KR20060070621A - Method of preparing initiator for producing artificial marble, initiator composition for producing artificial marble and artificial marble composition comprising same - Google Patents

Abstract

The present invention relates to a method for producing an initiator for preparing artificial marble, an initiator composition for preparing artificial marble, and an artificial marble composition comprising the same, wherein the method for preparing the initiator is prepared by mixing tertiary butyl hydroperoxide with a first solvent. Removing moisture from the peroxide; It provides a method for producing an initiator for preparing artificial marble comprising the step of reacting the water-removed tertiary butyl hydroperoxide and maleic anhydride in a second solvent at a low temperature.

The initiator for artificial marble according to the present invention can be used as an initiator for acrylic monomers, unsaturated acid monomers, acrylic resins, unsaturated resins, and the like. In addition, the initiator of the present invention exhibits excellent transparency after initiation and curing when used in acrylic artificial marble which is excellent in resin transparency and curing transparency, excellent in productivity and workability, and easy to mold, and particularly requires high transparency and room temperature curing. Excellent curing property can be exhibited during curing. In addition, there is no defect in the appearance at the time of fast workability and rapid demolding by maintaining excellent room temperature curability, and has the property that curing at room temperature is quickly and completely hardened to facilitate release.

Artificial Marble, Acrylic, Initiator, Active Oxygen

Description

TECHNICAL OF PREPARING INITIATOR FOR PRODUCING ARTIFICIAL MARBLE, INITIATOR COMPOSITION FOR PRODUCING ARTIFICIAL MARBLE AND ARTIFICIAL MARBLE COMPOSITION COMPRISING SAME}

[Industrial use]

The present invention relates to a method for producing an initiator for preparing artificial marble, an initiator composition for preparing artificial marble, and an artificial marble composition comprising the same, and more particularly, a method for preparing an initiator for manufacturing artificial marble, which is easy to handle and has high productivity, and an initiator for preparing artificial marble. A composition and an artificial marble composition comprising the same.

[Prior art]

Recently, high quality artificial marble, which is widely used as building interior materials, is classified into two types, acrylic and unsaturated polyester, depending on the base resin used. Among them, acrylic type has been continuously increasing in demand for various applications recently due to the transparent and luxurious texture, balanced mechanical properties and excellent weather resistance due to the characteristics of the resin itself. For example, the tops of various counter tops such as sink tops, vanity tops, reception desks of banks and securities stores, interior wall materials of merchandise stores, partitions, bathtubs, sink bowls, washbasins and interior sculptures. It is widely used around the world.

Unlike unsaturated polyester resins, acrylic resins have a very high polymerization shrinkage during molding, and defects due to shrinkage such as think marks tend to appear on the appearance of the final molded product, and release and demolding becomes difficult when molding at high temperatures to increase productivity. There are disadvantages. In addition, in order to obtain transparency, which is a characteristic of acrylic artificial marble, yellowing does not occur during curing and there should be no deformation. In particular, the use of an initiator is required to enable rapid curing at room temperature in order to improve productivity.

As a conventional initiator, benzoic peroxide, azobisisobutyronitrile, methyl ethyl ketone peroxide, tert-butylpere used in many unsaturated polyester resins BMC (bulk molding compound), SMC (sheet molding compound) and acrylic artificial marble Initial curing was carried out using the same amount by weight of oxybenzoylate, di-tert-benzoyl peroxide, benzoyl peroxide, tertiary butyl peroxy maleate and the like.

Tertiary butyl peroxy maleate is mainly used among the above-mentioned initiators, but all conventional initiators including the same have problems of not completely curing at room temperature or progressing remarkably slowly when used in acrylic artificial marble. Therefore, there was a problem that a yellowed surface is made during the manufacture of white artificial marble.

 The present invention has been made to solve the above problems, and an object of the present invention is to provide a method for producing an initiator for preparing artificial marble excellent in storage safety, workability and ease of handling.

Another object of the present invention is to provide an initiator composition for preparing artificial marble comprising an initiator prepared by the above method.

Another object of the present invention is to provide an artificial marble composition comprising the initiator composition prepared by the above-described method.

In order to achieve the above object, the present invention is to remove the moisture from the tertiary butyl hydro peroxide by mixing tertiary butyl hydro peroxide with an aromatic and aliphatic solvent; It provides a method for producing an initiator for preparing artificial marble comprising the step of reacting the water-removed tertiary butyl hydroperoxide and maleic anhydride in a solvent at a low temperature.

The present invention provides tertiary butyl peroxy maleate powder having an average particle diameter of 1000 microns to 0.0001 microns; Plasticizers; And it provides an initiator composition for preparing artificial marble comprising a filler.

The present invention also 100 parts by weight of a thermosetting resin containing a double bond; And it provides an artificial marble composition comprising 0.1 to 10 parts by weight of the initiator composition with respect to 100 parts by weight of the thermosetting resin.

Hereinafter, the present invention will be described in more detail.

The present invention relates to a method for preparing an initiator capable of initiating and curing a double bond of an acrylic resin or a monomer thereof, or an unsaturated resin or a monomer thereof, that is, a thermosetting resin, and an initiator composition comprising the same. The initiator composition of the present invention is excellent in storage safety, workability, and ease of handling, and initiates a curing reaction of an acrylic resin, and can be particularly useful in manufacturing artificial marble. In addition, the initiator composition of the present invention promotes the curing reaction so that the curing reaction of the acrylic resin occurs completely and quickly, and also enables the production of a cured cured product, especially artificial marble having a unique white color without change over time.

The initiator preparation method of the present invention first removes moisture from tertiary butyl peroxy peroxide. This water removal process is the first solvent which has affinity with tertiary butyl peroxy peroxide and is separated from H ₂ O, for example benzene, toluene, hexane, xylene, cocosol (trade name, SK Chemicals, mixed aromatic solvents). ), Heptane, octane, butyl acetate, cellosolve acetate and the like can be used.

The water removal process is described in more detail, and comprises tertiary butyl hydroperoxide and a solvent in a weight ratio of 1 to 100: 1 to 100 by weight. At this time, the mixing temperature is carried out at -20 to 30 ℃, the mixing rate is preferably 500 to 2000rpm. After completing the mixing process, the water is separated by standing for 5 minutes to 10 hours. Subsequently, in order to further remove traces and small amounts of water, a step of adding and stirring a dehydrating agent such as anhydrous magnesium sulfite and anhydrous sodium sulfite may be further performed. The amount of the dehydrating agent may be used about 0.1 to 30 parts by weight based on 100 parts by weight of the total mixture, but is not limited thereto. If a dehydrating agent is used, a filtration process is carried out to remove the dehydrating agent to obtain the water-removed tertiary butyl hydroperoxide and solvent mixture.

Maleic anhydride and a second solvent are added to the obtained tertiary butyl hydroperoxide and the first solvent mixture, followed by mixing. At this time, the mixing process is preferably performed for 1 minute to 20 hours at -20 to 30 ℃. When the mixing step is carried out at a high temperature higher than 30 ° C, the tertiary butyl hydroperoxide may decompose and explode, and the yield is low, which is not preferable. Moreover, when it carries out below -20 degreeC, reaction time becomes remarkably slow and reaction is not made or it becomes too late, and it is unpreferable. The reaction time is not particularly limited, but if it is carried out for a long time, the productivity is lowered, so it is preferable to carry out during this time.

The mixing ratio of the tertiary butyl hydroperoxide and maleic anhydride is preferably 1 to 100: 1 to 100 by weight. If it is out of this mixing ratio, since a yield falls, it is not preferable.

Representative examples of such solvents include aromatic organic solvents such as benzene, toluene or xylene, naphthene and aliphatic organic solvents such as hexane, heptane, octane or tetrahydrofuran, butyl acetate, ethyl cellulose or butyl cellulose; The same ketone ester and ether type organic solvent can be used.

This process forms the desired product, tertiary butyl peroxy maleate. Then, to increase the purity of tertiary butyl peroxy maleate, a general purification process may be further carried out. The purification process may be performed several times to wash and filter the unreacted substance by adding 100 to 1000 parts by weight of water to 100 parts by weight of the obtained tertiary butyl peroxy maleate, and then, the filtered product is 25 to 100 The drying step for 48 hours may be further carried out. At this time, the active oxygen content of the tertiary butyl peroxy maleate after complete drying is 8.51 ± 0.01.

It is also possible to further use additives such as surfactants and catalysts in the mixing process. The surfactant may include lauric acid, linear alkyl benzene sulfonic acid, alpha olefin sulfonate, sodium laurylether sulfate, sodium lauryl sulfate, sodium lauryl sulfate, and sodium lauryl sulfate. Lauryl Sulfate, Ammonium Laurylether Sulfate, Ammonium Lauryl Sulfate, Triethanolamine Lauryl Sulfate, Sodium Cocoyl Iethionate Anionic surfactants such as sodium lauryl sarcosinate can also be used. Or oleic acid, Triethanolamine Esterquaternary, Imidazoline Quarternary, Cetyl Trimethyl Ammonium Chloride, or Lauryl Trimethyl Ammonium Methyl Sulfate Cationic surfactants such as Coconut Diethanol Amide, Coconut Monoethanol Amide, Lauryl Diethanol Amide, Ethylene Glycol MonoStearate Nonionic surfactants such as ethylene glycol distearate, polyvinyl alcohol, and the like may be used.

The amount of the surfactant used is preferably 10 to 2000 parts by weight. If the amount of the surfactant is out of the above range, the yield and purity are low, which is not preferable.

Phosphoric acid, sulfuric acid, nitric acid, zirconium, sodium or zinc may be used as the catalyst, and the amount thereof is preferably 10 to 2000 parts by weight. When the amount of the catalyst used is outside the above range, the yield and purity are lowered, which is not preferable.

Subsequently, the tertiary butyl peroxy maleate prepared in the above process may be ground to prepare a powder having an average particle diameter of 1000 microns to 0.0001 microns, preferably 0.5 microns to 0.0001 microns. Thus, when tertiary butyl peroxy maleate powder which carries out a grinding | pulverization process and an average particle diameter which falls in the range mentioned above is used, it is preferable because it shows the effect more excellent when used as an initiator and a hardening | curing agent composition.

If the average particle diameter of the tertiary butyl peroxy malate powder is smaller than 0.001 micron, it can decompose upon long-term storage, and if it is larger than 1000 micron, the surface area is relatively small, so that the decomposition time is considerable. This is not desirable late.

The amount of active oxygen of the tertiary butyl peroxy maleate prepared by the above process is 8.43 ± 0.001 to 8.51 ± 0.001 (that is, 8.429 to 8.511) when the purity is 99 to 100%, and the amount of active oxygen varies depending on the purity. When the purity is 70%, about 5.5 is shown.

The tertiary butyl peroxy malate prepared in the above process may be applied to the artificial marble manufacturing process as a solid, but in order to control the convenience of use, reaction rate, etc., it is more preferable to prepare and use it as a composition. .

The initiator composition for preparing artificial marble of the present invention comprises tertiary butyl peroxy malate powder, plasticizer and filler having an average particle diameter of 1000 microns to 0.0001 microns, preferably 0.5 microns to 0.0001 microns. At this time, the mixing ratio of the tertiary butyl peroxy maleate powder, the plasticizer and the filler is preferably 1 to 100: 10 to 1000: 0.01 to 50 parts by weight.

The plasticizer may include dioxy phthalate, dioctyl adipate, diisodecyl phthalate, dioctyl adipate, dina (diisononyl adipate), trioctyl triisononyl trimellitate, triisononyl triellitate Mellitate, dioctyl maleate, citric acid ester (Citrocizer, Aekyung Petrochemical), adipic acid polyester (trade name: Nonpcizer, Aekyung Petrochemical), adipic acid ester system ( Trade name: Olicizerr), 2,2,4-trimethyl-1,3-pentanediol diisobutyrate, trimethylphthalate plasticizer (Lgflex BET), neopentyl glycol plasticizer (Lgflex EBN) or liquid paraffin wax Any plasticizer or silicone oil, paraffin wax available can be used.

The filler serves to increase the layer separation prevention and dispersion effect, and the filler may be used zinc oxide, zinc stearic acid, ammonium zinc carbonate, ammonium zinc chloride, zinc acetic acid, silica and extender pigments.

In addition, as the heat stabilizer, methylenephosphonic acid (methylenephosphonic acid) or melamine cyanurate may be further used. The amount of the heat stabilizer may be used in an amount of 0.01 to 1 part by weight based on 100 parts by weight of the total initiator composition.

When the initiator composition of the present invention is used in the artificial marble composition, the curing speed is fast, there is no change over time after curing, and it is possible to prepare an excellent acrylic artificial marble while maintaining a beautiful and transparent bright color unique to acrylic.

The initiator composition of the present invention having such a configuration can be obtained by mixing tertiary butyl peroxy malate powder, plasticizer and filler, and the mixing process is performed for 1 minute to 10 hours at a speed of 1500 to 2000 rpm.

The temperature condition of 30 to -20 ℃ preferred, and the atmosphere is preferably carried out in N ₂ atmosphere. If the mixing process is carried out in the conditions outside the above conditions there is a risk of decomposition and fire is not preferable, and when mixing at a temperature below -20 ℃ is not preferable because the mixing does not occur smoothly.

The artificial marble composition comprising the initiator composition of the present invention comprises 100 parts by weight of a thermosetting resin including a double bond and 0.1 to 10 parts by weight of the initiator composition of the present invention with respect to 100 parts by weight of the thermosetting resin. When the content of the initiator composition is out of the range, it may not be preferable because it may affect the hardness and chemical resistance of the artificial marble properties, and even if an excess of 10 parts by weight is used, the use of more excess is not possible. It is not economically desirable.

As the thermosetting resin, an acrylic resin is typical, but in addition to the acrylic resin, thermosetting resins, monomers, and the like which can be used in the manufacture of artificial marble may be used. As the acrylic resin, methyl methacrylate, butyl methacrylate, methyl acrylate, styrene monomer or 2-hydroxyethyl methacrylate may be used.

In addition, additives generally used to prepare artificial marble, such as polymethyl methacrylate and aluminum hydroxide, may be further used.

Hereinafter, preferred examples and comparative examples of the present invention are described. However, the following examples are only one preferred embodiment of the present invention and the present invention is not limited to the following examples.

(Comparative Example 1)

100 parts by weight of maleic anhydride, 145 parts by weight of tertiary butyl hydroperoxide, 5 parts by weight of oleic acid surfactant and 30 parts by weight of 85% phosphoric acid were sequentially introduced into a reactor at 0 ° C., and then 1200 rpm. The reaction was slowly carried out for 9 hours while stirring at a rate and vacuum filtered to prepare tertiary butyl peroxy malate. The amount of active oxygen of the prepared tertiary butyl peroxy maleate was measured.

(Comparative Example 2)

100 parts by weight of maleic anhydride, 145 parts by weight of tertiary butyl hydroperoxide, 200 parts by weight of benzene nonpolar solvent, 5 parts by weight of oleic acid surfactant and 30 parts by weight of 85% phosphoric acid to a reactor at 0 ° C. with respect to 100 parts by weight of maleic anhydride. After sequentially being added, the reaction was slowly carried out for 9 hours while stirring at 1200 rpm, and vacuum filtered to prepare tertiary butyl peroxy maleate. The amount of active oxygen of the prepared tertiary butyl peroxy maleate was measured.

(Comparative Example 3)

100 parts by weight of maleic anhydride, 145 parts by weight of tertiary butyl hydroperoxide, 200 parts by weight of benzene nonpolar solvent, 5 parts by weight of oleic acid surfactant and 30 parts by weight of 85% phosphoric acid to a reactor at 0 ° C. with respect to 100 parts by weight of maleic anhydride. After the addition in turn, the reaction was slowly reacted for 9 hours while stirring at 1200 rpm and vacuum filtered. The filtration product was then completely dried at 40 ° C. for 72 hours to prepare tertiary butyl peroxy maleate. The amount of active oxygen of the prepared tertiary butyl peroxy maleate was measured.

(Comparative Example 4)

100 parts by weight of a benzene aromatic solvent and 145 parts by weight of tertiary butyl hydroperoxide based on 100 parts by weight of the aromatic solvent were added to a reactor at 0 ° C., stirred at a speed of 1000 rpm for 30 minutes, and left standing for 180 minutes Water was removed from the hydroperoxide. Subsequently, 100 parts by weight of maleic anhydride, 5 parts by weight of oleic acid surfactant and 30 parts by weight of 85% phosphoric acid catalyst were sequentially added to the reactor at 0 ° C., followed by stirring at 1200 rpm, 9 parts by weight of maleic anhydride and 100 parts by weight of maleic anhydride. The reaction was slowly reacted for hours and vacuum filtered. The filtration product was then completely dried at 40 ° C. for 72 hours to prepare tertiary butyl peroxy maleate. The amount of active oxygen of the prepared tertiary butyl peroxy maleate was measured.

(Comparative Example 5)

100 parts by weight of a benzene aromatic solvent and 145 parts by weight of tertiary butyl hydroperoxide based on 100 parts by weight of the aromatic solvent were added to a reactor at 0 ° C., stirred at a speed of 1000 rpm for 30 minutes, and left standing for 180 minutes Water was removed from the hydroperoxide. Subsequently, 100 parts by weight of maleic anhydride, 5 parts by weight of oleic acid surfactant and 30 parts by weight of 85% phosphoric acid catalyst were sequentially added to the reactor at 0 ° C., followed by stirring at 1200 rpm, 9 parts by weight of maleic anhydride and 100 parts by weight of maleic anhydride. The reaction was slowly reacted for hours and vacuum filtered. Subsequently, the filtered product was reinserted into the reactor, washed with 60 minutes by adding 400 parts by weight of distilled water, and completely dried at 40 ° C. for 72 hours to prepare tertiary butyl peroxy malate. The amount of active oxygen of the prepared tertiary butyl peroxy maleate was measured.

(Example 1)

100 parts by weight of a benzene aromatic solvent and 145 parts by weight of tertiary butyl hydroperoxide based on 100 parts by weight of the aromatic solvent were added to a reactor at 0 ° C., stirred at a speed of 1000 rpm for 30 minutes, and left standing for 180 minutes Water was removed from the hydroperoxide. Subsequently, 100 parts by weight of maleic anhydride, 50 parts by weight of tetrahydrofuran nonpolar solvent, 5 parts by weight of oleic acid surfactant, and 30 parts by weight of 85% phosphoric acid catalyst were sequentially added to the reactor at 0 ° C. in the reactor. Then, the mixture was slowly reacted for 9 hours with stirring at 1200 rpm and filtered under vacuum. Subsequently, the filtered product was reinserted into the reactor, washed with 60 minutes by adding 400 parts by weight of distilled water, and completely dried at 40 ° C. for 72 hours to prepare tertiary butyl peroxy malate. The amount of active oxygen of the prepared tertiary butyl peroxy maleate was measured.

(Example 2)

100 parts by weight of a benzene aromatic solvent and 145 parts by weight of tertiary butyl hydroperoxide based on 100 parts by weight of the aromatic solvent were added to a reactor at 0 ° C., stirred at a speed of 1000 rpm for 30 minutes, and left standing for 180 minutes Water was removed from the hydroperoxide. Subsequently, 100 parts by weight of maleic anhydride, 50 parts by weight of tetrahydrofuran nonpolar solvent, 5 parts by weight of oleic acid surfactant, and 30 parts by weight of 85% phosphoric acid catalyst were sequentially added to the reactor at 0 ° C. in the reactor. Then, the mixture was slowly reacted for 9 hours with stirring at 1200 rpm and filtered under vacuum. Subsequently, the filtrate product was re-injected into the reactor, and 400 parts by weight of distilled water was added thereto, followed by washing twice for 60 minutes, followed by complete drying at 40 ° C. for 72 hours to prepare tertiary butyl peroxy malate. The amount of active oxygen of the prepared tertiary butyl peroxy maleate was measured.

(Example 3)

100 parts by weight of a benzene aromatic solvent and 145 parts by weight of tertiary butyl hydroperoxide based on 100 parts by weight of the aromatic solvent were charged to a reactor at 0 ° C., stirred at a speed of 1000 rpm for 30 minutes, and allowed to stand for 180 minutes to provide tertiary butyl Water was removed from the hydroperoxide. Subsequently, 100 parts by weight of maleic anhydride, 50 parts by weight of tetrahydrofuran nonpolar solvent, 5 parts by weight of oleic acid surfactant and 10 parts by weight of phosphoric acid (85%) catalyst were added to the reactor at 0 ° C. in the reactor. After the addition, the mixture was slowly reacted for 9 hours while stirring at 1200 rpm, followed by vacuum filtration. Subsequently, the filtrate product was re-introduced into the reactor, 400 parts by weight of distilled water was added and washed three times, followed by complete drying at 40 ° C. for 72 hours to prepare tertiary butyl peroxy malate. The amount of active oxygen of the prepared tertiary butyl peroxy maleate was measured.

(Example 4)

100 parts by weight of a benzene aromatic solvent and 145 parts by weight of tertiary butyl hydroperoxide based on 100 parts by weight of the aromatic solvent were added to a reactor at 0 ° C., stirred at a speed of 1000 rpm for 30 minutes, and left standing for 180 minutes Water was removed from the hydroperoxide. Subsequently, 20 parts by weight of anhydrous magnesium sulfite was added to the reactor to completely remove traces and small amounts of water, and filtered to prepare anhydrous magnesium sulfite.

Subsequently, 100 parts by weight of maleic anhydride, 50 parts by weight of tetrahydrofuran nonpolar solvent, 5 parts by weight of olenic acid surfactant, and 30 parts by weight of phosphoric acid (85%) catalyst were added to the reactor at 0 ° C. After the addition in turn, the reaction was slowly reacted for 9 hours while stirring at 1200 rpm and vacuum filtered. Subsequently, the filtrate product was re-introduced into the reactor, 400 parts by weight of distilled water was added and washed three times, followed by complete drying at 40 ° C. for 72 hours to prepare tertiary butyl peroxy malate. The amount of active oxygen of the prepared tertiary butyl peroxy maleate was measured.

The active oxygen content of the tertiary butyl peroxy maleate prepared by the method of Examples 1 to 4 and Comparative Examples 1 to 5 is shown in Table 1 below.

Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Example 1 Example 2 Example 3 Example 4 Free radicals 2.58 2.72 3.51 4.25 5.11 5.96 6.13 6.13 8.509 water 30 32 46 50 60 70 72 72 99.99 Exterior Yellow paste Yellow paste Yellow paste Yellow powder Yellow powder White powder White powder White powder White powder

As shown in Table 1, the purity of the tertiary butyl peroxy maleate of Examples 1 to 4 prepared according to the manufacturing process of the present invention is very high compared to the material prepared according to the processes of Comparative Examples 1 to 5, In addition, it is excellent in color, and it can be seen that the amount of active oxygen also shows high purity active oxygen.

(Comparative Example 6)

The dioctylphthalate plasticizer and the tertiary butyl peroxy maleate prepared in Example 4 were added to a 75:25 weight ratio in a 0 ° C blender capable of high-speed stirring, and an initiator paste was prepared by high speed mixing for 5 hours.

Artificial marble composition by mixing 30% by weight of methyl methacrylate, 50% by weight of polymethyl methacrylate and 20% by weight of aluminum hydroxide with 1 part by weight of the initiator paste prepared in the above process with respect to 100 parts by weight of the polymethylmethacrylate. Was prepared.

(Comparative Example 7)

Dioctylphthalate plasticizer, tertiary butyl peroxy maleate prepared in Example 4, zinc stearic acid filler, methylenephosphonic acid heat stabilizer, melamine cyanurate heat stabilizer were added to a 0 ° C. blender capable of high speed stirring. An initiator paste was prepared by adding a 0.1: 0.1 weight ratio and mixing at high speed for 5 hours.

Artificial marble composition by mixing 30% by weight of methyl methacrylate, 50% by weight of polymethyl methacrylate and 20% by weight of aluminum hydroxide with 1 part by weight of the initiator paste prepared in the above process with respect to 100 parts by weight of the polymethylmethacrylate. Was prepared.

(Example 5)

Firstly, the tertiary butyl peroxy maleate prepared in Example 4 was completely ground using a rotary mill so as to have an average particle diameter of 1000 microns or less. Subsequently, a 0 ° C. blender capable of high speed stirring was used to prepare a dioctylphthalate plasticizer, pulverized tertiary butyl peroxy maleate, zinc stearic acid filler, methylenephosphonic acid thermal stabilizer, melamine cyanurate thermal stabilizer and 66.9: 25: 8: 0.1. The mixture was mixed at a weight ratio of 0.1 by weight, and the mixture was mixed at high speed for 5 hours to prepare an initiator paste.

Artificial marble composition by mixing 30% by weight of methyl methacrylate, 50% by weight of polymethyl methacrylate and 20% by weight of aluminum hydroxide with 1 part by weight of the initiator paste prepared in the above process with respect to 100 parts by weight of the polymethylmethacrylate. Was prepared.

The sedimentability, 25 ° C. shelf life and appearance of the initiator pastes of Comparative Examples 6 to 7 and Example 5 were measured, and the results are shown in Table 2 below.

Item division Comparative Example 6 Comparative Example 7 Example 5 Remarks Sedimentation Layered oil Layered oil Layered Radish Plasticizer and Delamination 25 ℃ shelf life radish radish radish Purity, free radical reduction, no Exterior White paste White paste White paste

As shown in Table 2, it can be seen that the initiator composition prepared according to the manufacturing process of Example 5, which is the initiator composition manufacturing process of the present invention, has no sedimentation property, excellent storage property at 25 ° C, and good intrinsic appearance.

The initiator for artificial marble according to the present invention can be used as an initiator for acrylic monomers, unsaturated acid monomers, acrylic resins, unsaturated resins, and the like. In addition, the initiator of the present invention exhibits excellent transparency after initiation curing when used in acrylic artificial marble which is excellent in resin transparency, curing transparency, excellent productivity and workability, and is easy to mold, and particularly requires high transparency and room temperature curing. Excellent curing at room temperature can be exhibited. In addition, there is no defect in the appearance at the time of fast workability and rapid demolding by maintaining excellent room temperature curability, and has the property that curing at room temperature is quickly and completely hardened to facilitate release.

Claims (16)

Mixing tertiary butyl hydroperoxide with a first solvent to remove moisture from the tertiary butyl hydroperoxide; Reacting the water-removed tertiary butyl hydroperoxide and maleic anhydride in a second solvent at a low temperature The manufacturing method of the initiator for manufacturing artificial marble containing the process. The method for producing an initiator for producing artificial marble according to claim 1, further comprising adding a dehydrating agent to the mixture obtained after mixing the tertiary butyl hydroperoxide and the first solvent. The method of claim 1, wherein the first solvent is selected from the group consisting of benzene, toluene, hexane, xylene, cocosol, heptane, octane, butyl acetate, and cellosolve acetate. The method of claim 1, wherein the mixing ratio of the tertiary butyl hydroperoxide and the first solvent is 1 to 100: 1 to 100 by weight. The method of claim 1, wherein the water removal step is carried out at -20 to 30 ℃. The method of claim 1, wherein the second solvent is an aromatic organic solvent selected from the group consisting of benzene, toluene and xylene, naphthalene and aliphatic organic solvent selected from the group consisting of hexane, heptane, octane and tetrahydrofuran, and Method of producing an initiator for preparing artificial marble, which is selected from the group consisting of ketone esters and ether-based solvents selected from the group consisting of butyl acetate, ethyl cellulose and butyl cellulose. The method of claim 1, wherein the mixing ratio of tertiary butyl hydroperoxide and maleic anhydride is in a weight ratio of 10 to 100: 1 to 100. The method of claim 1, wherein the reaction step is carried out at a temperature of 30 to -20 ℃. The method of claim 1, wherein the tertiary butyl peroxy maleate is ground to further prepare a powder having an average particle diameter of 1000 microns to 0.0001 microns. 10. The method of claim 9, wherein the average particle diameter of the tertiary butyl peroxy malate powder is 0.5 micron to 0.0001 micron. Tertiary butyl peroxy maleate powder having an active oxygen amount of 8.429 to 8.511 when the purity is 90 to 100%; Plasticizers; And Filler Initiator composition for producing artificial marble comprising. The initiator composition of claim 11, wherein the average particle diameter of the tertiary butyl peroxy maleate powder is 1000 microns to 0.0001 microns. The initiator composition of claim 12, wherein the tertiary butyl peroxy maleate powder has an average particle diameter of 0.5 micron to 0.0001 micron. The initiator composition of claim 11, wherein the mixing step is performed by stirring at 30 to -20 ° C for 0.5 to 10 hours at a speed of 1500 to 2500 rpm. 100 parts by weight of a thermosetting resin including a double bond; And Tertiary butyl peroxy malate powder having an average particle diameter of 1000 microns to 0.0001 microns with respect to 100 parts by weight of the thermosetting resin; And 0.1 to 10 parts by weight of an initiator composition comprising a filler Artificial marble composition comprising a. Mixing tertiary butyl hydroperoxide with a first solvent to remove moisture from the tertiary butyl hydroperoxide; Preparing the initiator by reacting the water-removed tertiary butyl hydroperoxide and maleic anhydride in a second solvent at a low temperature; Mixing the initiator and the thermosetting resin A method for producing an artificial marble composition comprising a step.