KR101786625B1 - Surface-treated magnesium hydroxide, method for preparing the same and flame retarded composition - Google Patents
Surface-treated magnesium hydroxide, method for preparing the same and flame retarded composition Download PDFInfo
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- KR101786625B1 KR101786625B1 KR1020150150191A KR20150150191A KR101786625B1 KR 101786625 B1 KR101786625 B1 KR 101786625B1 KR 1020150150191 A KR1020150150191 A KR 1020150150191A KR 20150150191 A KR20150150191 A KR 20150150191A KR 101786625 B1 KR101786625 B1 KR 101786625B1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
- C09K21/04—Inorganic materials containing phosphorus
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
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- C08K3/0058—
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- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/06—Organic materials
- C09K21/12—Organic materials containing phosphorus
Abstract
The present invention relates to a surface-treated magnesium hydroxide, a process for producing the magnesium hydroxide, and a flame-retardant composition containing the same, wherein the surface-treated magnesium hydroxide is treated with a surface treatment agent containing phosphate substituted with a polyethylene glycol functional group .
The surface-treated magnesium hydroxide is imparted with hydrophobicity on its surface to improve the affinity with the polymer compound, so that the magnesium hydroxide has excellent dispersibility in the polymer compound, and flame retardancy and mechanical properties can be improved.
Description
The present invention relates to a surface-treated magnesium hydroxide, a method for producing the magnesium hydroxide, and a flame-retardant composition containing the magnesium hydroxide. More particularly, the present invention relates to a surface-treated magnesium hydroxide which has improved hydrophilicity on the surface and improved affinity with the polymer compound, And a method for producing the magnesium hydroxide, and a flame retardant composition containing the same, which can improve flame retardancy and mechanical properties.
Most of the flame-retardant polymer materials consist of polymer-free or halogen-free polymers with halogen molecules attached to the polymer structure and an internal hardening material based on organohalogen compounds.
Such a polymer material has excellent flame retardancy and does not deteriorate mechanical properties, but exhibits some disadvantages. They have no self-extinguishing capacity and release harmful and corrosive by-products that are toxic to large amounts of smoke and the environment during the thermal oxidative degradation process.
If magnesium hydroxide powder is used as a sealant in a polymeric material, such technical and environmental (ecological) disadvantages are eliminated. The water chemically bonded by the thermal decomposition of the magnesium hydroxide is liberated, thereby promoting self-extinguishing action and releasing harmless, non-corrosive by-products produced in the magnesium hydroxide during the thermal oxidative decomposition.
The disadvantage of using magnesium hydroxide as a sealant in synthetic resins is that it exhibits sufficient flame resistance only when a large amount of magnesium hydroxide is mixed with the synthetic resin. The amount thereof is in most cases in the range of 40% by weight to 65% by weight in the polymer compound. It is extremely difficult to uniformly mix such a large amount of magnesium hydroxide into the polymer material. This is because the polymer is a nonpolar linear structure composed of a long chain in most cases, while the magnesium hydroxide molecule is very polar and hydrophilic.
Moreover, after mixing such a large amount of magnesium hydroxide into the polymer material, some physical properties of the material, particularly impact strength, ductility and relative elongation, are reduced. The degree of the property deterioration depends on the uniform dispersibility of the magnesium hydroxide in the polymer structure. Water isolated from the magnesium hydroxide has been found to exert self-extinguishing action when the closest location is located, and a sufficiently flammable V-0 grade can be obtained when there is complete dispersion of the magnesium hydroxide. Particularly, the dispersibility has a decisive influence on the mechanical properties of the polymer.
As a method used for bringing about positive results in physical properties in mixing the magnesium hydroxide into the polymer material, there is a method of surface-treating the powdered magnesium hydroxide particles before mixing (JP-A-2002-285162, Japanese Patent Application Laid-Open No. 2001-226676, Japanese Patent Laid-Open No. 2003-253266, Japanese Laid-open Patent Application No. 2003-129056).
The surface treatment of suitable powdered magnesium hydroxide particles satisfies all of the above-mentioned complex requirements such as flame retardance, workability, practical properties, etc., and magnesium oxide of a given amount is mixed with the polymer substance without any problem using a normal mixing machine . A properly selected surface active agent enhances the mutual binding force between the magnesium hydroxide and the polymer, achieves uniform dispersion of the magnesium hydroxide particles in the compound, and improves flame retardancy and mechanical properties.
Japanese Patent No. 60243155, U.S. Patent No. 4,098,762 and U.S. Patent No. 5,143,965 disclose an alkali salt based on higher fatty acids having an aliphatic chain having a carbon number of 8 to 30, or an alkyl sulfate corresponding thereto, an alkyl A surface active agent based on an alkali salt of a sulfonic acid salt, an alkylaryl sulfonic acid salt or a sulfosuccinic acid ester, and the like have been used. In particular, surface active agents such as sodium stearate, sodium or potassium oleate have been used.
The use of alkoxysilanes for the surface treatment of magnesium hydroxide is disclosed in PCT WO 90/13516, but does not disclose specific alkoxysilanes.
Silane coupling agents such as vinylsilane and aminosilane, higher fatty acids such as stearic acid, and the like have been used as surface treatment agents that are commercially available.
However, magnesium hydroxide using these surface treatment agents still does not have sufficient dispersibility in the polymer, so that it is necessary to develop a surface treatment agent having excellent dispersibility in order to improve flame resistance and mechanical properties.
Disclosure of the Invention An object of the present invention is to provide a surface-treated magnesium hydroxide which is excellent in dispersibility into the polymer compound and can improve flame retardancy and mechanical properties as hydrophobicity is imparted to the surface to improve affinity with the polymer compound will be.
Another object of the present invention is to provide a process for producing the surface-treated magnesium hydroxide.
It is another object of the present invention to provide a flame retardant composition comprising the surface-treated magnesium hydroxide.
According to one embodiment of the present invention, there is provided a magnesium hydroxide surface-treated with a surface-treating agent containing phosphate substituted with a polyethylene glycol functional group.
The phosphate containing the polyethylene glycol substituent may be any one selected from the group consisting of a compound represented by the following formula (1), a compound represented by the following formula (2), and a mixture thereof.
[Chemical Formula 1]
(2)
In the general formulas (1) and (2), each R is independently a linear alkyl group having 8 to 30 carbon atoms or a branched alkyl group, and each n is independently an integer of 1 to 10.
The magnesium hydroxide can be surface-treated with the compound represented by Formula 1 and the compound represented by Formula 2.
The weight ratio of the compound represented by Formula 1 to the compound represented by Formula 2 may be 9: 1 to 5: 5.
The surface-treated magnesium hydroxide may contain the surface treating agent in an amount of 0.5 to 10 parts by weight based on 100 parts by weight of the magnesium hydroxide.
According to another embodiment of the present invention, there is provided a process for preparing a surface-treated magnesium hydroxide, which comprises the step of surface-treating magnesium hydroxide with a surface-treating agent containing phosphate substituted with polyethylene glycol functional groups do.
According to another embodiment of the present invention, there is provided a flame retardant composition comprising a polymer resin and the surface-treated magnesium hydroxide.
The surface-treated magnesium hydroxide of the present invention is imparted with hydrophobicity on the surface to improve the affinity with the polymer compound, so that it is excellent in dispersibility into the polymer compound, and flame retardancy and mechanical properties can be improved.
1 is a graph showing the sedimentation rate of surface-treated magnesium hydroxide in paraffin oil measured in Test Example 2 of the present invention.
Hereinafter, the present invention will be described in more detail.
The surface-treated magnesium hydroxide according to an embodiment of the present invention is surface-treated with a surface treating agent containing phosphate substituted with a polyethylene glycol functional group.
The phosphate substituted with the polyethylene glycol functional group can impart hydrophobicity to the magnesium hydroxide to improve the affinity with the polymer compound. As a result, the magnesium hydroxide surface-treated with the surface-treating agent containing a phosphate substituted with the polyethylene glycol functional group has excellent dispersibility in a polymer resin and exhibits improved flame retardancy and mechanical properties.
The polyethylene glycol functional group of the phosphate substituted with the polyethylene glycol functional group is a functional group containing an ethylene oxide repeating unit (-CH 2 CH 2 O-), and the oxygen at one end of the ethylene oxide repeating unit is connected to the phosphorus of the phosphate . The polyethylene glycol functional group may be substituted one or two times in the phosphate. The following formula (1) or (2) specifically exemplifies the case where the polyethylene glycol functional group is substituted by 1 or 2 of the above-mentioned phosphate.
Specifically, the phosphate containing the polyethylene glycol substituent may be any one selected from the group consisting of a compound represented by the following formula (1), a compound represented by the following formula (2), and a mixture thereof.
[Chemical Formula 1]
(2)
In the compound represented by Chemical Formula 1 or the compound represented by Chemical Formula 2, the hydroxyl group (-OH) and the polyethylene glycol substituent of the phosphate serve to bind to the magnesium surface, and the alkyl group imparts hydrophobicity to the magnesium hydroxide .
At this time, the surface treating agent may include the compound represented by Formula 1 and the compound represented by Formula 2 at the same time. In this case, the weight ratio of the compound represented by Formula 1 to the compound represented by Formula 2 may be 9: 1 to 5: 5, and preferably 3: 1 to 2: 1. The compound represented by the formula (1) has a better binding force with the surface of magnesium, and the compound represented by the formula (2) is more excellent in imparting hydrophobicity to the magnesium hydroxide. Therefore, the weight ratio of the compound represented by the formula (1) and the compound represented by the formula (2) can be appropriately selected in consideration of the binding force with the magnesium and the degree of hydrophobicity desired to be imparted to the magnesium hydroxide.
The surface-treated magnesium hydroxide may include the surface treating agent in an amount of 0.5 to 10 parts by weight, preferably 1 to 6 parts by weight, based on 100 parts by weight of the magnesium hydroxide. If the content of the surface treatment agent is less than 0.5 parts by weight, the effect of the present invention can not be sufficiently obtained. If the amount exceeds 10 parts by weight, undesirable effects such as bleeding out may occur.
The surface treatment agent may further include magnesium hydroxide surface treatment agents conventionally used in addition to the phosphate substituted with the polyethylene glycol functional group. Examples of the surface treatment agents of magnesium hydroxide which are commonly used include alkaline salts based on higher fatty acids having 8 to 30 carbon atoms or the corresponding alkylsulfates, alkylsulfonates, alkylarylsulfonates or sulfosuccinates; Alkoxysilanes; The dialcohol amino salt or alcoholate salt of alcohol phosphate ester or its metal salt, especially the diethanol amino salt of diolyl alcohol phosphate ester, the sodium salt of lauryl alcohol phosphate ester, the diethanol amino salt of stearyl alcohol phosphate ester, The sodium salt of alcohol phosphate ester, and the diethanol amino salt of arachyl alcohol phosphate ester; Silane coupling agents such as vinyl silane and aminosilane, higher fatty acids such as stearic acid, phosphoric acid, and the like.
The method for preparing a surface-treated magnesium hydroxide according to another embodiment of the present invention includes a step of surface-treating magnesium hydroxide with a surface-treating agent containing a phosphate substituted with the polyethylene glycol functional group.
As a method for surface-treating the magnesium hydroxide with a surface-treating agent containing a phosphate substituted with the polyethylene glycol functional group, any of the conventional surface treatment methods of magnesium hydroxide can be used. However, the surface of the surface containing the phosphate substituted with the polyethylene glycol functional group Methods such as spraying, wet surface treatment, or treating the surface can be preferably used to uniformly adhere the treating agent to the surface of the magnesium hydroxide particles.
More specifically, a surface treatment agent containing a phosphate substituted with the polyethylene glycol functional group may be added while stirring the magnesium hydroxide using a Henschel mixer or the like.
The flame retardant composition according to another embodiment of the present invention comprises a polymer compound as a base resin and the surface-treated magnesium hydroxide as a sealant.
The phosphate substituted with the polyethylene glycol functional group can impart hydrophobicity to the magnesium hydroxide to improve the affinity with the polymer compound.
Examples of the polymer compound include polyolefin resins such as polyethylene-based and polypropylene-based resins.
In addition, the flame retardant composition may be a solid plastic product manufactured through molding such as extrusion of the composition as well as a state of a fluid composition. For example, the flame retardant composition may be used as a cover for electric wires or the like, and may preferably be a flame retardant resin composition for covering a non-halogen wire.
Hereinafter, embodiments of the present invention will be described in detail so that those skilled in the art can easily carry out the present invention. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
(Preparation Example: Preparation of magnesium hydroxide)
Magnesium chloride (MgCl 2) and the mixed aqueous solution of ethyl sodium (Mg = 1.0 mol / L, acetate soda = 1.5 mol / L, 30 ℃) 40 L to 2 mol / L hydroxide sodium solution (30 ℃) 34 L of And the resultant solution was added with stirring to conduct coprecipitation reaction. The reaction product was hydrothermally treated at 160 ° C for 5 hours in a high-pressure reactor. After cooling to 100 占 폚 or lower, it was taken out from the high-pressure reactor, followed by filtration, washing with water, drying and pulverization to obtain magnesium hydroxide. The obtained magnesium hydroxide had a thickness of 0.09 mu m, a width of 2.2 mu m and an aspect of 24.
(Example 1: Preparation of surface-treated magnesium hydroxide)
6 kg of distilled water was added to 2 kg of magnesium hydroxide prepared in the above Preparation Example, and 60 g of the surface treatment agent dissolved in 1 kg of separately prepared water was added thereto. Stirred for 30 minutes at room temperature, filtered, and dried at 110 to 130 ° C to obtain surface-treated magnesium hydroxide.
Wherein the surface treatment agent is a compound represented by the general formula (1) wherein R is an alkyl chain of C 12 H 15 and n is 3, and the surface-treated magnesium hydroxide has a surface treatment agent containing 3 By weight.
(Example 2: Preparation of surface-treated magnesium hydroxide)
The surface-treated magnesium hydroxide was prepared in the same manner as in Example 1, except that 40 g of the surface treatment agent was used in Example 1. At this time, the surface-treated magnesium hydroxide contained 2 parts by weight of the surface treatment agent relative to 100 parts by weight of the magnesium hydroxide.
(Example 3: Preparation of surface-treated magnesium hydroxide)
The surface-treated magnesium hydroxide was prepared in the same manner as in Example 1, except that 20 g of the surface treatment agent was used in Example 1. At this time, the surface-treated magnesium hydroxide contained the surface treating agent in an amount of 1 part by weight based on 100 parts by weight of the magnesium hydroxide.
(Comparative Example 1)
The surface-treated magnesium hydroxide was prepared in the same manner as in Example 1, except that 40 g of the surface treatment agent containing stearic acid was used instead of the compound represented by the formula (1). At this time, the surface-treated magnesium hydroxide contained 2 parts by weight of the surface treatment agent relative to 100 parts by weight of the magnesium hydroxide.
(Comparative Example 2)
The same procedure as in Example 1 was carried out except that magnesium hydroxide without surface treatment was used.
[Test Example 1: Measurement of flame retardancy and elongation]
50 to 60% by weight of the surface-treated magnesium hydroxide prepared in Examples and Comparative Examples and 40 to 50% by weight of polypropylene (PP, homogeneous polymer, melt flow index specified at 5 g / 10 min at 230 DEG C, 2.16 kg) the PP-Mg (OH) 2 mixture consisting% was extruded by an extruder (Werner & Pfleiderer ZSK 30) standing from 200 to 230 ℃ and pellets. The prepared specimen was manufactured by injecting at an extruder temperature of 230 ° C.
The flame retardancy and elongation of the specimen were measured, and the results are shown in Table 1 below.
Content (parts by weight)
content(%)
content(%)
(LOI)
(%)
1.0
1.0
1.0
2.0
2.0
2.0
3.0
3.0
3.0
2.0
2.0
2.0
1) Flammability (LOI): The oxygen limiting index
Referring to Table 1 above, it can be seen that the surface-treated magnesium hydroxide produced in the examples is superior in flame retardancy to magnesium hydroxide which has been surface-treated with magnesium hydroxide or stearic acid which is prepared in the comparative example. Accordingly, the content of magnesium hydroxide to be added in order to impart sufficient flame retardancy to the PP can be reduced. In addition, since the mechanical properties are lowered as the amount of magnesium hydroxide added increases, it can be seen that the improvement in mechanical properties can be greatly improved by reducing the amount of magnesium hydroxide added.
In addition, the magnesium hydroxide surface-treated with stearic acid prepared in the above Comparative Example exhibited an elongation of less than 20%, while the magnesium hydroxide surface-treated with the compound represented by the formula (1) Which is a significant increase.
[ Test Example 2: Measurement of dispersibility]
In order to measure the dispersibility of the surface-treated magnesium hydroxide prepared in Example 1 in the polymer resin, the surface-treated magnesium hydroxide prepared in Example 1 was dispersed in paraffin oil, And the results are shown in Fig.
Also, for the magnesium hydroxide prepared in Comparative Examples 1 and 2, the sedimentation rate was measured in the same manner as described above, and the results are also shown in FIG.
1, 100% sedimentation occurred within 150 minutes of the surface-untreated magnesium hydroxide, and 100% sedimentation occurred within 220 minutes of magnesium hydroxide surface-treated with stearic acid. On the other hand, In the case of the magnesium hydroxide surface-treated with the surface treatment agent, only about 10% of the sedimentation occurred after 220 minutes, and the sedimentation was not completed even after 24 hours. That is, it can be understood that the magnesium hydroxide surface-treated with the surface-treating agent of the present invention is superior in dispersibility in the polymer compound as compared with magnesium hydroxide surface-treated with stearic acid.
Claims (6)
The phosphate containing the polyethylene glycol substituent is a mixture of a compound represented by the following formula (1) and a compound represented by the following formula (2)
Wherein the weight ratio of the compound represented by Formula 1 to the compound represented by Formula 2 is from 9: 1 to 5: 5.
[Chemical Formula 1]
(2)
(In the formulas (1) and (2)
Each R is independently a linear alkyl group or branched alkyl group having 8 to 30 carbon atoms,
Each n is independently an integer of 3 to 4)
Wherein the surface-treated magnesium hydroxide contains 0.5 to 10 parts by weight of the surface treatment agent per 100 parts by weight of the magnesium hydroxide.
The phosphate containing the polyethylene glycol substituent is a mixture of a compound represented by the following formula (1) and a compound represented by the following formula (2)
Wherein the weight ratio of the compound represented by Formula 1 to the compound represented by Formula 2 is from 9: 1 to 5: 5.
[Chemical Formula 1]
(2)
(In the formulas (1) and (2)
Each R is independently a linear alkyl group or branched alkyl group having 8 to 30 carbon atoms,
Each n is independently an integer of 3 to 4)
The surface-treated magnesium hydroxide according to claim 1
≪ / RTI >
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003253266A (en) | 2002-03-01 | 2003-09-10 | Sakai Chem Ind Co Ltd | Flame-retardant, method for production thereof and flame-retardant resin composition containing the same |
| CN101284921A (en) | 2007-04-11 | 2008-10-15 | 广州市啊啦棒建材有限公司 | Superfine magnesium hydrate polyethylene fire retardant composite material and preparation process thereof |
| JP2009114016A (en) * | 2007-11-06 | 2009-05-28 | Shiraishi Calcium Kaisha Ltd | Magnesium hydroxide flame retarder, its manufacturing method, and flame retardant composition |
| JP2009249389A (en) | 2008-04-01 | 2009-10-29 | Shiraishi Calcium Kaisha Ltd | Magnesium hydroxide flame retardant and flame-retardant polymer composition |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003253266A (en) | 2002-03-01 | 2003-09-10 | Sakai Chem Ind Co Ltd | Flame-retardant, method for production thereof and flame-retardant resin composition containing the same |
| CN101284921A (en) | 2007-04-11 | 2008-10-15 | 广州市啊啦棒建材有限公司 | Superfine magnesium hydrate polyethylene fire retardant composite material and preparation process thereof |
| JP2009114016A (en) * | 2007-11-06 | 2009-05-28 | Shiraishi Calcium Kaisha Ltd | Magnesium hydroxide flame retarder, its manufacturing method, and flame retardant composition |
| JP2009249389A (en) | 2008-04-01 | 2009-10-29 | Shiraishi Calcium Kaisha Ltd | Magnesium hydroxide flame retardant and flame-retardant polymer composition |
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