CN102443126A - Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam - Google Patents
Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam Download PDFInfo
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- CN102443126A CN102443126A CN2011102572355A CN201110257235A CN102443126A CN 102443126 A CN102443126 A CN 102443126A CN 2011102572355 A CN2011102572355 A CN 2011102572355A CN 201110257235 A CN201110257235 A CN 201110257235A CN 102443126 A CN102443126 A CN 102443126A
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Abstract
The invention discloses a low-temperature foaming phenolic resin which is prepared from the following components in parts by weight: 100 parts of phenol, 40-65 parts of paraformaldehyde, 0.5-3.5 parts of catalyst and 1-6 parts of amine compound. In addition, the invention also discloses a preparation method of the low-temperature foaming phenolic resin and a preparation method of modified phenolic foam of the low-temperature foaming phenolic resin. The low-temperature foaming phenolic resin can foam at 5-25 degrees; and the modified phenolic foam prepared from the low-temperature foaming phenolic resin is applicable to the low-temperature one-step molding technology, and has the advantages of short curing time and high production efficiency.
Description
Technical field
The present invention relates to the method for low-temp foaming resol and preparation method thereof and modified phenolic foam.
Background technology
The cellular insulant of resol production have thermal conductivity low, do not fire, low smoke and non-toxic, characteristic cheaply, the existing history for many years of phenol formaldehyde foam is that fire line is best in the insulating foam.Although these advantages are arranged; But phenol formaldehyde foam is not used widely in insulation market; Major cause is that resol will just can obtain ideal cured phenolic foam under heating condition; This method energy consumption is high, processing is cumbersome, efficient is low, and product crisp, fall foam, these have all limited it and have applied.
For this reason, one Chinese patent application number 03106510 (denomination of invention: the working method and the resin of processing that are used for the resol of normal-temperature continuous casting foaming) but disclose and a kind ofly done the method that composite catalyst prepares high ortho position, low viscous normal temperature foamed phenolic resin with alkali and MOX etc. at normal temperatures; U.S. Pat 5693684 discloses a kind of preparation method of cast phenol formaldehyde foam and resol, with sodium hydroxide, trolamine etc. as catalyzer.These two kinds of prior aries all are to be raw material with the liquid formaldehyde, need carry out vacuum hydro-extraction, produce waywardly, and can produce a large amount of phenolic wastewater, cause environmental pollution.
Summary of the invention
The object of the invention is exactly the deficiency that overcomes above-mentioned prior art, and a kind of low-temp foaming resol and preparation method thereof is provided, and provide a kind of contain this low-temp foaming resol and the method for modified phenolic foam.
The objective of the invention is to realize through following technical scheme:
A kind of low-temp foaming resol is prepared from the component of following weight part:
Wherein said catalyzer is sodium hydroxide or triethylamine,
Said aminated compounds is urea or urea.
A kind of preparation method of above-mentioned low-temp foaming resol may further comprise the steps:
1) with phenol and catalyst mix, add Paraformaldehyde 96 80 ℃ of left and right sides gradation, after adding whole Paraformaldehyde 96s, reacted again 30 minutes;
2) be warming up to 90～95 ℃, reacted 30 minutes;
3) be cooled to about 85 ℃, add aminated compounds, continue reaction 50 minutes.
A kind ofly contain above-mentioned low-temp foaming STUDY ON THE MODIFICATION OF PENOLIC RESIN PREPARATION OF PHENOLIC FOAM method, may further comprise the steps:
1) 100 parts in low-temp foaming resol, 1～4 part in tensio-active agent, 2～9 parts of whipping agents, 3～6 parts of alcohols properties-correcting agent, modified glue powder are stirred for 3～6 parts;
2) add 8～16 parts in solidifying agent, stirred 20 seconds～5 minutes;
3) in normal temperature environment, solidify 1～5 minute.
7, preparation method according to claim 6 is characterized in that:
Above-mentioned tensio-active agent is selected tween 80 or silicone oil for use, and said silicone oil preferably adopts silicone oil H330 or silicone oil DC-193.
Above-mentioned whipping agent is at least a in sherwood oil or the Skellysolve A, and when sherwood oil and Skellysolve A used simultaneously, sherwood oil was 3: 1 with the ratio of the weight part of Skellysolve A.
Above-mentioned alcohols properties-correcting agent is ethanol, and above-mentioned modified glue powder is a PNBR, and above-mentioned solidifying agent is a Phenylsulfonic acid class solidifying agent.
Compared with prior art; The preparation method of resol of the present invention is the synthetic LV of raw material, highly active resol with the Paraformaldehyde 96; This method process stabilizing, controllability are strong, and do not have waste water and produce, and prepared low-temp foaming resol can foam at 5-25 ℃.
The preparation method of modified phenolic foam of the present invention adopts single mode low-temperature primary forming technique, and set time is short; Only need can obtain in 2～5 minutes modification cystose and other goods of excellent performance, efficient is high, in addition; This method does not need investments such as barn, band saw processing, greatly reduces cost, reduces fixed investment; Only need several moulds just can continuously produce foam heat-insulating board and other goods of required specification, product appearance is attractive in appearance, does not fall foam, intensity height; Surface adhesion power is strong, and 3 groups of moulds can be produced the above warming plate of 100 sides daily.
Embodiment
Below in conjunction with specific embodiment explanation is done into-gone on foot to method of the present invention.
Embodiment 1
(1) preparation of low-temp foaming resol
In 2 tons of reaction kettles, add 15 kilograms in the sodium hydroxide of 800 kilograms of phenol, 30% (weight percent), stir, heat to 80 ℃; Divide 6 times and add 320 kilograms of Paraformaldehyde 96s, reacted 30 minutes, be warming up to 90～95 ℃; Reacted 30 minutes, and be cooled to 85 ℃ then, add 10 kilograms in urea; Reacted 50 minutes, and be cooled to normal temperature and obtain low-temp foaming resol, its viscosity is 2000CP/25 ℃.
(2) preparation of modified phenolic foam
100 parts of (weight parts of low-temp foaming resol with preparation in (1); As follows) and 4 parts of tween 80s, 6 parts of sherwood oils, 3 parts of ethanol, 3 parts of modified glue powders; 9 parts of Phenylsulfonic acids of back adding stir; Stir at normal temperatures after 20 seconds and inject die cavity, solidify the modified phenolic foam plate and the goods that obtain solidifying excellence after 2 minutes.
Embodiment 2
100 parts in low-temp foaming resol, silicone oil H3302 part, 4 parts of Skellysolve As, 3 parts of ethanol, 3 parts of modified glue powders with preparation in (1); Add 11 parts of Phenylsulfonic acids after stirring, stir and inject die cavity obtains solidifying excellence after 5 minutes modified phenolic foam plate and goods after 2 minutes.
Embodiment 3
100 parts in low-temp foaming resol, silicone oil DC-1934 part, 5 parts of ethanol, 9 parts of Skellysolve As, 6 parts of modified glue powders with preparation in (1); Add 3 parts of xylene monosulfonic acids, 7 parts of tosic acid after stirring, stir and inject die cavity obtains solidifying excellence after 3 minutes modified phenolic foam plate and goods after 5 minutes.
Embodiment 4
100 parts in low-temp foaming resol, silicone oil DC-1934 part, 4 parts of ethanol, 6 parts of sherwood oils, 2 parts of Skellysolve As, 5 parts of modified glue powders with preparation in (1); Add 3 parts of xylene monosulfonic acids, 7 parts of tosic acid after stirring, stir and inject die cavity obtains solidifying excellence after 3 minutes modified phenolic foam plate and goods after 5 minutes.
Claims (10)
1. low-temp foaming resol is characterized in that being prepared from the component of following weight part:
Wherein said catalyzer is sodium hydroxide or triethylamine,
Said aminated compounds is: urea or urea.[wkl]
2. the preparation method of the said low-temp foaming resol of claim 1 may further comprise the steps:
1) with phenol and catalyst mix, add Paraformaldehyde 96 80 ℃ of left and right sides gradation, after adding whole Paraformaldehyde 96s, reacted again 30 minutes;
2) be warming up to 90～95 ℃, reacted 30 minutes;
3) be cooled to about 85 ℃, add aminated compounds and continue reaction 50 minutes.
3. one kind contains right and requires 1 said low-temp foaming STUDY ON THE MODIFICATION OF PENOLIC RESIN PREPARATION OF PHENOLIC FOAM method, it is characterized in that may further comprise the steps:
1) 100 parts in low-temp foaming resol, 1～4 part in tensio-active agent, 2～9 parts of whipping agents, 3～6 parts of alcohols properties-correcting agent, modified glue powder are stirred for 3～6 parts;
2) add 8～16 parts in solidifying agent, stirred 20 seconds～5 minutes;
3) in normal temperature environment, solidify 1～5 minute.
4. preparation method according to claim 3 is characterized in that: said tensio-active agent is selected tween 80 or silicone oil for use.
5. preparation method according to claim 4 is characterized in that: described silicone oil is silicone oil H330 or silicone oil DC-193.
6. preparation method according to claim 3 is characterized in that: said whipping agent is at least a in sherwood oil or the Skellysolve A.
7. preparation method according to claim 6 is characterized in that: when sherwood oil and Skellysolve A used simultaneously, sherwood oil was 3: 1 with the ratio of the weight part of Skellysolve A.
8. preparation method according to claim 3 is characterized in that: said alcohols properties-correcting agent is ethanol.
9. preparation method according to claim 3 is characterized in that: said modified glue powder is a PNBR.
10. preparation method according to claim 3 is characterized in that: said solidifying agent is a Phenylsulfonic acid class solidifying agent.
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| CN2011102572355A CN102443126A (en) | 2011-09-02 | 2011-09-02 | Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam |
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| CN2011102572355A CN102443126A (en) | 2011-09-02 | 2011-09-02 | Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766243A (en) * | 2012-07-25 | 2012-11-07 | 胡玉 | Room-temperature foamable phenolic resin and method for preparing phenolic foams by same |
| CN102936325A (en) * | 2012-11-13 | 2013-02-20 | 中国林业科学研究院林产化学工业研究所 | High-solid-content foamable urea modified A-stage phenolic resin and preparation method thereof |
| CN102977547A (en) * | 2012-10-08 | 2013-03-20 | 山东莱芜润达新材料有限公司 | Low temperature rapid-foaming phenol formaldehyde foam thermal insulation board preparation method |
| CN103214642A (en) * | 2013-04-23 | 2013-07-24 | 王博 | Normal-temperature foamed modified phenolic resin and method for producing high-performance fireproof heat preservation plate by using normal temperature foamed modified phenolic resin |
| CN103254381A (en) * | 2013-05-17 | 2013-08-21 | 江苏文昌电子化工有限公司 | Preparation method of nitrogenous phenolic resin in one-step synthesis process |
| 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 |
| CN103848951A (en) * | 2014-03-20 | 2014-06-11 | 新疆科西嘉新材料有限公司 | Method for continuously producing expandable phenolic resin |
| CN103849113A (en) * | 2014-03-20 | 2014-06-11 | 新疆科西嘉新材料有限公司 | Method for preparing expandable phenolic resin containing phenolic foam broken material |
| CN103865017A (en) * | 2014-03-25 | 2014-06-18 | 江苏锋芒复合材料科技集团有限公司 | Environment-friendly phenolic resin preparation process without wastewater discharge |
| CN103865016A (en) * | 2014-03-20 | 2014-06-18 | 新疆科西嘉新材料有限公司 | Preparation method of expandable phenolic resin |
| CN104404770A (en) * | 2014-12-16 | 2015-03-11 | 山东圣泉新材料股份有限公司 | Amino resin composition for flame-retardant wet curtain and preparation method and application thereof |
| CN107083017A (en) * | 2017-06-14 | 2017-08-22 | 济南大学 | A kind of normal temperature can send out synthesis and the foaming method of phenolic resin |
| CN108192055A (en) * | 2017-12-11 | 2018-06-22 | 安徽美克思科技有限公司 | A kind of synthesis technology of aramid fiber honeycomb nitrile rubber modified phenolic resin |
| CN109280326A (en) * | 2018-09-14 | 2019-01-29 | 营口象圆新材料工程技术有限公司 | A kind of phenolic board and preparation method thereof that rock wool is modified |
-
2011
- 2011-09-02 CN CN2011102572355A patent/CN102443126A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766243B (en) * | 2012-07-25 | 2015-03-25 | 胡玉 | Room-temperature foamable phenolic resin and method for preparing phenolic foams by same |
| CN102766243A (en) * | 2012-07-25 | 2012-11-07 | 胡玉 | Room-temperature foamable phenolic resin and method for preparing phenolic foams by same |
| CN102977547A (en) * | 2012-10-08 | 2013-03-20 | 山东莱芜润达新材料有限公司 | Low temperature rapid-foaming phenol formaldehyde foam thermal insulation board preparation method |
| CN102936325A (en) * | 2012-11-13 | 2013-02-20 | 中国林业科学研究院林产化学工业研究所 | High-solid-content foamable urea modified A-stage phenolic resin and preparation method thereof |
| CN102936325B (en) * | 2012-11-13 | 2014-04-16 | 中国林业科学研究院林产化学工业研究所 | High-solid-content foamable urea modified A-stage phenolic resin and preparation method thereof |
| CN103214642A (en) * | 2013-04-23 | 2013-07-24 | 王博 | Normal-temperature foamed modified phenolic resin and method for producing high-performance fireproof heat preservation plate by using normal temperature foamed modified phenolic resin |
| CN103254381A (en) * | 2013-05-17 | 2013-08-21 | 江苏文昌电子化工有限公司 | Preparation method of nitrogenous phenolic resin in one-step synthesis process |
| 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 |
| CN103848951A (en) * | 2014-03-20 | 2014-06-11 | 新疆科西嘉新材料有限公司 | Method for continuously producing expandable phenolic resin |
| CN103849113A (en) * | 2014-03-20 | 2014-06-11 | 新疆科西嘉新材料有限公司 | Method for preparing expandable phenolic resin containing phenolic foam broken material |
| CN103865016A (en) * | 2014-03-20 | 2014-06-18 | 新疆科西嘉新材料有限公司 | Preparation method of expandable phenolic resin |
| CN103848951B (en) * | 2014-03-20 | 2016-01-27 | 新疆美克思新材料股份有限公司 | A kind of method of continuous seepage expandable phenolic resin |
| CN103865016B (en) * | 2014-03-20 | 2016-01-27 | 新疆美克思新材料股份有限公司 | A kind of preparation method of expandable phenolic resin |
| CN103849113B (en) * | 2014-03-20 | 2016-01-27 | 新疆美克思新材料股份有限公司 | A kind of preparation method of the expandable phenolic resin containing phenol formaldehyde foam particle |
| CN103865017A (en) * | 2014-03-25 | 2014-06-18 | 江苏锋芒复合材料科技集团有限公司 | Environment-friendly phenolic resin preparation process without wastewater discharge |
| CN104404770A (en) * | 2014-12-16 | 2015-03-11 | 山东圣泉新材料股份有限公司 | Amino resin composition for flame-retardant wet curtain and preparation method and application thereof |
| CN107083017A (en) * | 2017-06-14 | 2017-08-22 | 济南大学 | A kind of normal temperature can send out synthesis and the foaming method of phenolic resin |
| CN108192055A (en) * | 2017-12-11 | 2018-06-22 | 安徽美克思科技有限公司 | A kind of synthesis technology of aramid fiber honeycomb nitrile rubber modified phenolic resin |
| CN109280326A (en) * | 2018-09-14 | 2019-01-29 | 营口象圆新材料工程技术有限公司 | A kind of phenolic board and preparation method thereof that rock wool is modified |
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Application publication date: 20120509 |