CN101302304B - Preparation of epoxide resin based foam material - Google Patents
Preparation of epoxide resin based foam material Download PDFInfo
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- CN101302304B CN101302304B CN2008100340101A CN200810034010A CN101302304B CN 101302304 B CN101302304 B CN 101302304B CN 2008100340101 A CN2008100340101 A CN 2008100340101A CN 200810034010 A CN200810034010 A CN 200810034010A CN 101302304 B CN101302304 B CN 101302304B
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Abstract
The invention discloses a method for preparing an epoxide resin foaming material. The method comprises the following steps that: 1. according to the mass ratio, epoxide resins, foaming agents, foam stabilizing agents and addition agents are respectively picked up and evenly mixed with high-speed stirring; 2. the mixture obtained is put in an oven with a temperature of between 40 and 80 DEG C and pre-heated for 0.5 to 1 hour, and the mixture is taken out and cooled down to a temperature of between 25 and 35 DEG C; 3. The mixture is added with curing agents and evenly mixed; 4. the mixture is put in a stainless steel mold and heated at the temperature of between 40 to 80 DEG C for 0.5 to 2 hours, and the mixture is cooled down to the room temperature and taken out, and finally the finished products are obtained. By controlling reaction conditions, the invention realizes the association control of the chemical foaming and the curing molding of epoxy, and the foaming multiplying factor is as high as 2.7, and products prepared by the method are good in water resistance, chemical corrosion resistance and strength. The method of the invention has the advantages of easy buying of materials, simple operation and easy industrialization, and provides a new path for preparing thermosetting foaming materials.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of preparation method of epoxide resin based foam material.
Background technology
Characteristics such as epoxy foam is low because of its apparent density, light weight and structure are tough and tensile, and have than more excellent mechanical property, electric property, water tolerance and the chemical resistance of conventional urethane and polystyrene foamed plastics and higher thermostability etc., have broad application prospects in industries such as automobile, aerospace, biology, electronics, ocean goods, coating, medicine, thereby caused people's attention.Yet, because compact structure, abscess are fine and close and epoxide resin based foam material that have certain physical strength requires to foam and the synergistic effect of solidification process, promptly carrying out synchronously of foaming and solidification process synthesized the difficulty for preparing thereby greatly increased its foam material.So far, only have few scientists be devoted to epoxide resin based foam material preparation and performance study thereof.The method that can be used for preparing epoxide resin based foam material at present has: physics method, mechanical process and foaming.Yet all there is complicated operation in various degree in above-mentioned three kinds of reaction methods, stirring is uneven, cost is high, and generation toxic gas, product pattern are difficult to problems such as control, are difficult to large-scale production.Up to now, the domestic research report of not seeing the foaming of relevant epoxide resin based foam material as yet and solidifying collaborative processes.Therefore develop a kind of modern design, advanced technology, convenient and simple, with low cost, the bubble compact substance is equal, expansion ratio is high, reaction conditions is gentle, method that can the scale production epoxide resin based foam material is significant.
Summary of the invention
The object of the present invention is to provide a kind of with low cost, reaction conditions is gentle, can large-scale production the preparation method of epoxide resin based foam material.
The preparation method of the epoxide resin based foam material that the present invention proposes comprises the following steps: to comprise the following steps: a kind of preparation method of epoxide resin based foam material
A. according to mass ratio 100: (0.2～5): the ratio of (0.2～3) takes by weighing Resins, epoxy, whipping agent, suds-stabilizing agent respectively and mixes under 600～1000 rev/mins of high-speed stirring, wherein said Resins, epoxy is selected from a kind of in the bisphenol A type epoxy resin, described whipping agent is selected from a kind of in the azo compound, and described suds-stabilizing agent is selected from a kind of in the Tweens tensio-active agent;
B. the mixture that step a is obtained placed 20～100 ℃ of baking oven preheatings 15 minutes～1 hour, took out then and was chilled to 20～40 ℃;
C. to step b make mixture in add massfraction be 10%～25% solidifying agent of Resins, epoxy 600～1000 rev/mins of high-speed stirring until mixing, wherein said solidifying agent is selected from a kind of in the low Temperature Curing Agent for Epoxy Resin;
D. the mixture that step c is obtained places stainless steel mould 20～100 ℃ of heating 0.5～2 hour, is chilled to then to take out after the room temperature promptly to obtain the finished product epoxide resin based foam material.
Step a further adds auxiliary agent when blending epoxy, whipping agent, suds-stabilizing agent, the mass ratio of Resins, epoxy and auxiliary agent is 100: (x～70), described auxiliary agent are Powdered packing material.
The useful result of invention is as follows: the present invention is a kind of by gate ring epoxy resins foaming and solidified collaborative processes in principle, in, low temperature prepares the method for epoxide resin based foam material down, belong to chemical method and foam.Chemical blowing process is a kind of effective plastic foamed method, and its principle is to be accompanied by chemical reaction to produce gas and foam in foaming process.The key distinction of other foaming methods such as this method and mechanical process and physics method is temperature.For in, the foam materials that obtains even structure, abscess densification under the cryogenic preparation condition, have certain physical strength, can adopt the two-step approach of chemical foaming, this method can be divided into pre-frothing and two processes of foamed solidification moulding.In the pre-frothing process, whipping agent joins in the liquid mixture, and chemical reaction produces gas and forms solution-air solution, and with the increase of gas volume, gas evolution makes and forms a large amount of nuclei of bubbles and then expand into foams in the resin system; In the foamed solidification moulding process, foaming process makes foam further grow up and forms nuclei of bubbles and the supersaturated gas that is evenly distributed; The polycondensation that solidifying agent caused simultaneously makes the visco-elasticity of reaction system raise gradually, and flowability descends gradually, and final reaction is finished, and reaches curing molding, finally forms stable cavernous structure.The present invention is by the chemical foaming of gate ring epoxy resins and the collaborative processes of curing molding, select Resins, epoxy, whipping agent and solidifying agent reaction, by pre-frothing with introduce the collaborative processes that suds-stabilizing agent is controlled its chemical foaming and curing molding, the preparation epoxide resin based foam material.In this reaction system, can be by changing the oxirane value of Resins, epoxy, the kind of whipping agent, suds-stabilizing agent and solidifying agent and add-on, addition sequence, temperature of reaction and reaction times wait the expansion ratio of control material and intensity etc.Particularly: one, the present invention makes epoxy foaming and curing molding process synergic carry out by the control production technique, be to produce in the Resins, epoxy foaming system when having the foams of foam structure in a large number, by curing molding fixed foam body, obtain the goods that hard bubble; Two, the present invention can prepare expansion ratio up to epoxide resin based foam material 2.7, varying strength; Three, the product of the present invention preparation has good mechanical performance, electric property, water tolerance and chemical resistance and higher thermostability etc.; Four, raw material of the present invention is easy to get, and is simple to operate, and plant and instrument is easy, the expansion ratio height, and intensity is easily controlled, and it is convenient to handle, and is easy to industrialization, for the control preparation of porous plastics provides new approach.
Description of drawings
Fig. 1 is the alveolar layer sectional view of embodiment 1.
Embodiment
Below by drawings and Examples the present invention is described in further detail, a kind of preparation method of epoxide resin based foam material comprises the following steps:
A. according to mass ratio 100: (0.2～5): the ratio of (0.2～3) takes by weighing Resins, epoxy, whipping agent, suds-stabilizing agent respectively and mixes under 600～1000 rev/mins of high-speed stirring, wherein said Resins, epoxy is selected from a kind of in the bisphenol A type epoxy resin, described whipping agent is selected from a kind of in the azo compound, and described suds-stabilizing agent is selected from a kind of in the Tweens tensio-active agent;
B. the mixture that step a is obtained placed 20～100 ℃ of baking oven preheatings 15 minutes～1 hour, took out then and was chilled to 20～40 ℃;
C. to step b make mixture in add massfraction be 10%～25% solidifying agent of Resins, epoxy 600～1000 rev/mins of high-speed stirring until mixing, wherein said solidifying agent is selected from a kind of in the low Temperature Curing Agent for Epoxy Resin;
D. the mixture that step c is obtained places stainless steel mould 20～100 ℃ of heating 0.5～2 hour, is chilled to then to take out after the room temperature promptly to obtain the finished product epoxide resin based foam material.
Step a further adds auxiliary agent when blending epoxy, whipping agent, suds-stabilizing agent, the mass ratio of Resins, epoxy and auxiliary agent is 100: (18～70), described auxiliary agent are Powdered packing material.
Embodiment 1
(1) according to mass ratio 100: 3: 1: 18 ratio takes by weighing bisphenol A type epoxy resin, Diisopropyl azodicarboxylate, tween-80, light calcium carbonate and talcous mixture respectively and mixes under 600～1000 rev/mins high-speed stirring;
(2) mixture in the step (1) is placed 75 ℃ baking oven preheating take out after 0.5 hour, be chilled to 30 ℃;
(3) in step (2), add the triethylene tetramine solidifying agent of Resins, epoxy massfraction 10% in the gained mixture, in 600～1000 rev/mins high-speed stirring until mixing;
(4) mixture in the step (3) is placed stainless steel mould,, take out after being chilled to room temperature, promptly obtain product of the present invention in 75 ℃ of heating 1 hour.
The product that embodiment 1 obtains characterizes the pattern of product, intensity, expansion ratio etc. by electronic universal tester etc., as illustrated in fig. 1 and 2, this foam material by the bubble compact substance all, the closed pore of expansion ratio～2.7, aperture～0.1mm forms; The bending and the compressive strength of material are respectively 7.18N/cm
2And 2.42N/cm
2
Embodiment 2
In the step (2), cooling temperature changes 25 ℃ into, in the step (3), the adding umber of triethylene tetramine is 25% of a Resins, epoxy massfraction, other conditions and step and embodiment 1 are identical, the gained foam material by the bubble compact substance all, the closed pore of expansion ratio～2.4, aperture～0.05mm forms, the bending and the compressive strength of material are respectively 10.69N/cm
2And 3.76N/cm
2
Embodiment 3
In the step (2), cooling temperature changes 20 ℃ into, in the step (3), replace triethylene tetramine as solidifying agent with diethylenetriamine, other conditions and step and embodiment 1 are identical, the gained foam material by the bubble compact substance all, the closed pore of expansion ratio～2.2, aperture～0.06mm forms, the bending and the compressive strength of material are respectively 10.5N/cm
2And 3.65N/cm
2
Embodiment 4
In the step (1), do not add auxiliary agent, (2) preheating temperature is 80 ℃, and other conditions and step and embodiment 1 are identical, the gained foam material by the bubble compact substance all, the closed pore of expansion ratio～3, aperture～0.2mm forms, the bending and the compressive strength of material are respectively 3.70N/cm
2And 1.90N/cm
2
Embodiment 5
According to mass ratio 100: 3: 1: 70 ratio took by weighing the talcous mixture of bisphenol A type epoxy resin, Diisopropyl azodicarboxylate, tween-80, light calcium carbonate and auxiliary agent respectively, place 80 ℃ baking oven preheating to take out after 0.5 hour in this mixture, be chilled to 30 ℃; Other conditions and step and embodiment 1 are identical, the gained foam material by the bubble compact substance all, the closed pore of expansion ratio～2, aperture～0.04mm forms, the bending and the compressive strength of material are respectively 6.42N/cm
2And 2.35N/cm
2
Embodiment 6
According to mass ratio 100: 0.2: 1: 18 ratio took by weighing bisphenol A type epoxy resin, Cellmic C 121, tween-80, light calcium carbonate and talcous mixture respectively, place 100 ℃ baking oven preheating to take out after 0.5 hour in this mixture, be chilled to 30 ℃; Other conditions and step and embodiment 1 are identical, the gained foam material by the bubble compact substance all, the closed pore of expansion ratio～1.5, aperture～0.01mm forms, the bending and the compressive strength of material are respectively 7.82N/cm
2And 2.96N/cm
2
Described content only is 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 (1)
1. the preparation method of an epoxide resin based foam material comprises the following steps:
A. according to mass ratio 100: (0.2～5): the ratio of (0.2～3) takes by weighing Resins, epoxy, whipping agent, suds-stabilizing agent respectively and mixes under 600～1000 rev/mins of high-speed stirring, wherein said Resins, epoxy is selected from a kind of in the bisphenol A type epoxy resin, described whipping agent is selected from a kind of in the azo compound, and described suds-stabilizing agent is selected from a kind of in the Tweens tensio-active agent;
B. the mixture that step a is obtained placed 20～100 ℃ of baking oven preheatings 15 minutes～1 hour, took out then and was chilled to 20～40 ℃;
C. until mixing, wherein said solidifying agent is selected from a kind of in the low Temperature Curing Agent for Epoxy Resin to 10%～25% the solidifying agent that adds massfraction and be Resins, epoxy in the mixture that step b makes 600～1000 rev/mins of high-speed stirring;
D. the mixture that step c is obtained places stainless steel mould 20～100 ℃ of heating 0.5～2 hour, is chilled to then to take out after the room temperature promptly to obtain the finished product epoxide resin based foam material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100340101A CN101302304B (en) | 2008-02-28 | 2008-02-28 | Preparation of epoxide resin based foam material |
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| CN2008100340101A CN101302304B (en) | 2008-02-28 | 2008-02-28 | Preparation of epoxide resin based foam material |
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| CN101302304A CN101302304A (en) | 2008-11-12 |
| CN101302304B true CN101302304B (en) | 2011-04-27 |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863747A (en) * | 2012-09-25 | 2013-01-09 | 中国工程物理研究院化工材料研究所 | High-temperature-resistance high-strength epoxy foam plastic and preparation method thereof |
| JP2015055667A (en) * | 2013-09-10 | 2015-03-23 | ヤマハ株式会社 | Keyboard instrument |
| CN104530463A (en) * | 2014-12-26 | 2015-04-22 | 上海材料研究所 | Preparation method of epoxy resin foamed plastic |
| CN106566192A (en) * | 2015-10-13 | 2017-04-19 | 河南卓尔航空科技有限公司 | Foaming material |
| CN106398122B (en) * | 2016-10-13 | 2018-06-08 | 常州大学 | A kind of graphene epoxy resin composite foam material and preparation method thereof |
| CN113248873A (en) * | 2021-06-25 | 2021-08-13 | 江苏中科聚合新材料产业技术研究院有限公司 | Low-density conductive wave-absorbing epoxy resin foam material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4410639A (en) * | 1983-04-20 | 1983-10-18 | Albany International Corp. | Curing polyepoxide resin binders in high density syntactic foam forming compositions |
| CN1314925A (en) * | 1998-08-27 | 2001-09-26 | 亨凯尔公司 | Storage-stable compositions useful for the production of structural forms |
| CN1626578A (en) * | 2003-11-04 | 2005-06-15 | 日东电工株式会社 | Steel-plate-reinforcement resin composition, steel plate reinforcing sheet, and reinforcing method of steel plate |
-
2008
- 2008-02-28 CN CN2008100340101A patent/CN101302304B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4410639A (en) * | 1983-04-20 | 1983-10-18 | Albany International Corp. | Curing polyepoxide resin binders in high density syntactic foam forming compositions |
| CN1314925A (en) * | 1998-08-27 | 2001-09-26 | 亨凯尔公司 | Storage-stable compositions useful for the production of structural forms |
| CN1626578A (en) * | 2003-11-04 | 2005-06-15 | 日东电工株式会社 | Steel-plate-reinforcement resin composition, steel plate reinforcing sheet, and reinforcing method of steel plate |
Non-Patent Citations (5)
| Title |
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| 278. |
| 278.;张京珍等.泡沫塑料成型加工 第一版.化学工业出版社,2005,49-50. * |
| 张京珍等.泡沫塑料成型加工 第一版.化学工业出版社,2005,49-50. |
| 钱志屏.泡沫塑料 第一版.中国石化出版社,1998,281-282. |
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