition of thermosetting resin after modified processing reduces.On the whole, silane coupler is utilized
KH550 is modified, and 3-8% dosages all play a role, 5% content will more other resins it is more quite a lot of.
Claims (8)
- A kind of 1. low water absorbable phenolic resin insulating cement, it is characterised in that：The phenolic resin insulating cement is in parts by weight by 155 Part~190 parts of phenol, 14 parts~20 parts of NaOH solution, 270 parts~345 parts of formalin and 4.7 parts~15 parts of γ- Aminopropyl triethoxysilane forms；The NaOH solution be mass fraction 40%~50% the NaOH aqueous solution, the formaldehyde Solution is the formalin of mass fraction 37%~39%；A kind of preparation method of described low water absorbable phenolic resin insulating cement is carried out according to the following steps：First, weigh in parts by weight 155 parts~190 parts phenol, 14 parts~20 parts of NaOH solution, 270 parts~345 parts of first Aldehyde solution and 4.7 parts~15 parts of gamma-aminopropyl-triethoxy-silane；The formalin weighed is divided into two parts of A and B, wherein A Quality be that 70%~85%, the B quality of formalin gross mass is the 15%~30% of formalin gross mass；It is described NaOH solution is the NaOH aqueous solution of mass fraction 40%~50%, and the formalin is the first of mass fraction 37%~39% The aldehyde aqueous solution；2nd, the phenol for taking step 1 to weigh is added in container, is melted at a temperature of 40 DEG C~50 DEG C, is then added step 1 and is weighed NaOH solution, obtain mixed solution, react 8min~12min；3rd, A is added into step 2 mixed liquor, is warming up to 70 DEG C~75 DEG C, then add γ-aminopropyl three that step 1 weighs Ethoxysilane, then heat up, treat that temperature reaches 80 DEG C~85 DEG C, react 1h ± 5min；4th, 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；5th, after reaction terminates, less than 40 DEG C is cooled to and pours out the material in container, obtains phenolic resin.
- A kind of 2. low water absorbable phenolic resin insulating cement according to claim 1, it is characterised in that：Step 1 is by weight Number weighs 172 parts of phenol.
- A kind of 3. low water absorbable phenolic resin insulating cement according to claim 1, it is characterised in that：Step 1 is by weight Number weighs 17 parts of NaOH solution.
- 4. a kind of low water absorbable phenolic resin insulating cement according to claim 1, it is characterised in that step 1 is by weight Number weighs 310 parts of formalin.
- A kind of 5. low water absorbable phenolic resin insulating cement according to claim 1, it is characterised in that：Step 1 is by weight Number weighs 7.2 parts of gamma-aminopropyl-triethoxy-silane.
- A kind of 6. low water absorbable phenolic resin insulating cement according to claim 1, it is characterised in that：NaOH described in step 1 Solution is the NaOH aqueous solution of mass fraction 40%.
- A kind of 7. low water absorbable phenolic resin insulating cement according to claim 1, it is characterised in that：Step 1 A quality For the 80% of formalin gross mass.
- A kind of 8. low water absorbable phenolic resin insulating cement according to claim 1, it is characterised in that：Step 1 B quality For the 20% of formalin gross mass.
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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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| 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 |
| CN104403261A (en) * | 2014-09-04 | 2015-03-11 | 中国建筑材料科学研究总院 | Inorganic material-modified phenolic foam insulation material with low water absorption and preparation method thereof |
| 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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2016
- 2016-03-15 CN CN201610150193.8A patent/CN105754062B/en active Active
Patent Citations (6)
| 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 |
| CN104403261A (en) * | 2014-09-04 | 2015-03-11 | 中国建筑材料科学研究总院 | Inorganic material-modified phenolic foam insulation material with low water absorption and preparation method thereof |
| 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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