CN102250445A - Method for preparing phenolic foamed plastic - Google Patents
Method for preparing phenolic foamed plastic Download PDFInfo
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- CN102250445A CN102250445A CN2011101503979A CN201110150397A CN102250445A CN 102250445 A CN102250445 A CN 102250445A CN 2011101503979 A CN2011101503979 A CN 2011101503979A CN 201110150397 A CN201110150397 A CN 201110150397A CN 102250445 A CN102250445 A CN 102250445A
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- cardanol
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- resole
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Abstract
The invention relates to a method for preparing a phenolic foamed plastic. The phenolic foamed plastic is produced by the conventional method; and the method comprises the following steps of: reacting phenol with a formaldehyde solution in the presence of an alkaline catalyst to obtain A-stage phenolic resin; and blending with conventional curing agent, surfactant and foaming agent, foaming, and curing to obtain phenolic foam. Anacardol replaces partial phenol for reaction, and a mass ratio of the anacardol to the phenol is 1:5-1:1. By the method, the cost of the phenolic foam is greatly reduced, the toughness of the foam is improved, the brittleness of the foam is reduced, and the phenolic foam is a product with good market prospect.
Description
Technical field
The present invention relates to a kind of phenolic foamed plastics preparation method, prepared foam toughness improves, and cost reduces, and is a kind of product of good market prospects.
Background technology
Phenolic foamed plastics is a class novel foamed plastic that grew up in recent years, so that its flame resistivity is good, the amount of being fuming is low, high warm nature is good, stable performance, adiabatic heat insulation, sound insulation, easy-formation processing and weather resistance and rank the prostatitis of all porous plastics preferably, be called as " the emerging lagging material of the third generation " or " king of insulation ".After nineteen sixty, a lot of serious fire take place in utilities building both at home and abroad, and death by accident mostly is because toxic gas suffocates and causes, and causes that the public and official are to the particularly attention of synthetic materials fire safety problem of building materials.The excellent properties of low toxicity, flame retardant resistance phenolic resin foam makes it the high speed development that elicitation technique is developed.European and American countries all extensively adopts the PF foam to replace traditional polymkeric substance and mineral to be basic lagging material at the public building design aspect.In a word, the phenolic foamed plastics industry has become advanced technology, product diversification, emerging development industry that automation degree of equipment is the highest.
The main component of phenolic foamed plastics is a resol, is formed by petrochemical industry based raw material phenol and formaldehyde addition polycondensation.The production of resol and use meeting bring to a certain degree pollution to environment, influence the whole ecological environment.In the production of resol, produce a large amount of waste water, mainly phenols and aldehyde material in the waste water, produce by raw material phenol and formaldehyde, if the not treated meaning of taking up the post of of phenolic wastewater is discharged, all can bring serious harm to the mankind, fish and farm crop, and the processing of phenolic wastewater can increase product cost greatly.Along with the enhancing day by day of human environment consciousness and crisis of resource, how to fully utilize biomass resource effectively and replace petrochemical material to prepare that phenol formaldehyde foam is own to be mentioned strategic height by many countries and take in.In recent years, (cashew nut shell, CNSL) application at chemical field comes into one's own the biomass resource cashew shell liquid day by day.Because of the primary structure of cashew nut shell oil having the monoene or the diolefin long-chain of one 15 carbon on the position between phenol, so both had the feature of phenolic compound, the flexibility of aliphatic long-chain compound is arranged again.Therefore if can replace phenol, then can overcome the fragility of common phenol formaldehyde foam, enlarge its Application Areas with cashew nut shell oil.
Summary of the invention
In order to solve the relatively poor problem of toughness of the phenol formaldehyde foam that prior art exists, the invention provides a kind of phenol formaldehyde foam preparation method, at first adopt cardanol partly to replace phenol to prepare A stage resin, further prepare phenolic foamed plastics, effectively reduce cost, improved the toughness of phenolic foamed plastics simultaneously.
Technical scheme of the present invention is: a kind of phenol formaldehyde foam preparation method, produce according to a conventional method, phenol and formaldehyde solution reacted in the presence of basic catalyst obtain resole, obtain phenol formaldehyde foam then with after solidifying agent, tensio-active agent and the whipping agent blend of routine, foaming, the curing, react with cardanol instead of part phenol, the mass ratio of cardanol and phenol is 1:5 to 1:1.
Used basic catalyst is any one in sodium hydroxide, potassium hydroxide, calcium oxide or the magnesium oxide.
Used cardanol is a cashew shell liquid.
Use mineral acid or organic acid to be neutralizing agent in the reaction, described mineral acid is a hydrochloric acid, one or more in phosphoric acid and the sulfuric acid, and described organic acid is a formic acid, acetate, oxalic acid, one or more in the-sulfinic acid.
Used solidifying agent is sulfuric acid, phosphoric acid and tosic acid; Tensio-active agent is a soil temperature-80; Whipping agent is a Skellysolve A.
Beneficial effect:
The present invention can make the phenol formaldehyde foam cost reduce greatly, and toughness is improved simultaneously, and its compressive strength (volume compression 10%) reaches 100-150 KPa, falls the slag rate and reduces to 1.0-2.0%.
Embodiment:
A kind of phenol formaldehyde foam preparation method, with cardanol instead of part phenol, the mass ratio of cardanol and phenol is 1:5 to 1:1, and all the method for preparing phenol formaldehyde foam with routine is identical for other: in reaction flask, add cardanol, phenol, formaldehyde solution and basic catalyst, be warming up to 80-90 ℃, stop heating, the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, be cooled to 70 ℃, add neutralizing agent to pH6-7.Decompression dehydration to solid content is 78-82%, and stopped reaction gets the garnet resole.Resole and conventional solidifying agent, tensio-active agent and whipping agent blend with preparation foam in 70-80 ℃ of baking oven, obtain phenolic foamed plastics after the curing.Solidifying agent can be sulfuric acid, phosphoric acid, tosic acid, and tensio-active agent can be soil temperature-80, and whipping agent can be Skellysolve A.
Neutralizing agent can be mineral acid or organic acid.Mineral acid can be a hydrochloric acid, one or more in phosphoric acid and the sulfuric acid.Organic acid can be a formic acid, acetate, oxalic acid, one or more in the-sulfinic acid.
Cardanol is a cashew shell liquid.
Under above-mentioned experiment condition, the phenolic foamed plastics performance that obtains is tested: density≤40kg/cm3; Rate of closed hole 〉=90%; Its compressive strength (compression 10%) reaches 100-150 KPa, falls the slag rate and reduces to 1.0-2.0 %; Thermal conductivity (10 ℃)≤0.02W/ (mk); 150 ℃ of maximum operation (service) temperatures; Critical oxygen index 〉=45%; Maximum smoke density≤3.0%; Dimensional stability (V/V)≤2.0%; Water-intake rate≤7.0%.
Embodiment 1
Phenol 100g, cardanol 20g, formaldehyde 155 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 78%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween-80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain phenolic foamed plastics after the curing.
The modified by cardanol phenolic foamed plastics performance that obtains is tested: density≤40kg/cm
3Rate of closed hole 〉=90%; Its compressive strength (compression 10%) reaches 100-150 KPa, falls the slag rate and reduces to 1.0-2.0%; Thermal conductivity (10 ℃)≤0.02W/ (mk); 150 ℃ of maximum operation (service) temperatures; Critical oxygen index 〉=45%; Maximum smoke density≤3.0%; Dimensional stability (V/V)≤2.0%; Water-intake rate≤7.0%.
Its toughness determination data contrasts as following table with the data of phenolic foamed plastics:
| The sample title | Compressive strength (KPa) | Fall slag rate (%) |
| The modified by cardanol phenolic foamed plastics | 100-150 | 1.0-2.0 |
| Phenolic foamed plastics | 20-30 | 10.2-12.6 |
Phenolic foamed plastics is not add cardanol to make in the table.
?
Embodiment 2
Phenol 100g, cardanol 22g, formaldehyde 165 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 80%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween-80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 3
Phenol 100g, cardanol 28g, formaldehyde 170 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 85%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 4
Phenol 100g, cardanol 30g, formaldehyde 172 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 87%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween-80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 5
Phenol 100g, cardanol 32g, formaldehyde 175 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 83%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween-80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 6
Phenol 100g, cardanol 35g, formaldehyde 178 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 79%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween-80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 7
Phenol 100g, cardanol 38g, formaldehyde 180 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 82%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween-80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 8
Phenol 100g, cardanol 40g, formaldehyde 183 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 83%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 9
Phenol 100g, cardanol 42g, formaldehyde 185 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 77%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 10
Phenol 100g, cardanol 45g, formaldehyde 188 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 78%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 11
Phenol 100g, cardanol 50g, formaldehyde 191 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 79%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 12
Phenol 100g, cardanol 54g, formaldehyde 193 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 82%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 13
Phenol 100g, cardanol 60g, formaldehyde 200 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 83%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 14
Phenol 100g, cardanol 64g, formaldehyde 198 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 125%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 15
Phenol 100g, cardanol 80g, formaldehyde 215 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 80%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Embodiment 16
Phenol 100g, cardanol 100g, formaldehyde 210 g, basic catalyst sodium hydroxide is transferred pH to 9-10, is warming up to 80-90 ℃, stops heating, and the reaction system heat release is warming up to 100 ℃, meets the requirements to reacting viscosity, is cooled to 70 ℃, adds neutralizing agent to pH6-7.Decompression dehydration to solid content is 79%, and stopped reaction gets the garnet resole.With resole and 50% sulphuric acid soln, tween 80 and the Skellysolve A blend of preparation, in 70-80 ℃ of baking oven, foam, obtain the modified by cardanol phenolic foamed plastics after the curing.
Claims (4)
1. phenol formaldehyde foam preparation method, produce according to a conventional method, phenol and formaldehyde solution reacted in the presence of basic catalyst obtain resole, obtain phenol formaldehyde foam then with after solidifying agent, tensio-active agent and the whipping agent blend of routine, foaming, the curing, it is characterized in that: react with cardanol instead of part phenol, the mass ratio of cardanol and phenol is 1:5 to 1:1.
2. phenol formaldehyde foam preparation method as claimed in claim 1 is characterized in that: described basic catalyst is any one in sodium hydroxide, potassium hydroxide, calcium oxide or the magnesium oxide;
Phenol formaldehyde foam preparation method as claimed in claim 1 is characterized in that: use mineral acid or organic acid to be neutralizing agent in the reaction, described mineral acid is a hydrochloric acid, in phosphoric acid and the sulfuric acid one or more, described organic acid is a formic acid, acetate, oxalic acid, one or more in the-sulfinic acid.
3. phenol formaldehyde foam preparation method as claimed in claim 1 is characterized in that: described phenol formaldehyde ratio is 1:2.5.
4. phenol formaldehyde foam preparation method as claimed in claim 1 is characterized in that: used cardanol is a cashew shell liquid.
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| CN2011101503979A CN102250445A (en) | 2011-06-07 | 2011-06-07 | Method for preparing phenolic foamed plastic |
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| CN2011101503979A CN102250445A (en) | 2011-06-07 | 2011-06-07 | Method for preparing phenolic foamed plastic |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746613A (en) * | 2012-07-05 | 2012-10-24 | 同济大学 | Preparation method for phosphate ester flame retardant toughening phenolic foam material |
| CN102746612A (en) * | 2012-07-05 | 2012-10-24 | 同济大学 | Preparation method for halogen-free flame-retardant toughened phenolic foamed plastics |
| CN103013038A (en) * | 2012-12-27 | 2013-04-03 | 北京莱恩斯高新技术有限公司 | Cardanol modified phenolic aldehyde foam and preparation method thereof |
| CN103289305A (en) * | 2013-05-24 | 2013-09-11 | 同济大学 | Preparation method of borate modified phenolic foam material |
| CN106279597A (en) * | 2016-08-08 | 2017-01-04 | 合肥永佳新材料科技有限公司 | A kind of modified amido sulfoacid water reducer and preparation method thereof |
| CN106565923A (en) * | 2016-11-02 | 2017-04-19 | 中国林业科学研究院林产化学工业研究所 | Silicon-containing epoxy anacardol-group phenolic resin, and preparation method and application of silicon-containing epoxy anacardol-group phenolic resin |
| CN106749944A (en) * | 2016-12-22 | 2017-05-31 | 沈阳化工大学 | A kind of phenolic foam resin of N trihydroxy methyls Methacrylamide etherificate and preparation method thereof |
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| CN101033307A (en) * | 2006-03-10 | 2007-09-12 | 上海尖端工程材料有限公司 | Method of preparing pnenolic aldehyde foam from modified foamable phenolic resin |
| CN101768326A (en) * | 2010-01-15 | 2010-07-07 | 上海虞城新型建材有限公司 | Preparation method of modified phenolic resin and application thereof |
| CN101955596A (en) * | 2009-07-13 | 2011-01-26 | 上海赛星节能科技有限公司 | Preparation method of polydimethylsiloxane modified phenolic foam |
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Patent Citations (3)
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| CN101033307A (en) * | 2006-03-10 | 2007-09-12 | 上海尖端工程材料有限公司 | Method of preparing pnenolic aldehyde foam from modified foamable phenolic resin |
| CN101955596A (en) * | 2009-07-13 | 2011-01-26 | 上海赛星节能科技有限公司 | Preparation method of polydimethylsiloxane modified phenolic foam |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746613A (en) * | 2012-07-05 | 2012-10-24 | 同济大学 | Preparation method for phosphate ester flame retardant toughening phenolic foam material |
| CN102746612A (en) * | 2012-07-05 | 2012-10-24 | 同济大学 | Preparation method for halogen-free flame-retardant toughened phenolic foamed plastics |
| CN103013038A (en) * | 2012-12-27 | 2013-04-03 | 北京莱恩斯高新技术有限公司 | Cardanol modified phenolic aldehyde foam and preparation method thereof |
| CN103013038B (en) * | 2012-12-27 | 2014-07-16 | 北京莱恩斯高新技术有限公司 | Cardanol modified phenolic aldehyde foam and preparation method thereof |
| CN103289305A (en) * | 2013-05-24 | 2013-09-11 | 同济大学 | Preparation method of borate modified phenolic foam material |
| CN106279597A (en) * | 2016-08-08 | 2017-01-04 | 合肥永佳新材料科技有限公司 | A kind of modified amido sulfoacid water reducer and preparation method thereof |
| CN106565923A (en) * | 2016-11-02 | 2017-04-19 | 中国林业科学研究院林产化学工业研究所 | Silicon-containing epoxy anacardol-group phenolic resin, and preparation method and application of silicon-containing epoxy anacardol-group phenolic resin |
| CN106749944A (en) * | 2016-12-22 | 2017-05-31 | 沈阳化工大学 | A kind of phenolic foam resin of N trihydroxy methyls Methacrylamide etherificate and preparation method thereof |
| CN106749944B (en) * | 2016-12-22 | 2019-01-01 | 沈阳化工大学 | A kind of phenolic foam resin and preparation method thereof of N- trihydroxy methyl Methacrylamide etherificate |
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Application publication date: 20111123 |