CN108659454A - Modified phenolic foam thermal insulation material and preparation method thereof - Google Patents
Modified phenolic foam thermal insulation material and preparation method thereof Download PDFInfo
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- CN108659454A CN108659454A CN201810584329.5A CN201810584329A CN108659454A CN 108659454 A CN108659454 A CN 108659454A CN 201810584329 A CN201810584329 A CN 201810584329A CN 108659454 A CN108659454 A CN 108659454A
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- 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
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- 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
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- 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
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- 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
- C08J2497/00—Characterised by the use of lignin-containing materials
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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Abstract
The invention discloses a kind of modified phenolic foam thermal insulation materials and preparation method thereof, wherein the preparation method includes：1) in the presence of a solvent, by after 1 5h of cetyl trimethylammonium bromide and montmorillonite hybrid reaction, taking precipitate M1；2) sediment M1 obtained in step 1) is placed in aluminum salt solution and/or magnesium salt solution after mixing and takes precipitation, sediment M2 is made；3) sediment M2 obtained in step 2) is placed under conditions of temperature is 200 400 DEG C and is roasted, modified montmorillonoid is made；4) it foams after mixing modified montmorillonoid obtained, sodium lignin sulfonate and foaming agent in phenolic resin, step 3), mixture M 3 is made；5) under conditions of temperature is 70 80 DEG C, cure after curing agent mixing is added into mixture M 3, modified phenolic foam thermal insulation material is made.Realizing has the effect of better fire resistance and heat-insulating property.
Description
Technical field
The present invention relates to phenolic aldehyde foam thermal insulation material fields, and in particular, to modified phenolic foam thermal insulation material and its system
Preparation Method.
Background technology
Phenolic aldehyde foam thermal insulation material is as a kind of common thermal insulation material type, with performances such as its good sound absorptions by wide
General application.It is that its thermal coefficient as an important index of thermal insulation material, meanwhile, for materials such as buildings
When, often to its fire protecting performance, higher requirements are also raised.
Therefore it provides a kind of having lower heat insulating coefficient, to have better heat-insulating property, while having preferably
The problem of modified phenolic foam thermal insulation material of fire protecting performance and preparation method thereof is urgent need to resolve of the present invention.
Invention content
For the above-mentioned prior art, it is an object of the invention to overcome in the prior art phenolic aldehyde foam thermal insulation material often prevent
Fiery performance is difficult to meet the problem of more requirement of harsh environment, a kind of with lower heat insulating coefficient to provide, thus
With better heat-insulating property, while the modified phenolic foam thermal insulation material and preparation method thereof with better fire protecting performance.
To achieve the goals above, the present invention provides a kind of preparation methods of modified phenolic foam thermal insulation material, wherein
The preparation method includes：
1) it in the presence of a solvent, by after cetyl trimethylammonium bromide and montmorillonite hybrid reaction 1-5h, takes
Sediment M1；
2) sediment M1 obtained in step 1) is placed in aluminum salt solution and/or magnesium salt solution after mixing and takes precipitation, made
Obtain sediment M2；
3) sediment M2 obtained in step 2) is placed under conditions of temperature is 200-400 DEG C and is roasted, be made modified and cover
De- soil；
4) it foams after mixing modified montmorillonoid obtained, sodium lignin sulfonate and foaming agent in phenolic resin, step 3),
Mixture M 3 is made；
5) under conditions of temperature is 70-80 DEG C, cure after curing agent mixing is added into mixture M 3, modified phenol is made
Aldehyde cellular insulant.
The present invention also provides a kind of according to modified phenolic foam thermal insulation material made from preparation method described above.
Through the above technical solutions, the present invention is in the presence of a solvent, by cetyl trimethylammonium bromide and illiteracy
De- soil hybrid reaction so that cetyl trimethylammonium bromide can be modified montmorillonite, displace between cheating engaging layer
Inorganic ions such as a large amount of magnaliums, and alkyl is injected between montmorillonite, increase the gap between each level of montmorillonite, then into one
Above-mentioned sediment is placed in aluminum salt solution and/or magnesium salt solution after immersion and roasts by step, modified montmorillonoid is made, then change above-mentioned
Cure after property montmorillonite and phenolic resin, sodium lignin sulfonate and foaming agent mixed foaming, makes through above-mentioned material and mode system
The modified phenolic foam thermal insulation material obtained has better fire protecting performance and heat-insulating property.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Specific implementation mode
The specific implementation mode of the present invention is described in detail below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
The present invention provides a kind of preparation methods of modified phenolic foam thermal insulation material, wherein the preparation method includes：
1) it in the presence of a solvent, by after cetyl trimethylammonium bromide and montmorillonite hybrid reaction 1-5h, takes
Sediment M1；
2) sediment M1 obtained in step 1) is placed in aluminum salt solution and/or magnesium salt solution after mixing and takes precipitation, made
Obtain sediment M2；
3) sediment M2 obtained in step 2) is placed under conditions of temperature is 200-400 DEG C and is roasted, be made modified and cover
De- soil；
4) it foams after mixing modified montmorillonoid obtained, sodium lignin sulfonate and foaming agent in phenolic resin, step 3),
Mixture M 3 is made；
5) under conditions of temperature is 70-80 DEG C, cure after curing agent mixing is added into mixture M 3, modified phenol is made
Aldehyde cellular insulant.
The present invention in the presence of a solvent, by cetyl trimethylammonium bromide and montmorillonite hybrid reaction so that
Cetyl trimethylammonium bromide can be modified montmorillonite, displace a large amount of magnaliums between cheating engaging layer etc. it is inorganic from
Son, and alkyl is injected between montmorillonite, increase the gap between each level of montmorillonite, further sets above-mentioned sediment
It is roasted after being impregnated in aluminum salt solution and/or magnesium salt solution, modified montmorillonoid is made, then by above-mentioned modified montmorillonoid and phenolic aldehyde tree
Cure after fat, sodium lignin sulfonate and foaming agent mixed foaming, makes through modified phenolic foam made from above-mentioned material and mode
Thermal insulation material has better fire protecting performance and heat-insulating property.
In a kind of preferred embodiment of the present invention, in step 1), the solvent is selected from water and/or ethyl alcohol.
In further preferred embodiment, in step 1), mixed process is by cetyl trimethylammonium bromide and molten
After agent mixes and is warming up to 60-80 DEG C under agitation, montmorillonite mixing is added thereto.
In one kind more preferably embodiment, relative to the solvent of 100mL, the cetyl trimethyl bromination
The dosage of ammonium is 2-5g, and the dosage of the montmorillonite is 8-15g.
In another preferred embodiment, in step 2), the aluminium salt is selected from aluminum nitrate and/or aluminium chloride, the magnesium salts
Selected from magnesium nitrate and/or magnesium sulfate.
Further include drying sediment M2, and dry in step 2) in a kind of preferred embodiment of the present invention
Dry process is to be placed under conditions of temperature is 80-120 DEG C to carry out.
In further preferred embodiment, roasting time is 2-3h in step 3).
In a kind of preferred embodiment of the present invention, in step 4), the phenolic aldehyde tree relative to 100 parts by weight
The dosage of fat, the modified montmorillonoid is 5-20 parts by weight, and the dosage of the sodium lignin sulfonate is 2-10 parts by weight, the hair
The dosage of infusion is 5-10 parts by weight；
In step 5), relative to the mixture M 3 of 100 parts by weight, the dosage of the curing agent is 5-15 parts by weight.
The foaming agent and the curing agent can be selected from type commonly used in the art, for example, a kind of preferred reality
It applies in mode, the foaming agent is selected from pentane；
The curing agent is selected from p-methyl benzenesulfonic acid and/or benzene sulfonic acid.
The present invention also provides a kind of according to modified phenolic foam thermal insulation material made from preparation method described above.
The present invention will be described in detail by way of examples below.
Embodiment 1
1) after 2g cetyl trimethylammonium bromides and 100mL water being mixed under agitation and being warming up to 60 DEG C, to
After 8g montmorillonite hybrid reactions 1h wherein is added, taking precipitate M1；
2) sediment M1 obtained in step 1) is placed in aluminum nitrate solution and magnesium nitrate solution after mixing and takes precipitation, made
Sediment M2 be placed in temperature be 80 DEG C under conditions of dry；
3) sediment M2 obtained in step 2) is placed under conditions of temperature is 200 DEG C and roasts 2h, modified cover is made and takes off
Soil；
4) by modified montmorillonoid obtained, 2 parts by weight sulfomethylated lignins in 100 parts by weight of phenolic resin, 5 parts by weight steps 3)
It foams after sour sodium and the mixing of 5 parts by weight pentanes, mixture M 3 is made；
5) under conditions of temperature is 70 DEG C, the mixing of 5 parts by weight p-methyl benzenesulfonic acid is added into 100 parts by weight mixture Ms 3
After cure, modified phenolic foam thermal insulation material A1 is made.
Embodiment 2
1) after 5g cetyl trimethylammonium bromides and 100mL ethyl alcohol being mixed under agitation and being warming up to 80 DEG C,
After 15g montmorillonite hybrid reactions 5h is added thereto, taking precipitate M1；
2) sediment M1 obtained in step 1) is placed in aluminum nitrate solution and magnesium nitrate solution after mixing and takes precipitation, made
Sediment M2 be placed in temperature be 120 DEG C under conditions of dry；
3) sediment M2 obtained in step 2) is placed under conditions of temperature is 400 DEG C and roasts 3h, modified cover is made and takes off
Soil；
4) by modified montmorillonoid obtained, 10 parts by weight lignin in 100 parts by weight of phenolic resin, 20 parts by weight steps 3)
It foams after sodium sulfonate and the mixing of 10 parts by weight pentanes, mixture M 3 is made；
5) under conditions of temperature is 80 DEG C, it is mixed that 15 parts by weight p-methyl benzenesulfonic acid are added into 100 parts by weight mixture Ms 3
Cure after conjunction, modified phenolic foam thermal insulation material A2 is made.
Embodiment 3
1) 3g cetyl trimethylammonium bromides and 50mL water and 50mL ethyl alcohol are mixed and is heated up under agitation
To after 70 DEG C, after 12g montmorillonite hybrid reactions 3h is added thereto, taking precipitate M1；
2) sediment M1 obtained in step 1) is placed in aluminum nitrate solution and magnesium nitrate solution after mixing and takes precipitation, made
Sediment M2 be placed in temperature be 100 DEG C under conditions of dry；
3) sediment M2 obtained in step 2) is placed under conditions of temperature is 300 DEG C and roasts 3h, modified cover is made and takes off
Soil；
4) by modified montmorillonoid obtained, 5 parts by weight lignin in 100 parts by weight of phenolic resin, 10 parts by weight steps 3)
It foams after sodium sulfonate and the mixing of 8 parts by weight pentanes, mixture M 3 is made；
5) under conditions of temperature is 75 DEG C, it is mixed that 10 parts by weight p-methyl benzenesulfonic acid are added into 100 parts by weight mixture Ms 3
Cure after conjunction, modified phenolic foam thermal insulation material A3 is made.
Embodiment 4
It is prepared according to the preparation method of embodiment 1, unlike, mixed process is to be placed directly within 20 DEG C in step 1)
Under conditions of mix, modified phenolic foam thermal insulation material A4 is made.
Embodiment 5
It is prepared according to the preparation method of embodiment 2, unlike, the dosage of the cetyl trimethylammonium bromide
For 1g, and roasting time is 1h in step 3), and modified phenolic foam thermal insulation material A5 is made.
Embodiment 6
It is prepared according to the preparation method of embodiment 3, unlike, the dosage of the modified montmorillonoid is 2 parts by weight,
The dosage of the sodium lignin sulfonate is 1 parts by weight, and modified phenolic foam thermal insulation material A6 is made.
Comparative example 1
It is prepared according to the preparation method of embodiment 1, unlike, it is added without cetyl trimethylammonium bromide, is made
Obtain modified phenolic foam thermal insulation material D1.
Comparative example 2
It is prepared according to the preparation method of embodiment 2, unlike, without step 2), modified phenolic foam is made
Thermal insulation material D2.
Comparative example 3
It is prepared according to the preparation method of embodiment 3, unlike, it is added without modified montmorillonoid, sodium lignin sulfonate,
Modified phenolic foam thermal insulation material D3 is made.
Test case
Above-mentioned A1-A6 and D1-D3 is detected into its fire resistance rating according to GB8624, while detecting its thermal coefficient, is obtained
The results are shown in Table 1.
Table 1
| Number | Fire resistance rating | Thermal coefficient (W/mK) |
| A1 | A | 0.018 |
| A2 | A | 0.019 |
| A3 | A | 0.018 |
| A4 | A | 0.020 |
| A5 | B1 | 0.023 |
| A6 | B1 | 0.022 |
| D1 | B1 | 0.031 |
| D2 | B1 | 0.032 |
| D3 | B2 | 0.028 |
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
1. a kind of preparation method of modified phenolic foam thermal insulation material, which is characterized in that the preparation method includes：
1) in the presence of a solvent, by after cetyl trimethylammonium bromide and montmorillonite hybrid reaction 1-5h, precipitation is taken
Object M1；
2) sediment M1 obtained in step 1) is placed in aluminum salt solution and/or magnesium salt solution after mixing and takes precipitation, be made heavy
Starch M2；
3) sediment M2 obtained in step 2) is placed under conditions of temperature is 200-400 DEG C and is roasted, modified montmorillonoid is made；
4) it foams, is made after mixing modified montmorillonoid obtained, sodium lignin sulfonate and foaming agent in phenolic resin, step 3)
Mixture M 3；
5) under conditions of temperature is 70-80 DEG C, cure after curing agent mixing is added into mixture M 3, modified phenolic bubble is made
Foam thermal insulation material.
2. preparation method according to claim 1, wherein in step 1), the solvent is selected from water and/or ethyl alcohol.
3. preparation method according to claim 1 or 2, wherein in step 1), mixed process is by cetyl trimethyl
After ammonium bromide and solvent mix and be warming up to 60-80 DEG C under agitation, montmorillonite mixing is added thereto.
4. preparation method according to claim 3, wherein relative to the solvent of 100mL, the cetyl front three
The dosage of base ammonium bromide is 2-5g, and the dosage of the montmorillonite is 8-15g.
5. preparation method according to claim 1 or 2, wherein in step 2), the aluminium salt is selected from aluminum nitrate and/or chlorine
Change aluminium, the magnesium salts is selected from magnesium nitrate and/or magnesium sulfate.
6. preparation method according to claim 1 or 2, wherein further include in step 2) sediment M2 is dried, and
Drying course is to be placed under conditions of temperature is 80-120 DEG C to carry out.
7. preparation method according to claim 1 or 2, wherein roasting time is 2-3h in step 3).
8. preparation method according to claim 1 or 2, wherein in step 4), the phenolic aldehyde relative to 100 parts by weight
The dosage of resin, the modified montmorillonoid is 5-20 parts by weight, and the dosage of the sodium lignin sulfonate is 2-10 parts by weight, described
The dosage of foaming agent is 5-10 parts by weight；
In step 5), relative to the mixture M 3 of 100 parts by weight, the dosage of the curing agent is 5-15 parts by weight.
9. preparation method according to claim 1 or 2, wherein the foaming agent is selected from pentane；
The curing agent is selected from p-methyl benzenesulfonic acid and/or benzene sulfonic acid.
10. modified phenolic foam thermal insulation material made from a kind of preparation method according to any one of claim 1-9.
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| CN201810584329.5A CN108659454A (en) | 2018-06-08 | 2018-06-08 | Modified phenolic foam thermal insulation material and preparation method thereof |
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| CN201810584329.5A CN108659454A (en) | 2018-06-08 | 2018-06-08 | Modified phenolic foam thermal insulation material and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450630A (en) * | 2013-08-09 | 2013-12-18 | 江苏德明新材料有限公司 | Preparation method of environment-friendly phenol aldehyde-inorganic composite heat insulating material |
| CN104924706A (en) * | 2015-05-20 | 2015-09-23 | 北京化工大学 | Preparation method for composite material with hydrotalcite-imvite laminate alternating structure |
| CN106832754A (en) * | 2017-03-22 | 2017-06-13 | 广东电网有限责任公司电力科学研究院 | A kind of phenol-formaldehyde resin modified material and its application |
| CN107216601A (en) * | 2017-06-30 | 2017-09-29 | 李欢 | A kind of humic acid modified enhancing phenolic foam material and preparation method thereof |
-
2018
- 2018-06-08 CN CN201810584329.5A patent/CN108659454A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450630A (en) * | 2013-08-09 | 2013-12-18 | 江苏德明新材料有限公司 | Preparation method of environment-friendly phenol aldehyde-inorganic composite heat insulating material |
| CN104924706A (en) * | 2015-05-20 | 2015-09-23 | 北京化工大学 | Preparation method for composite material with hydrotalcite-imvite laminate alternating structure |
| CN106832754A (en) * | 2017-03-22 | 2017-06-13 | 广东电网有限责任公司电力科学研究院 | A kind of phenol-formaldehyde resin modified material and its application |
| CN107216601A (en) * | 2017-06-30 | 2017-09-29 | 李欢 | A kind of humic acid modified enhancing phenolic foam material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 丁彤等编写: "《中国化工产品大全 下》", 30 October 1994, 北京：化学工业出版社 * |
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