Radiation-protective lanthanide-containing compounds

FIELD: chemistry.

SUBSTANCE: invention relates to lanthanide-containing compounds, consisting of a copolymer of ethyl methacrylate and 3-allylpentanedione-2,4 (100:1), bonded through a β-diketonate group with a lanthanide (+3) ion, which in turn is bonded with molecules of a ligand which is β-diketone of general formula: , where Ln is a lanthanide (+3) ion (La3+, Pr3+, Nd3+, Sm3+, Eu3+, Gd3+ Tb3+, Dy3+, Ho3+, Er3+, Tm3+, Yb3+), n is the number of ethyl methacrylate links in the copolymer chain; m is the number of lanthanide-containing links in the copolymer chain; R1, R2, R3, R4 are organic radicals (CH3 - methyl, C6H5-phenyl): - R1=R2=R3=R4=CH3 - lanthanide (+3) ion, bonded with the polymer part of the compound through a pentanedione-2,4 fragment (acetyl acetone) and a ligand which is acetyl acetone; - R1 = R3 = CH3, R2=R4=C6H5 - lanthanide (+3) ion bonded with the polymer part of the compound through benzoyl acetone fragment and a ligand which is benzyol acetone; - R1=R2=R3=R4=C6H5 - lanthanide (+3) ion bonded with the polymer part of the compound through a dibenzoyl methane fragment and a ligand which is dibenzoyl methane; - R1=R3=R4=CH3, R2=C6H5 - lanthanide (+3) ion bonded with the polymer part of the compound through a benzoyl acetone fragment and a ligand which is acetyl acetone; - R1=R2=C6H5, R3=R4=CH3 - lanthanide (+3) ion bonded with the polymer part of the compound through a dibenzoyl methane fragment and a ligand which is acetyl acetone; - R1=R2=R3=C6H5, R4=CH3 - lanthanide (+3) bonded with the polymer part of the compound through a dibenzoyl methane fragment and a ligand which is benzoyl acetone. Said compounds have radiation-protective properties.

EFFECT: obtaining material which is optically transparent in the visible and ultraviolet range and resistant to ionising radiation.

1 ex, 1 tbl, 9 dwg

 

The invention relates to space and nuclear science, more specifically to a radiation resistant polymer materials.

Known organosilicon polymers subjected to modification Tris-β-diketonates REE (A.S. USSR №1840546). The modification in this case occurs on the hydroxyl groups of the polymer, designed for stitching (rejection) when applied to the product. The main disadvantage of these materials is their mechanical instability and weak adhesion to the surface of the product. Resulting in the installation and operation of the product with such a coating requires extremely careful handling. In addition, the optical transparency of the material does not meet the requirements of space science.

The closest analogues to the claimed polymers are acrylate polymer materials (A.S. USSR №1029584), derived from acrylate polymers containing carboxyl groups by reacting them with Tris-β-diketonates of rare earth elements (REE).

where Ln is a lanthanide ion (+3), n is the number of lanthanide-containing links in the chain (co)polymer, R1, R2- organic radical (methyl, phenyl).

However, these materials have a number of disadvantages: the presence of free carboxyl groups in the polymer do not provide to rodinnou stability of metal structures, the corrosion of metal structures, in particular aluminum, to which they are applied; when applied to non-metallic coating of the same carboxyl groups, the material is subjected to hydrolysis and, consequently, delamination of the coating from the workpiece; radiation resistance is insufficient.

The technical objective of the proposed solutions is the development of optically transparent in the visible and ultraviolet region (co)polymer material that is resistant to ionizing (electromagnetic and corpuscular radiation capable of protecting the surface from these radiations, thus not exposed to the moisture of the air and non-corrosive metal parts.

To solve the technical problem it is suggested to use compounds consisting of a polymer part, directly linked through a β-diketonate group with the lanthanide ion (+3), which, in turn, is associated with molecules of the ligand, which represents a β-diketone, the General formula

where Ln is a lanthanide ion (+3) (La3+Pr3+Nd3+Sm3+, Eu3+, Gd3+, Tb3+, Dy3+, Ho3+Er3+Tm3+, Yb3+);

n is the number of links methacrylate in the copolymer chain;

m - the number of lanthanide-containing links in the chain of the copolymer;

R1, R , R3, R4organic radicals (CH3is methyl,6H5is phenyl):

- R1=R2=R3=R4=CH3polymer connection part connects the lanthanide ion (+3) through a fragment of pentanedione-2,4 (acetylacetone), the ligand is an acetylacetone;

- R1=R3=CH3, R2=R4=C6H5polymer connection part connects the lanthanide ion (+3) through a fragment of benzoylacetone, the ligand is benzoylacetone;

- R1=R2=R3=R4=C6H5the connection part connects the lanthanide ion (+3) through the fragment dibenzoylmethane, the ligand is dibenzoylmethane;

- R1=R3=R4=CH3, R2=C6H5the connection part connects the lanthanide ion (+3) through a fragment of benzoylacetone, the ligand is an acetylacetone;

- R1=R2=C6H5, R3=R4=CH3- the connection part connects the lanthanide ion (+3) through the fragment dibenzoylmethane, the ligand is an acetylacetone;

- R1=R2=R3=C6H5, R4=CH3the connection part connects the lanthanide ion (+3) through the fragment dibenzoylmethane, the ligand is benzoylacetone;

resistant to ionizing (electromagnetism and corpuscular the time radiation and able to protect them from the surface, to which they are applied.

Unlike the prototype of the proposed connection does not contain easily susceptible to hydrolysis and corroding metal surface carboxyl groups, which results in greater durability of products during storage and operation, and extends the possible range of their use, in particular, the possibility of their use as radiation-resistant materials in the terrestrial environment.

To obtain the claimed compound at room temperature to a solution of polymeric material with β-diketonate fragments to add a solution of Tris-β-diketonate REE. This creates a chemical equilibrium between ion binding REE β-diketonate fragment (co)polymer material and the actual β-diketonate ligand Tris-β-diketonate. After the application of lanthanide-containing (co)polymer solution on the surface of the product, one molecule of β-diketonate ligand evaporates together with the solvent and the interaction goes to the end, the resulting compound of formula (I)

where R1, R2, R3, R4- organic radicals, n is the number of links methacrylate in the polymer chain, and m is the number of lanthanide-containing units in the polymer chain, Ln is a lanthanide ion (+3).

The claimed compounds have the IR spectrum revealed the processes for coordinated molecules of β-diketones and β-diketonate fragment of the polymer connection parts of the absorption bands of stretching vibrations ν(-CO-CH 2-CO)enol.β-deketand ν(C=C)enol. β-diket.lying in the region of 1600 cm-1In the UV absorption spectrum the absorption band in the region of 270-320 nm. due to π→π*electronic transitions (Nakamoto K. Infrared spectra of inorganic and coordination compounds. - M.: Mir, 1966. - 411 S.; Bellamy L. New data on the infrared spectra of complex molecules. - M.: Mir, 1971. - 318 S.; Neiland OA and other Structure and tautomeric transformations of β-dicarbonyl compounds. - Riga: Knowledge, 1977. - 448 S.).

Figure 1 shows the dynamics of changes in UV transmission spectra of copolymer of ethyl methacrylate and 3-allylpalladium-2,4 (100:1), containing 1.2 wt.% holmium depending on the time of UV-irradiation: 1-0 h, 2-4 h, 3-10 h 4-24 h, 5-40 h; figure 2 shows the dynamics of changes in UV transmission spectra of copolymer of ethyl methacrylate and acrylic acid (100:1), containing 1.2 wt.% holmium depending on the time of UV-irradiation: 1-0 h, 2-24 h, 3-28 h, 4-34 h, 5-46 h; figure 3 presents induced absorption spectrum of a copolymer of ethyl methacrylate and 3-allylpalladium-2,4 (100:1), containing 1.2 wt.% holmium at the time of exposure to UV radiation: 1-4 h, 2-10 h, 3-24 h, 4-40 h; 4 - dynamics of change in the UV spectrum of induced absorption of a copolymer of ethyl methacrylate and acrylic acid (100:1), containing 1.2 wt.% holmium, in the process of UV-irradiation: 1-24 h, 2-28 h, 3-34 h, 4-46 h; figure 5 - transmission spectrum is of polymera methacrylate and 3-allylpalladium-2,4 (100:1), containing 1.2 wt.% holmium, before irradiation by protons (1) and after irradiation with protons E=500 Kev, f=1•1013particles/cm2(2); figure 6 - transmission spectrum of a copolymer of ethyl methacrylate and 3-allylpalladium-2,4 (100:1), containing 1.2 wt.% holmium, before irradiation by protons (1) and after (2) E=500 Kev, f=1•1014particles/cm2; figure 7 is a transmission spectrum of a copolymer of ethyl methacrylate and 3-allylpalladium-2,4 (100:1), containing 1.2 wt.% holmium, before irradiation by protons (1) and after (2) E=500 Kev, f=1•1015particles/cm2; Fig - dynamics of change in the spectrum of induced absorption of a copolymer of ethyl methacrylate and 3-allylpalladium-2,4 (100:1), containing 1.2 wt.% holmium, during proton irradiation at E=500 Kev, and f, is equal to: 1•1013particles/cm2- (1), 1•1014particles/cm2- (2) and 1•1015particles/cm2- (3); figure 9 - dynamics of change in the spectrum of induced absorption of a copolymer of ethyl methacrylate and acrylic acid (100:1), containing 1.2 wt.% holmium, in the process of irradiation by protons with E=cm and f, is equal to: 4•1014particles/cm2- (1); 6•1014particles/cm2- (2); 8•1014particles/cm2- (3); 1•1015particles/cm2- (4).

Here is an example of a specific implementation.

To obtain the claimed compounds containing as Ln the holmium was taken a 20% solution of copolymer in toluene obtained the C methacrylate, and 3-allylpalladium-2,4, in a molar ratio of 100:1, previously washed free from acid 0,05 m NaOH solution.

In a polymer base with a volume of 30 ml (26,28 g) with constant stirring and a temperature of 25°C was introduced Tris-acetylacetonate holmium 3 water mass 0,2357 g, dissolved in 1 ml of 1,4-dioxane, and stirred for 2 hours. Flowing a chemical reaction can be described by the following scheme:

To conduct a comparative test was made prototype sample is a copolymer of ethyl methacrylate and acrylic acid (100:1), containing 1.2 wt.% holmium (+3), General formula

To do this in 1080 ml of a 20% toluene solution of the polymer basis of the prototype, pre-washed free from acid 0,05 m NaOH solution at 30°C was injected 2,48 g trihydrate Tris-acetylacetonate holmium, pre-dissolved in 30 ml of 1,4-dioxane.

As one of the indicators of corrosion resistance of acrylate polymer materials is an acid number were measured acid number:

- polymers of the claimed compounds and prototype;

- polymers, washed free from acid 0,05M alkali solution, the claimed compounds and prototype;

solutions holinesterzoy copolymers of the claimed compounds and the prototype.

Acid number was determined by the churchyard-23955-80, p. As can be seen, the acid number of the copolymer of ethyl methacrylate, 3-allylpalladium-2,4 significantly lower than that of a copolymer of ethyl methacrylate and acrylic acid (see table).

Table
Information on the acid numbers of the prototype and the claimed substance
Copolymer of ethyl methacrylate and 3-allylpalladium-2,4 (100:1)Copolymer of ethyl methacrylate and acrylic acid (100:1)
NephropathyWashedWashed, containing 1.2 wt.% holmiumNephropathyWashedWashed, containing 1.2 wt.% holmium
Acid number, mg KOH/g0,440,010,041,900,650,70

The use of leaching polymer base has allowed more than 15 times lower values of acid number in both samples, however, for a copolymer of ethyl methacrylate with acrylic acid is th value of the acid number is still high and makes it unacceptable as coatings for metal surfaces. Introduction Tris-acetylacetonate holmium in a polymer base leads to a slight increase of the acid number in both samples, but in the case of the claimed substance is below the allowable standards for polyacrylate lacquer (0.1 mg KOH/g). Low value acid number indirectly confirms its corrosion resistance to metal structures.

Resistance to UV radiation was estimated by the change of the absorption spectra of the quartz plates coated with valmistamisele (1.2 wt.%) polymer coatings before and after exposure.

The solution holinesterzoy (1.2 wt.%) samples varnishes were applied to the plane-parallel plate of quartz KU-1 and dried at 60°C up to degree 3 (slipcast surface). When drying was obtained polymer coating of the inventive substance (I) and its prototype (II), containing 1.2 wt.% holmium.

Irradiation of the quartz plates coated with valmistamisele polymer coating (I) and (II) was produced by the lamp DB-PD contact close (within 2 mm). To measure the energy of UV radiation of this lamp was not possible, therefore, all these studies are quantitative in nature. Recording absorption spectra were carried out before and after irradiation spectrometer SPECORD UV VIS range from 28000 to 50000 cm-1(357-200 nm), 0-100 absorption.

The analysis of the absorption spectra of the quartz plate coated with a layer of polymer coating (I) (1), prototype (II) (Figure 2) showed a higher resistance to UV radiation of the first sample compared to its prototype, which is more clearly seen in the spectra of induced absorption in both samples.

Induced absorption spectrum was obtained by subtraction of a transmission spectrum of the unirradiated sample from the spectrum of the irradiated sample. Induced absorption spectrum of polymer coating (I) (Figure 3) show that the degradation of the optical properties unlike its prototype (II) (Figure 4) is much less, instead of reducing the transparency of the coating (increased absorption) in the field of 230-320 nm, the transmittance is increased, as indicated by negative values of induced absorption. The greatest effect of increasing the transparency of the inventive substance (I) is in the range of 300 nm and up to 38% at the time of exposure 4 hours Further exposure to UV radiation leads to increased absorption of the sample, but starting from 24 h begins to decrease and stabilize at 32% at the time of irradiation 32-40 hours Under irradiation valmistamisega prototype (II) the effect of increasing the transparency was observed. By contrast, when exposure time equal to 24 hours, there is an increase in light absorption by 40% in the field of 240-340 nm. Pogloshena the sample prototype (II) continuously increases with time of exposure and time of exposure to 46 h reaches 60%.

Similarly, there were obtained compounds with other lanthanides. To do this in 30 ml of polymer base with constant stirring and t=25°C were introduced 3-water Tris-acetylacetonate corresponding lanthanide in number, for example: La3+- 0,2238 g WG3+- 0,2247 g, Nd3+- 0,2262 g Sm3+- 0,229 g Eu3+- 0,2298 g, Gd3+- 0,232 g, Tb3+- 0,2329 g Dy3+- 0,2346 g, H3+- 0,2367 g, Tm3+- 0,2375 g Yb3+- 0,2394,

The variation of the optical properties of the claimed compounds containing other lanthanides, like valmistamisele claimed connection. At the time of exposure to UV radiation 40 h the decrease in the absorption of the inventive compounds in the range of 300 nm, containing other ions of the lanthanides, amounted to: La3+~20%, WG3+~30%of Nd3+~10%, Sm3+~30%of Eu3+~20%, Gd3+~10%, Tb3+~20%, Dy3+~30%of Er3+~30%, Tm3+~50%of Yb3+~50%.

Resistance to proton radiation as in the case of UV radiation, was estimated by the change of the absorption spectra of the inventive polymeric coating containing 1.2 wt.% holmium deposited on a quartz plate KU-1. Proton irradiation was performed at the cascade accelerator KG-500 in Sri NP MSU. When the irradiation was used proton energy (E) 500 Kev and fluence (f) 1·1013-1015particles/cm2(F=1015particles/cm2recruited within 30 minutes). Tol is in cover was taken about 0.5 mm, that is certainly more mileage proton energy of 500 Kev in the substance.

From the absorption spectra (Figure 5-7) and spectra of the induced absorption of the inventive substance (I) (Fig) proton irradiated with the same energy (E=500 Kev) observed similar compared to UV-irradiation, the picture changes in the transmittance of the polymer coating to the increase in the number of bombarding particles. Thus, when f=1 to 1013particles/cm2and 1·1014particles/cm2observed increase in optical transparency of the samples in the range of 300 nm to 5 and 20%, respectively, when f=1·1015particles/cm2there is a reduction optical transparency to 20% of the initial light transmission.

As can be seen from the spectra induced absorption (Fig.9) prototype (II)containing 6 wt.% holmium, under the same conditions of irradiation by protons (E=500 Kev and f=1·1015particles/cm2), there is a reduction optical properties (absorption increases) more than 20%. Given the fact that in the inventive polymer coating (I) the content of holmium 5 times less than in the prototype (II), and optical properties he also reduced by 20%, it follows that the claimed compounds of General formula (I) are more resistant to proton radiation in comparison with the prototype.

Increased resistance to ionizing radiation lanthanide-containing polymers of light is Ana with the dissipation of the energy of radiation around the carbon skeleton of the polymer, i.e. reradiation through fluorescence (luminescence) in the soft (thermal or visible radiation. Since the quantum yield of luminescence of β-diketonate complex compounds of europium (III) increases in the following series: Tris-acetylacetonates<Tris-benzoylacetonate<Tris-dibenzoylmethane, it follows that the stability of the inventive compounds (I) in which:

- R1=CH3, R2=C6H5,

- R1=R2=C6H5,

will be higher than when R1=R2=CH3.

Thus, the claimed connection:

1) have a low acid number, which confirms their corrosion resistance to metal structures;

2) have a higher resistance to UV and proton radiation than the prototype;

3) use as a radiation-protective coatings.

Lanthanide-containing compounds consisting of a copolymer of ethyl methacrylate and 3-allylpalladium-2,4 (100:1), linked through a β-diketonate group with the lanthanide ion (+3), which in turn is associated with molecules of the ligand, which represents a β-diketone, the General formula:

where Ln is a lanthanide ion (+3) (La3+Pr3+Nd3+Sm3+, Eu3+, Gd3+, Tb3+, Dy3+, Ho3+Er3+Tm3+, Yb3+),
n is the number C is egnew methacrylate in the copolymer chain;
m - the number of lanthanide-containing links in the chain of the copolymer;
R1, R2, R3, R4, organic radicals (CH3is methyl,6H5is phenyl):
- R1=R2=R3=R4=CH3- lanthanide ion (+3)associated with the polymer portion connecting through a fragment of pentanedione-2,4 (acetylacetone) and ligand represents acetylacetone,
- R1=R3=CH3, R2=R4=C6H5- lanthanide ion (+3)associated with the polymer portion connecting through a fragment of benzoylacetone and ligand representing benzoylacetone,
- R1=R2=R3=R4=C6H5- lanthanide ion (+3)associated with the polymer part of the connection through the fragment dibenzoylmethane and ligand, representing dibenzoylmethane,
- R1=R3=R4=CH3, R2=C6H5- lanthanide ion (+3)associated with the polymer portion connecting through a fragment of benzoylacetone and ligand represents acetylacetone,
- R1=R2=C6H5, R3=R4=CH3- the lanthanide ion (+3) associated with the polymer part of the connection through the fragment dibenzoylmethane and ligand represents acetylacetone,
- R1=R2=R3=C6H5, R4=CH3- lanthanide ion (+3)associated with polymers is part of the connection through the fragment dibenzoylmethane and ligand, representing benzoylacetone with radiation-safe properties.



 

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