CN103865016A - Preparation method of expandable phenolic resin - Google Patents
Preparation method of expandable phenolic resin Download PDFInfo
- Publication number
- CN103865016A CN103865016A CN201410106895.7A CN201410106895A CN103865016A CN 103865016 A CN103865016 A CN 103865016A CN 201410106895 A CN201410106895 A CN 201410106895A CN 103865016 A CN103865016 A CN 103865016A
- Authority
- CN
- China
- Prior art keywords
- phenolic resin
- reaction
- preparation
- expandable phenolic
- paraformaldehyde
- 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.)
- Granted
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 28
- 229920001568 phenolic resin Polymers 0.000 title claims abstract description 25
- 239000005011 phenolic resin Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 229930040373 Paraformaldehyde Natural products 0.000 claims abstract description 16
- 229920002866 paraformaldehyde Polymers 0.000 claims abstract description 16
- 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
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 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 20
- 239000011347 resin Substances 0.000 abstract description 20
- 239000006260 foam Substances 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 4
- 239000003607 modifier Substances 0.000 abstract 2
- 238000007599 discharging Methods 0.000 abstract 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 17
- 229920003987 resole Polymers 0.000 description 6
- 238000007711 solidification Methods 0.000 description 5
- 230000008023 solidification Effects 0.000 description 5
- 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
- 230000015572 biosynthetic process Effects 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
- 238000003786 synthesis reaction Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 206010000269 abscess Diseases 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
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin 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 invention relates to a preparation method of expandable phenolic resin. The preparation method of the expandable phenolic resin comprises the following steps: preparing the following raw materials in parts by weight: 1000 parts of phenol, 700-750 parts of paraformaldehyde, 20-40 parts of catalyst and 40-80 parts of modifier; adding phenol, paraformaldehyde and catalyst into a reaction kettle, controlling temperature to be 60-90 DEG C, and performing a reaction for 3 hours; controlling reaction temperature to be 70 DEG C, adding the modifier into the reaction kettle, performing the reaction for 0.5 hour, cooling, and discharging, so that the expandable phenolic resin is obtained. Compared with the prior art, viscosity of the synthesized resin can be 3000-4000cps, heat produced in a curing process is less, the obtained phenolic resin is fine and smooth in foam and high in strength.
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., especially for the external-wall heat-insulation material resol used that foams, viscosity is more than 10000cps.Full-bodied resol has a lot of shortcomings in foam process, and as batch mixing difficulty, the row that flows in foaming process is poor, and expansion ratio is low etc., therefore need to reduce the viscosity of foamed phenolic resin.
Reducing the viscosity of resin has several different methods, 1., add solvent in resin, and as water etc.; 2., reduce level of response in resin building-up process.Method adds solvent in 1., can cause the foam of final foaming of poor quality, and as many in middle abscess, intensity is low etc.2. method reduces resin reaction degree, causes in resin expanded process thermal discharge large, and heartburn phenomenon appears in foam.
Summary of the invention
Object of the present invention is exactly to provide in a kind of solidification process thermal discharge little in order to overcome the defect that above-mentioned prior art exists, prepared phenol formaldehyde foam exquisiteness, 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 to reactor, controlling temperature is 60～90 ℃, reacts 3 hours;
(3) temperature of reaction is controlled to 70 ℃, adds wherein properties-correcting agent, continue reaction 0.5h, cooling discharge prepares expandable phenolic resin.
Described paraformaldehyde is that massfraction is 96% paraformaldehyde.
Described catalyzer is ammoniacal liquor or triethylamine.
Described properties-correcting agent is carboxamide.
Reaction in step (2) is first to react 1h at 60 ℃, is then warming up to 90 ℃ of reaction 2h.
Compared with prior art, the present invention has adopted mole proportioning of higher phenol and formaldehyde, effectively reduces the content of methylol in resol, can reduce the release of heat in resin curing process; Before pyroreaction, there is one section of low-temp reaction, the addition reaction that low-temp reaction is synthesis phase, when resin is synthesized, addition reaction energy can be more abundant, and while not only making resin solidification, thermal discharge reduces, and more can reduce the content of resin Free-formaldehyde; In last resin, add carboxamide, formaldehyde reaction free in resin generates urea-formaldehyde resin, greatly reduces the content of formaldehyde in resin.The synthetic resin viscosity of the present invention can be at 3000～4000cps, and in solidification process, thermal discharge is little, prepared phenol formaldehyde foam exquisiteness, 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, the catalyzer of use is ammoniacal liquor;
(2) phenol, paraformaldehyde, catalyzer are placed in to reactor, controlling temperature is 60 ℃, reacts 1 hour, then temperature is elevated to 90 ℃, continues reaction 2 hours;
(3) temperature of reaction is controlled to 70 ℃, add wherein properties-correcting agent carboxamide, continue reaction 0.5h, cooling discharge prepares expandable phenolic resin, the resol preparing is detected, and 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 preparing, thermal discharge is little, prepared phenol formaldehyde foam exquisiteness, 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:
Paraformaldehyde paraformaldehyde 700, catalyst of triethylamine 20, properties-correcting agent carboxamide 40 that phenol 1000, massfraction are 96%;
(2) phenol, paraformaldehyde, catalyzer are placed in to reactor, react for first reacting 1h at 60 ℃, be then warming up to 90 ℃ of reaction 2h;
(3) temperature of reaction is controlled to 70 ℃, adds wherein properties-correcting agent, continue reaction 0.5h, 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:
Paraformaldehyde 750, catalyst ammonia water 40, properties-correcting agent carboxamide 80 that phenol 1000, massfraction are 96%;
(2) phenol, paraformaldehyde, catalyzer are placed in to reactor, react for first reacting 1h at 60 ℃, be then warming up to 90 ℃ of reaction 2h;
(3) temperature of reaction is controlled to 70 ℃, adds wherein properties-correcting agent, continue reaction 0.5h, cooling discharge prepares expandable phenolic resin.
Because the present invention has adopted mole proportioning of higher phenol and formaldehyde, effectively reduce the content of methylol in resol, can reduce the release of heat in resin curing process; Before pyroreaction, there is one section of low-temp reaction, the addition reaction that low-temp reaction is synthesis phase, when resin is synthesized, addition reaction energy can be more abundant, and while not only making resin solidification, thermal discharge reduces, and more can reduce the content of resin Free-formaldehyde; In last resin, add carboxamide, formaldehyde reaction free in resin generates urea-formaldehyde resin, greatly reduces the content of formaldehyde in resin.
Claims (5)
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 to reactor, controlling temperature is 60～90 ℃, reacts 3 hours;
(3) temperature of reaction is controlled to 70 ℃, adds wherein properties-correcting agent, continue reaction 0.5h, 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 is that massfraction is 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.
5. the preparation method of a kind of expandable phenolic resin according to claim 1, is characterized in that, the reaction in step (2) is first to react 1h at 60 ℃, is then warming up to 90 ℃ of reaction 2h.
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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103865016A true CN103865016A (en) | 2014-06-18 |
| CN103865016B CN103865016B (en) | 2016-01-27 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| 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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| Country | Link |
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| CN (1) | CN103865016B (en) |
Cited By (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 |
Cited By (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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103865016B (en) | 2016-01-27 |
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| C06 | Publication | ||
| PB01 | Publication | ||
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| C53 | Correction of patent of invention or patent application | ||
| CB02 | Change of applicant information |
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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Free format text: CORRECT: APPLICANT; FROM: XINJIANG KEXI NEW MATERIAL CO., LTD. TO: XINJIANG MAX TECHNOLOGY DEVELOPMENT CO., LTD. |
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Address after: 832200 Xinjiang Uygur Autonomous Region Changji County Manasi County River Tower Industrial Park S area 301 - 1 plain forest farm territory Applicant after: XINJIANG KEXIJIA NEW MATERIAL CO., LTD. Address before: 832200, Xinjiang Uygur Autonomous Region, Changji County, Manasi County tower River Industrial Park S District 301 - 1 plain forest farm Applicant before: Xinjiang Max Technology Development Co., Ltd. |
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| C14 | Grant of patent or utility model | ||
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160127 Termination date: 20190320 |