Method of stabilization of alkali metals peroxisalts and a device for its realization

FIELD: chemical industry; a method and a device of alkali metals peroxysalts stabilization.

SUBSTANCE: the invention is intended for a chemical industry and may be used at production of oxygen-containing bleaching agents and synthetic detergents. In the vacuum drier 3 supplied with a rake-type rabble 10 and a weight-measuring device 12, the main original material is supplied from a reserve tank 1. Then it is vacuumized simultaneously with the solution of a coating material located in a measuring container 17, connected by lines 21, 22 and 13 with the device of a dryer 3 vacuumizing. Then mix the main original material with the solute of the coating material at a residual pressure of no more than 13.33 kPa. Increase the pressure in the vacuum drier 3 up to the atmospheric pressure or exceeding it by no more than 10 kPa spasmodically by an air supply from a source 28. The produced product is exposed to a vacuum drying up to the required moisture, making control of the moisture content by a change of the weight of the dryer 3 contents with the help of the weight-measuring device 12. Stability of the finished product is 59.0-69.0 %, consumption of the coating material - 0.9-1.8 mass %, the share of the active oxygen - 13.8-14.4 mass %.

EFFECT: the invention ensures production of oxygen-containing bleaching agents and synthetic detergents.

10 cl, 1 dwg, 2 tbl

 

Group of inventions relates to the chemical industry and can be used to obtain oxygen-containing bleaching products on the basis of peroxisome alkali metals (hereinafter proxool), such as, for example, peroxosulfates sodium carbonate, peroxosulfates borate of sodium, which are also used as components of synthetic detergents (CMC);

Using peroxisome as components of CMC is limited by their lack of stability during storage, especially under conditions of high temperature and humidity, in the presence of aggressive (aluminosilicate) of CMC components. Especially melatonin is peroxosulfates sodium carbonate (hereinafter CRC), which even at room temperature and without air loses 2/3 of its initial content of active oxygen (AK) after one year, at 100°With through the day.

The main factors causing the loss of active oxygen in peroxisome are, along with high temperature and humidity, in the first place, impurities of heavy metals (salts, oxides)that fall into particles peroxysalts of feedstock in the synthesis process or components of the CMC because of its chemical nature. Therefore, the most important criterion chemical stability peroxone is maintaining the content of active oxygen (AK) as in the conditions is x storage under normal conditions, and in compositions CMC.

Exposure to aggressive environments and adverse weather conditions is compensated by using a large number of chemicals (organic and/or polymeric compounds, aqueous solutions of neutral salts of alkaline or alkaline earth metals, acids etc)that add to the original solutions in the process of obtaining peroxisome or to the finished product as a protective coating material on the particles.

The desirability of use in the detergent compositions of peroxisome coated, especially PKN, has acquired great importance in recent years, given recent in industry for the production of detergents tend to use in detergent compositions more aggressive components such as aluminosilicate components (zeolite), the effect of which is usually compensated by the use of large quantities of coating reagent (encapsulation) to 7-12% weight/weight. The initial contents of the AK in this case is reduced, which is undesirable as to achieve the desired whitening effect requires the use of additional quantities peroxysalts, which increases the cost of the CMC.

Known method of stabilizing particles PKN, namely, that on the fine material in a continuous flow centrifugation his chere the C region is continuously generated mist is applied to the molten coating material (WO No. 93/04982, IPC 01 15/10, publ. 1993).

Known method of stabilizing PKN applying the coating material sprayed onto the particles of the aqueous solution covering the reagent mixing in the mixer and subsequent drying in a fluidized layer, and the coating is applied during the many aisles of processed particles through the mixer and separate dryer (RU # 2137704, IPC 01 15/10, publ. 1999).

Closest to the proposed invention is a method of stabilizing PKN by spraying the particles of aqueous coating material (magnesium sulfate or chloride of magnesium, calcium, strontium or barium) from the calculation of 0.07 to 0.3 mol per mol PKN. Thus treated PKN dried for 42 hours at 50°and a residual pressure of 3 mm Hg (us No. 4325933, IPC 01 31/00, 01 15/037, publ., 1982).

It is also known a device for applying coating material to the solid particles peroxysalts, of an alkali metal containing mixer, the feed system of the particles of source material, including the cumulative capacity of the metering device, the delivery system solution covering material comprising a measuring container with a metering device and a vacuum dryer (US No. 4325933, IPC 01 31/00, 01 15/037, publ. 1982).

Known methods and devices do not deliver the desired quality of product due to technological N. the preparation of processed particles to the coating roll coating. Initial particle peroxysalts have developed porous structure and contain air, flue gases used in their production process, which occupy 40-65% of the inner volume of the particle. The oxygen present in the air together with the residual capillary moisture create a constant internal tension in capillary-porous body of the core particles with the coating. If the surface layer is non-uniform moisture through the pores of the coating material supplied to the inside of the particles, is connected with the capillary moisture and together with oxygen to decompose the product. If the coating material forms a continuous homogeneous layer, with increasing core temperature of the air inside the kernel expands and breaks the capillary-porous body core. This greatly increases the area of contact with the external moisture, which in result leads to decomposition of the product.

The technical result of the proposed method and device is to increase the stability of peroxisome with a protective coating.

This technical result is achieved by the fact that in the known method of stabilizing peroxisome by mixing solid particles of the base material with a solution of coating material and subsequent vacuum drying before mixing the core material and the coating solution mA is Arial subjected to separate evacuation, the main material vacuum while heating to 55°and the mixing is carried out initially in vacuum with subsequent stepwise raising the pressure to atmospheric or redundant. In addition, a solution of coating material use amount 0,215-0,235 volume of the base material. In addition, the vacuum at all stages is carried out at a residual pressure of not more than 13,33 kPa mainly in 0,67-4,6 kPa. In addition, raising the pressure to atmospheric or excessive exercise during the time period in the range of 0.5-1.0 minutes, and the excess pressure is not greater than 10 KPa.

This technical result is also achieved by the fact that in the known device for applying coating material to the solid particles peroxysalts, of an alkali metal containing the delivery system of particles of the base material, including the cumulative capacity of the metering device, the delivery system solution covering material comprising a measuring container with a metering device, and a vacuum dryer, storage capacity for particles of the base material and a measuring container for mortar coating material is communicated with a vacuum dryer, a vacuum dryer equipped with a stirrer system and a compressed air supply, a measuring container for mortar coating material is connected to the vacuum system the vacuum with the Shilka and compressed air. In addition, vacuum dryer has a cylindrical shape and is horizontal. In addition, the mixer vacuum dryer is grabavoy. In addition, vacuum dryer equipped with a weighing device.

Proxool in the form of particles, which is suitable for stabilization according to the present invention can be manufactured using any known process. The kernel (core) particles peroxysalts may include various additives in a wide range of shared content in accordance with known theoretical and practical knowledge. As the coating material may be used any known stabilizing reagent or a mixture, soluble in water, the concentration of a stabilizing agent selected from a calculation that it would obtain coverage at least 0.8 weight/weight%.

The drawing shows a diagram of the device for stabilizing peroxisome on the proposed method.

The device includes an accumulation tank 1 to the base material installed at the exit gate 2; horizontal vacuum dryer 3 has a cylindrical shape with an inlet pipe 4 and outlet pipe 5, provided with a jacket for heating inputs 6,7 and outputs 8,9, horizontal grabavoy mixer 10 with the actuator 11 and weighing device 12; working on the awn vacuum dryer 3 is connected to a vacuum system (not shown) in line 13, equipped with manovacuummeter 14 and the shut-off valve 15; a vacuum dryer 3 connected to a storage tank 1 for granular material in line 16; the device also includes a measuring tank 17 for a solution of the coating material, which is equipped with a shut-off valve 18 installed at the inlet into the measuring tank through the line 19 and is connected to the vacuum system consistently over the line 20 with shut-off valve 21 and lines 22 and 13, and with a vacuum dryer 3 through the outlet 23 with shut-off valve 24 in line 25; in addition, on lines 22 and 26 with shut-off valve 27 measuring capacity 17 is also connected with a source of air supply 28 and to the input socket 4 vacuum dryer 3. The device is also equipped with monovakuumetr 29, mounted on the line 20, the sensor 30 for liquid mounted in a measuring tank 17 and the transmitter 31 for bulk materials installed in the storage tank 1.

The stabilization of the particles peroxysalts, of using the proposed device is as follows: in the accumulation tank 1 of the production cycle the peroxysalts heated core material in the form of particles and/or granules with a diameter of 100-1200 μm, preferably with a diameter of 600-1000 μm, the filling of the measuring vessel 1 is controlled by the sensor 31. When closed, the shut-off valve 24 through the open valve 2 in line 16 of bulk products is served in a vacuum dryer 3 in volume, not exceeding 50% of its internal volume, the weight of the submitted product is fixed weighing device 12. A solution of coating material selected concentration, containing one or more reagents, line 19 through the open shut-off valve 18 is fed into the measuring container 17 amount 0,215-0,235 volume of the base material filed in a vacuum dryer 3. The filling of the measuring vessel 17 is controlled by the transmitter 30. In the jacket of the dryer 3 serves coolant temperature 40-55°C.

Shut-off valves 18, 27 and the valve 2 is closed and the shut-off valves 15 and 21 open. Include a vacuum system and, when working grabavoy the mixer 10 through 13 vaccum working cavity vacuum dryer 3 and simultaneously measuring tank 17 with a solution of coating material. When the preset residual pressure, controlled by monovakuumetr 14 and 29, monitor the reduction of weight of the contents of the vacuum dryer 3 weighing device 12. Upon reaching the calculated mass, opens the shutoff valve 24 and line 25 through the inlet 4 into the vacuum dryer 3 from the measuring tank 17 is fed a solution of coating material. After 3-5 minutes of intensive mixing of the contents of the vacuum dryer 3 are closed, the valves 15, 21 and 24, opens the shutoff valve 27 and from the source 28 through line 26 for the period BP is like 0.5 to 1.0 minutes, fill the air the whole system devices working in vacuum mode, raising the pressure to atmospheric or excess is not more than 10 kPa. This process is controlled by manufacyurer 14. The result is an abrupt pressure rise in the vacuum dryer 3 creates a pressure differential between the pressure in the inner cavity of the engine and the pressure on the outer covering of the shell of the particles in the dryer. Then close the shutoff valve 27 to open the valve 15, and the system again vacuumized for drying particles coated with stirring. The drying process intensify heated by coolant temperature 40-55°With a shirt in a vacuum dryer 3 and controlled by changing the mass of the contents of the vacuum dryer 3 by means of the weighing device 12. When reaching into the product of a given moisture content, turn off the vacuum system, open the valve 27 and fill system of the device, the gas or air from a source 28, raising the system pressure to atmospheric. Through the flanged outlet 5 vacuum dryer 3 ready stabilized particles served in the receiving tank for the finished product (not shown) and sent for packing. Close the valve 27 to open the valve 2 and the device is ready for the next cycle.

In the pumping process with simultaneous heating of the interior is Anna core cavity of the treated parts are the air, flue gases, impurities of heavy metals other volatile gases and part of the capillary and crystallization of moisture. Thus, particles peroxysalts, prepare for the next technological step - coating the surface of particles of the coating material by mechanical mixing of the particles peroxysalts, with a solution of coating material in a vacuum, as the vacuum is sharply reduced chemical activity of oxygen in the oxidation of metals.

The difference between the pressure in the inner cavity of the core particles (granules) and the pressure on the outer side of the covering material promotes uniform distribution of coating material on the surface of the particles and fixed by pressure to the entire surface area of the particles and the mutual adsorption between the core material particles and a covering material in a partially filled capillary channels. Moreover, the unfilled part of the capillary channels of the particle remains under vacuum and thus relieves the internal stress of the particles, which reduces the surface area. The processes lead to a decrease of hygroscopicity of peroxisome and preservation of their oxidative activity on the source level for a long time.

The process of stabilization of peroxisome according to the invention allows significant is entrusted to increase their stability, due to the removal from the gas and capillary moisture, instead of which partially penetrates the mortar coating material (stabilizing solution), which forms a strong coating that prevents access of air and moisture inside the kernel from the outside.

Table 1 presents the test results confirming the effectiveness of the proposed method and device for example, stabilization of PKN obtained by the method described in patent RU No. 2164215.

The stability of the samples was estimated by the method of EATING 10005, by comparing the content of AK in the original and stabilized materials before and after the test in the climatic chamber, by mixing with the zeolite in a ratio of 50/50 and aging at a temperature of 32°C and a relative humidity of 80% within 48 hours.

The content of AK in the samples was determined by the method EAT 07278.

Table 2 presents comparative qualitative characteristics of PKN stabilized according to the invention and a known manner by spraying a solution of coating material in a fluidized bed. As a coating material was used a solution of sodium sulfate. The table shows the average test result of 10 samples.

The dissolution rate PKN, stabilized by the proposed method, according to the international standard contact to JSO 311123-1976 high, the time ratio is eastwoodiae dissolution of 90% of the sample, does not exceed 2.5 minutes.

From the data presented in tables 1 and 2, it is seen that using the proposed method and device for stabilizing peroxisome alkali metals can improve their stability in comparison with known methods for 5-10 units to reduce the consumption of covering material in 3-5 times and to maintain a high initial concentration of active oxygen in the product.

Table 2
IndicatorsSource PKNPKN stabilized
According to the inventionAccording to the method
Mass fraction of active oxygen, % (average)13,613,811,8
The average particle size, microns650-950650-950670-1100
Wt. the proportion of sodium sulfate, %-0,9-1,83,6-4,5
Wt. fraction of moisture, %2,00,8-1,00,8-1,0
Bulk density, g/DM312141200-12101210-1310
Stability5559-69 (in Russian)53-56

1. Method one hundred and the waste utilization technologies of peroxisome alkali metals by mixing solid particles of the base material with a solution of coating material and subsequent vacuum drying, characterized in that before mixing the core material and the coating solution of the material subjected to separate the vacuum, and the main material vacuum while heating and mixing is carried out initially in vacuum with subsequent stepwise raising the pressure to atmospheric or redundant.

2. The method according to claim 1, characterized in that the evacuation of the base material lead when heated to 55°mainly to 40-50°C.

3. The method according to claim 1 or 2, characterized in that the lifting of the pressure to atmospheric or excessive exercise during the time period in the range of 0.5-1.0 min, while the pressure not greater than 10 kPa.

4. The method according to claim 1, characterized in that the solution of coating material use amount 0,215÷0,235 volume of the base material.

5. The method according to claim 1, characterized in that the vacuum at all stages is carried out at a residual pressure of not more than 13,33 kPa, mainly when 0,67÷4,6 kPa.

6. Device for stabilizing peroxisome alkali metals in the form of solid particles containing the delivery system of the base material, including the cumulative capacity of the metering device, the delivery system solution covering material comprising a measuring container with a metering device and a vacuum dryer, characterized in that the cumulative capacity is ü for the base material and a measuring container for mortar coating material is communicated with a vacuum dryer, and vacuum dryer equipped with a stirrer system and a compressed air supply.

7. The device according to claim 6, characterized in that the measuring container for mortar coating material is connected to the vacuum system vacuum dryer and compressed air.

8. The device according to claim 6 or 7, characterized in that the vacuum dryer has a cylindrical shape and is horizontal.

9. The device according to claim 8, characterized in that the mixer vacuum dryer is grabavoy.

10. The device according to claim 6 or 7, characterized in that the vacuum dryer equipped with a weighing device.



 

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