RU2368414C1 - Device for solid matter desublimation - Google Patents

Abstract

FIELD: process engineering.

SUBSTANCE: proposed device comprises two desublimators with orifices to feed desublimated product vapor and cold carrier gas. Aforesaid desublimators have vapor-gas distributed chambers with grates and sublimators, mixing chamber and ready-product separation units. Aforesaid horizontal mixing chamber has its lower part representing truncated part of a cylinder or cone, while upper part represents a variable-cross section box. Ratio of maximum-to-minimum cross sectional areas makes 1.25 to 2.

EFFECT: high-quality, finely- and ultra-dispersed mixes in products with volume not over 5 mg.

4 dwg, 1 tbl

Description

Technical field

The invention relates to desublimation technology and can be used in the chemical and pharmaceutical industries to obtain a mixture of finely and ultrafine materials in small volumes of the product.

State of the art

A device for fractional desublimation of solids from a mixture of gas with vapors [Application 3730747 Germany 4, B01D / 00. // publ. in B.I. No. 20 dated March 30, 1989]. The device is a cylinder-conical apparatus, in the lower part of which are placed nozzles for supplying steam of a desublimated product. These nozzles are located parallel to the axis of the apparatus. There is another row of nozzles for supplying cold gas mounted on the side wall of the apparatus. Nozzles placed on the side wall of the device are inclined to the axis of the device at an angle (0.17-0.75) π radians. The device is equipped with an additional apparatus or unit for separating solid desublimated particles and gas flow.

The disadvantage of this apparatus is the inability to obtain a mixture of finely and ultrafine materials in small volumes of the product.

Closest to the proposed invention in technical essence and the achieved result, i.e. the prototype is a device for desublimation of solids [RF Patent No. 2229918 publ. in B.I. No. 16 dated 06/10/2004], which includes two desublimators with openings for supplying steam of a desublimated product and cold carrier gas, equipped with steam and gas distribution chambers with gratings and sublimators, knots for separating the finished product and a mixing chamber, in the lower part of which there are slotted openings with guides, moreover, on one wall of the chamber they are located at identical angles to the axis of the apparatus in the range of 30 ° -75 °, and on the opposite wall - at different angles increasing from 30 ° to 75 °.

The disadvantage of the prototype is the inability to obtain a high-quality mixture of finely and ultrafine materials in product volumes of up to 5 mg.

SUMMARY OF THE INVENTION

The inventive task was to create a device for desublimation of solids, which would allow to obtain a mixture of finely and ultrafine materials in product volumes up to 5 mg.

This object is achieved in that the device for desublimation of solids includes two desublimators with holes for supplying steam of the desublimated product and cold carrier gas, equipped with steam and gas distribution chambers with gratings and sublimators, a mixing chamber and units for separating the finished product, while the mixing chamber is horizontal the lower part of the chamber is a truncated part of the cylinder or cone, and the upper is made in the form of a box of variable cross section, and the ratio of the areas the maximum and minimum sections is 1.25-2.

Information confirming the possibility of carrying out the invention

Figure 1 presents a front view of a device for desublimation of solids.

Figure 2 presents a view A, including a side view of the device, and a device for separating the finished product, including a filter and a collector of the finished product, as well as sections A-A and B-B, which show sections of the mixing chamber having a maximum and minimum cross section, respectively .

The device for desublimation of solids contains two sublimators 1, 2, two steam and gas distribution chambers with gratings 3, 4 and two desublimators 5, 6 connected tangentially by their upper parts to the lower part of the displacement chamber 7 located horizontally, as well as a device for separating the finished product, including filter 8 and the finished product collector 9. In the lower part, the mixing chamber is a truncated part of the cylinder or cone, and the upper one is made in the form of a box of variable section, and the ratio of the areas th and minimum sections is 1.25-2.

The device operates as follows.

For example, phthalic anhydride and benzoic acid, respectively, are loaded into sublimators 1, 2. The resulting vapor of phthalic anhydride and benzoic acid enters the gas distribution chambers 3 and 4. Next, the vapor of the corresponding substances enters the desublimators 5, 6. The vapor of phthalic anhydride and benzoic acid is mixed with a cooling agent (air). As a result, phthalic anhydride is obtained at the outlet of the desublimator 5, and benzoic acid at the outlet of the desublimator 6.

The consumption of cold air is 3.2 m ³ / hour. The particle size of phthalic anhydride and benzoic acid at the outlet of the corresponding desublimators was (5-12) microns and (10-27) microns, respectively.

The temperature of the gas-solid particle flows at the outlet of the desublimators 5, 6 is about 31 ° C. Then, gas-solid particles flows are introduced tangentially into the lower part of the mixing chamber 7. Pre-mixing of desublimated products occurs. The final mixing is performed when the gas-solid particles flow in the horizontal section of the mixing chamber due to disturbances received by the stream when moving it from the section of the maximum section of the box part to the minimum and vice versa. The resulting mixture is discharged from the mixing chamber and enters the filter 8 and the finished product collector 9.

The table shows the results of the analysis of individual samples taken from the finished mixture.

Mixture composition Sample number one 2 3 four 5 The average concentration,% Phthalic anhydride 53.7 54.8 55,2 52.8 53,2 53.94 The deviation of the content in the sample from the average value,% -0.24 0.86 1.26 -1.14 -0.74 Benzoic acid 46.3 45,2 44.8 47.2 46.8 46.06 The deviation of the content in the sample from the average value,% 0.24 -0.86 -1.26 1.14 0.74

The weight of the sample is 5 mg. The analysis was performed on a SPECORD-M 40 spectrophotometer.

The proposed device allows to obtain fine and ultrafine mixtures of high quality. The effect of high-quality mixing is achieved at a sample level of 5 mg.

Claims (1)

A device for desublimation of solids, comprising two desublimators with openings for supplying steam of a desublimated product and a cold carrier gas, equipped with steam and gas distribution chambers with gratings and sublimators, a mixing chamber and units for separating the finished product, characterized in that the mixing chamber is horizontal, while the bottom part of the chamber is a truncated part of the cylinder or cone, and the upper one is made in the form of a box of variable section, and the ratio of the maximum areas to imalnogo cross sections of 1.25-2.

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