KR101565281B1 - Insulating Material Compositions for Having Inorganic Foam Material, Process for preparing Insulating Materials and Insulating Materials Prepared Therefrom - Google Patents
Insulating Material Compositions for Having Inorganic Foam Material, Process for preparing Insulating Materials and Insulating Materials Prepared Therefrom Download PDFInfo
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- KR101565281B1 KR101565281B1 KR1020150057216A KR20150057216A KR101565281B1 KR 101565281 B1 KR101565281 B1 KR 101565281B1 KR 1020150057216 A KR1020150057216 A KR 1020150057216A KR 20150057216 A KR20150057216 A KR 20150057216A KR 101565281 B1 KR101565281 B1 KR 101565281B1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
- C08G8/32—Chemically modified polycondensates by organic acids or derivatives thereof, e.g. fatty oils
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/065—Hydrides or carbides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
Abstract
Description
The present invention relates to a heat insulating material composition using an inorganic foaming agent, a method for manufacturing a heat insulating material, and a heat insulating material produced therefrom. More particularly, the present invention relates to a heat insulating material composition, a method of manufacturing a heat insulating material, and a method of manufacturing a heat insulating material using an inorganic foaming agent capable of improving the heat insulating property by lowering thermal conductivity in the production of a phenolic resin foam by using silicon carbide (SiC), which is an inorganic foaming agent, And a heat insulating material produced therefrom.
Currently, most of the insulation materials used in Korea and abroad are insulation materials made of polystyrene (PS) foam, polyurethane (PU) foam and glass fiber. Polystyrene foam and polyurethane foam insulation have the advantage of being light in weight and excellent in warmth, but they are easily burned and poisonous gas is generated during combustion. In addition, glass fiber insulation has a very good flame retardancy, but its thermal insulation is poor and glass fiber itself is harmful to the human body.
In order to overcome these problems, many researches and alternative materials have been developed. Among them, substitute materials using phenol resin having excellent flame retardancy have been developed as polymeric resins. Phenol resin is a thermosetting resin with excellent heat resistance and has a very high self-ignition temp. Of 480 ° C. Water (H 2 O) and carbon dioxide (CO 2 ) And less generation of toxic gas. Phenolic resin foams made from these phenolic resins have little thermal deformation even at high temperatures because of their excellent heat resistance. In addition, the thermal conductivity of phenolic resin foam is similar to conventional insulation and is very strong in chemical action and solvent. Therefore, phenol resin foam can be used for various indoor, exterior decoration, molding, and the like, which are required to be nonflammable, and is also used as a structural material for railway vehicles and aircraft, and its application range is very wide.
In addition, the phenolic resin foam exhibits flame retardancy, heat resistance, low ductility and lowest thermal conductivity as compared with the conventional organic compound-based heat insulating material. When a contact is made with a flame, a carbonized film is formed on the surface to prevent flame propagation, And the shape is not changed. In the case of foreign countries, phenol resin foam is commonly used as a building insulation material, especially ceiling material. In most cases, a phenol resin phenol resin is used in the form of a resol-type phenol resin, especially a basic catalyst such as NaOH, NH 3 and the like in a reaction molar ratio (F / P) A phenol resin which is produced by using a resol type phenol resin is used.
Such a phenol resin foam using a phenol resin is usually obtained by stirring an additive such as a foam stabilizer, a plasticizer, a foaming agent, a curing agent, a flame retardant, etc. to a predetermined proportion of a phenol resin.
At this time, since the contained phenol resin accounts for 70 to 90% by weight of the total composition, it largely influences the overall physical properties of the foam. Particularly, the amount of water contained in the phenol resin greatly influences the heat insulating performance of the phenolic resin foam. When the amount of water contained in the phenol resin is too small, the water content is favorable for the heat insulating performance, but the viscosity is too high, If it is difficult to control in the process and contains too much water, the heat insulating performance is deteriorated and the adhesive force of the phenol resin foam becomes low, so that it becomes impossible to produce the laminate type foam. Therefore, the moisture content and viscosity contained in the phenol resin It is important to control it.
Thus, conventionally, after the phenol resin addition and condensation reaction, the degassing process is separately performed to remove the moisture contained in the phenol resin. However, since the artificial moisture removal of the degassing process causes the viscosity of the phenol resin to increase exponentially, It is not easy to control and it is not smoothly mixed with other additives and it is difficult to apply it to the production of phenol resin foam.
As a conventional technology relating to a heat insulating material composition, Patent Document 0001 discloses a resin composition comprising a resol type phenol resin, a curing agent, a foaming agent and a foaming agent, wherein the resol type phenol resin has a moisture content of 4.0% cps < / RTI > or less " However, the phenol resin foam prepared by the above composition has disadvantages in that the heat conductivity is not satisfactory by using an organic compound such as butane as a foaming agent and the heat insulating property is not excellent.
Therefore, it is inevitable to develop a new technology for producing a product having excellent heat insulation property by lowering the thermal conductivity by preparing a phenol resin foam by varying the kind of the foaming agent in the heat insulating material composition.
Disclosure of the Invention The present invention has been conceived in order to solve the above problems. It is an object of the present invention to provide a heat insulating material composition using an inorganic foaming agent capable of producing a product having excellent heat insulating property by lowering thermal conductivity by producing phenolic resin foam using silicon carbide as a foaming agent of a heat insulating material composition. A method for manufacturing a heat insulating material, and a heat insulating material manufactured from the method.
In order to achieve the above object, the present invention provides a solution means.
The present invention relates to a resin composition comprising 100 parts by weight of a resol type phenolic resin, 5 to 10 parts by weight of silicon carbide (SiC) as a foaming agent, 5 to 10 parts by weight of a curing agent and 2 to 5 parts by weight of a foaming agent, 5 to 10% by weight, and a viscosity at 25 DEG C of 4,000 to 9,000 mPa / s. The present invention also provides a heat insulating material composition using the inorganic foaming agent.
The present invention also relates to a thermosetting resin composition comprising 100 parts by weight of a resol-type phenol resin having a water content of 5 to 10% by weight and a viscosity at 25 DEG C of 4,000 to 9,000 mPa / s, 5 to 10 parts by weight of silicon carbide (SiC) To 10 parts by weight of a foaming agent, and 2 to 5 parts by weight of a foaming agent, and foaming and curing the phenolic resin foam composition.
The present invention also provides a heat insulating material having a thermal conductivity of 0.018 W / mK or less.
Means for solving the other specific problems according to the present invention are described in the detailed description of the invention.
The present invention having the above-described configuration can be expected to have the following technical and economic effects.
First, the heat insulating material composition according to the present invention is advantageous in that it can foam a foam using silicon carbide as a foaming agent, thereby lowering the thermal conductivity of the phenol resin foam, thereby manufacturing a product having excellent heat insulation.
Second, there is an advantage that it is useful as an eco-friendly construction material in which formaldehyde is hardly released in the heat insulating material itself, and therefore, there is little release of formaldehyde, and toxic gases and soot are not generated even in the case of fire.
Hereinafter, a heat insulating material composition, a method of manufacturing a heat insulating material, and a heat insulating material manufactured from the inorganic foaming agent according to the present invention will be described in detail.
First, the heat insulating material composition using the inorganic foaming agent comprises 100 parts by weight of a resol-type phenol resin, 5 to 10 parts by weight of silicon carbide (SiC) as a foaming agent, 5 to 10 parts by weight of a curing agent and 2 to 5 parts by weight of a foaming agent, The resin has a moisture content of 5 to 10% by weight and a viscosity at 25 DEG C of 4,000 to 9,000 mPa / s.
The resol type phenol resin among the constituents of the heat insulating material composition has a water content of 10.0 wt% or less and a viscosity at 25 DEG C of 4,000 to 9,000 mPa / s. It is easy. As a specific example, it is preferable to use Neolite OG-5000 manufactured by KANAMI HIZATSU CO., LTD. As a phenol resin for a resol-type insulating material in order to keep the open cell ratio, the heat insulation property and the flame retardancy high.
The resol type phenol resin has a pH of 6.5 to 7.5 and is excellent in terms of storage stability and self-polymerization prevention because of neutralization of the resin. The water content is 5 to 10% by weight and the viscosity at 25 ° C is 4,000 to 9,000 mPa / s (measured by Brookfield viscometer), the viscosity of the conventional resol-type phenol resin is very low compared to the moisture content of the resin. Therefore, the phenol resin foam has a low viscosity, And is suitable for insulation.
The heat insulating material composition using the inorganic foaming agent of the present invention contains a foaming agent to facilitate foaming of the resol-type phenol resin. The use of silicon carbide (SiC) as the foaming agent is a major feature of the present invention. The silicon carbide is reacted with water contained in the resol-type phenol resin to cause a hydrolysis reaction by reacting according to the following chemical formula to generate hydrogen (H 2 ) to form a foam in the phenol resin.
SiC + 2H 2 O? SiO 2 + 2H 2
The silicon carbide is used in an amount of 5 to 10 parts by weight based on 100 parts by weight of the resol-type phenol resin. When the amount of the silicon carbide is less than 5 parts by weight, foaming is not properly performed. When the amount is more than 10 parts by weight, And an unstable cell structure may be generated.
Further, the heat insulating material composition using the inorganic foaming agent of the present invention includes a curing agent to help the phenolic resin foam to cure while maintaining a desired foaming speed, improve the appearance of the product, and maintain the mechanical strength. The curing agent is not particularly limited as long as it is a curing agent capable of curing the resol-type phenolic resin. Examples of the curing agent include phosphoric acid, arylsulfonic acid, paratoluenesulfonic acid, phenolsulfonic acid, benzenesulfonic acid, xylenesulfonic acid, sulfuric acid, and the like. Commercially available curing agents include xylenesulfonic acid , Para-toluenesulfonic acid (PTSA), phosphoric acid and the like of Samjung Chemical Co., Ltd. can be used. In the present invention, the above-mentioned curing agent may be used as the above-described components, but it is preferably a non-aqueous dispersion curing agent, more preferably an aryl sulfonic acid (COOH), which is dispersed at a high concentration of 75% or more in polyethylene glycol, ethylene glycol, acid. If the curing agent is dispersed in water or a water-containing curing agent is used, the water contained in the curing agent may deteriorate the physical properties of the heat insulating material even if the water content of the resol-type phenol resin is low.
The curing agent is used in an amount of 6 to 15 parts by weight based on 100 parts by weight of the resol-type phenol resin. When the amount of the curing agent is less than 6 parts by weight, curing and foaming of the heat insulating material are not sufficiently performed. The speed becomes too fast, so that it is difficult to control the heat insulating material in the manufacturing process, and the heat insulating material may be corroded.
The heat insulating material composition using the inorganic foaming agent of the present invention contains a foaming agent in order to uniformly control the foam shape and size, excellent heat insulation property, foam stabilization and uniform distribution upon foaming of the resol type phenolic resin. The foam stabilizer may be a surfactant and may be any foam stabilizer that can be used in the formation of a heat insulating material. Examples thereof include silicone compounds such as polydimethyl siloxane and the like, polyoxyethylene and polyoxyethylene Polyoxypropylene derivatives, polyoxyethylene glycol, polyoxyethylene / polyoxypropylene random copolymer or polyoxyethylene / polyoxypropylene block copolymer, polyoxyethylene alkylphenol condensation product, polyoxyethylene alkyl ether At least one member selected from the group consisting of polyethylene glycol fatty acid esters, polyoxyethylene castor ethers, polyoxyethylene hydrogenated castor ethers, polyoxyethylene amines and polyoxyethylene lauryl ethers . ≪ / RTI > As a commercially available foam stabilizer, a non-ionic foam stabilizer of Hangan Chemical Co., Ltd., a nonionic foam stabilizer of Southeast Sumitomo Corporation, and SM3210P of KCC Co., Ltd. can be used.
Such a foam stabilizer is used in an amount of 2 to 5 parts by weight based on 100 parts by weight of the resol-type phenol resin. If the amount is less than 2 parts by weight, foaming of the heat insulating material may not be smoothly performed. There is a problem that the heat insulating material is broken and it is difficult to use the heat insulating material.
The heat insulating material composition using the inorganic foaming agent of the present invention may include aliphatic alcohol and polyammonium phosphate as an additive in order to improve the cell structure and flame retardancy of the heat insulating material more stably. As the aliphatic alcohol, propylene glycol, glycerin and the like can be used. The content of the additive varies depending on the use of the phenolic resin foam, and the aliphatic alcohol may be used in an amount of 2 to 5 parts by weight based on 100 parts by weight of the resol-type phenol resin, and the polyammonium phosphate may be used in an amount of 5 to 8 parts by weight.
Such a heat insulating material composition can be produced by mixing the above-mentioned constituent components. That is, the foamable phenolic resin composition may contain all of the constituent components immediately before preparation of the phenol foam, and the constituent components may be stored separately before the preparation.
The method for producing a heat insulating material according to the present invention can produce a phenol foam by foaming and curing the heat insulating material composition described above. The foaming and curing of the phenol resin foam can be carried out by heating to 60 to 80 캜, stirring at a constant speed, and then atmospheric pressure or pressure foaming can be employed in the mold. The foaming agent, the foam stabilizer and the additive may be added to the resol-type phenol resin in advance, or may be added simultaneously with the curing agent. For example, the phenol resin foam composition is mixed with the resol-type phenol resin at a temperature of 22 to 25 ° C for 30 seconds at a speed of 2000 to 3000 rpm using a high-speed stirrer. When the stirring speed is out of the above range, mixing of all the components is uneven, so that a foam exhibiting good physical properties can not be obtained.
The mold can be used without particular limitation as long as it is a mold capable of externally releasing moisture generated during the curing reaction of the phenol resin foam composition. The size of the mold is designed to be 250 mm x 250 mm x 200 mm in width x length x height In order to increase the density of the foam, an SUS steel plate of 220 mm x 220 mm x 1 mm in width x length x height can be placed and cured.
Thus, the mold into which the heat insulating material composition is injected is cured and foamed in an oven at 60 to 80 ° C for 3 to 8 minutes to obtain a heat insulating material. The curing and foaming may be carried out at room temperature, but foaming is preferably carried out in an oven in order to obtain a yield of the foam, discharge of moisture and formation of a good foam. If the foaming is carried out at a high temperature exceeding 80 캜 The cells of the heat insulating material may be poor due to too rapid curing and foaming, and when foaming at less than 60 ° C, foaming may not occur sufficiently and the quality of the product may become poor.
As described above, the heat insulating material produced by the present invention has a thermal conductivity of 0.018 W / mK or less, a density of 35 to 60 kg / m3, a strength of 0.30 to 0.45 Mpa, and a thermal conductivity of 0.018 W / mK or less, Can be effectively reduced, and the density and the strength are included in the above-mentioned range, so that the present invention can be applied to various applications.
In addition, the appearance of the heat insulating material produced in the present invention has a weak black color, and each cell is foamed without a hole in the barrier wall in a closed cell state. When the bubble size and the distribution at the time of foaming, the insulation material (foam) is excellent, it means that the insulation and the low ductility are excellent. When the ratio of the bubbles of the insulation material having independent pores (independent bubble ratio) is more than 90% . The bubble size of the foam is usually in the range of 50 to 500 mu m, and the average pore size of the heat insulating material produced in the present invention falls within the range of 100 to 400 mu m.
Since the heat insulating material according to the present invention is foamed using a resol-type phenolic resin having flame retardancy, the flame retardancy of the foam is exhibited without the need of a separate flame retardant agent, which is excellent in terms of environment, production process, and production cost. Also,
The insulation material according to the present invention contains a phenol resin having a low water content and a non-aqueous dispersion curing agent while minimizing the moisture effect of the foam and facilitating the workability. At the same time, the heat insulating property, flame retardancy, It can be used as a substitute material for solving the problems of styrofoam and urethane foam insulation which are widely used as existing insulation materials, and various applications of industrial insulation and building materials of high-function insulation materials are expected.
Hereinafter, the present invention as described above can be better understood by the following examples, and the examples are for illustrative purposes only, and the present invention is not limited by these examples.
≪ Example 1 >
The resol type phenol resin was prepared by mixing 8 g of silicon carbide as a foaming agent, 7 g of para-toluenesulfonic acid (PTSA) as a curing agent, 10 g of a polyol as a foaming agent ( (250 mm x 250 mm x 200 mm) with stirring at room temperature (2500 rpm) at room temperature, followed by heating at 70 ° C Insulating material was prepared by foaming in an oven for 5 minutes. The water content was measured by the Karl Fischer method and the viscosity was measured at 25 ° C using a Brookfield DV-II + Pro Programmable Viscometer using a # 64 Spindle.
≪ Examples 2 to 7 >
As compared with Example 1, only the difference in the mixing ratio of the constituent components was adjusted as shown in Table 1 below, and the rest were the same to produce a heat insulator.
Resol type phenol resin 100 g
≪ Comparative Example 1 &
Compared with Example 1, only a composition of 3 g of polyoxyethylene castor ether as a foaming agent, 5 g of n-pentane as a blowing agent and 8 g of PTSA as a curing agent was used in 100 g of a resol type phenolic resin having a moisture content of 2.9% by weight and a viscosity of 12,400 cps And the remaining parts were the same.
≪ Comparative Example 2 &
Compared with Example 1, only a composition obtained by mixing 3 g of polyoxyethylene castor ether as a foaming agent, 5 g of n-pentane as a blowing agent and 9 g of PTSA as a curing agent was used in 100 g of a resol type phenolic resin having a moisture content of 9.0 wt% and a viscosity of 7,200 cps And the remaining parts were the same.
Various physical properties of the heat insulating materials prepared in Examples 1 to 7 and Comparative Examples 1 and 2 were measured as follows.
<Experimental Example 1> Measurement of thermal conductivity
The heat insulating materials prepared in Examples 1 to 7 and Comparative Examples 1 and 2 were set to a size of 300 mm in width and length, respectively, and the low temperature plate and the high temperature plate were set to 10 ° C. and 30 ° C., respectively. The results are shown in Table 2 below. ≪ tb > < TABLE >
≪ Experimental Example 2 >
The insulation materials prepared in Examples 1 to 6 and Comparative Examples 1 and 2 were measured using a tensile strength meter (UTM, manufactured by Lloyd) according to ASTN D1621, and the results are shown in Table 2 below.
<Experimental Example 3> Density Measurement
The heat insulating materials prepared in Examples 1 to 7 and Comparative Examples 1 and 2 were measured by measuring the weight and volume at 200 mm in length, height and height, respectively, and were measured in accordance with JIS A 9511: 2006R. Are shown in [Table 2].
(W / mK)
(MPa)
(Kg / m3)
<Analysis of Test Results>
In the performance comparison table [Table 2], which is a result of various tests for the above Examples 1 to 7 and Comparative Examples 1 and 2, Examples 1 and 2, which are insulators made of the phenol resin foam composition according to the present invention, Strength and density as compared with those of Examples 3 to 7 and Comparative Examples 1 and 2 which were out of the range, and it can be seen that the results are remarkably superior to the comparative examples in all respects.
The scope of protection of the present invention is limited only by the matters described in the claims, and those skilled in the art can improve and modify the technical idea of the present invention in various forms. Accordingly, such improvements and modifications will fall within the scope of the present invention as long as they are obvious to those skilled in the art.
Claims (7)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109401183A (en) * | 2018-10-25 | 2019-03-01 | 太尔胶粘剂(广东)有限公司 | A kind of phenolic foam material and its preparation method and application for polishing |
| KR20200002663A (en) * | 2018-06-29 | 2020-01-08 | 주식회사 한국특수불연 | Method for manufacturing heat insulating material having foam structure using resol type phenol resin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000119424A (en) | 1998-10-16 | 2000-04-25 | Asahi Chem Ind Co Ltd | Foam of phenolic resin containing inorganic material |
| JP2014159713A (en) * | 2013-02-20 | 2014-09-04 | Nisshin Steel Co Ltd | Method of manufacturing composite building material |
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2015
- 2015-04-23 KR KR1020150057216A patent/KR101565281B1/en active IP Right Grant
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000119424A (en) | 1998-10-16 | 2000-04-25 | Asahi Chem Ind Co Ltd | Foam of phenolic resin containing inorganic material |
| JP2014159713A (en) * | 2013-02-20 | 2014-09-04 | Nisshin Steel Co Ltd | Method of manufacturing composite building material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20200002663A (en) * | 2018-06-29 | 2020-01-08 | 주식회사 한국특수불연 | Method for manufacturing heat insulating material having foam structure using resol type phenol resin |
| KR102121517B1 (en) * | 2018-06-29 | 2020-06-26 | 주식회사 한국특수불연 | Method for manufacturing heat insulating material having foam structure using resol type phenol resin |
| CN109401183A (en) * | 2018-10-25 | 2019-03-01 | 太尔胶粘剂(广东)有限公司 | A kind of phenolic foam material and its preparation method and application for polishing |
| CN109401183B (en) * | 2018-10-25 | 2021-12-10 | 太尔胶粘剂(广东)有限公司 | Phenolic foam material for polishing and preparation method and application thereof |
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