Heterogenic sensibiliser and method of water photoremediation

FIELD: chemistry.

SUBSTANCE: invention relates to chemistry and chemical technology, namely to synthesis of modified silicagels, containing molecules of substituted phthalocyanines covalently bound with them, and their application for water photoremediation. Method of water photoremediation with application of radiation of visible range in presence of oxygen and heterogenic sensibiliser of general formula: , where R=H is either SPh; X is anion; n=4-8; M=Zn, AlL, GaL, SiLz; L=Cl, OH; M=1-4.

EFFECT: invention makes it possible to carry out efficient purification of water from bacteriological contamination.

2 cl, 3 tbl, 11 ex

 

The present invention relates to chemistry and chemical technology, namely the synthesis of modified silica gels containing covalently associated molecules substituted phthalocyanines, as well as the application of these silica gels for Photobacterium water.

Known cationic phthalocyanines, representing poly(dialkylaminomethyl)substituted phthalocyanine zinc and aluminum, which are sensitizers of singlet oxygen production under the action of visible light, and the way Photobacterium water using these phthalocyanines [RF patent №2281953, CL C02F 1/30, 2006]. The positive charge of cationic groups ensures the interaction of these sensitizers with negatively charged outer membrane of microorganisms, contamination and effective photodynamic inactivation. Despite its high efficiency, this method has a major drawback, which is the need for subsequent removal of dye from solution. This operation is carried out using a specially designed selective filters, which greatly complicates and increases the cost of the process, and, nevertheless, does not guarantee in all cases, complete removal of the sensitizer and the products of its photodegradation of solution.

This lack deprived heterogeneous (solid-phase) sensibilized the market of singlet oxygen production. Solid sensitizers can be easily separated from the water after the process is complete, the photo radiation by simple filtering.

Known heterogeneous sensitizers for inactivation of microorganisms obtained by the adsorption of dyes with lightfastness from 4 to 8 points on an inert carrier [A. Yoshino, I. Iwami. US Patent No. 4 520 072]. However, the adsorbed dye can decorrelates and move in aqueous solution, thereby causing chemical pollution.

This lack deprived of heterogeneous sensitizers, the active phase in which covalently grafted to the media.

Known heterogeneous sensitizers for inactivation of microorganisms obtained by chemical grafting to the granules aminopropiophenone silica gel phthalocyanines non-transition metals (zinc, aluminum, gallium and silicon) [RF patent №2447027, CL C02F 1/30, 2010 - prototype]. However, these sensitizers are not active.

The objective of the invention is the synthesis of heterogeneous sensitizers containing as the active phase of substituted phthalocyanines covalently associated with aminopropiophenone silica gel having high Photobacterium activity, as well as the development method Photobacterium water with acquired sensitizers.

The problem is solved by the synthesis of heterogeneous sensibilise the Directors, you can imagine the following General formula

where R=H or SPh;

X is an anion;

n=4-8;

M=Zn, AlL, GaL, SiL2;

L=Cl, OH;

m>1.

Get these sensitizers by proshivkoi chloromethylphosphonic phthalocyanines MPc(CH2Cl)nand MPc[(SPh)4](CH2Cl)nmodified aminopropiophenone the silica and subsequent processing of the products obtained amines, such as 2-dimethylaminoethanol. Modification aminopropionic silica produce single or multiple treatment solution of 3-bromopropylamine hydrobromide.

As a result, the media appear amino group, more remote from the silica gel.

Example of modifying aminopropiophenone silica gel single handle 3-bromopropylamine with subsequent inoculation of octachloronaphthalene silicon and quaternization of the last 2-dimethylaminoethanol shown in the diagram. The structure of heterogeneous sensitizer 3MD-am/5 m-SiPcChol7obtained by inoculation of policyinformation silicon to aminopropiophenone the silica gel diasorb-250 Amin, modified triple handle 3-bromopropylamine below. Processing bromopropylamine can be performed any number of times and, respectively, to obtain larger the f value m.

Join phthalocyanine as possible on primary and secondary amino groups of the modified diasorb, however, given the spatial factors in the reaction participates preferably at primary and not a secondary amino group. In the resulting sensitizers grafted phthalocyanine more mobile and forms a sphere of larger radius than using unmodified diasorb. This increases the possibility of contact phthalocyanine with bacteria in the water, the deeper its penetration into the bacterium and, thus, increases the efficiency of disinfection of water.

Heterogeneous sensitizers containing as the active phase phthalocyanines of formula MPc(Chol)nabsorb visible light range with a wavelength in the region from 600 to 750 nm. Heterogeneous sensitizers of formula MPc[(SPh)4]Cholncontaining thienylene groups absorb light in the region from 600 to 800 nm. Thienylene substituents in position 3 is located outside the plane of phthalocyaninato the tubes and prevent the convergence of the phthalocyanine molecules and formation of inactive π-π dimers and aggregates, which positively affects their antimicrobial activity.

The task is also achieved by providing a method of potoo is uttarayana water using the above-described heterogeneous sensitizers and radiation of the visible range in the presence of oxygen.

Used for the synthesis of polychloroethene phthalocyanines are chlorotoluene phthalocyanines by known methods, for example described in the patent of the Russian Federation 2405785, C07D 47/22, 2010

As modifiable media can be used aminopropiophenone silica gels with different pore size, such as diasorb-250 Amin, diasorb-750 Amin.

The invention is illustrated by the following examples.

Example 1

Modification aminopropiophenone silica

To 5 g aminopropiophenone silica gel (Diasorb-250 Amin, Diasorb-750 Amin) add 1 g of 3-bromopropylamine hydrobromide in 20 ml of dioxane. The mixture is heated for 2 h in a boiling water bath. Then the product is filtered, washed with water, alkali solution and again with water until neutral reaction of the mother liquor. Modified medium (MD-250am, MD-750am) is dried at a temperature of 80-90°C.

Three-time processing aminopropionic silica as described above gives a spacer containing up to four aminopropylene links (modified media 3MD-250am, 3MD-750am, m<4 in the General formula).

Example 2

Heterogeneous sensitizer, a modified MD-250am/5 m-SiPcChol7

To 2 g MD-250am in 20 ml of DMF added 0.01 g (10 mmol) octakis(chloromethyl)phthalocyanine silicon in 10 ml of DMF. The mixture is heated at 80-90°C to bleaching solution in t is an increase of about 40 minutes To the resulting suspension add 0.3 ml of 2-dimethylaminoethanol and the mixture is again heated at 80-90°C for 40 minutes the Precipitate was separated, washed with water and dried. The content of the dye in the sample is 5 mmol/1 g of the carrier.

Example 3

Heterogeneous sensitizer-modified 3MD-am/5 m-SiPcChol7

Get like that shown in example 2, using 3MD-250am instead of MD-250am.

Example 4

Heterogeneous sensitizer, a modified MD-750am/5 m-SiPcChol7

Get analogously to example 2, using MD-750am instead of MD-250am.

Example 5

Heterogeneous sensitizer-modified 3MD-750am/5 m-SiPcChol7

Get analogously to example 2, using 3MD-750am instead of MD-250am.

Example 6

Heterogeneous sensitizer MD-750am/2.5 μm-ZnPc(SPh)4Chol8

For the synthesis taken klimatisierung Tetra-3-phenyldiethanolamine zinc content 9 chloromethylene groups (% Cl 22.97) phenyl rings. Proof provisions chloromethylene groups is a shift signal of these protons in the spectrum of TMR (5,0 M. D.), different from the shift of the protons of CH2Cl groups directly related to phtalocyanines ring (5,5-5,8).

The solution 0,00360 g (2.5 μm) klimatisierung Tetra-3-phenylthio-phthalocyanine zinc in 6 ml of DMF is added to a suspension of 1 g MD-750am in 10 ml of DMF. The mixture is heated at 70-90°C for 30-40 minutes until the discoloration of the solution is then added to the mixture of 0.33 g (0,0035 M) 2-dimethylaminoethanol and the mixture is heated at 80-90°C for another 30-40 minutes The precipitate was separated, washed with acetone, water and dried. Full binding taken in response klimatisierung of tetraphenylnaphthalene with the carrier network of heterogeneous sensitizer containing dye 2.5 μm per 1 g of the carrier.

Example 7

Heterogeneous sensitizer, a modified MD-250am/5 m-AlPc(SPh)4Chol6

To 2 g MD-250am in 20 ml of DMF add 0,0134 g (10 mmol) heptanes(chloromethyl)Tetra-3-phenyldiethanolamine chloramine in 10 ml of DMF. The mixture is heated at 80-90°C for about 40 min until the discoloration of the solution. To the resulting suspension add 0.3 ml of 2-dimethylaminoethanol and the mixture is again heated at 80-90°C for 40 minutes the Precipitate was separated, washed with water and dried. The content of the dye in the sample is 5 mmol/g of carrier.

Example 8

Heterogeneous sensitizer MD-250am/1.5 μm-GaPcChol7

Get by the method of example 2, using gallium complex octachloronaphthalene phthalocyanine in an amount of 0.004 g (3 μm).

Example 9

The determination of the activity of heterogeneous sensitizers D-am/5 m-SiPcChol7MD-am/5 m-SiPcChol7and 3MD-am/5 m-SiPcChol7in photoinactivation of bacteria E. coli (pXen7) method bioluminescence

To determine Photobacterium activity of heterogeneous photosensitizers used bacterial bioluminescent test system based on genetically engineered strain is. coli (pXen7), bioluminescence which is due to the cloned full lux-operon from the glowing soil entomopathogenic bacteria Photorhabdus luminescens. The intensity of the bioluminescence of bacteria, preincubating with heterogeneous photosensitizers, before and after irradiation were recorded using a luminometer "Biotox-6" (Moscow) in cuvettes with a volume of 1.5 ml with 1 ml of the sample at room temperature. The intensity of bioluminescence was expressed in relative units.

In the test tube was introduced 2 ml of suspension biosensor - genetically engineered bacterial strain E. coli pXen7, suspended in distilled water to a concentration of 3×107CFU/ml, and heterogeneous photosensitizer. Samples were incubated in the dark for 10 minutes Experienced the sample was irradiated with white light source acomp (50 mW/cm2). Irradiation of the experimental samples and the incubation of a dark control was performed under stirring. After irradiation or dark incubation of the samples for 2 min, the media was allowed to settle to the bottom and selected in 1 ml of the supernatant liquid for measuring bioluminescence.

Incubation without access of light bacterial biosensor to 40 min with samples of heterogeneous photosensitizers in concentration in terms of the active substance 20 μm did not lead to a decrease in the level of bioluminescence (survival) compared the biosensor without additives photosensitizers or in the presence of media (diasorb-250 Amin, Diasorb 750 Amin) without photosensitizers. This reflects the absence of dark toxicity data samples.

The results are shown in table 1.

Table 1
Data Photobacterium bacteria E. coli pXen7 in water in the presence of heterogeneous photosensitizers
DoseThe level of bioluminescence, %
D-am/5 m-SiPcChol7(comparative prototype)MD-am/5 m-SiPcChol73MD-am/5 m-SiPcChol7
0 j/cm2(dark control)100100100
135 j/cm283±659±630±4
270 j/cm264±537±48±2

From table 1 it follows that the level of bioluminescence (survival of bacteria after treatment modified sensitizers much less, and the processing efficiency increases with increasing V. the penalties modifications that is, when increasing the length of the spacer connecting the active phase (phthalocyanine) media. So, among the studied new heterogeneous photosensitizers based on silicon phthalocyanines with both the chosen modes of irradiation (doses of 135 or 270 j/cm2most high Photobacterium activity has sample 3MD-am/5 m-SiPcChol7.

Example 10

The determination of the activity of heterogeneous sensitizers D-am/5 m-SiPcChol7MD-am/5 m-SiPcChol7and 3MD-am/5 m-SiPcChol7in photoinactivation of bacteria E. coli (pXen7) method bioluminescence carried out similarly to example 9.

The results are shown in table 2.

From table 2 it follows that the processing efficiency increases with increasing degree of modification, that is, when increasing the length of the spacer connecting the active phase (phthalocyanine) media. So, among the studied new heterogeneous photosensitizers based on silicon phthalocyanines with both the chosen modes of irradiation (doses of 135 or 270 j/cm2most high Photobacterium activity has sample 3MD-am/5 m SiPcChol7.

Table 2
Data Photobacterium bacteria E. coli pXen7 in water in the presence of heterogeneous photosensitizers
DoseThe level of bioluminescence, %
D-am/5 m-SiPcChol7MD-750aM/5 m-SiPcChol73MD-am/5 m-SiPcChol7
0 j/cm2(dark control)100100100
135 j/cm260±538±424±3
270 j/cm227±314±22±1

Example 11

The determination of the activity of heterogeneous sensitizers D-am/5 m-AlPc(SPh)4Chol6and MD am/5 m-AlPc(SPh)4Chol6in photoinactivation of bacteria E. coli (pXen7) method bioluminescence carried out similarly to example 9.

The results are shown in table 3.

Table 3
Data Photobacterium bacteria E. coli pXen7 in water in the presence of heterogeneous photosensitizers
DoseThe level of bioluminescence, %
MD-am/5 m-AlPc(SPh)4Chol6
0 j/cm2(dark control)100100
180 j/cm271±643±4

From table 3 it follows that the efficiency of processing in the modification increases. Thus, the dose of light in 180 j/cm2when using the modified drug MD-am/5 m-AlPc(SPh)4Chol6leads to a greater reduction in bioluminescence bacteria than when using D-am/5 m-AlPc(SPh)4Chol6that proves more effective the disinfection.

From examples 9, 10 and 11, it follows that the elongation of the spacer between the active phase (phthalocyanine) and the surface of the silica gel significantly increases the activity of heterogeneous sensitizers in photoinactivation of microorganisms in the aquatic environment.

Thus, heterogeneous sensitizers according to the invention have significantly higher Photobacterium activity than the sensitizers of the prototype, and how Photobacterium water use is more efficient than the method on the prototype.

1. Heterogeneous sensitizer General formula

where R=Nlib SPh;
X is an anion;
n=4-8;
M=Zn, AlL, GaL, SiL2;
L=Cl, OH;
m=1-4.

2. How Photobacterium water using sensitizer and radiation of the visible range in the presence of oxygen, characterized in that use heterogeneous sensitizer sensitizer under item 1.



 

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