CN106317764B - A kind of method of modifying improving phenolic resin toughness and anti-flammability - Google Patents
A kind of method of modifying improving phenolic resin toughness and anti-flammability Download PDFInfo
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- CN106317764B CN106317764B CN201610763179.5A CN201610763179A CN106317764B CN 106317764 B CN106317764 B CN 106317764B CN 201610763179 A CN201610763179 A CN 201610763179A CN 106317764 B CN106317764 B CN 106317764B
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- phenolic resin
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- flammability
- toughness
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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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
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
- C08G8/32—Chemically modified polycondensates by organic acids or derivatives thereof, e.g. fatty oils
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The present invention relates to a kind of for improving the method for modifying of phenolic resin toughness and anti-flammability, this is used to improve the method for modifying of phenolic resin toughness and anti-flammability the following steps are included: being put into reactor after tung oil is mixed with phenolic resin, and it is slowly added to polyvinyl butyral, obtain phenolic resin mixed liquor；Phenolic resin mixed liquor is distilled, is condensed, a phenol-formaldehyde resin modified is obtained；Nano cupric oxide is supported in montmorillonite, modified montmorillonoid is obtained；It by modified montmorillonoid and a phenol-formaldehyde resin modified heat together, is cooled to after room temperature and opens reaction kettle cover again, take out phenol-formaldehyde resin modified crude liquid and be filtered purification, obtain finished product.Provided by the present invention for improving modification of the method for modifying of phenolic resin toughness and anti-flammability by toughener to phenolic resin progress toughness enhancing, then by by the phenolic resin heat together after modified montmorillonoid and toughening, the anti-flammability of phenolic resin is improved, the raising of toughness and flame retardant property keeps the purposes of phenolic resin wider.
Description
Technical field
The present invention relates to a kind of method of modifying of resin, more particularly to one kind is for improving phenolic resin toughness and anti-flammability
Method of modifying.
Background technique
2402 phenolic resin are a kind of 100% fat-soluble phenolic resin, are butyl rubber, natural gum, butadiene-styrene rubber, fourth silica gel
The vulcanizing agent of equal rubber, is especially used for the vulcanization of butyl rubber, improves the heat resistance of butyl rubber.In coatings industry, 2402 phenol
Urea formaldehyde can be used for producing the original in outdoor enamel, floor paint, marine paint, antirust paint, water-based ink and thin-layer rust-preventative oil product
Material, heating manufactured nitrate paint paint film in coating with drying oil has good gloss.In production terylene insulating tape, oil pipe
In the industrial gummed tape field of dope etc., 2402 phenolic resin also serve as vulcanizing agent, reinforcing agent and tackifier and use, to improve
Product service performance and service life.
With the development of society, before 2402 phenolic resin are in an increasingly wide range of applications in other field of industrial production
Scape, but influenced by nature, for example the brittleness of 2402 phenolic resin is bigger, poor fire, poor electrical performance etc., so that
In some industrial circles, the use scope of 2402 phenolic resin is still by various limitations.
Summary of the invention
The technical problem to be solved by the embodiment of the invention is that the brittleness for 2402 phenolic resin is bigger, fire-retardant
Property is poor so that in some industrial circles, the use scope of 2402 phenolic resin still by various limitations the problem of, propose one
Plant the method for modifying for improving phenolic resin toughness and anti-flammability.
In order to solve the above-mentioned technical problem, the embodiment of the invention provides one kind for improving phenolic resin toughness and fire-retardant
The method of modifying of property, this is used to improve the method for modifying of phenolic resin toughness and anti-flammability the following steps are included: by tung oil and phenol
It is put into reactor after urea formaldehyde mixing, and is slowly added to polyvinyl butyral, obtain phenol after high-speed stirred 2h at 250 DEG C
Urea formaldehyde mixed liquor；Phenolic resin mixed liquor is distilled, then condensation process, obtains a phenol-formaldehyde resin modified；By receiving
Nano cupric oxide is supported in montmorillonite by rice copper oxide and the mass ratio 1:50 of montmorillonite, obtains modified montmorillonoid；It will be modified
Montmorillonite and a phenol-formaldehyde resin modified heat together 2h in reaction kettle in acid condition, are cooled to after room temperature and open reaction again
Kettle cover takes out phenol-formaldehyde resin modified crude liquid；Phenol-formaldehyde resin modified crude liquid is filtered purification, obtain phenol-formaldehyde resin modified at
Product.
Wherein, the mass ratio of the tung oil, phenolic resin and the polyvinyl butyral that are added in reactor is 100:100:3.
Wherein, the process for being slowly added to polyvinyl butyral is: uniformly adding the amount of polyvinyl butyral in 1h
Enter into reactor.
Wherein, it prepares the method for nano cupric oxide: cupric oxide powder is dissolved in 15wt%H2O2In solution, reaction is moved into
1h is stirred in kettle, 18h is reacted at 180 DEG C, is cooled to room temperature after reaction, by obtained product dehydrated alcohol and distillation
Water is centrifugated after successively washing removal impurity, and finally nano oxidized copper powders can be obtained in drying.
Wherein, nano oxidized copper powders the preparation method of modified montmorillonoid: are dissolved in 10wt%H2O2In solution, then
Montmorillonite is added, after mixing evenly under the conditions of reaction temperature is 35 DEG C, stands 5h, filtering drying obtains modified montmorillonoid.
Wherein, the mass ratio of modified montmorillonoid and a phenol-formaldehyde resin modified is 1:10.
Wherein, reactor temperature is 60 DEG C.
The implementation of the embodiments of the present invention has the following beneficial effects: provided by the present invention for improve phenolic resin toughness and
The method of modifying of anti-flammability directly carries out the modification of toughness enhancing by toughener to phenolic resin, and then passing through will be nano oxidized
Copper is supported in montmorillonite, by the phenolic resin heat together after montmorillonite and toughening, improves the anti-flammability of phenolic resin, toughness and
The raising of flame retardant property keeps the purposes of phenolic resin wider.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is that a kind of process for improving the method for modifying of phenolic resin toughness and anti-flammability provided by the invention is illustrated
Figure.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The present invention provides a kind of for improving the method for modifying of phenolic resin toughness and anti-flammability, referring to Figure 1, Fig. 1
It is provided by the invention a kind of for improving the flow diagram of the method for modifying of phenolic resin toughness and anti-flammability.This is used to mention
The method of modifying of high phenolic resin toughness and anti-flammability the following steps are included:
(1), it using phenolic resin as raw material, is put into reactor after tung oil is mixed with phenolic resin, and is slowly added to gather
Vinyl butyral (mass ratio of tung oil, phenolic resin and polyvinyl butyral is 100:100:3), the high speed at 250 DEG C
Phenolic resin mixed liquor is obtained after stirring 2h.The process for being slowly added to polyvinyl butyral is: by the polyethylene in 1h
The amount of butyral is even added in reactor.
(2), phenolic resin mixed liquor is distilled, then condensation process, obtains a phenol-formaldehyde resin modified.
(3), cupric oxide powder is dissolved in 15wt%H2O2In solution, moves into reaction kettle and stir 1h, it is anti-at 180 DEG C
Answer 18h, be cooled to room temperature after reaction, by obtained product dehydrated alcohol and distilled water successively wash removal impurity after from
Heart separation, finally nano oxidized copper powders can be obtained in drying.Nano oxidized copper powders are dissolved in 10wt%H2O2In solution,
Then montmorillonite is added, after mixing evenly under the conditions of reaction temperature is 35 DEG C, stands 5h, filtering drying obtains modified cover and takes off
Soil.Wherein, the mass ratio 1:50 of nano cupric oxide and montmorillonite.
(4), according to the mass ratio of modified montmorillonoid and a phenol-formaldehyde resin modified be 1:10 amount by modified montmorillonoid with
The heat together 2h in reaction kettle, temperature are 60 DEG C to phenol-formaldehyde resin modified in acid condition, are opened again after being cooled to room temperature
Kettle cover is reacted, phenol-formaldehyde resin modified crude liquid is taken out.
(5), phenol-formaldehyde resin modified crude liquid obtained in step (4) is filtered purification, obtains phenol-formaldehyde resin modified
Finished product.
The implementation of the embodiments of the present invention has the following beneficial effects: provided by the present invention for improve phenolic resin toughness and
The method of modifying of anti-flammability directly carries out the modification of toughness enhancing by toughener to phenolic resin, and then passing through will be nano oxidized
Copper is supported in montmorillonite, by the phenolic resin heat together after montmorillonite and toughening, improves the anti-flammability of phenolic resin, toughness and
The raising of flame retardant property keeps the purposes of phenolic resin wider.
The above is merely preferred embodiments of the present invention, be not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (5)
1. a kind of for improving the method for modifying of phenolic resin toughness and anti-flammability, which comprises the following steps:
(1), it using phenolic resin as raw material, is put into reactor after tung oil is mixed with phenolic resin, and be slowly added to polyethylene
Butyral obtains phenolic resin mixed liquor at 250 DEG C after high-speed stirred 2h, the tung oil that is added in the reactor,
The mass ratio of the phenolic resin and the polyvinyl butyral is 100:100:3；
(2), phenolic resin mixed liquor obtained in step (1) is distilled, then condensation process, obtains a modified phenolic
Resin；
(3), nano cupric oxide is supported in montmorillonite by nano cupric oxide and the mass ratio 1:50 of montmorillonite, obtains modified illiteracy
De- soil；
(4), a phenol-formaldehyde resin modified obtained in modified montmorillonoid and step (2) is total in reaction kettle in acid condition
The mass ratio of hot 2h, the modified montmorillonoid and a phenol-formaldehyde resin modified is 1:10, is cooled to after room temperature and opens reaction again
Kettle cover takes out phenol-formaldehyde resin modified crude liquid；
(5), phenol-formaldehyde resin modified crude liquid obtained in step (4) is filtered purification, obtains the finished product of phenol-formaldehyde resin modified.
2. according to claim 1 for improving the method for modifying of phenolic resin toughness and anti-flammability, which is characterized in that
In step (1), the process for being slowly added to the polyvinyl butyral is: in 1h that the amount of the polyvinyl butyral is equal
It is even to be added in the reactor.
3. according to claim 1 for improving the method for modifying of phenolic resin toughness and anti-flammability, which is characterized in that
In step (3), cupric oxide powder the method for preparing the nano cupric oxide: is dissolved in 15wt%H2O2In solution, reaction is moved into
1h is stirred in kettle, 18h is reacted at 180 DEG C, is cooled to room temperature after reaction, by obtained product dehydrated alcohol and distillation
Water is centrifugated after successively washing removal impurity, and finally nano oxidized copper powders can be obtained in drying.
4. according to claim 1 or 3 for improving the method for modifying of phenolic resin toughness and anti-flammability, feature exists
In nano oxidized copper powders the preparation method of the modified montmorillonoid: are dissolved in 10wt%H in step (3)2O2Solution
In, montmorillonite is then added, after mixing evenly under the conditions of reaction temperature is 35 DEG C, stands 5h, filtering drying obtains modified illiteracy
De- soil.
5. according to claim 1 for improving the method for modifying of phenolic resin toughness and anti-flammability, which is characterized in that
In step (4), the reactor temperature is 60 DEG C.
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| CN201610763179.5A CN106317764B (en) | 2016-08-30 | 2016-08-30 | A kind of method of modifying improving phenolic resin toughness and anti-flammability |
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| CN201610763179.5A CN106317764B (en) | 2016-08-30 | 2016-08-30 | A kind of method of modifying improving phenolic resin toughness and anti-flammability |
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| CN106317764B true CN106317764B (en) | 2019-03-29 |
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| CN107378804A (en) * | 2017-08-09 | 2017-11-24 | 安徽昌悌进出口贸易有限公司 | A kind of resin base high cooling efficiency emery wheel material |
| CN107602786B (en) * | 2017-09-18 | 2019-10-29 | 成都道立福科技有限公司 | A kind of preparation method of tung oil-modified phenolic resin |
| CN110667708A (en) * | 2019-09-29 | 2020-01-10 | 重庆千能实业有限公司 | Vehicle roof with high-efficiency heat insulation function |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387822A (en) * | 2014-11-27 | 2015-03-04 | 青岛市市南区隆德中医药研究所 | Matt coating paint |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387822A (en) * | 2014-11-27 | 2015-03-04 | 青岛市市南区隆德中医药研究所 | Matt coating paint |
Non-Patent Citations (2)
| Title |
|---|
| 改性酚醛树脂的研究进展;刘世强等;《热固性树脂》;20160930;第31卷(第05期);64-70 |
| 酚醛树脂高性能化改性研究进展;伊廷会;《热固性树脂》;20010730;第16卷(第04期);29-33 |
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Effective date of registration: 20210416 Address after: 441299 Baozhuang village, Huancheng, Zaoyang City, Xiangyang City, Hubei Province (Chemical Industrial Park) Patentee after: Zaoyang Cixiang Medical Technology Co.,Ltd. Address before: 441200, Xiangfan City, Hubei province Jujube city Wangjiawan Village Patentee before: ZAOYANG ZHONGCHENG CHEMICAL Co.,Ltd. |