CN102295821B - Production method of phenolic foam wall insulation material - Google Patents
Production method of phenolic foam wall insulation material Download PDFInfo
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- CN102295821B CN102295821B CN2011101765651A CN201110176565A CN102295821B CN 102295821 B CN102295821 B CN 102295821B CN 2011101765651 A CN2011101765651 A CN 2011101765651A CN 201110176565 A CN201110176565 A CN 201110176565A CN 102295821 B CN102295821 B CN 102295821B
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Abstract
The invention discloses a production method of a phenolic foam wall insulation material. The production method comprises (1) preparing raw materials of phenol, paraformaldehyde for industrial purposes, sodium hydroxide, acrylamide and water, (2) putting phenol, sodium hydroxide and water into a reactor, heating, and adding slowly paraformaldehyde for industrial purposes into the reactor, (3) putting acrylamide into the reactor and heating slowly, (4) adding water, chloropropylene oxide and sodium hydroxide into the reactor, heating and stirring, (5) cooling, adding formic acid into the reactor and carrying out dehydration, and (6) mixing an epoxy modified phenolic resin obtained by the step 5, an organic silicone foam stabilizer, n-pentane and one or more of p-toluenesulfonic acid, benzenesulfonic acid, phosphoric acid and sulfuric acid, and pouring the mixture into a mold for foaming to obtain a desired product. The phenolic foam wall insulation material produced by the production method has the advantages of low cost, energy saving and fire resistance. Compared with similar products, the phenolic foam wall insulation material has low water absorption and strong ageing resistance, and thus the phenolic foam wall insulation material can be utilized widely for the field of thermal insulation building walls.
Description
Technical field
The invention belongs to technical field of polymer materials, relate to a kind of working method of phenol formaldehyde foam wall heat insulation material.
Background technology
In recent years, along with deepening continuously of dwelling construction energy conservation and improving constantly of energy conservation standard, China introduces and has developed many novel power-saving technologies and material, and in residential housing, vigorously promotes the use.Wall heat insulation material should have good heat insulation effect; Good fire resistance is arranged again; For example CCTV building fire and Shanghai residential building fire, all bad with having adopted fire resistance polystyrene foam plate or polyurethane foam plate are relevant as wall heat insulation material, have caused serious disaster; Many loss of life and personal injury, fortune loss have beaten alarm bell for society again.As everyone knows, characteristics such as phenolic foam material has light weight, heat-proof quality is good, rigidity is big, stable performance the more important thing is; It belongs to nonflammable material, and the smoke density in its when burning is low, not fusion, no dropping, and low production cost; Thereby progressively obtained people's approval; Yet this phenolic foam material is compared with other lagging materials, still exists the higher defective of water-intake rate, and this possibly cause its heat-insulating property to descend along with the increase of water regain.The higher reason of phenol formaldehyde foam water-intake rate is, volatile component such as water penetrates cell wall during the resol foamed solidification and behind the phenolic resin curing, thereby on cell wall, forms hole or depression.These holes or depression have been quickened the displacement of whipping agent and air, cause thermal conductivity raising, water-intake rate to improve.The existence of hole or depression is to cause the major cause that the physical strength of phenolic foams reduces, fragility increases and water-intake rate increases.And when phenol formaldehyde foam sheet material was applied to wall insulation system, these defectives may cause the moisture in the foam board absorbing environmental, thereby reduced its heat insulation effect widely.Therefore, how to reduce its water-intake rate, strengthen its aging-resistant ability, become and promoted problem that needing to demand solution in this material urgently on a large scale.
Summary of the invention
The technical problem that the present invention will solve is; Defective to the known technology existence; A kind of working method of phenol formaldehyde foam wall heat insulation material is provided; The phenol formaldehyde foam wall heat insulation material product that this method is produced has the characteristic of low water absorption and stronger resistance of aging, can be widely used in wall insulation system.
Technical solution of the present invention is that the working method of a kind of phenol formaldehyde foam wall heat insulation material that is provided is to adopt following raw material and process step to make phenol formaldehyde foam wall heat insulation material product:
(1), by following weight ratio backup raw material:
(2), get step (1) and be equipped with phenol, sodium hydroxide, water and drop in the reaction kettle, be warming up to 70～85 ℃, slowly add step (1) and be equipped with industrial Paraformaldehyde 96, add in 1 hour;
(3), get step (1) and be equipped with acrylic amide and drop in the reaction kettle, slowly be warming up to 95～110 ℃, kept 95～110 ℃ of temperature 30～90 minutes.The acrylic amide that this step adds, its molecular energy embeds in the resol molecular chains through two keys, and when phenolic resin curing its amide functional group can with the reactive group crosslinking curing, generate three-dimensional crosslinking structure, improve the cross-linking density of product;
(4), reactor temperature is reduced to 40 ℃, add 10～60 parts in water, 5～25 parts of epoxy chloropropane, 2～10 parts in sodium hydroxide, be warming up to 50～70 ℃, stirred 1～6 hour.This step adopts epoxychloropropane modified resol, through the introducing of epoxide group, increases cross-linking density when solidifying, and strengthens cell wall intensity and elasticity, and increases resin integral intensity, withstand voltage shock-resistant ability and elasticity;
(5), reactor temperature is reduced to 40 ℃, in reaction kettle, slowly add while stirring formic acid totally 1～9 part with the pH value of regulating mixture in the still to neutrality, dewater 20～70 parts, must epoxy modified phenolic resin;
(6), get by following weight ratio 30～40:1～1.3:2～2.5:1.9～2.2 in regular turn and inject preset die after in step (5) gained epoxy modified phenolic resin and tensio-active agent silicon foams stablizer, whipping agent Skellysolve A and solidifying agent tosic acid, Phenylsulfonic acid, phosphoric acid, the sulfuric acid one or more are dissolved in 0.4～0.5 part of water mixing and stirring; The foaming of use ordinary method, the foaming density range is 30～80kg/m
3, promptly get phenol formaldehyde foam wall heat insulation material product of the present invention, use ordinary method that products obtained therefrom is carried out water-intake rate by GB/T 8810-88 national standard and detect to such an extent that water-intake rate (%) is measured result such as following table:
The phenol formaldehyde foam wall heat insulation material detects form
The invention has the beneficial effects as follows, can be known by above detection table that the censorship phenol formaldehyde foam wall heat insulation material that the present invention produces compares the phenol formaldehyde foam wall heat insulation material that traditional technology is produced, water-intake rate is significantly reduced.The present invention is through above-mentioned innovation; Through strengthening the cross-link intensity and the cross-linking density of resol molecular chain; The cell wall thickness and the rebound resilience of product have been improved; Volatile matters such as moisture and whipping agent are to the puncture degree of foam wall when having reduced the resol foaming, thereby have reduced the water-intake rate of product effectively, have improved product resistance of aging and other physicals.Phenol formaldehyde foam wall heat insulation material product of the present invention has that cost is low, energy-conservation, the fp advantage, and water-intake rate is low compared with similar products, resistance of aging is strong, can be widely used in the heat-preserving building wall field.
Embodiment:
Embodiment 1:
(1), backup raw material: phenol 350 ㎏, industrial Paraformaldehyde 96 175 ㎏, sodium hydroxide 1.5 ㎏, acrylic amide 5 ㎏, water 60 ㎏;
(2), get step (1) and be equipped with phenol, sodium hydroxide, water and drop in the reaction kettle, be warming up to 70～85 ℃, slowly add step (1) and be equipped with industrial Paraformaldehyde 96, add in 1 hour;
(3), get step (1) and be equipped with acrylic amide and drop in the reaction kettle, slowly be warming up to 95～110 ℃, kept 95～110 ℃ of temperature 30～90 minutes;
(4), reactor temperature is reduced to 40 ℃, add water 10 ㎏, epoxy chloropropane 5 ㎏, sodium hydroxide 2 ㎏, be warming up to 50～70 ℃, stirred 1 hour;
(5), reactor temperature is reduced to 40 ℃, in reaction kettle, slowly add while stirring formic acid totally 1 ㎏ with the pH value of regulating mixture in the still to neutrality, 20 ㎏ that dewater, epoxy modified phenolic resin;
(6), get and inject preset die after step (5) gained epoxy modified phenolic resin 30 ㎏, silicon foams stablizer 1kg, Skellysolve A 2kg and tosic acid 1.92kg are dissolved in 0.4kg water mixing and stirring; The foaming of use ordinary method, the foaming density range is 30kg/m
3, promptly get phenol formaldehyde foam wall heat insulation material product of the present invention.
Embodiment 2:
(1), backup raw material: phenol 400 ㎏, industrial Paraformaldehyde 96 225 ㎏, sodium hydroxide 2 ㎏, acrylic amide 25 ㎏, water 120 ㎏;
Step (2)～(3) are with embodiment 1;
(4), reactor temperature is reduced to 40 ℃, add water 60 ㎏, epoxy chloropropane 25 ㎏, sodium hydroxide 10 ㎏, be warming up to 50～70 ℃, stirred 6 hours;
(5), reactor temperature is reduced to 40 ℃, in reaction kettle, slowly add while stirring formic acid totally 9 ㎏ with the pH value of regulating mixture in the still to neutrality, 70 ㎏ that dewater, epoxy modified phenolic resin;
(6), get step (5) gained epoxy modified phenolic resin 40 ㎏, silicon foams stablizer 1.3k g, Skellysolve A 2.5kg and be dissolved in 0.5kg water mixing and stirring by the composite tosic acid of any weight ratio, Phenylsulfonic acid, phosphoric acid, sulfuric acid 2.2kg after inject preset die; The foaming of use ordinary method, foaming density is 80kg/m
3, promptly get phenol formaldehyde foam wall heat insulation material product of the present invention.
Claims (1)
1. the working method of a phenol formaldehyde foam wall heat insulation material, this method system adopts following raw material and step:
(1), by following weight ratio backup raw material:
(2), get step (1) and be equipped with phenol, sodium hydroxide, water and drop in the reaction kettle, be warming up to 70～85 ℃, slowly add step (1) and be equipped with industrial Paraformaldehyde 96, add in 1 hour;
(3), get step (1) and be equipped with acrylic amide and drop in the reaction kettle, slowly be warming up to 95～110 ℃, kept 95～110 ℃ of temperature 30～90 minutes;
(4), reactor temperature is reduced to 40 ℃, add 10～60 parts in water, 5～25 parts of epoxy chloropropane, 2～10 parts in sodium hydroxide, be warming up to 50～70 ℃, stirred 1～6 hour;
(5), be cooled to 40 ℃, in reaction kettle, slowly add while stirring formic acid totally 1～9 part with the pH value of regulating mixture in the still to neutrality, dewater 20～70 parts, must epoxy modified phenolic resin;
(6), get by following weight ratio 30～40:1～1.3:2～2.5:1.9～2.2 in regular turn and inject preset die after in step (5) gained epoxy modified phenolic resin and silicon foams stablizer, Skellysolve A and tosic acid, Phenylsulfonic acid, phosphoric acid, the sulfuric acid one or more are dissolved in 0.4～0.5 part of water mixing and stirring; The foaming of use ordinary method, the foaming density range is 30～80kg/m
3, promptly get phenol formaldehyde foam wall heat insulation material product of the present invention.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101765651A CN102295821B (en) | 2011-06-28 | 2011-06-28 | Production method of phenolic foam wall insulation material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101765651A CN102295821B (en) | 2011-06-28 | 2011-06-28 | Production method of phenolic foam wall insulation material |
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| Publication Number | Publication Date |
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| CN102295821A CN102295821A (en) | 2011-12-28 |
| CN102295821B true CN102295821B (en) | 2012-10-31 |
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| CN2011101765651A Expired - Fee Related CN102295821B (en) | 2011-06-28 | 2011-06-28 | Production method of phenolic foam wall insulation material |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102838831B (en) * | 2012-09-28 | 2014-01-08 | 湖南中野高科技特种材料有限公司 | Method for recycling phenolic aldehyde foam wastes |
| CN103739797A (en) * | 2013-12-05 | 2014-04-23 | 天津昭鑫电材科技有限公司 | Environmental protection phenol formaldehyde resin and production method thereof |
| CN103755905B (en) * | 2014-01-06 | 2016-02-17 | 湖南中野高科技特种材料有限公司 | The production method of high-strength polymethacrylimide modified phenolic resins foam |
| CN103980817A (en) * | 2014-04-15 | 2014-08-13 | 天长市开林化工有限公司 | Novel rust-conversion coating material with rust |
| CN104559046B (en) * | 2015-02-03 | 2016-09-07 | 中南大学 | Acetylenylbenzene azo novolac foam and preparation method thereof between one |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1594811A (en) * | 1976-12-31 | 1981-08-05 | Unilever Ltd | Phenolic resin foams |
| CN101724133A (en) * | 2009-12-18 | 2010-06-09 | 谢建军 | Method for producing phenolic resin by utilizing paraformaldehyde |
| CN101962429A (en) * | 2009-07-24 | 2011-02-02 | 苏州美克思科技发展有限公司 | Modified foaming phenolic resin and manufacturing method thereof |
| CN101974164A (en) * | 2010-11-16 | 2011-02-16 | 山东大学 | Preparation process of high foaming phenolic resin foam material |
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2011
- 2011-06-28 CN CN2011101765651A patent/CN102295821B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1594811A (en) * | 1976-12-31 | 1981-08-05 | Unilever Ltd | Phenolic resin foams |
| CN101962429A (en) * | 2009-07-24 | 2011-02-02 | 苏州美克思科技发展有限公司 | Modified foaming phenolic resin and manufacturing method thereof |
| CN101724133A (en) * | 2009-12-18 | 2010-06-09 | 谢建军 | Method for producing phenolic resin by utilizing paraformaldehyde |
| CN101974164A (en) * | 2010-11-16 | 2011-02-16 | 山东大学 | Preparation process of high foaming phenolic resin foam material |
Non-Patent Citations (1)
| Title |
|---|
| 李少堂等.环氧改性聚醚增韧酚醛树脂及其泡沫.《复合材料——基础、创新、高效：第十四届全国复合材料学术会议论文集（上）》.2006,221-224. * |
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