Novel monomer and polymer materials

FIELD: chemistry.

SUBSTANCE: method of producing hybrid organic-inorganic material comprises the following steps: (a) peptisation of material of inorganic particles selected from oxides, sulphides, sulphates, phosphates, arsenides and arsenates of noble metals and mixtures thereof, in anhydrous sulphuric acid or hydrogen fluoride, to obtain a solution of material of inorganic particles; (b) fractionation of the solution obtained at step (a) to obtain a solution of inorganic particles having particle size ranging from 5 nm to 100 nm; (c) mixing the fractionated solution obtained at step (b) with an organic solvent; (d) reacting the mixture from step (c) with a solution of a reactive organic monomer with silane functional groups in an organic solvent.

EFFECT: method of obtaining hybrid organic-inorganic monomer material enables to obtain monomer materials which combine desired products of material of inorganic particles and an organic monomer, in addition to unique nanoparticle properties.

15 cl

 

The level of technology

1. The scope of the invention

The present invention relates to new Monomeric materials and polymeric materials containing the new Monomeric materials.

2. Description of the prior art

Known composite materials containing inorganic particles and a polymer resin. In particular, the so-called "hybrid organic-inorganic nanocomposites are in active research. Receiving involves attaching organic fragments to the surface of the inorganic nanoparticles. This can be done either by grafting organic fragments to pre-formed nanoparticles (what is referred to as postsinteticescuu modification), or the introduction of organic fragment during the synthesis of nanoparticles (modification in situ).

Niederberger (Niederberger) and others, Chem. Mater. 2004, 16, 1202-1208, describes the modification of in situ surface of particles of titanium dioxide. This method comprises adding titanium tetrachloride to a mixture of benzyl alcohol and dopamine or 4-tert-butylcatechol. Functionalized particles soluble in various solvents and suitable for convenient measurement of physical properties, such as width of the energy gap.

Tahir (Tahir) and others, Angew. Chem. Int. Ed. 2006, 45, 908-912, reveals active polymeric ester that can be used in the IAOD to as in situ, and postsinteticescuu functionalization. For functionalization of nanocrystals of titanium dioxide in situ, TiCl4was introduced into the solution of polymer ligand in benzyl alcohol. This solution was stirred for two days at 80°C in argon atmosphere. Postfunctionalist was performed by sealing a mixture of nanowires of TiO2and 10 ml of polymer ligand in benzyl alcohol.

Lee and others, Chem. Mater. 2001, 13, 1137-1142 reveal the hybrid material of the optical thin film containing PMMA (polymethylmethacrylate) with integral realconsolemode groups - titanium dioxide. This material has a high refractive index. The material was obtained by polymerization of methyl methacrylate (MMA) and 3-(trimethoxysilyl)prophylatically (MSMA) in the presence of benzoyl peroxide (BPO) as an initiator. After two hours of polymerization at 60°C was added dropwise a homogeneous solution in tetrahydrofuran (THF) deionized water and Ti(OBu)4. The mixture was reacted for a further 2 hours at 60°C.

The materials of the previous technologies are either surface modified inorganic nanoparticles or dispersion of inorganic nanoparticles in the organic resin.

The present invention is to provide Monomeric materials containing inorganic nanoparticles having kovalan is but associated with their surface, at least one ethylene-unsaturated organic fragment.

Another objective of this invention is to provide homopolymers of new monomers of the present invention.

Another objective of the present invention is to provide heteropolymer containing as a first monomer, a monomer of the present invention, and as the second organic monomer monomer.

Another object of the present invention is to provide a method of obtaining a hybrid monomers according to the present invention.

Summary of invention

In the first embodiment, this invention relates to hybrid organic-inorganic Monomeric material containing inorganic nanoparticles with covalently bound to their surface, at least one polymerized fragment, preferably, the ethylene-unsaturated organic fragment.

In the second embodiment, this invention relates to polymeric material containing hybrid organic-inorganic material of the first variant implementation of the invention. This polymeric material can be homopolymers hybrid Monomeric material or it may be heteropolymers hybrid monomer and the usual PR is ancescao monomer.

In the third embodiment, this invention relates to a method for producing a hybrid organic-inorganic Monomeric material containing stages:

a) peptization of inorganic material particles in an inorganic acid to obtain a solution of an inorganic material particle;

b) fractionating the solution obtained in stage a)to a slurry of inorganic particles having a size range of particles from 5 nm to 100 nm;

C) mixing the fractionated solution obtained in stage b)with an organic solvent S1;

g) the reaction mixture from stage b) with a solution in an organic solvent S2 reactive organic monomer with wilanowie functional groups.

Not everyone inorganic material suitable for the formation of nanosized particles or suitable for use in the present invention. Examples of suitable compounds include the oxides, sulfides, sulfates, phosphates, arsenides, arsenate base metals, which can be covalently functionalized on the surface of the particles of the reactive fragment.

Inorganic particles may be amorphous or they can be crystalline. In many cases, crystalline materials are preferred because these materials have a more pronounced physical is the cue properties than amorphous materials.

It was found that the materials according to the invention is particularly suitable for the production of polymer resins having excellent optical properties with regard to transparency and refractive index. In this context, preferred inorganic materials are those which have a high refractive index, i.e. the index of refraction at least to 1.6, preferably at least 2. Suitable examples include titanium dioxide, zinc oxide, zinc sulfide, lead sulfide, and the like. In this context, the titanium oxide is a preferred material, in particular crystalline form of anatase and rutile.

The term "refractive index" or "PP", as used here, refers to the refractive index of the material at the wavelength of light emitted by a sodium (589 nm).

In the monomers of the present invention, a conventional organic monomers bind to the surface of inorganic particles through covalent bond. Preferably, this covalent bond is a bond of the silicon atom with the surface of inorganic particles. This link is generated by the interaction of inorganic particles with reactive celanova functional monomer. Preferred are monomers having ethylene-unsaturated goinoutwest.

The reaction of the inorganic particles with reactive celanova functional monomer can be carried out by reacting a reactive silane functional monomer with pre-formed inorganic particle (potentes) or by creating inorganic particles in the presence of a reactive silane functional monomer (in situ). The reaction postsynthesis preferred.

Hybrid Neorganicheskie-organic monomers of the present invention induce specific interest as building blocks for hybrid Neorganicheskie-organic polymers. For the purpose of polymerization of hybrid monomers have the properties of organic monomer from which they were obtained, and the polymers can be formed using the reaction conditions, catalysts, polymerization initiators, polymerization and cross-linking agents known to specialists.

Hybrid monomers can react with itself, forming homopolymers or they can react with other monomers, forming heteropolymer. Heteropolymer may have respective monomers, statistically distributed in them, or they can be in the form of a so-called block copolymers, that is, the resulting polymer chains contain oligomeric segments gamopolis the nuclear biological chemical (NBC nature.

The resulting polymer resin, in particular transparent, it is believed, form a new class of compounds, for which the inventors propose a genetic name "aptamer", reflecting their dual hallmark as of nanosized particles and polymeric materials. Specific subclass aptameric materials formed by materials that are based on crystalline inorganic particles. For this subclass of materials, the inventors propose the name "castamere". Another important subclass of these materials represents those that have desirable optical properties; for this subclass, the inventors propose the name "optovolokonnye". It will be clear that optovolokonnye materials may belong to the subclass kristallnach materials or may not belong.

Detailed description of the invention

The invention will be further illustrated by detailed description get crystalrose material based on titanium dioxide with attractive optical properties, including a high degree of transparency and high refractive index. It is clear that the method may be modified using various inorganic starting materials, using different reactive Milanovich functional monomial is s, using different solvents, etc.

The preferred starting material titanium dioxide is one of the commercially available titanium dioxide sold as having a crystallite size in the range of nanometers. However, such materials typically include particles which are much larger than indicated in the manufacturer's specifications may result in agglomeration. Further suppose that the amorphous material is formed during the production processes for these materials are titanium dioxide, which bind the crystals of titanium dioxide of nanoscale in a single material.

To form aptamer, it is usually necessary to disagglomerated source material titanium dioxide by dissolving it in strong acid. The acid must be strong enough not only to particiapate particles, but also to dissolve amorphous titanium dioxide, which connects the nanocrystals together. It is possible that the processing of a strong acid also causes some recrystallization of the nanocrystalline particles.

In the case of titanium dioxide is very little acid strong enough to meet the above requirements. Suitable acids include hydrofluoric acid and anhydrous sulfuric acid, and anhydrous sulfuric acid is preferred.

Material titanium dioxide) is t with concentrated sulfuric acid and the mixture is heated to a temperature of about 200°C. The temperature of the support is about 5 minutes. The solution is then cooled to room temperature, preferably, using a bath of ice. The cooled solution is mixed with water. The resulting suspension is filtered through a series of filter media with decreasing pore size to remove particles of micrometer size. Get a clear solution.

This clear solution is subjected to dialysis to remove sulfate anions, dissolved cations Ti4+and particles of TiO2less than 5 nm. Preferably, the dialysis removes all particles of TiO2less than 15 nm. During dialysis the pH of the support is about 1, using a 0.1 normal aqueous HCl.

Volume detalizirovannoi solution is reduced to one-third part by evaporation of the greater part of the water present in the solution. After evaporation, the concentration of TiO2will be, preferably, about 5 g per 100 ml At this point, add concentrated HCl to form a 3-molar solution.

The acidified solution is then mixed with an organic solvent S1. This solvent must be miscible with water, and he must be a suitable solvent for the reactive monomer with wilanowie functional groups. In this example, using N,N-dimethylacetamide (DMAA). Usually acidified aqueous solution is diluted 2-6 times organic will dissolve the LEM.

The solution of nanoparticles of titanium dioxide in DMAA is mixed with 3-(trimethoxysilyl)propylmercaptan (CAS number 2530-85-0) in DMAA. The reaction temperature is 80°C, and the reaction time is about 1 hour. Use an ultrasonic bath to facilitate what is essentially occurs in a heterogeneous reaction, even if it is a transparent solution.

After the reaction cieniowania completed, to the reaction product, water is added, forcing cieniowanie particles of titanium dioxide to come out of solution. The resulting suspension is centrifuged for 10 minutes at 5000 rpm Obtained granules dissolved in DMAA and the solution is evaporated to remove all remaining water. Cieniowanie particles also form transparent solutions with other solvents, such as N,N-dimethylformamide (DMF) and acetonitrile, and monomers such as N,N-dimethylacrylamide. Other suitable monomers include N,N-dimethylacrylamide and mixtures of this acrylamide and the corresponding methacrylamide.

Optional, this solubility can be improved by mixing the solution silverbank particles in DMF with trioctylphosphine (TOPO, CAS number 78-50-2), 5% by weight relative to the TiO2. The nanoparticles may further be stabilized reactive polymers such as oligomers and polymers of the above acrylic monomers is IDA and methacrylamide.

For the polymerization reaction cieniowanie particles dissolved in a suitable monomer. The residue after zentrifugenbau can be dissolved directly in the monomer or it may first be dissolved in nemonoman a solvent such as DMAA. In the latter case, the solution is subsequently mixed with the selected monomer and the solvent is then removed, e.g. by evaporation. It is important that at the beginning of the polymerization reaction of the monomer mixture mainly contain no solvent.

The solution silverbank particles in N,N-dimethylacrylamide will polimerizuet, adding photoinitiator (Darocur 4265, Ciba-Geigy), or thermally with azo-visitbotanical (AIBN) or other radical initiator. Formed a viscous transparent solution, which utverjdayut in plastic with UV irradiation.

Resin of N,N-dimethylacrylamide and methacrylate modified nanoparticles of titanium dioxide have excellent optical properties in terms of transparency and high refractive index. For best results, the refractive index of the crystal particles of titanium dioxide are preferred compared to amorphous particles, and particles of rutile is preferred in comparison with particles of anatase.

Size patinirovannaya particles can be determined by atomic force microscopy (AFM). Suppose that the particle size is m less than about 20 nm contributing less to the high refractive index resin [see Caseri (W.Caseri), Macromol. Rapid. Commun. 21, 705-722 (2000)]. Therefore, the monomer, preferably, does not contain significant quantities of particles of titanium dioxide with a size below 20 nm.

Particles of titanium dioxide having a size substantially greater than 20 nm is not preferable in the optical resin, because such particles cause light absorption and Rayleigh scattering. Found that the process described above leads to the solution of the particles of titanium dioxide, which does not actually contain crystallites of titanium dioxide is greater than 20 nm. Unexpectedly, the final stage of filtration is carried out with gasket filter having a pore size of 0.2 micrometer (200 nm). On average, about 10% of the initial amount of titanium dioxide is retained on filter paper.

Stage dialysis is used to remove dissolved ions Ti4+and SO42-and particles of titanium dioxide of less than about 5 nm. Good results were obtained with a dialysis tubing Spectra/Por type 7, available from Spectrum in Gardenia, California, USA. Dialysis can be further optimized by the selection environment, which removes essentially all particles of titanium dioxide of less than 10 nm, preferably, essentially removes all particles of titanium dioxide of less than 15 nm.

The refractive index of the optical resin obtained as described above, is a function of volume percentage of particles of duoci is titanium, present in the resin. Resin of the present invention can contain up to 50% titanium dioxide by volume, which corresponds to about 80% by weight.

A high degree of transparency and high refractive index optical resins of this invention make these materials particularly suitable for a large number of optical applications such as lenses, refractometers, and the like. The application is of special interest in the use of these resins for the encapsulation of light-emitting diode (LED) chips.

On the interface of two optical materials with different refractive indices can occur two types of reflection. The first is a well-known full reflection, which occurs when the angle of the incident beam lies outside the so-called cone of Snell's law. This type of reflection can be mentioned as a classic, or Snell's law, reflection. In addition, there is a second form of reflection that occurs within the cone of Snell's law. It represents a partial reflection, which is proportional to the ratio of the areas of the respective refractive indices.

Thanks semiconductor materials used in LED chips, these chips or matrices have a very high index of refraction: usually about 2.2 for green and blue LED-s, and about 3.4 for the red LED. IU the odes of production of these chips will inevitably lead to LED-am, having a flat surface on the light emitting side. Flat surface at the interface with the surrounding air is the fact that a lot of light emitted from the LED is reflected back into the LED chip. In other words, the surface of the partition LED/air has a small cone of Snell's law, leading to the lack of efficiency of the glow.

Standard LED-s capsulebuy in the hemisphere of the transparent resin. The spherical surface section of the air-resin leads to much lower reflection. However, the refractive index of the materials used for these vertices hemispheres, is typically around 1.5, which leads to a significant decrease of the refractive index in the flat surface section LED/dome. As a result, the encapsulation leads to only a moderate reduction in light loss due to reflection.

The optical resin of the present invention may be arranged so as to have a very high refractive indices. For example, a resin containing 50 % by volume of PbS (PP=4,0) in the organic matrix, with PP=1,5, has a refractive index of 2.75. Resin on the basis of titanium dioxide can be arranged so that PP reached a value of about 2.2. Rheological properties of these materials make it feasible to form them into the desired spherical shape. Reflection Snell such structures of nams is th decreases.

Although dome LED, made of optical resin with high PP, significantly reduce the reflection loss at the interface LED/dome, part of the improvement is removed increased partial reflection on the boundary surface of the dome/air. This is due to the high incidence of PP on this last interface. It was found that the reflection loss can be reduced further by providing layers dome with low PP, even if this measure increases the number of reflecting surfaces.

For green or blue LED with PP 2,2, an optimal design of the encapsulation includes a dome-shaped core having PP 2,2 (i.e. identical to that of the LED chip, the first hemispherical shell with PP is 1.81, and the second hemispherical shell having PP 1,22. This layered dome has a reflection loss of 3.8% compared to the reflection loss of 14% for monolithic dome with PP to 2.2. Significant improvement will be with the material with PP at least 2.

Improving the efficiency of light received with this layered dome, comes from the fact that a partial reflection is proportional to the ratio of the areas of the respective refractive indices.

Resins having a refractive index of 2.2 and 1,81 can be packaged using the process described above. Transparent resin having a PP is Colo 1,22, currently not available. The best practically available selection of uses for the outer electron shell resin with PP about from 1.3 to 1.4, such resins known in the art.

The same design encapsulation of the core/shell/shell can be used for encapsulation of the red LED with PP 3,4. Although not optimal for this configuration (PP dome is significantly lower than that of the LED chip), the lower reflection loss, however, significantly (30%).

1. A method of obtaining a hybrid organic-inorganic Monomeric material containing stage:
a) peptization of the inorganic material particles selected from the oxides, sulfides, sulfates, phosphates, arsenides and arsenate base metals and mixtures thereof, in anhydrous sulfuric acid or hydrogen fluoride, to obtain the solution of the inorganic material particle;
b) fractionating the solution obtained in stage a)to a slurry of inorganic particles having the interval of particle size from 5 nm to 100 nm;
C) mixing the fractionated solution obtained in stage b)with an organic solvent;
g) the reaction mixture from stage b) with a solution in an organic solvent reactive organic monomer with wilanowie functional groups.

2. The method according to claim 1, where dissolve the b stage C) is identical to the solvent at the stage d).

3. The method according to claim 1 or 2, where the inorganic material particles are selected from materials having a refractive index at least to 1.6, preferably at least a 2.0.

4. The method according to claim 1, where the inorganic material particles selected from the group consisting of titanium dioxide, zinc oxide, zinc sulfide, lead sulfide, and mixtures thereof.

5. The method according to claim 4, where the material of the inorganic particle is a titanium dioxide.

6. The method according to claim 5, where the material of the inorganic particles is an anatase, rutile, or their mixture.

7. The method according to claim 5, where the material of the inorganic particles is a rutile.

8. The method according to claim 1, where stage b) contains filtering.

9. The method according to claim 1, where stage b) contains dialysis.

10. The method according to claim 1, where the solution obtained in stage b), contains inorganic particles having a particle size of from 15 to 50 nm.

11. The method according to claim 1, where the solution obtained in stage b), contains inorganic particles having a particle size of about 20 nm.

12. The method according to claim 1, where the solvent used in stage C), is mixed with water.

13. The method according to item 12, where the solvent used in stage C), selected from the group consisting of N,N-dimethylacetamide, N,N-dimethylformamide (DMF) and acetonitrile.

14. The method according to claim 1, where the reactive organic monomer with wilanowie functional groups contains this the len-unsaturated fragment.

15. The method according to 14, where reactive organic monomer with wilanowie functional groups contains a fragment of acrylamide or methacrylamide.



 

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31 cl, 11 dwg, 9 ex

FIELD: chemistry.

SUBSTANCE: invention can be used in production of titanium dioxide when processing material which contains titanium and iron, for example ilmenite concentrates. The method of producing titanium dioxide involves the following steps: (a) reacting iron-containing titanium ore with an aqueous solution of NH4F at temperature 100-120°C, pressure of 1-2 bars and pH of approximately 6.5-7.0; (b) filtering the obtained aqueous suspension with subsequent separation into a precipitate fraction which contains ammonium fluoroferrates, and a filtrate fraction which contains ammonium fluorotitanates; (c) hydrolysis of the obtained filtrate fraction thereby obtaining a solid component which is ammonium fluorooxotitanate; (d) thermal hydrolysis of the solid component obtained at step (c).

EFFECT: high degree of utilisation of raw material, high output and whiteness of the product, as well as simplification of the process and reduction of amount of wastes.

17 cl, 4 dwg

FIELD: chemistry.

SUBSTANCE: for titanium dioxide treatment at first the basic material in the form of titanium dioxide water suspension is prepared at pH value equal or less than 3 or at pH value equal or more than 10, then water-soluble tin and zirconium compounds are added as well as water-soluble tin and zirconium compounds are added as well as water-soluble compounds of at least one additional element selected from the group including aluminium, silicon and titanium at pH equal or less than 3 or equal or more than 10, then obtained mixture is brought to pH in the range from 6 to 8. The pigment obtained with this method is claimed as well as its application in paints, varnishes and plastics compositions.

EFFECT: enhanced photostability of pigment based on titanium dioxide while keeping its optical properties.

17 cl, 3 ex

FIELD: chemistry; construction.

SUBSTANCE: present invention relates to obtaining titaniferous products, used in production of construction and paint materials, as well as welding electrodes. The method of obtaining titaiferous product from a sphene concentrate involves decomposition of the concentrate for 2.5-5.0 hours by dilution with a solution of sulphuric acid while boiling, with transfer of titanium into the sulphuric acid solution, and calcium and silicon into the primary residue and separation of the primary residue. After separation of the primary residue, the sulphuric acid solution is concentrated until attaining titanium concentration of 150-200 g/l in terms of titanium dioxide. The obtained suspension is settled, forming a secondary residue, which is separated from the concentrated sulphuric acid and combined with the primary residue. The concentrated sulphuric acid then subjected to thermal hydrolysis and the combined residue is treated with aluminium phosphate, obtaining calcium-silica filler.

EFFECT: increased photochemical activity of titaniferous product and reduced content of phosphorous in it, as well as improved service characteristics of the calcium-silica filler.

6 cl, 5 ex

FIELD: chemistry.

SUBSTANCE: modification of titanium dioxide by metal oxides involves titanium dioxide treatment in water suspension by solutions of magnesium, or aluminium, or nickel formiates obtained by reaction of aqueous formic acid solution with the indicated metals or their carbonates or hydroxides. Formic acid quantity is stechiometric or exceeds stechiometric quantity by 20-100%. Further the suspension is dried in dispersion dryer with heating of titanium dioxide with applied salts at 200-700°C for 1-60 minutes.

EFFECT: reduced temperature of titanium dioxide modification without surface contamination with hardly removable anions, or anatase form transmutation into rutile form.

2 cl, 9 ex

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