CN106317764A - Modification method for improving toughness and flame retardance of phenolic resin - Google Patents
Modification method for improving toughness and flame retardance of phenolic resin Download PDFInfo
- Publication number
- CN106317764A CN106317764A CN201610763179.5A CN201610763179A CN106317764A CN 106317764 A CN106317764 A CN 106317764A CN 201610763179 A CN201610763179 A CN 201610763179A CN 106317764 A CN106317764 A CN 106317764A
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- phenolic resin
- modified
- toughness
- flammability
- modifying
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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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention relates to a modification method for improving toughness and flame retardance of phenolic resin. The modification method for improving toughness and flame retardance of phenolic resin comprises steps as follows: tung oil and phenolic resin are mixed and placed in a reactor, polyvinyl butyral is slowly added, and a phenolic resin mixed liquid is obtained; the phenolic resin mixed liquid is distilled and condensed, primary modified phenolic resin is obtained; nanometer copper oxide is supported on montmorillonite and modified montmorillonite is obtained; the modified montmorillonite and the primary modified phenolic resin are heated, a reactor cover is opened after the mixture is cooled to the room temperature, a modified phenolic resin rough liquid is taken out for filtration and purification, and a finished product is obtained. According to the modification method for improving toughness and flame retardance of phenolic resin, phenolic resin is subjected to toughness enhancement modification by the aid of a toughening agent, then modified montmorillonite and phenolic resin with toughness enhanced are heated, the flame retardance of phenolic resin is improved, and phenolic resin with toughness and flame retardance improved has wider application.
Description
Technical field
The present invention relates to the method for modifying of a kind of resin, particularly relate to a kind of for improving phenolic resin toughness and anti-flammability
Method of modifying.
Background technology
2402 phenolic resin are a kind of 100% fat-soluble phenolic resin, are butyl rubber, natural gum, butadiene-styrene rubber, fourth silica gel
Deng the vulcanizing agent of rubber, especially for the sulfuration of butyl rubber, improve the thermostability of butyl rubber.In coatings industry, 2402 phenol
It is former that urea formaldehyde can be used for producing in outdoor enamel, floor paint, marine paint, antirust paint, water color ink and thin-layer rust-preventative oil product
Material, the nitrate paint paint film in coating made with drying oil heating has good gloss.Producing 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 viscosifier and use, in order to improve
Product serviceability and life-span.
Along 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 affected by nature, the fragility of such as 2402 phenolic resin is bigger, poor fire, poor electrical performance etc. so that
In some industrial circles, the range of 2402 phenolic resin is still by various restrictions.
Summary of the invention
Embodiment of the present invention technical problem to be solved is, the fragility for 2402 phenolic resin is bigger, fire-retardant
Property is poor so that in some industrial circles, the range of 2402 phenolic resin is still by the problem of various restrictions, it is proposed that one
Plant the method for modifying for improving phenolic resin toughness and anti-flammability.
In order to solve above-mentioned technical problem, embodiments provide a kind of for improving phenolic resin toughness and fire-retardant
The method of modifying of property, this method of modifying being used for improving phenolic resin toughness and anti-flammability comprises the following steps: by Oleum Verniciae fordii and phenol
Put in reactor after urea formaldehyde mixing, and be slowly added to polyvinyl butyral resin, at 250 DEG C, obtain phenol after high-speed stirred 2h
Urea formaldehyde mixed liquor；Phenolic resin mixed liquor is distilled, then condensation process, obtain a phenol-formaldehyde resin modified；By receiving
Nano cupric oxide is supported in montmorillonite by the mass ratio 1:50 of rice copper oxide and montmorillonite, obtains modified montmorillonoid；By modification
Montmorillonite is total to hot 2h in acid condition with a phenol-formaldehyde resin modified in reactor, opens reaction after being cooled to room temperature again
Kettle cover, takes out the thick liquid of phenol-formaldehyde resin modified；Carry out thick for phenol-formaldehyde resin modified liquid filtering and purify, obtain the one-tenth of phenol-formaldehyde resin modified
Product.
Wherein, the Oleum Verniciae fordii, the phenolic resin that add in reactor are 100:100:3 with the mass ratio of polyvinyl butyral resin.
Wherein, the process being slowly added to polyvinyl butyral resin is: the amount of polyvinyl butyral resin uniformly added in 1h
Enter in reactor.
Wherein, the method preparing nano cupric oxide: cupric oxide powder is dissolved in 15wt%H2O2In solution, move into reaction
Stirring 1h in still, react 18h at 180 DEG C, reaction is cooled to room temperature, by the product dehydrated alcohol obtained and distillation after terminating
Water washs centrifugation after the removal of impurity successively, is finally dried and i.e. can get nano cupric oxide powder.
Wherein, the preparation method of modified montmorillonoid: nano oxidized copper powders is dissolved in 10wt%H2O2In solution, then
Add montmorillonite, after stirring under the conditions of reaction temperature is 35 DEG C, stand 5h, filtering drying, obtain 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.
Implement the embodiment of the present invention, have the advantages that the present invention provides 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, then by by nano oxidized
Copper is supported in montmorillonite, by montmorillonite with toughness reinforcing after phenolic resin altogether heat, improve the anti-flammability of phenolic resin, toughness and
The raising of fire resistance makes the purposes of phenolic resin wider.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
In having technology to describe, the required accompanying drawing used is briefly described, it should be apparent that, the accompanying drawing in describing below is only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to
Other accompanying drawing is obtained according to these accompanying drawings.
Fig. 1 is the flow process signal of a kind of method of modifying for improving phenolic resin toughness and anti-flammability that the present invention provides
Figure.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments wholely.Based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under not making creative work premise
Embodiment, broadly falls into the scope of protection of the invention.
The invention provides a kind of method of modifying for improving phenolic resin toughness and anti-flammability, refer to Fig. 1, Fig. 1
It it is the schematic flow sheet of a kind of method of modifying for improving phenolic resin toughness and anti-flammability that the present invention provides.This is used for carrying
The method of modifying of high phenolic resin toughness and anti-flammability comprises the following steps:
(1), with phenolic resin as raw material, put in reactor after Oleum Verniciae fordii is mixed with phenolic resin, and be slowly added to gather
Vinyl butyral (Oleum Verniciae fordii, phenolic resin are 100:100:3 with the mass ratio of polyvinyl butyral resin), at 250 DEG C at a high speed
Phenolic resin mixed liquor is obtained after stirring 2h.The process being slowly added to polyvinyl butyral resin is: by described polyethylene in 1h
The amount of butyral is even added in reactor.
(2), phenolic resin mixed liquor is distilled, then condensation process, obtain a phenol-formaldehyde resin modified.
(3), cupric oxide powder is dissolved in 15wt%H2O2In solution, move into and reactor stirs 1h, anti-at 180 DEG C
Answering 18h, reaction is cooled to room temperature after terminating, the product dehydrated alcohol obtained and distilled water are washed successively after the removal of impurity from
The heart separates, and is finally dried and i.e. can get nano cupric oxide powder.Nano oxidized copper powders is dissolved in 10wt%H2O2In solution,
It is subsequently adding montmorillonite, after stirring under the conditions of reaction temperature is 35 DEG C, stands 5h, filtering drying, obtain modified illiteracy and take off
Soil.Wherein, the mass ratio 1:50 of nano cupric oxide and montmorillonite.
(4), according to modified montmorillonoid and a phenol-formaldehyde resin modified the amount that mass ratio is 1:10 by modified montmorillonoid with
One time phenol-formaldehyde resin modified is total to hot 2h in acid condition in reactor, and temperature is 60 DEG C, opens after being cooled to room temperature again
Reaction kettle cover, takes out the thick liquid of phenol-formaldehyde resin modified.
(5), by the thick liquid of phenol-formaldehyde resin modified of gained in step (4) carry out filtering purifying, obtain phenol-formaldehyde resin modified
Finished product.
Implement the embodiment of the present invention, have the advantages that the present invention provides 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, then by by nano oxidized
Copper is supported in montmorillonite, by montmorillonite with toughness reinforcing after phenolic resin altogether heat, improve the anti-flammability of phenolic resin, toughness and
The raising of fire resistance makes the purposes of phenolic resin wider.
These are only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and
Within principle, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (7)
1. the method for modifying being used for improving phenolic resin toughness and anti-flammability, it is characterised in that comprise the following steps:
(1), with phenolic resin as raw material, put in reactor after Oleum Verniciae fordii 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；
(2), the phenolic resin mixed liquor of gained in step (1) is distilled, then condensation process, obtain a modified phenolic
Resin；
(3), by the mass ratio 1:50 of nano cupric oxide and montmorillonite, nano cupric oxide is supported in montmorillonite, obtains modified illiteracy
De-soil；
(4), modified montmorillonoid is total in acid condition with a phenol-formaldehyde resin modified of gained in step (2) in reactor
Hot 2h, opens reaction kettle cover again after being cooled to room temperature, take out the thick liquid of phenol-formaldehyde resin modified；
(5), by the thick liquid of phenol-formaldehyde resin modified of gained in step (4) carry out filtering purifying, obtain the finished product of phenol-formaldehyde resin modified.
Method of modifying for improving phenolic resin toughness and anti-flammability the most according to claim 1, it is characterised in that
In step (1), the mass ratio of the described Oleum Verniciae fordii added in described reactor, described phenolic resin and described polyvinyl butyral resin
For 100:100:3.
Method of modifying for improving phenolic resin toughness and anti-flammability the most according to claim 2, it is characterised in that
In step (1), the process being slowly added to described polyvinyl butyral resin is: in 1h, the amount by described polyvinyl butyral resin is equal
Even join in described reactor.
Method of modifying for improving phenolic resin toughness and anti-flammability the most according to claim 1, it is characterised in that
In step (3), the method preparing described nano cupric oxide: cupric oxide powder is dissolved in 15wt%H2O2In solution, move into reaction
Stirring 1h in still, react 18h at 180 DEG C, reaction is cooled to room temperature, by the product dehydrated alcohol obtained and distillation after terminating
Water washs centrifugation after the removal of impurity successively, is finally dried and i.e. can get nano cupric oxide powder.
5., according to the method for modifying for improving phenolic resin toughness and anti-flammability described in claim 1 or 4, its feature exists
In, in step (3), the preparation method of described modified montmorillonoid: nano oxidized copper powders is dissolved in 10wt%H2O2Solution
In, it is subsequently adding montmorillonite, after stirring under the conditions of reaction temperature is 35 DEG C, stands 5h, filtering drying, obtain modified illiteracy
De-soil.
Method of modifying for improving phenolic resin toughness and anti-flammability the most according to claim 1, it is characterised in that
In step (4), the mass ratio of described modified montmorillonoid and a phenol-formaldehyde resin modified is 1:10.
7., according to the method for modifying for improving phenolic resin toughness and anti-flammability described in claim 1 or 6, its feature exists
In, in step (4), described reactor temperature is 60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Publication Number | Publication Date |
|---|---|
| CN106317764A true CN106317764A (en) | 2017-01-11 |
| CN106317764B CN106317764B (en) | 2019-03-29 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107602786A (en) * | 2017-09-18 | 2018-01-19 | 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 |
-
2016
- 2016-08-30 CN CN201610763179.5A patent/CN106317764B/en active Active
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 |
|---|
| 伊廷会: "酚醛树脂高性能化改性研究进展", 《热固性树脂》 * |
| 刘世强等: "改性酚醛树脂的研究进展", 《热固性树脂》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107602786A (en) * | 2017-09-18 | 2018-01-19 | 成都道立福科技有限公司 | A kind of preparation method of tung oil-modified phenolic resin |
| 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 |
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| Publication number | Publication date |
|---|---|
| CN106317764B (en) | 2019-03-29 |
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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. |