CN103865016B - A kind of preparation method of expandable phenolic resin - Google Patents
A kind of preparation method of expandable phenolic resin Download PDFInfo
- Publication number
- CN103865016B CN103865016B CN201410106895.7A CN201410106895A CN103865016B CN 103865016 B CN103865016 B CN 103865016B CN 201410106895 A CN201410106895 A CN 201410106895A CN 103865016 B CN103865016 B CN 103865016B
- Authority
- CN
- China
- Prior art keywords
- phenolic resin
- reaction
- paraformaldehyde
- expandable phenolic
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 22
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 229930040373 Paraformaldehyde Natural products 0.000 claims abstract description 16
- 229920002866 paraformaldehyde Polymers 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 5
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 125000003917 carbamoyl group Chemical group [H]N([H])C(*)=O 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 229920005989 resin Polymers 0.000 abstract description 21
- 239000011347 resin Substances 0.000 abstract description 21
- 230000015572 biosynthetic process Effects 0.000 abstract description 7
- 238000003786 synthesis reaction Methods 0.000 abstract description 7
- 238000007711 solidification Methods 0.000 abstract description 6
- 230000008023 solidification Effects 0.000 abstract description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 17
- 239000006260 foam Substances 0.000 description 6
- 229920003987 resole Polymers 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 4
- 238000007259 addition reaction Methods 0.000 description 4
- 229920001807 Urea-formaldehyde Polymers 0.000 description 2
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 201000006549 dyspepsia Diseases 0.000 description 1
- 208000024798 heartburn Diseases 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Phenolic Resins Or Amino Resins (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The present invention relates to a kind of preparation method of expandable phenolic resin, get the raw materials ready according to following component and weight part content: phenol 1000, paraformaldehyde 700-750, catalyzer 20-40, properties-correcting agent 40-80; Phenol, paraformaldehyde, catalyzer are placed in reactor, and control temperature is 60 ~ 90 DEG C, reacts 3 hours; Temperature of reaction controlled at 70 DEG C, add properties-correcting agent wherein, continue reaction 0.5h, namely cooling discharge prepares expandable phenolic resin.Compared with prior art, the resin viscosity of the present invention's synthesis can at 3000 ~ 4000cps, and in solidification process, thermal discharge is little, and obtained phenol formaldehyde foam is fine and smooth, and intensity is high.
Description
Technical field
The present invention relates to exterior-wall heat insulation polymkeric substance, especially relate to a kind of preparation method of expandable phenolic resin.
Background technology
Current generally higher for the foam viscosity of resol used of phenolic resin foam lagging material, substantially at 6000 ~ 15000cps not etc., to foam resol used especially for external-wall heat-insulation material, viscosity is at more than 10000cps.Full-bodied resol has a lot of shortcoming in foam process, and as batch mixing is difficult, in foaming process, flowing row is poor, and expansion ratio is low, therefore needs the viscosity reducing foamed phenolic resin.
Reduce the viscosity of resin and have multiple method, 1., add solvent, as water etc. in resin; 2., level of response in resin synthesis process is reduced.Method 1. in add solvent, the foam of final foaming can be caused of poor quality, and as Intermediate cells is many, intensity is low.2. method reduces resin reaction degree, and cause thermal discharge in resin expanded process large, heartburn phenomenon appears in foam.
Summary of the invention
Object of the present invention is exactly provide thermal discharge in a kind of solidification process little to overcome defect that above-mentioned prior art exists, and obtained phenol formaldehyde foam is fine and smooth, the preparation method of the expandable phenolic resin that intensity is high.
Object of the present invention can be achieved through the following technical solutions:
A preparation method for expandable phenolic resin, adopts following steps:
(1) get the raw materials ready according to following component and weight part content:
Phenol 1000, paraformaldehyde 700-750, catalyzer 20-40, properties-correcting agent 40-80;
(2) phenol, paraformaldehyde, catalyzer are placed in reactor, control temperature is 60 ~ 90 DEG C, reacts 3 hours;
(3) temperature of reaction controlled at 70 DEG C, add properties-correcting agent wherein, continue reaction 0.5h, namely cooling discharge prepares expandable phenolic resin.
Described paraformaldehyde to be massfraction be 96% paraformaldehyde.
Described catalyzer is ammoniacal liquor or triethylamine.
Described properties-correcting agent is carboxamide.
Reaction in step (2) is first at 60 DEG C of reaction 1h, is then warming up to 90 DEG C of reaction 2h.
Compared with prior art, present invention employs higher phenol and the mol ratio of formaldehyde, effectively reduce the content of methylol in resol, the release of heat in resin curing process can be reduced; Have one section of low-temp reaction before pyroreaction, low-temp reaction is the addition reaction of synthesis phase, and when making resins synthesis, addition reaction can be more abundant, and when not only making resin solidification, thermal discharge reduces, and more can reduce the content of resin Free-formaldehyde; Add carboxamide in last resin, formaldehyde reaction free in resin generates urea-formaldehyde resin, greatly reduces the content of formaldehyde in resin.The resin viscosity of the present invention's synthesis can at 3000 ~ 4000cps, and in solidification process, thermal discharge is little, and obtained phenol formaldehyde foam is fine and smooth, and intensity is high.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
A preparation method for expandable phenolic resin, adopts following steps:
(1) processing compound:
Phenol: 1000g, 96% formaldehyde: 731g, catalyzer: 30g, properties-correcting agent: 60g, wherein, the properties-correcting agent of use is carboxamide, and the catalyzer of use is ammoniacal liquor;
(2) phenol, paraformaldehyde, catalyzer are placed in reactor, control temperature is 60 DEG C, reacts 1 hour, then temperature is elevated to 90 DEG C, continues reaction 2 hours;
(3) temperature of reaction is controlled at 70 DEG C, add properties-correcting agent carboxamide wherein, continue reaction 0.5h, namely cooling discharge prepares expandable phenolic resin, detect the resol prepared, its detected result is as follows: VIS=3200cps, NV=82.5%, GT=60sec, FF=0.7%.Can find out, in the expandable phenolic resin solidification process prepared, thermal discharge is little, and obtained phenol formaldehyde foam is fine and smooth, and intensity is high.
Embodiment 2
A preparation method for expandable phenolic resin, adopts following steps:
(1) get the raw materials ready according to following component and weight part content:
Phenol 1000, massfraction are paraformaldehyde paraformaldehyde 700, catalyst of triethylamine 20, the properties-correcting agent carboxamide 40 of 96%;
(2) phenol, paraformaldehyde, catalyzer being placed in reactor, reacting for first reacting 1h at 60 DEG C, be then warming up to 90 DEG C of reaction 2h;
(3) temperature of reaction controlled at 70 DEG C, add properties-correcting agent wherein, continue reaction 0.5h, namely cooling discharge prepares expandable phenolic resin.
Embodiment 3
A preparation method for expandable phenolic resin, adopts following steps:
(1) get the raw materials ready according to following component and weight part content:
Phenol 1000, massfraction are paraformaldehyde 750, catalyst ammonia water 40, the properties-correcting agent carboxamide 80 of 96%;
(2) phenol, paraformaldehyde, catalyzer being placed in reactor, reacting for first reacting 1h at 60 DEG C, be then warming up to 90 DEG C of reaction 2h;
(3) temperature of reaction controlled at 70 DEG C, add properties-correcting agent wherein, continue reaction 0.5h, namely cooling discharge prepares expandable phenolic resin.
Owing to present invention employs higher phenol and the mol ratio of formaldehyde, effectively reduce the content of methylol in resol, the release of heat in resin curing process can be reduced; Have one section of low-temp reaction before pyroreaction, low-temp reaction is the addition reaction of synthesis phase, and when making resins synthesis, addition reaction can be more abundant, and when not only making resin solidification, thermal discharge reduces, and more can reduce the content of resin Free-formaldehyde; Add carboxamide in last resin, formaldehyde reaction free in resin generates urea-formaldehyde resin, greatly reduces the content of formaldehyde in resin.
Claims (4)
1. a preparation method for expandable phenolic resin, is characterized in that, the method adopts following steps:
(1) get the raw materials ready according to following component and weight part content:
Phenol 1000, paraformaldehyde 700-750, catalyzer 20-40, properties-correcting agent 40-80;
(2) phenol, paraformaldehyde, catalyzer are placed in reactor, control temperature is 60 ~ 90 DEG C, reacts 3 hours, and wherein reaction is for first reacting 1h at 60 DEG C, is then warming up to 90 DEG C of reaction 2h;
(3) temperature of reaction controlled at 70 DEG C, add properties-correcting agent wherein, continue reaction 0.5h, namely cooling discharge prepares expandable phenolic resin.
2. the preparation method of a kind of expandable phenolic resin according to claim 1, is characterized in that, described paraformaldehyde to be massfraction be 96% paraformaldehyde.
3. the preparation method of a kind of expandable phenolic resin according to claim 1, is characterized in that, described catalyzer is ammoniacal liquor or triethylamine.
4. the preparation method of a kind of expandable phenolic resin according to claim 1, is characterized in that, described properties-correcting agent is carboxamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410106895.7A CN103865016B (en) | 2014-03-20 | 2014-03-20 | A kind of preparation method of expandable phenolic resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410106895.7A CN103865016B (en) | 2014-03-20 | 2014-03-20 | A kind of preparation method of expandable phenolic resin |
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| Publication Number | Publication Date |
|---|---|
| CN103865016A CN103865016A (en) | 2014-06-18 |
| CN103865016B true CN103865016B (en) | 2016-01-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410106895.7A Expired - Fee Related CN103865016B (en) | 2014-03-20 | 2014-03-20 | A kind of preparation method of expandable phenolic resin |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111393A (en) * | 2015-08-31 | 2015-12-02 | 沈阳化工大学 | Preparation method of foamable phenolic resin |
| CN111349202A (en) * | 2020-04-30 | 2020-06-30 | 江阴市威腾铝箔合成材料有限公司 | Preparation method of phenolic resin and phenolic foam material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101020736A (en) * | 2007-03-12 | 2007-08-22 | 谢建军 | Production process of foamed phenolic resin with high strength and low density |
| CN102443126A (en) * | 2011-09-02 | 2012-05-09 | 王博 | Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam |
| CN102617818A (en) * | 2012-04-10 | 2012-08-01 | 北京林业大学 | Preparation method of biological oil modified phenolic resin for foaming |
-
2014
- 2014-03-20 CN CN201410106895.7A patent/CN103865016B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101020736A (en) * | 2007-03-12 | 2007-08-22 | 谢建军 | Production process of foamed phenolic resin with high strength and low density |
| CN102443126A (en) * | 2011-09-02 | 2012-05-09 | 王博 | Low-temperature foaming phenolic resin, preparation method thereof and preparation method of modified phenolic foam |
| CN102617818A (en) * | 2012-04-10 | 2012-08-01 | 北京林业大学 | Preparation method of biological oil modified phenolic resin for foaming |
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| CN103865016A (en) | 2014-06-18 |
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Address after: 832200, the Xinjiang Uygur Autonomous Region, Changji County Manasi River Industrial Park S District 301 - 1 plain forest farm territory Applicant after: Xinjiang Max Technology Development Co., Ltd. Address before: 832200, the Xinjiang Uygur Autonomous Region Changji Hui Autonomous Prefecture Manasi County River Industrial Park S District 301 - 1 plain forest farm territory Applicant before: XINJIANG KEXIJIA NEW MATERIAL CO., LTD. |
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