Method of obtaining basic zinc carbonates

FIELD: chemistry.

SUBSTANCE: invention can be used in chemical industry. Method of obtaining basic zinc carbonates includes chemical conversion of coarse-dispersed zinc oxide in water solution of carbon dioxide and ammonia, further formation of target product, its filtration, drying, condensation and return of gaseous products to the stage of chemical conversion. Chemical conversion of zinc oxide into basic zinc carbonate is performed in ammonia-carbonate water solution in heterogenic conditions with molar ratio carbon dioxide:ammonia, equal 1:(5-9), temperature 15-50 °C and atmospheric pressure.

EFFECT: invention makes it possible to obtain amorphous sediments of pentazinc hexahydroxodicarbonate Zn5(CO3)2(OH)6 of stoichiometric composition with particle size, which does not exceed 50 nm, to simplify the process, reduce energy consumption and ecological load on the environment.

1 dwg, 3 tbl, 5 ex

 

The invention relates to a technology for major carbon zinc salts, which can be used as raw materials and intermediate products in the pharmaceutical, microelectronics, chemical, tire, paint and oil industries.

A known method of producing hydroxocobalamin Nickel by dissolving the specified metal in ammonium carbonate solution at elevated temperature and subsequent deposition of the desired product by distillation of the ammonia, and the dissolution of Nickel are in the presence taken separately or in combination with each other nitric acid, ammonium nitrate and Nickel content of nitrate-ion 2-50% with respect to the mass of dissolved metal [description of the invention to as. the USSR №1518307 from 16.10.1987, IPC4C01G 53/06, publ. 30.10.1989]. Because Nickel belongs to the d-metals of the fourth period of the periodic system of chemical elements of Mendeleev, and zinc, the present method can be successfully extended to zinc.

The disadvantages of this method include the variable composition of the finished product, the low productivity of the process, its frequency and low efficiency of each operation, the presence of large amounts of wastewater due to the necessity of washing the obtained precipitation from nitrate ions. In addition, the process which engages stage, flowing at elevated temperatures, resulting hardware complexity of the method and additional energy consumption.

Closest to the proposed method to the technical essence is a method of obtaining a basic carbonate salts, in particular zinc and its oxides, which comprises dissolving (as one of the stages of the process of chemical transformation) metal-containing compounds of zinc ammonium carbonate solution (as a particular case of an aqueous solution of carbon dioxide and ammonia) followed by the formation of the target product, filtering, drying, condensation and return of the gaseous products at the stage of dissolution, and as a metal-containing compound used is inactive (or rather coarse) zinc oxide [description of the invention to the patent of Russian Federation №2043301 from 25.06.1991, MPK C01G 3/00, C01G 3/02, C01G 9/00, C01G 9/02, C01G 51/04, C01G 51/06, C01G 53/04, C01G 53/06, publ. 10. 90.1995]. The result is improved performance of the continuous process stream due to the intensification of the process steps, it is possible to obtain active oxides. In addition, due to trapping gas emissions, the regeneration liquid effluent and re-use them in the process receive waste clean technology.

However, this method has significant drawbacks. P and the temperature increase of the process monohydrate ammonia decomposes and accordingly, changing the concentration of carbonate-ammonium solution, which leads to variability in the composition of the final product (so-called floating, non-stoichiometric composition). In the literature [see NS Nikolaev, V.V. Ivanov, A.A. Shubin. Synthesis of highly dispersed forms of zinc oxide: chemical precipitation and thermolysis. Journal of Siberian Federal University. Chemistry. 2010. series 3, No. 2, p.160-170] noted the existence of several forms of a basic carbonate of zinc, such as Zn5(CO3)2(OH)6(mineral hydrozincite), Zn3CO3(OH)4, hydrates Zn3CO3(OH)4·2H2O, Zn4CO3(OH)6·2H2O. So the finished product is a complex mixture of these substances.

In addition, the method is implemented at temperatures and pressures higher than ambient temperature and normal atmospheric pressure, resulting hardware complexity of the process and additional energy. At the stage of washing the finished product from the impurity cations and anions requires a large amount of water and its subsequent costly cleanup.

It is also known [see NS Nikolaev, V.V. Ivanov, A.A. Shubin. Synthesis of highly dispersed forms of zinc oxide: chemical precipitation and thermolysis. Journal of Siberian Federal University. Chemistry. 2010. series 3, No. 2, p.160 and 170]that the particle size of the primary carbonate C the NCA affects the size of oxide particles, resulting in the process of thermal decomposition. The process of evaporation in this way leads to the formation of coarse particles of carbonate and gidroksicarbonata zinc, and as a result of their thermolysis obtained, as shown by the results of x-ray phase analysis of coarse particles.

The problem solved by the present invention and the technical result achieved are obtaining amorphous precipitation gidroksicarbonata zinc Zn5(CO3)2·(OH)6(hexahydrobenzylcarbonate pentazine) stoichiometric composition with a particle size not exceeding 50 nm, and in simplifying the process, reducing energy consumption for its implementation and reducing the environmental impact on the natural environment.

To solve the problem and achieve the stated technical result in the production method of the main carbon zinc salts, including chemical transformation of metal-containing zinc compounds in an aqueous solution of carbon dioxide and ammonia, followed by the formation of the target product, filtering, drying, condensation and return of the gaseous products through chemical transformation, and as a metal-containing compound used coarse zinc oxide, chemical conversion of zinc oxide in a basic carbonate of the Inca is carried out in ammonium carbonate aqueous solution in a heterogeneous conditions at a molar ratio of carbon dioxide:ammonia equal to 1:(5 to 9) the temperature of 15-50°C and atmospheric pressure.

Thus, the method of obtaining basic carbonate salts of zinc (Zn) includes chemical transformation (dissolution) of the metal-containing zinc compounds in an aqueous solution of carbon dioxide (CO2) and ammonia (NH3(in ammonium carbonate solution), followed by the formation of the target product, filtering, drying, condensation and return of such gaseous substances, such as ammonia and small amounts of carbon dioxide into chemical transformations (dissolution), and as a metal-containing compound used coarse (inactive) zinc oxide (ZnO), chemical conversion of zinc oxide in basic zinc carbonate is carried out in ammonium carbonate aqueous solution in a heterogeneous conditions at a molar ratio of CO2:NH3equal to 1:(5-9), the temperature of 15-50°C and atmospheric pressure.

The results of x-ray phase analysis of the original and the synthesized compounds and the products of their thermolysis of illustrating the invention, are summarized in Tables 1 and 2 and presented in the diffraction pattern (see drawing).

The particle size of the ZnO crystallites was determined from the broadening of the form x-ray diffraction profile (see the diffraction pattern of ZnO powder). Based on the experimentally defined values true physical broadening of the line β (half-width d is fractional reflections from the analyte, grad), you can determine the average crystallite size D (nm), using equation Selyakova-sherrer:

D=Kλ/βcosθHKL,

where K - the coefficient of 0.94 for x-ray analysis;

λ is the wavelength of x-ray radiation (nm);

cosθHKLcosine of the scattering angle (dimensionless quantity).

Thus, the product of thermolysis of Zn5(CO3)2(OH)6obtained by dissolving zinc oxide in an aqueous solution of carbon dioxide and ammonia at a molar ratio of CO2:NH3equal to 1:(5 to 9)is zinc oxide with an average particle size equal to 10-50 nm.

Analyze the essential features of the invention.

Chemical conversion of zinc oxide in basic zinc carbonate is carried out in ammonium carbonate aqueous solution in a heterogeneous environment. Unlike the closest analogue where to get the homogeneous saturated solution of Aminatou of zinc and its subsequent evaporation with a selection of basic carbonates of zinc, of variable composition, in the present technical solution of the original solid crystalline zinc oxide is transferred to the solid basic zinc carbonate without getting saturated solution of Aminatou zinc. This greatly simplifies the technology by eliminating stages of evaporation and washing the precipitate. In addition, reduced environmental load of the surrounding nature is th environment. Remain constant with respect to the stoichiometric composition of Zn5(CO3)2(OH)6in crystalline form with a predominance of amorphous phase after thermal decomposition (thermolysis) allows to obtain a final product with a particle size of zinc oxide 10-50 nm. Such small particles have unique features and are used in the manufacture of components of semiconductor devices, electrical contact materials, UV filters, solar cells, sensors, catalysts, sorbents, and so on, in contrast to the properties of coarse particles known method [see RF patent №2043301], which do not possess such properties.

Heterogeneous chemical conversion of zinc oxide in basic zinc carbonate is carried out in an aqueous solution of carbon dioxide and ammonia at a molar ratio of CO2:NH3equal to 1:(5-9).

With decreasing molar relationship CO2:NH3the dissolution of zinc oxide in ammonium carbonate aqueous solution is less than 1:5, for example, 1:4.5 or below leads to the disappearance in precipitation of amorphous phase and enlargement of the particles in the crystalline phase, while increasing the molar ratio of the CO2:NH3more than 1:9, for example, 1:9.5 or above significantly increases the time of conversion of zinc oxide in basic zinc carbonate.

The results of the experiments and the following various molar ratios of CO 3and NH3summarized in Table 3.

Chemical conversion of zinc oxide is carried out at a temperature of 15-50°C. the temperature of the dissolution below 15°C 10°C and below, leads to a significant decrease in the rate of the process of obtaining basic zinc carbonate, and the temperature rises above 50°C 55°C or higher, leads to rapid decomposition of an aqueous solution of ammonia monohydrate and volatilization of gaseous ammonia, which changes the composition of the carbonate-ammonia solution and, as a consequence, the composition of the final product (non-stoichiometric composition of basic carbonate of zinc).

Chemical conversion of zinc oxide is carried out at atmospheric pressure. This pressure provides a stable and secure process that reduces energy consumption and simplifies its implementation in practice.

Implementation of the invention consider the following examples.

Example 1 (comparative). Getting gidroksicarbonata zinc Zn5(CO3)2(OH)6using homogeneous process.

The process is conducted at atmospheric pressure and a temperature of 25°C. In a reaction flask of 200 ml are placed hanging zinc oxide by weight of 1 g and the addition of ammonium bicarbonate by weight of 1.18, Then is added 100 ml of 0.24 M aqueous solution of ammonia. Included magnetic stirrer. Stirring is carried out for 2 hours the solution becomes homogeneous (pH 10,57). Next, the resulting solution was evaporated to 50 ml, and the reaction flask precipitation of basic zinc carbonate, which is separated by filtration and dried at 60°C for six hours.

As shown by the results of x-ray phase analysis, the precipitate is a mixture of coarse ZnCO3and Zn5(CO3)2(OH)6after thermolysis which is obtained ZnO with a particle size greater than 1 μm. The size was determined from the broadening of the form x-ray diffraction profile on the diffractometer DRON-2 (Cu K2- radiation, λ=1,54Å, graphite monochromator on the reflected beam) with a scanning speed of 2 deg/min

Homogeneous method proposed in the prototype, it is not possible to obtain basic zinc carbonate specified composition Zn5(CO3)2(OH)6and particles of zinc oxide with a size of 10-50 nm.

Example 2. Getting Zn5(CO3)2(OH)6in the heterogeneous conditions of the process of transformation with a molar ratio of CO2and NH3- 1:1.

The process is conducted at atmospheric pressure and room temperature. Hanging zinc oxide by weight of 2 g and ammonium hydrogen carbonate and 0.8 g placed in chemical beaker of 500 ml and add 200 ml of distilled water (molar ratio of CO2:NH3- 1:1). Stirring of the reaction mixture is carried out in such a way that th is would be solid ZnO and formed during the reaction the basic zinc carbonate were suspended. Experience time is 24 hours. The precipitate is filtered and dried at 60°C for six hours.

The results of x-ray phase analysis showed that the precipitate is crystalline Zn5(CO3)2(OH)6with a large particle size (see Table 2) from 10 to 100 μm. Particle size was determined using an optical microscope NU-2E.

Examples 3 and 4. Getting Zn5(CO3)2(OH)6in the heterogeneous conditions of the process of transformation with the recommended molar ratio of CO2and NH3.

The process is conducted at atmospheric pressure and room temperature of 20°C. a portion of the zinc oxide by weight of 0.5 g is placed in a chemical beaker (200 ml) and add 75 ml of distilled water. Stirring of the reaction mixture is carried out so that the solid zinc oxide and basic zinc carbonate were suspended. Later in the reaction mixture depending on experience type:

- the first option - 75 milliliters of binary aqueous solution of ammonium bicarbonate (NH4HCO3) and an aqueous solution of ammonia (NH3·H2O) with concentrations of 3,3÷10-2M and 13.2÷10-2M, respectively, the molar ratio of CO2:NH3- 1:5, experience time is 24 hours;

- the second option - 75 milliliters of binary aqueous solution of hydrocarb the Nata ammonia and aqueous ammonia with a concentration of 3.3÷10 -2M and 2.64÷10-1M, respectively, the molar ratio of CO2:NH3- 1:9, experience time is 48 hours.

The obtained precipitation was filtered and dried at 60°C for six hours.

The results of x-ray phase analysis shows that the sediments represent the crystal structure of Zn5(CO3)2(OH)6with small particle size from 20 to 50 nm and a high content of amorphous phase (see Table 3). The size was determined from the broadening of the form x-ray diffraction profile on the diffractometer DRON-2 (Cu K2- radiation, λ=1,54Å, graphite monochromator on the reflected beam) with a scanning speed of 2 deg/min

There is a possibility to use different molar ratio of CO2and NH3in the range between 1:5 and 1:9. The obtained crystal structures and their sizes will meet the stated requirements.

Example 5. Getting Zn5(CO3)2(OH)6in the heterogeneous conditions of the transformation process in pilot conditions.

In a reactor with a volume of 20 liters with anchor stirrer was placed 1 kg of zinc oxide (GOST 10262-73, qualification "H") and 0.4 kg of ammonium bicarbonate was then added to 16 l of an aqueous solution of ammonia with a concentration of 1.84 M (molar ratio of CO2:NH3- 1:7). The synthesis was carried out at a temperature of 20°C for 48 hours. The precipitate, after which Otdelenia from the mother liquor, dried at 50°C for 24 hours. The results of x-ray phase analysis shows that the sediment is crystals of Zn5(CO3)2(OH)6with small particle size and high content of amorphous phase. After thermal decomposition of the obtained crystal grains of zinc oxide with an average size of 20 nm.

Implementation of this technology on an industrial scale, for example, with basic carbon zinc salts in an amount up to 50 kg of above-mentioned conditions flow method proportionally increase.

As a result of implementation of the invention is substantially simplified way to obtain the primary carbon zinc salts of carbonate-ammonia solutions were obtained amorphous precipitation of gidroksicarbonata zinc stoichiometric composition and a particle size not exceeding 50 nm. Decreased energy consumption for the process. Decreased environmental burden on the environment.

Table 1
The results of x-ray phase analysis of the source connections
The research objectCard number database JCPDSHee is practical formula objects of study
Zinc oxide36-1451ZnO
The ammonium bicarbonate44-1483NH4HCO3

Table 2
The results of x-ray phase analysis of the synthesized compounds and the products of their thermolysis
The research objectCard number database JCPDSChemical formula of research objectsThe number cards solid product of thermolysis database JCPDSThe qualitative composition of the products of thermolysis
Basic zinc carbonate72-1100Zn5(CO3)2(OH)679-0205ZnO

Table 3
The results of heterogeneous chemical ol the rotation of zinc oxide in basic zinc carbonate
The molar ratio of CO2:NH3Qualitative and phase composition of the products of dissolution according to x-ray phase analysis
1:10Zn5(CO3)2(OH)6crystal structure with small particle size and the content of amorphous phase
1:9Zn5(CO3)2(OH)6crystal structure with small particle size and the content of amorphous phase
1:7Zn5(CO3)2(OH)6crystal structure with small particle size and the content of amorphous phase
1:5Zn5(CO3)2(OH)6crystal structure with an average particle size of
1:3Zn5(CO3)2(OH)6crystal structure with a large particle size
1:1Zn5(CO3)2(OH)6crystal structure with a large particle size

The method of obtaining the main carbon zinc salts, including chemical transformation of metal-containing compounds qi is the AC in an aqueous solution of carbon dioxide and ammonia, followed by the formation of the target product, its filtering, drying, condensation and return of the gaseous products through chemical transformation, and as a metal-containing compound used coarse zinc oxide, characterized in that the chemical conversion of zinc oxide in basic zinc carbonate is carried out in ammonium carbonate aqueous solution in a heterogeneous conditions at a molar ratio of carbon dioxide: ammonia = 1:(5-9), the temperature of 15-50°C and atmospheric pressure.



 

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2 dwg, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to cold curing epoxide compositions and can be used in making structures, including large-sized structures, from polymer composite materials by vacuum infusion in engineering fields. The epoxide composition includes an epoxide base containing epoxy-diane resin, an active diluent and a curing system based on an amine curing agent and a surfactant, characterised by that the epoxy-diane resin used is a resin or a mixture of resins with molecular weight 340-430, the active diluent used has viscosity of up to 0.1 Pa·s, the amine curing agent is a mixture of a curing agent basedd on an aromatic amine and a cold curing catalyst, and the curing system further includes a heterocyclic imidazole-type compound and a nanomodifier. The technical result is preparation of a high-technology epoxy composition, curable without the need for additional heat and without a large exothermic effect, and characterised by improved physical and mechanical properties.

EFFECT: composition is characterised by high modulus of elasticity of 3,8-4,2 GPa, which allows its use in making deformation-resistant articles from polymer composite materials with higher structural strength.

7 cl, 3 tbl, 12 ex

FIELD: medicine.

SUBSTANCE: group of inventions refers to medicine, particularly to magnetic nanoparticles for treating and/or preventing cancer, prepared of ferric oxides or pure iron containing an oxide-containing layer, wherein at least one therapeutically active substance is bound to said particles. Releasing at least one therapeutically active substance is caused or initiated, or accelerated substantially by a variable magnetic field.

EFFECT: group of inventions provides reducing the uncontrolled release of the therapeutically active substances during nanoparticle delivery to cancer cells.

13 cl, 11 ex

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