CN102816410A - Polyetheramine toughened phenol formaldehyde foam and preparation method thereof - Google Patents
Polyetheramine toughened phenol formaldehyde foam and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyetheramine toughened phenol formaldehyde foam and a preparation method thereof. The polyetheramine toughened phenol formaldehyde foam comprises the following components in parts by weight: 100 parts of polyetheramine modified phenol formaldehyde resin, 3-10 parts of surfactant, 5-15 parts of foaming agent and 5-20 parts of curing agent. The preparation method comprises the following steps: after sequentially adding the curing agent, surfactant and foaming agent into the polyetheramine modified phenol formaldehyde resin, stirring at high speed, injecting into a mold, and heating to foam and form, thereby obtaining the polyetheramine toughened phenol formaldehyde foam, which has the advantages of less shedding and high toughness and is a heat insulating material with excellent properties.
Description
Technical field
The present invention relates to a phenol formaldehyde foam, particularly a kind of polyetheramine toughening metlbond foam and preparation method thereof.
Background technology
Porous plastics is because of thermal conductivity is low, in light weight, easy construction is more and more in use heat insulation, field of thermal insulation; But several kinds of porous plastics at present commonly used such as urethane, rubber and plastic, PS, Vilaterm etc. exist shortcomings such as easy firing, the amount of being fuming is big, toxicity is high, heat resisting temperature is low, make it in practical application, particularly receive very big restriction in the application aspect boats and ships, the building.
Phenol formaldehyde foam (Phenolic Foam; Be called for short PF) be a kind of fire prevention of excellent performance, heat insulation, sound insulation, lightweight, energy-saving material; Thermal conductivity has only 0.018～0.042 W/mk; Heat-insulating property is superior to PS (PS), urethane (PU), Vilaterm (PE) etc., and the lagging material more traditional than mineral wool, jelutong bukit, perlite, glass wool etc. is high more than 1 times, have again simultaneously foams such as PS, PU, PE far away from flame retardant property.Advantages such as that phenolic foamed plastics has is inexpensive, fire resistance good, do not burn, the amount of being fuming is little, the flame resistant penetrance is good, therefore developed country's research and development are quite active abroad, and oneself adopts in fields such as boats and ships, buildings in a large number.Phenolic foamed plastics is to develop kind faster in the at present external synthetic foam, and consumption increases rapidly in recent years, and range of application constantly enlarges.The world consumption amount is less than 100 tons before nineteen sixty-eight, reaches 3.2 ten thousand tons in 1976, and to 1986 oneself reach 40,000 tons, reach 8.5 ten thousand tons the nineties, at present above 200,000 tons.Phenol formaldehyde foam becomes " candidate that lagging material is new ", more and more comes into one's own.For example, oneself accounts for 25% of syntactic foam plastics total amount the phenolic foamed plastics of the FSU, and annual growth reaches 38%.U.S.'s phenolic foamed plastics output in 1980 is 5000 tons, and 1985 is 50,000 tons, is 10 times before 5 years.Simultaneously, the U.S. is applied to phenol formaldehyde foam high-tech areas such as submarine, boats and ships, space flight and aviation industry at first.Phenolic foamed plastics has accounted for 46% in the used sound-insulating material of building trade.Japan's construction is economized the decree of promulgation " phenolic foamed plastics is as Modular building thing flame resistant material ", and market scale has reached annual several ten thousand tons.As the material of sealing with the control intensity of a fire, phenolic foam board is all installed in the many large-scale apartment of urban architectures such as Marseille, Lyons on the wall with phenolic foamed plastics in France.Simultaneously, because aspects such as Highrise buildings, communications and transportation, shipping industry, aircraft industry, space technology have proposed strict requirement to the thermostability of syntactic foam plastics, flame retardant resistance etc. in recent years, therefore, phenolic foamed plastics receives people and payes attention to widely.
Phenolic aldehyde foam thermal insulation material has following significant advantage:
1, the oxygen index of uninflammability phenolic aldehyde foam thermal insulation material is that flame retardant resistance is best in all organic insulation materials greater than 40.
2, the thermal conductivity of the low phenolic aldehyde foam thermal insulation material of thermal conductivity is that thermal conductivity is minimum in all lagging materials.
3, the low phenolic aldehyde foam thermal insulation material of smoke density and toxicity is that smoke density and toxicity are minimum in all organic insulation materials, and smoke density such as PS, rubber and plastic, Vilaterm, polyurethane foam and toxicity are all very high.
When 4, the strong phenol formaldehyde foam of anti-flame breakthrough power was seen naked light, the surface formed knot carbon, and the phenomenon of thawing is curled, do not had to no dropping, nothing.After overdoing, the surface forms the graphite linings of structural carbon, has effectively protected the foamy inner structure.Anti-flame ability can reach and do not penetrated 100 millimeters more than 1 hour, is best in all organic insulation materials.
5, anticorrosive anti-aging power is high
Phenolic aldehyde foam thermal insulation material is curing molding, and long-term exposure does not have obvious catabiosis in the sun.Obviously be longer than other material work-ing life.The almost corrosion of all mineral acid, organic acid and the salt of ability.
6, the use temperature of the high phenolic aldehyde foam thermal insulation material of thermostability is-190～+ 150 ℃, is the widest in all organic insulation materials, and thermostability is also best.
But the compressive strength≤180KPa of common phenol formaldehyde foam, shock strength≤110J/m simultaneously,
2, fall slag rate>=10%, have the deadly defect that matter is crisp, intensity is low and be prone to slag, it has seriously hindered phenol formaldehyde foam and has applied on a large scale.
Summary of the invention
One of the object of the invention is in order to solve that existing phenol formaldehyde foam matter is crisp, intensity is low and to be prone to the problem of slag and a kind of polyetheramine toughening metlbond foam and preparation method thereof is provided.
Technical scheme of the present invention
A kind of polyetheramine toughening metlbond foam calculates by weight, and its composition and content are following:
100 parts in polyethex amine modification resol
3～10 parts in tensio-active agent
5～15 parts of whipping agents
5～20 parts in solidifying agent
Wherein said polyethex amine modification resol is prepared by a method comprising the following steps:
(1), the mol ratio of control phenol and formaldehyde between 1:1.5～2, it is 7.5～10 that phenol and formaldehyde are mixed the pH value that the back adds sodium hydroxide solution control reaction system, stirring also heat temperature raising to 60～80 ℃ insulation reaction a 30～60min gets reaction solution A;
(2), 3%～20% the polyetheramine that in the reaction solution A of step (1) gained, adds phenol weight is warming up to 85-95 ℃, insulation reaction 60～90min, stopped reaction is cooled to room temperature and gets reaction solution B;
(3), in the reaction solution B of step (2) gained, drip phosphoric acid, control pH value is 6.5～7.5, promptly obtains polyethex amine modification resol;
Described tensio-active agent is a tween-80;
Described whipping agent is a pentane;
Described solidifying agent is calculated by mass percentage, and its composition and content are following:
Phosphoric acid 5%～60%
Tosic acid 20%～45%
Boric acid 5%～15%
Water 15%～40%
The preparation method of above-mentioned solidifying agent is about to phosphoric acid, tosic acid, boric acid and water mixed dissolution and promptly gets solidifying agent.
The preparation method of above-mentioned a kind of polyetheramine toughening metlbond foam, concrete steps are following:
Promptly in polyethex amine modification resol, add solidifying agent, tensio-active agent tween-80, whipping agent pentane successively after, high-speed stirring is mixed, and injects mould, the polyetheramine toughening metlbond foam is prepared in the foamable moulding.
Beneficial effect of the present invention
A kind of polyetheramine toughening metlbond foam of the present invention; Because adopting polyetheramine is toughner synthesizing polyether amine modified phenolic resins; Make the polyetheramine toughening metlbond foam through foaming again, kept traditional advantages such as low, the low cigarette of phenol formaldehyde foam thermal conductivity, anti-combustion, overcome that phenol formaldehyde foam is prone to slag, matter is crisp, intensity is low, the shortcoming of poor toughness simultaneously largely; Its compressive strength of polyetheramine toughening metlbond foam of final gained is measured with reference to the GB8813-1988 standard;>=210KPa, shock strength is measured with reference to the GB/T1043-1993 standard,>=230J/m
2, fall the slag rate and measure≤5% with reference to the GB/T12812-1991 standard.
In addition, the preparation method of a kind of polyetheramine toughening metlbond foam of the present invention, production technique and condition are simple, controlled, and used various chemical feedstockss are technical grade, therefore applicable to commercial scale prodn.
Embodiment
Through concrete embodiment the present invention is further set forth below, but do not limit the present invention.
The technical grade product that used various chemical feedstockss provide by the Shanghai traditional Chinese medicines in the various embodiments of the present invention.
Measuring the used instrument of compressive strength is the Sun 500 type universal testing machines that Italy-GALDABLNI produces;
Measuring the used instrument of shock strength is the JC-3002 type charpy impact test machine that Jiangdu absolute sincerity testing tool factory produces;
Fall the slag rate and measure, manually polish, calculate with reference to the GB/T12812-1991 standard.
Embodiment 1
A kind of polyetheramine toughening metlbond foam, its composition and content are following:
Polyethex amine modification resol 50g
Tensio-active agent 3g
Whipping agent 3g
Solidifying agent 4g
Wherein said polyethex amine modification resol is prepared by a method comprising the following steps:
(1), 90g phenol, 56g Paraformaldehyde 96 are added in the there-necked flask, add 10% sodium hydroxide solution 9g, heat temperature raising to 60 under the agitation condition～80 ℃, insulation reaction 30～60min gets reaction solution A;
(2), in the reaction solution A of step (1) gained, add 10g polyetheramine T-2000 and be warming up to 85-95 ℃, insulation reaction 60～90min, stopped reaction is cooled to room temperature and gets reaction solution B;
(3), dropping phosphoric acid control pH value is 6.5～7.5 in the reaction solution B of step (2) gained, obtains 163g polyethex amine modification resol;
Described tensio-active agent is a tween-80;
Described whipping agent is a pentane;
Described solidifying agent, its composition and content are following:
Phosphoric acid 29g (58%)
Tosic acid 11g (22%)
Boric acid 2.5g (5%)
Water 7.5g (15%)
The preparation method of above-mentioned solidifying agent is about to phosphoric acid, tosic acid, boric acid and water mixed dissolution and promptly gets solidifying agent.
The preparation method of above-mentioned a kind of polyetheramine toughening metlbond foam, concrete steps are following:
Promptly in polyethex amine modification resol, add solidifying agent, tensio-active agent tween-80, whipping agent pentane successively after, high-speed stirring 30s; Pour into fast in the mould of certain volume, closed die is in 70 ℃ of following foamed solidification 1h; Cooling, the demoulding, getting density is 70kg/m
3About the polyetheramine toughening metlbond foam.
The polyetheramine toughening metlbond foam of above-mentioned gained, its compressive strength is determined as 229KPa with reference to the GB8813-1988 standard, and shock strength is determined as 283J/m with reference to the GB/T1043-1993 standard
2, fall the slag rate and be determined as 3.1% with reference to the GB/T12812-1991 standard.
Embodiment 2
A kind of polyetheramine toughening metlbond foam, its composition and content are following:
Polyethex amine modification resol 50g
Tensio-active agent 5g
Whipping agent 7g
Solidifying agent 9g
Wherein said polyethex amine modification resol is prepared by a method comprising the following steps:
(1), 80g phenol, 66g Paraformaldehyde 96 are added in the there-necked flask, and add 10% sodium hydroxide solution 7g, heat temperature raising to 60 under the agitation condition～80 ℃, insulation reaction 30～60min gets reaction solution A;
(2), in the reaction solution A of step (1) gained, add 15g polyetheramine T-5000 and be warming up to 85-95 ℃, insulation reaction 60～90min, stopped reaction is cooled to room temperature and gets reaction solution B;
(3), dropping phosphoric acid control pH value is 6.5～7.5 in the reaction solution B of step (2) gained, obtains 164g polyethex amine modification resol;
Described tensio-active agent is a tween-80;
Described whipping agent is a pentane;
Described solidifying agent, its composition and content are following:
Phosphoric acid 3g (6%)
Tosic acid 22g (44%)
Boric acid 6g (12%)
Water 19g (38%)
The preparation method of above-mentioned solidifying agent is about to phosphoric acid, tosic acid, boric acid and water mixed dissolution and promptly gets solidifying agent.
The preparation method of above-mentioned a kind of polyetheramine toughening metlbond foam, concrete steps are following:
Promptly in polyethex amine modification resol, add solidifying agent, tensio-active agent tween-80, whipping agent pentane successively after, high-speed stirring 30s; Pour into fast in the mould of certain volume, closed die is in 70 ℃ of following foamed solidification 1h; Cooling, the demoulding, getting density is 40kg/m
3About the polyetheramine toughening metlbond foam.
The polyetheramine toughening metlbond foam of above-mentioned gained, its compressive strength is determined as 221KPa with reference to the GB8813-1988 standard, and shock strength is determined as 248J/m with reference to the GB/T1043-1993 standard
2, fall the slag rate and be determined as 4.2% with reference to the GB/T12812-1991 standard.
Embodiment 3
A kind of polyetheramine toughening metlbond foam, its composition and content are following:
Polyethex amine modification resol 50g
Tensio-active agent 2g
Whipping agent 5g
Solidifying agent 7g
Wherein said polyethex amine modification resol is prepared by a method comprising the following steps:
(1), 90g phenol, 50g Paraformaldehyde 96 are added in the there-necked flask, and add 10% sodium hydroxide solution 12g, heat temperature raising to 60 under the agitation condition～80 ℃, insulation reaction 30～60min gets reaction solution A;
(2), in the reaction solution A of step (1) gained, add 4g polyetheramine D-2000 and be warming up to 85-95 ℃, insulation reaction 60～90min, stopped reaction is cooled to room temperature and gets reaction solution B;
(3), dropping phosphoric acid control pH value is 6.5～7.5 in the reaction solution B of step (2) gained, obtains 152g polyethex amine modification resol;
Described tensio-active agent is a tween-80;
Described whipping agent is a pentane;
Described solidifying agent, its composition and content are following:
Phosphatase 11 5g (30%)
Tosic acid 18g (36%)
Boric acid 5g (10%)
Water 12g (24%)
The preparation method of above-mentioned solidifying agent is about to phosphoric acid, tosic acid, boric acid and water mixed dissolution and promptly gets solidifying agent.
The preparation method of above-mentioned a kind of polyetheramine toughening metlbond foam, concrete steps are following:
Promptly in polyethex amine modification resol, add solidifying agent, tensio-active agent tween-80, whipping agent pentane successively after, high-speed stirring 30s; Pour into fast in the mould of certain volume, closed die is in 70 ℃ of following foamed solidification 1h; Cooling, the demoulding, getting density is 50kg/m
3About the polyetheramine toughening metlbond foam.
The polyetheramine toughening metlbond foam of above-mentioned gained, its compressive strength is determined as 212KPa with reference to the GB8813-1988 standard, and shock strength is determined as 233J/m with reference to the GB/T1043-1993 standard
2, fall the slag rate and be determined as 4.8% with reference to the GB/T12812-1991 standard.
Embodiment 4
A kind of polyetheramine toughening metlbond foam, its composition and content are following:
Polyethex amine modification resol 50g
Tensio-active agent 3g
Whipping agent 5g
Solidifying agent 5g
Wherein said polyethex amine modification resol is prepared by a method comprising the following steps:
(1), 90g phenol, 60g Paraformaldehyde 96 are added in the there-necked flask, and add 10% sodium hydroxide solution 10g, heat temperature raising to 60 under the agitation condition～80 ℃, insulation reaction 30～60min gets reaction solution A;
(2), in the reaction solution A of step (1) gained, add 15g polyetheramine D-400 and be warming up to 85-95 ℃, insulation reaction 60～90min, stopped reaction is cooled to room temperature and gets reaction solution B;
(3), dropping phosphoric acid control pH value is 6.5～7.5 in the reaction solution B of step (2) gained, obtains 170g polyethex amine modification resol;
Described tensio-active agent is a tween-80;
Described whipping agent is a pentane;
Described solidifying agent, its composition and content are following:
Phosphatase 11 5g (30%)
Tosic acid 18g (36%)
Boric acid 5g (10%)
Water 12g (24%)
The preparation method of above-mentioned solidifying agent is about to phosphoric acid, tosic acid, boric acid and water mixed dissolution and promptly gets solidifying agent.
The preparation method of above-mentioned a kind of polyetheramine toughening metlbond foam, concrete steps are following:
Promptly in polyethex amine modification resol, add solidifying agent, tensio-active agent tween-80, whipping agent pentane successively after, high-speed stirring 30s; Pour into fast in the mould of certain volume, closed die is in 70 ℃ of following foamed solidification 1h; Cooling, the demoulding, getting density is 60kg/m
3About the polyetheramine toughening metlbond foam.
The polyetheramine toughening metlbond foam of above-mentioned gained, its compressive strength is determined as 223KPa with reference to the GB8813-1988 standard, and shock strength is determined as 266J/m with reference to the GB/T1043-1993 standard
2, fall the slag rate and be determined as 3.9% with reference to the GB/T12812-1991 standard.
The above content is merely the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (10)
1. a polyetheramine toughening metlbond foam is characterized in that calculating by weight, and its composition and content are following:
100 parts in polyethex amine modification resol
3～10 parts in tensio-active agent
5～15 parts of whipping agents
5～20 parts in solidifying agent
Wherein said polyethex amine modification resol is prepared by a method comprising the following steps:
(1), the mol ratio of control phenol and formaldehyde between 1:1.5～2, phenol and formaldehyde are mixed the back add sodium hydroxide solution and control the pH value 7.5～10, heat temperature raising to 60 under the agitation condition～80 ℃, insulation reaction 30～60min gets reaction solution A;
(2), 3%～20% the polyetheramine that in the reaction solution A of step (1) gained, adds phenol weight is warming up to 85-95 ℃, insulation reaction 60～90min, stopped reaction is cooled to room temperature and gets reaction solution B;
(3), in the reaction solution B of step (2) gained, drip phosphoric acid, control pH value is 6.5～7.5, promptly obtains polyethex amine modification resol;
Described tensio-active agent is a tween-80;
Described whipping agent is a pentane;
Described solidifying agent is calculated by mass percentage, and its composition and content are following:
Phosphoric acid 5%～60%
Tosic acid 20%～45%
Boric acid 5%～15%
Water 15%～40%;
The preparation method of above-mentioned solidifying agent is about to phosphoric acid, tosic acid, boric acid and water mixed dissolution and promptly gets solidifying agent.
2. a kind of polyetheramine toughening metlbond foam as claimed in claim 1 is characterized in that calculating by weight, and its composition and content are following:
100 parts in polyethex amine modification resol
4～10 parts in tensio-active agent
6～14 parts of whipping agents
8～18 parts in solidifying agent.
3. a kind of polyetheramine toughening metlbond foam as claimed in claim 2 is characterized in that calculating by weight, and its composition and content are following:
100 parts in polyethex amine modification resol
6 parts in tensio-active agent
6 parts of whipping agents
8 parts in solidifying agent
Wherein said solidifying agent is calculated by mass percentage, and its composition and content are following:
Phosphoric acid 58%
Tosic acid 22%
Boric acid 5%
Water 15%.
4. a kind of polyetheramine toughening metlbond foam as claimed in claim 2 is characterized in that calculating by weight, and its composition and content are following:
100 parts in polyethex amine modification resol
10 parts in tensio-active agent
14 parts of whipping agents
18 parts in solidifying agent
Described solidifying agent is calculated by mass percentage, and its composition and content are following:
Phosphoric acid 6%
Tosic acid 44%
Boric acid 12%
Water 38%.
5. a kind of polyetheramine toughening metlbond foam as claimed in claim 2 is characterized in that calculating by weight, and its composition and content are following:
100 parts in polyethex amine modification resol
4 parts in tensio-active agent
10 parts of whipping agents
14 parts in solidifying agent
Described solidifying agent is calculated by mass percentage, and its composition and content are following:
Phosphoric acid 30%
Tosic acid 36%
Boric acid 10%
Water 24%.
6. a kind of polyetheramine toughening metlbond foam as claimed in claim 2 is characterized in that calculating by weight, and its composition and content are following:
100 parts in polyethex amine modification resol
6 parts in tensio-active agent
10 parts of whipping agents
10 parts in solidifying agent
Described solidifying agent is calculated by mass percentage, and its composition and content are following:
Phosphoric acid 30%
Tosic acid 36%
Boric acid 10%
Water 24%.
7. like claim 1,2,3,4,5 or 6 described a kind of polyetheramine toughening metlbond foams, it is characterized in that it is 10% that described polyethex amine modification resol prepares the concentration of sodium hydroxide solution described in the step of process (1).
8. a kind of polyetheramine toughening metlbond foam as claimed in claim 7 is characterized in that it is D-230, D-400, D-2000, T-2000, T-3000 or T-5000 that described polyethex amine modification resol prepares the polyetheramine described in the step of process (3).
9. like the preparation method of claim 1,2,3,4,5 or 6 described a kind of polyetheramine toughening metlbond foams, it is characterized in that step is following:
Promptly in polyethex amine modification resol, add solidifying agent, tensio-active agent tween-80, whipping agent pentane successively after, high-speed stirring is mixed, and injects mould, the foamable moulding promptly gets the polyetheramine toughening metlbond foam.
10. the polyethex amine modification resol described in a kind of polyetheramine toughening metlbond foam as claimed in claim 8 is characterized in that being prepared by a method comprising the following steps:
(1), the mol ratio of control phenol and formaldehyde between 1:1.5～2, phenol and formaldehyde are mixed the back add sodium hydroxide solution and control the pH value 7.5～10, heat temperature raising to 60 under the agitation condition～80 ℃, insulation reaction 30～60min gets reaction solution A;
(2), 3%～20% the polyetheramine that in the reaction solution A of step (1) gained, adds phenol weight is warming up to 85-95 ℃, insulation reaction 60～90min, stopped reaction is cooled to room temperature and gets reaction solution B;
(3), in the reaction solution B of step (2) gained, drip phosphoric acid, control pH value is 6.5～7.5, promptly obtains polyethex amine modification resol.
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| CN106543640A (en) * | 2016-12-02 | 2017-03-29 | 天津科技大学 | A kind of preparation method of modifying nanometer cellulose phenol formaldehyde foam |
| CN106832164A (en) * | 2017-02-27 | 2017-06-13 | 天津市居安泰科技有限公司 | A kind of rigid foam preparation method of tripolycyanamide amino resin |
| CN106893057A (en) * | 2017-03-03 | 2017-06-27 | 肖圣洁 | A kind of preparation method of melmac toughener |
| CN107325478A (en) * | 2017-08-03 | 2017-11-07 | 合肥泓定科技有限公司 | Exterior wall phenolic-aldehyde heat-insulation board and preparation method thereof |
| CN112708089A (en) * | 2019-10-25 | 2021-04-27 | 北华大学 | Preparation method of flexible lignin phenolic resin for foaming |
| CN115386323A (en) * | 2022-09-06 | 2022-11-25 | 江西省永晟科技有限公司 | Preparation method and application of novel phenolic resin adhesive |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106543640A (en) * | 2016-12-02 | 2017-03-29 | 天津科技大学 | A kind of preparation method of modifying nanometer cellulose phenol formaldehyde foam |
| CN106832164A (en) * | 2017-02-27 | 2017-06-13 | 天津市居安泰科技有限公司 | A kind of rigid foam preparation method of tripolycyanamide amino resin |
| CN106832164B (en) * | 2017-02-27 | 2019-11-08 | 天津市居安泰科技有限公司 | A kind of preparation method of rigid foam tripolycyanamide amino resin |
| CN106893057A (en) * | 2017-03-03 | 2017-06-27 | 肖圣洁 | A kind of preparation method of melmac toughener |
| CN107325478A (en) * | 2017-08-03 | 2017-11-07 | 合肥泓定科技有限公司 | Exterior wall phenolic-aldehyde heat-insulation board and preparation method thereof |
| CN112708089A (en) * | 2019-10-25 | 2021-04-27 | 北华大学 | Preparation method of flexible lignin phenolic resin for foaming |
| CN115386323A (en) * | 2022-09-06 | 2022-11-25 | 江西省永晟科技有限公司 | Preparation method and application of novel phenolic resin adhesive |
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Application publication date: 20121212 |