CN106589801B - A kind of synthetic method of high oxygen index (OI) phenolic resin - Google Patents
A kind of synthetic method of high oxygen index (OI) phenolic resin Download PDFInfo
- Publication number
- CN106589801B CN106589801B CN201611207579.4A CN201611207579A CN106589801B CN 106589801 B CN106589801 B CN 106589801B CN 201611207579 A CN201611207579 A CN 201611207579A CN 106589801 B CN106589801 B CN 106589801B
- Authority
- CN
- China
- Prior art keywords
- phenolic resin
- boron
- oxygen index
- high oxygen
- synthetic method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
- C08L61/14—Modified phenol-aldehyde condensates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C08J2361/14—Modified phenol-aldehyde condensates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
-
- 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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
A kind of synthetic method of high oxygen index (OI) phenolic resin is related to the synthetic method that phenolic resin provides a kind of high oxygen index (OI) phenolic resin for the high-grade fireproof performance that phenolic resin foam thermal insulation material can be achieved.Two steps of solidification of modified synthesis and foamed phenolic resin including expandable phenolic resin, are as follows：It will be added in the system of phenol, paraformaldehyde, basic polymerization catalyst for the boron-containing compound of interior modification, carry out polymerisation, obtain expandable phenolic resin modified in boron；It will be pre-processed with silane coupling agent for the boron-containing compound of outer modification, pretreated outer modified boron compound is added in expandable phenolic resin modified in boron, cured after inorganic filler, pore creating material, foam stabilizer, curing agent is added, obtains high oxygen index (OI) phenolic resin.
Description
Technical field
The present invention relates to phenolic resin, more particularly, to a kind of synthetic method of high oxygen index (OI) phenolic resin.
Background technology
China's fire of high-rise building takes place frequently, and causes huge property loss and casualties.Currently, construction material is fire-retardant
Problem has become the hot spot paid close attention to both at home and abroad.With China's construction material to it is energy saving/heat preservation and flame retardant property require it is further
It improves, the demand of fire retardant exterior wall thermal insulation material will further increase.Phenolic resin class A foam A thermal insulation material has both fire-retardant, light just
The excellent characteristic such as matter, safety is a kind of quality-high and inexpensive self-flame-retardant foamed plastics, will not melt in combustion
Melt, also not will produce stream drop.It is to improve the conventional method for the shortcomings of its brittleness is big, but compare that toughener is added into phenolic resin
The heat-resisting of phenolic resin, fire resisting and corrosion resistance can be declined after the phenolic resin for being not added with altered contents, toughening.Mesh
It is preceding that there has been no A grades of phenolic foam materials to emerge.
Fire retardant is to improve material flame resistance, reduce material and be ignited probability and inhibit helping of being propagated further of flame
Agent.Fire retardant can be divided into addition type and response type two major classes, the former refers to polymerizeing and the main chain in high polymer in polycondensation process
Or the group with fire retardation is introduced on side chain to reach fire-retardant purpose；The latter refer in polymer material forming process,
It is distributed in material, is divided into as inorganic and organic two class, since organic fire-retardant decomposition product toxicity is big, cigarette by physical mixed
The shortcomings of mist is big is just gradually replaced by inorganic combustion inhibitor such as zinc borate.Zinc borate has significant fire-retardant and smoke suppressing effect, also
High temperature molten drop (high temperature molten drop is the Ignition sources of danger) can be reduced, helps to generate porous carbon layer in material combustion, and this carbon
Layer can be B2O3Stablize, when being used in compounding with antimony oxide, halogen containing flame-retardant, aluminium hydroxide, magnesium hydroxide, has good
Synergistic effect, can reduce the dosage of other fire retardants while improving oxygen index (OI).In addition, zinc borate has under nontoxic, high temperature
The features such as not generating toxic gas is a kind of fire retardant of green non-pollution.
The existing report that phenolic resin is modified using boron-containing compound, such as boron in boron-containing compound and expandability phenol
Complexation reaction occurs for urea formaldehyde, generates phenolic resin Chinese patent CN1844233, the Chinese patent CN101531769 of boron modification,
But the phenolic resin oxygen index (OI) raising obtained by this method is limited, and flame retardant property needs to be further increased.Also have in phenol in document
Boron-containing compound is added in urea formaldehyde building-up process and carries out outer modified Chinese patent CN104650785A, Chinese patent
CN104004319A, but in the work, boron-containing compound is not preprocessed and is directly added into system, causes boron-containing compound
Very weak with the interaction of phenolic aldehyde, most of boron-containing compound fails to be dispersed in phenolic system, greatly reduces and mixes
The effect of miscellaneous modification.But these work be limited to expandable phenolic resin synthesis or phenolic resin solidification and etc.
A certain step introduces boron and is modified, there is not yet it is modified to be carried out at the same time inside and outside substep to phenolic resin with boron simultaneously.
Invention content
The purpose of the present invention is to provide one kind of the high-grade fireproof performance of achievable phenolic resin foam thermal insulation material
The synthetic method of high oxygen index (OI) phenolic resin.
The present invention includes two steps of solidification of the modified synthesis and foamed phenolic resin of expandable phenolic resin, specific to walk
It is rapid as follows：
1) it will be added in the system of phenol, paraformaldehyde, basic polymerization catalyst for the boron-containing compound of interior modification, into
Row polymerisation obtains expandable phenolic resin modified in boron；
2) it will be pre-processed with silane coupling agent for the boron-containing compound of outer modification, by pretreated outer modified boron
Compound is added in expandable phenolic resin modified in the boron that step 1) obtains, and inorganic filler, pore creating material, foam stabilizing is added
Cured after agent, curing agent, obtains high oxygen index (OI) phenolic resin.
In step 1), borate can be used in the boron-containing compound for interior modification, and the borate can be selected from boron
At least one of acid, zinc borate, iron borate, calcium boride etc.；The phenol, paraformaldehyde, basic polymerization catalyst, for interior
The mass ratio of modified boron-containing compound can be：(20~60) ︰ (20~60) ︰ (10~40) ︰ (0.1~10)；The alkalinity is poly-
It closes catalyst and can be selected from least one of potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, magnesium hydroxide etc.；It is described
The thick expandable phenolic resin that viscosity is 1000~6000PaS when modified expandable phenolic resin is 25 DEG C in boron.
In step 2), the boron-containing compound for outer modification can be selected from boron powder, boric acid, zinc borate, iron borate, boron
At least one of sand, calcium boride, diboron trioxide etc.；The silane coupling agent can be selected from KH560, KH550, KH540,
At least one of KH530 etc.；Modified expandable phenolic resin, inorganic filler, pore creating material, foam stabilizer, solidification in the boron
The mass ratio of agent can be (20~70) ︰ (5~50) ︰ (0.1~5) ︰ (0.1~4) ︰ (0.1~10) ︰ (0.1~10)；It is described inorganic
Filler can be selected from least one of aluminium hydroxide, magnesium hydroxide, silica, sodium metasilicate etc.；The pore creating material can be selected from just
At least one of pentane, hydrogen peroxide, AC foaming agents etc.；The foam stabilizer can be selected from tween, organic foam stabilizer, 12
At least one of sodium alkyl sulfate, neopelex, castor oil polyoxyethylene ether etc.；The optional bin cure of curing agent
At least one of acid, phosphoric acid, p-methyl benzenesulfonic acid etc.；The cured temperature can be 40~100 DEG C, and the cured time can be 5
~10min.
Although phenol formaldehyde foam will not melt in combustion, also not will produce stream drop, have excellent anti-flammability,
The advantages that high thermal stability and low smoke density, fire retardant degree is considerably beyond being currently being widely used the bubbles such as polystyrene, polyurethane
Foam material, and dense smoke and poison gas will not be distributed, but the close of the rigid aromatic ring of its structure methylene connection is piled up so that resin
Matrix becomes fragile, thus the slag-off phenomenon of phenol formaldehyde foam is serious, brittleness is big, surface is also easy to produce the weakness such as stress crack, toward phenolic aldehyde tree
It is the conventional method for improving the shortcomings of its brittleness is big that toughener is added in fat, but compared to the phenolic aldehyde tree for being not added with altered contents
Fat, the heat-resisting of phenolic resin, fire resisting and corrosion resistance can be declined after toughening.There has been no A grades of high fire-retardance phenolic aldehyde to steep at present
Foam material emerges.
The present invention be on the basis of existing phenolic resin foam thermal insulation material production technology, to expandable phenolic resin into
The boron modification of row intramolecular, and it is outer to the progress of phenolic resin foam thermal insulation material by adding boron-containing compound in the curing process
It is modified, prepare the foam resin thermal insulation material with high flame resistance.
The main reason for phenol formaldehyde foam non-refractory be connected in phenolic resin phenyl ring C-C key bond energys it is relatively low, and phenol hydroxyl
Base stage is easily aoxidized, therefore easy to crack under the high temperature conditions and decomposition.First important technique measure of the present invention is by boracic
Compound (such as boric acid, calcium boride, iron boride or zinc borate) carries out intramolecular modification to expandable phenolic resin, in room temperature
With expandable phenolic resin the complex that complexation reaction generates boron modified phenolic resin, B-O keys can occur for lower boron compound
Bond energy is higher than C-C key bond energys, this contributes to the preparation of high oxygen index (OI) phenolic resin and the improvement of its high temperature resistance.
Second important technique measure of the present invention is introduced in the solidification process of foamed phenolic resin by silane idol
It is outer modified to join the pretreated boron-containing compound progress of agent, one layer is coated by the pretreated boric acid zinc surface of silane coupling agent
Silane coupling agent, coupling agent play the role of medium, and phenolic aldehyde and zinc borate are connected in the form of covalent bond, obtain strong boundary
Face interacts.In addition, boron-containing compound can absorb heat under ignition temperature by the evaporation of the crystallization water, object temperature of catching fire is reduced
Degree, and produce nonvolatile B2O3Glassy mass, is coated on polymer surfaces, and the glassy state protective layer of this densification also rises
To the effect of isolation film, and boric acid can promote to generate a large amount of carbon (increase of carbon means that flammable effusion object is reduced), have fine
Flame-retardant smoke inhibition effect.
The invention has the advantages that on the basis of existing phenolic resin foam thermal insulation material production technology, pair can send out
Property phenolic resin carry out intramolecular boron modification, and in the solidification process of foamed phenolic resin by add boron-containing compound into
Row is outer modified, develops the foam resin thermal insulation material of high fire-retardance high intensity.The present invention is using organic and inorganic materials
It is compound, by the inside and outside modification of boron-containing compound, it is greatly improved the temperature classification of phenolic resin material, and keep its higher
Heat insulation effect has the excellent heat-insulating property of phenol formaldehyde foam and high-grade flame retardant property concurrently, light and fire retardant, can be widely applied to outer
In wall outer heat preservation system.
Specific implementation mode
The present invention be on the basis of existing phenolic resin foam thermal insulation material production technology, to expandable phenolic resin into
The boron modification of row intramolecular, and it is outer to the progress of phenolic resin foam thermal insulation material by adding boron-containing compound in the curing process
It is modified, prepare the foam resin thermal insulation material with high flame resistance.
The main reason for phenol formaldehyde foam non-refractory be connected in phenolic resin phenyl ring C-C key bond energys it is relatively low, and phenol hydroxyl
Base stage is easily aoxidized, therefore easy to crack under the high temperature conditions and decomposition.First important technique measure of the present invention is by boracic
Compound (such as boric acid, calcium boride, iron boride or zinc borate) carries out intramolecular modification to expandable phenolic resin, in room temperature
With expandable phenolic resin the complex that complexation reaction generates boron modified phenolic resin, B-O keys can occur for lower boron compound
Bond energy is higher than C-C key bond energys, this contributes to the improvement of high temperature resistance.
The mass ratio for synthesizing expandable phenolic resin is as follows：
Phenol 20~60；
Paraformaldehyde 20~60；
Basic polymerization catalyst 10~40；
Boron-containing compound 0.1~10 for interior modification.
The boron-containing compound for interior modification selects at least one in boric acid, zinc borate, calcium boride or iron borate
Kind.
The basic polymerization catalyst selects in potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, magnesium hydroxide
Select at least one.
Second important technique measure of the present invention is introduced in the solidification process of foamed phenolic resin by silane idol
It is outer modified to join the pretreated boron-containing compound progress of agent, one layer is coated by the pretreated boric acid zinc surface of silane coupling agent
Silane coupling agent, coupling agent play the role of medium, and phenolic aldehyde and zinc borate are connected in the form of covalent bond, obtain strong boundary
Face interacts.In addition, boron-containing compound can absorb heat under ignition temperature by the evaporation of the crystallization water, object temperature of catching fire is reduced
Degree, and produce nonvolatile B2O3Glassy mass, is coated on polymer surfaces, and the glassy state protective layer of this densification also rises
To the effect of isolation film, and boric acid can promote to generate a large amount of carbon (increase of carbon means that flammable effusion object is reduced) with good
Flame-retardant smoke inhibition effect.
The third important technique measure of the present invention is 30~90 mass parts of addition in the solidification process of phenolic resin
Inorganic compound (such as aluminium hydroxide, magnesium hydroxide, silica, sodium metasilicate) is used as filler, and improving, phenolic resin material is strong
While spending, it is remarkably improved temperature classification.
The mass ratio of foam resin solidification process is as follows：
The inorganic filler selects at least one in aluminium hydroxide, magnesium hydroxide, silica, sodium metasilicate.
The pore creating material selects at least one in pentane, hydrogen peroxide, AC foaming agents.
The foam stabilizer is in tween, organic foam stabilizer, lauryl sodium sulfate, neopelex, castor
It is selected in sesame oil polyoxyethylene ether at least one.
The curing agent selects at least one in sulfuric acid, phosphoric acid, p-methyl benzenesulfonic acid.
The boron-containing compound for outer modification can be selected from boron powder, boric acid, zinc borate, iron borate, borax, calcium boride,
At least one of diboron trioxide etc..
The above component is sequentially added into mixing kettle, 15~60s of high-speed stirred is quickly poured into mold, at 40~100 DEG C
5~10min of foamed solidification, cooling, demoulding.According to mold shape, the material of respective shapes is sent out；According to mold thickness, send out
The material of respective thickness；According to mould volume size, corresponding mixture is added, sends out the material of corresponding density.
Main performance index：
Apparent density (kg/m3)≤50
Thermal coefficient (W/mK) 0.025~0.030
Combustibility is B1 grades fire retardant
With 4 embodiments, the invention will be further described below.
Embodiment 1：
1000g phenol, 570g paraformaldehydes, 36g sodium hydroxides and 5g boric acid are sequentially added into mixing kettle, high-speed stirred
3min is warming up to 85 DEG C of reaction 2.5h, obtains the expandable phenolic resin of boron modification.
Embodiment 2：
Ultrasonic disperse 0.5h in 100mL95% ethyl alcohol is added in zinc borate 10g, adds 3wt%KH560, flow back 2h, centrifugation point
From washing is dried to obtain pretreated zinc borate.
Embodiment 3：
By 50g expandable phenolic resins, 10g aluminium hydroxides, 10g magnesium hydroxides, the pretreated boron of 0.4g Tween-80s, 8g
Sour zinc, 6g pentanes and 10g sulfuric acid/phosphoric acid mixed acid sequentially add mixing kettle, and high-speed stirred 15s is quickly poured into 0.004m3's
In template die, the glass mat of 3mm thickness is spread, closed die, the foamed solidification 10min at 80 DEG C is cooling, and demoulding obtains density
For 55kg/m3The high temperature resistance phenolic aldehyde foam insulating composite material of left and right.Referred to the oxygen of the obtained phenolic foam sheet of this method
Number up to 90.
Embodiment 4：
Change the zinc borate in above-described embodiment 2 into boric acid, remaining steps are the same as embodiment 2 and embodiment 3.With this method institute
The oxygen index (OI) of obtained phenolic foam sheet may be up to 85.
Claims (10)
1. a kind of synthetic method of high oxygen index (OI) phenolic resin, it is characterised in that modified synthesis including expandable phenolic resin and
Two steps of solidification of foamed phenolic resin, are as follows：
1) it will be added in the system of phenol, paraformaldehyde, basic polymerization catalyst, gathered for the boron-containing compound of interior modification
Reaction is closed, expandable phenolic resin modified in boron is obtained；The phenol, basic polymerization catalyst, changes for interior paraformaldehyde
The mass ratio of the boron-containing compound of property is：(20~60) ︰ (20~60) ︰ (10~40) ︰ (0.1~10)；
2) it will be pre-processed with silane coupling agent for the boron-containing compound of outer modification, pretreated outer modified boronation closed
Object is added in the boron that step 1) obtains in the expandable phenolic resin of modification, and inorganic filler is added, pore creating material, foam stabilizer, consolidates
Cured after agent, obtains high oxygen index (OI) phenolic resin；Modified expandable phenolic resin in the boron, is made at inorganic filler
Hole agent, foam stabilizer, curing agent mass ratio be (20~70) ︰ (5~50) ︰ (0.1~5) ︰ (0.1~4) ︰ (0.1~10).
2. a kind of synthetic method of high oxygen index (OI) phenolic resin as described in claim 1, it is characterised in that in step 1), institute
It is zinc borate or iron borate to state and use borate, the borate for the boron-containing compound of interior modification.
3. a kind of synthetic method of high oxygen index (OI) phenolic resin as described in claim 1, it is characterised in that in step 1), institute
It states basic polymerization catalyst and is selected from least one of potassium hydroxide, sodium hydroxide, calcium hydroxide, barium hydroxide, magnesium hydroxide；
The thick expandability phenolic aldehyde tree that viscosity is 1000~6000PaS when modified expandable phenolic resin is 25 DEG C in the boron
Fat.
4. a kind of synthetic method of high oxygen index (OI) phenolic resin as described in claim 1, it is characterised in that in step 2), institute
The boron-containing compound for outer modification is stated in boric acid, zinc borate, iron borate, borax, calcium boride, diboron trioxide at least
It is a kind of.
5. a kind of synthetic method of high oxygen index (OI) phenolic resin as described in claim 1, it is characterised in that in step 2), institute
It states silane coupling agent and is selected from least one of KH560, KH550, KH540, KH530.
6. a kind of synthetic method of high oxygen index (OI) phenolic resin as described in claim 1, it is characterised in that in step 2), institute
It states inorganic filler and is selected from least one of aluminium hydroxide, magnesium hydroxide, silica, sodium metasilicate.
7. a kind of synthetic method of high oxygen index (OI) phenolic resin as described in claim 1, it is characterised in that in step 2), institute
It states pore creating material and is selected from least one of pentane, hydrogen peroxide, AC foaming agents.
8. a kind of synthetic method of high oxygen index (OI) phenolic resin as described in claim 1, it is characterised in that in step 2), institute
It states foam stabilizer and is selected from tween, organic foam stabilizer, lauryl sodium sulfate, neopelex, castor oil polyoxy
At least one of vinethene.
9. a kind of synthetic method of high oxygen index (OI) phenolic resin as described in claim 1, it is characterised in that in step 2), institute
It states curing agent and is selected from least one of sulfuric acid, phosphoric acid, p-methyl benzenesulfonic acid.
10. a kind of synthetic method of high oxygen index (OI) phenolic resin as described in claim 1, it is characterised in that in step 2),
The cured temperature is 40~100 DEG C, and the cured time is 5~10min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611207579.4A CN106589801B (en) | 2016-12-23 | 2016-12-23 | A kind of synthetic method of high oxygen index (OI) phenolic resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611207579.4A CN106589801B (en) | 2016-12-23 | 2016-12-23 | A kind of synthetic method of high oxygen index (OI) phenolic resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106589801A CN106589801A (en) | 2017-04-26 |
| CN106589801B true CN106589801B (en) | 2018-11-13 |
Family
ID=58603581
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611207579.4A Active CN106589801B (en) | 2016-12-23 | 2016-12-23 | A kind of synthetic method of high oxygen index (OI) phenolic resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106589801B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108912290A (en) * | 2018-06-14 | 2018-11-30 | 新疆美克思新材料股份有限公司 | A kind of phenolic resin, phenolic foam material and its synthetic method |
| CN110817835A (en) * | 2018-08-14 | 2020-02-21 | 中国科学院上海硅酸盐研究所 | Porous carbon material and preparation method thereof |
| CN109575210A (en) * | 2018-11-30 | 2019-04-05 | 湖北中烟工业有限责任公司 | A kind of preparation method of heat-insulated compound resin |
| CN111040375B (en) * | 2019-12-27 | 2022-11-18 | 华东理工大学 | Nano-pore antioxidant resin-based composite material and preparation method thereof |
| CN114907741A (en) * | 2022-04-27 | 2022-08-16 | 首航科环(泉州)纳米涂料有限公司 | Environment-friendly hydrophobic nano coating and preparation method and use method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844233A (en) * | 2006-03-21 | 2006-10-11 | 上海胜星树脂涂料有限公司 | Method for preparing high temperature resistant phenol-formaldehyde foam composite thermal-insulating materials |
| CN101531769A (en) * | 2009-04-17 | 2009-09-16 | 上海应用技术学院 | Method for preparing high temperature resistance phenolic aldehyde foam insulating composite material |
| CN103073740A (en) * | 2013-01-29 | 2013-05-01 | 山东圣泉化工股份有限公司 | Preparation method of phenolic foamed plastic |
| CN103289305A (en) * | 2013-05-24 | 2013-09-11 | 同济大学 | Preparation method of borate modified phenolic foam material |
-
2016
- 2016-12-23 CN CN201611207579.4A patent/CN106589801B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844233A (en) * | 2006-03-21 | 2006-10-11 | 上海胜星树脂涂料有限公司 | Method for preparing high temperature resistant phenol-formaldehyde foam composite thermal-insulating materials |
| CN101531769A (en) * | 2009-04-17 | 2009-09-16 | 上海应用技术学院 | Method for preparing high temperature resistance phenolic aldehyde foam insulating composite material |
| CN103073740A (en) * | 2013-01-29 | 2013-05-01 | 山东圣泉化工股份有限公司 | Preparation method of phenolic foamed plastic |
| CN103289305A (en) * | 2013-05-24 | 2013-09-11 | 同济大学 | Preparation method of borate modified phenolic foam material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106589801A (en) | 2017-04-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106589801B (en) | A kind of synthetic method of high oxygen index (OI) phenolic resin | |
| JP3950980B2 (en) | Method for producing foam | |
| CN107674169A (en) | A kind of non-ignitable external wall insulation of A levels and preparation method thereof | |
| CN103333457B (en) | A kind of height presses down cigarette, high oxygen index phenolic fireproof insulating plate and preparation method thereof | |
| CN105367990A (en) | Heat-insulating fireproof material based on phenolic aldehyde hollow microspheres and preparation method thereof | |
| CN104017285A (en) | Novel heat-resistant and flame-retardant mixed thermal-insulation material and preparation method thereof | |
| CN101531769A (en) | Method for preparing high temperature resistance phenolic aldehyde foam insulating composite material | |
| CN106810778A (en) | A kind of preparation method of XPS | |
| CN103435970B (en) | A kind of modified phenolic foam for wall thermal insulating and preparation method thereof | |
| CN102604321A (en) | Flame retardant thermal insulation material and preparation method thereof | |
| CN106589792B (en) | A kind of composite phenol formaldehyde cellular insulant and preparation method thereof | |
| CN102888077A (en) | Method for preparing toughened phenolic foam board for exterior insulation of exterior building walls | |
| CN106220231A (en) | Exterior wall fire-retardant polyphenyl insulation material and preparation method thereof | |
| CN105733173B (en) | A kind of preparation method of energy-efficient phenolic foam board | |
| CN102514322A (en) | Flame-retardant thermal insulation material and preparation method thereof | |
| CN106221051A (en) | External wall flame-retardant thermal insulation material and preparation method thereof | |
| CN105694252A (en) | Foam polystyrene composition | |
| CN108912291B (en) | Toughened flame-retardant phenolic resin, phenolic foam material and preparation method thereof | |
| CN105348726B (en) | A kind of manufacture resistance to compression, that resist warping, hydrophobic, the method for fire-retardant heat insulation foamed material | |
| CN106589791A (en) | High-temperature ceramizable phenolic foam composite material and preparation method thereof | |
| CN104497476A (en) | Phenolic resin modified polystyrene foam and preparation method thereof | |
| CN106317664A (en) | External wall flame-retardant thermal insulation material and preparation method thereof | |
| CN103306387A (en) | A2 grade EPS modified fireproof insulation board and preparation and using method thereof | |
| CN111732814B (en) | High-performance fireproof flame-retardant phenolic foam and preparation method thereof | |
| CN106049695B (en) | A kind of fire-retardant heat insulation plate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210705 Address after: 251900 in Lubei high tech Development Zone, Wudi County, Binzhou City, Shandong Province Patentee after: Wudi Dexin Chemical Co.,Ltd. Address before: 831100 No.77, Beijing North Road, Changji Hui Autonomous Prefecture, Xinjiang Uygur Autonomous Region Patentee before: CHANGJI University |