The method of processing sahamalaza

 

(57) Abstract:

Describes the method of processing crystalline sahamalaza, including the processing of crystalline material in the fluidized bed, with additions of water at a content of 20-50 wt.% material within the processing time up to 4 h, followed by drying of the crystalline material, while he pseudogiants, and the fluidization is achieved through the upward flow of carrier gas, and the method is carried out at a temperature of 25-35°C. the Technical result - the formation of solid crystalline sahamalaza having high fluidity (flowability) and improved appearance. 3 C.p. f-crystals, 2 tab.

The present invention relates to the production of solid crystalline sahamalaza having high fluidity (flowability) and improved appearance.

Sahamalaza (4-chloro-4-deoxy - D-galactopyranosyl-1,6 - dichloro-1,6-dideoxy- -D - fructo-furanoside, otherwise known as 4,1',6'-trichloro-4, 1', 6'- trimethoxysilane sucrose) is a strong podslushivaet first described in patent GB 1543167. Crystal sahamalaza in the form of orthorhombic needles was described in the patent GB 2065646 A. the Problem with the crystalline materials of this tee is nnow structure, it is thus difficult to transfer from one container to another. Even in the laboratory under strict control is difficult to obtain a freely-current sahamalaza, and in terms of large scale production, the problem is complicated by the fact that the equipment for further processing, such as pumps, centrifuges and dryers, tends to destroy the crystals, thus additionally reducing performance fluidity (flowability). Thus, there is a need to get clean sahamalaza having a modified structure with high fluidity (flowability).

The state of flow of solids is usually assessed from the point of view of the flow velocity, as well as from the point of view of the angle of repose poured material. In the "Bulk Solids Handling: An Introduction To Practice And Technology", C. R. Woodcock and J. S. Mason, Leonard Hill, July 1987, page 31, the state of flow of solids in the form of particles roughly classified according to the angle of repose as follows:

25-30overy free-flowing,

30-38ofree-flowing,

38-45oaverage,

45-55osleepy,

more than 55omuch sleepy.

This shows that free-flowing Armenia is to receive sahamalaza, having the angle of repose is usually less than 40oand preferably within 34-38o. The state of the thread (flowability) of the solid substance in the form of particles can also be directly measured using a funnel, in which the material sample clock when it pours through the funnel of known dimensions (as described below with reference to examples, but also in CIT. the work of the "Bulk Solids Handling").

It was found that the crystalline sahamalaza obtained directly at the final stage of crystallization of the synthesis process, can be processed by a simple operation using standard equipment to provide greatly improved flow characteristics. The nature of the changes occurring in the material seems to be relatively complex and changing. It seems that processing removes small particles and modifies the size and shape of individual crystals, providing a more narrow distribution of particle sizes, and the crystals become more dense, more cubic shape. The treated product may actually have a larger overall size of the particles, but not always. In particular, it should be noted that the method is not a method of agglomeration, in which small particles SL is the buy provides a method for processing crystalline sahamalaza to remove small particles and modifying the size and shape of individual crystals thus to reduce the angle of repose and increase fluidity (flowability), including processing of crystalline material in the fluidized bed at ambient temperature with addition of water, followed by drying of the crystalline material, while he pseudogiants. Usually fluidization is achieved by the upward flow of the respective carrier gas, usually air. The method can be carried out in conventional dryers fluidized bed and granulators, for example, MP2 (firm Niro Limited"), which consists of four main areas:

the inlet of the air conditioning system;

modular (standard) containers for the above purposes;

dosing fluid; and

the exhaust system.

The drying air pumped by the fan through the inlet filter and heated, passing it over steam heat exchanger. Temperature control is carried out by mixing hot air from the heat exchanger with the ambient air through the valve.

Sahamalaza placed in the container for a product and pseudogout in a stream of warm air. In fluidized bed spray water using two nozzles for liquids that are put in place which give to the nozzle using a peristaltic pump. Pumped out the air passes through the filter to prevent the product from working chamber. The quantity of water added and the processing time can vary in a relatively wide range to provide the product with specific properties. In General, water should be supplied with the content of 20-50%, preferably 25-40%, more preferably 25-30 wt.% material during the treatment period lasting up to 4 hours, usually from 15 minutes to 2 hours, for example, from 1 to 1.5 hours at a temperature in the layer, say, 25-35oC, for example, about 30oC before the final stage of drying.

Preferably sift the source material in order to remove particles of non-standard sizes, and are usually the source materials have an average particle diameter of 100-200 m, the coefficient of variation (CV) of particle size is at least 48% (although a material with a coefficient of variation as low as 44% can still be improved), and the angle of repose equal 38-48o.

As described in Crystallisation, 3rd Edition, J. W. Mullin, Butterworth and Heinemann, 1993, distribution of particle size (P SD) (particle size) can usually be classified an average particle size and coefficient of variation. Coefm indicator associated with a standard deviation curve of the Gaussian distribution, and is usually expressed in percent:

< / BR>
Values of L84%, 5050%%(= Lmand L16%can be obtained from the curve of the average mass distribution. The higher the CV value, the wider the distribution, CV= 0 means the distribution of particles of only one size. The CV curve of the Gaussian distribution is 52%, but the product coming from the crystallizer for sugar, which is usually more appropriate distribution of the gamma function has a CV of about 50%.

Granulometric composition was measured using scattering of the laser beam, using the device Malvern Mastersizer.

For example, conducted a series of experiments using four different source materials - SMI SM2, SM3, SM4, usually weighing about 12 kg In Examples 6 and 10 shows the results of experiments, which used a smaller number of source materials, but added more water.

Angle of repose was measured as angle of repose poured material (i.e., the angle between the horizontal base and an inclined side conical mounds, formed after the material carefully poured through the funnel on a flat powernoise 25 mm and a diameter of 22 mm

A timer.

Procedure:

1. Put the funnel into the holder so that the upper part of the rod was at a distance of 20 cm above the table.

2. Weigh 50 g of the sample in a clean, dry 500 ml chemical glass.

3. The bottom of the funnel closed with a cap and put weighed sample into the upper part of the funnel. Under the stem of the funnel fills the glass.

4. Remove the cover and start to record the time during which the sample passes through the rod. Repeat this measurement two more times and record the average value of the three chronometrically.

5. If some part of the sample remains stuck to the funnel, then record the mass of the sample that has passed through the rod. Thus determine the amount of sample remaining in the funnel.

6. If the sample is not spilling across the web, then you can knock on the upper part of the funnel. If the sample will begin to pour through the funnel timing should be repeated lightly tapping on the top of the funnel. Necessarily make a record of what tapping is produced. If the material does not pass through the funnel even after tapping, you make a record that the material is not friable.

In nnye according to Examples 1 to 11.

From the results of that processing can significantly reduce the angle of repose and provides good characteristics of the material yield strength. In addition, the resulting product is usually a brilliant crystalline material, bright colors, reminiscent of powdered sugar (fine sugar).

1. The method of processing crystalline sahamalaza, including the processing of crystalline material in the fluidized bed, with the addition of water at a content of 20 to 50 wt.% material within the processing time up to 4 h, followed by drying of the crystalline material, while he pseudogiants, and the fluidization is achieved through the upward flow of carrier gas, and the method is carried out at a temperature of 25 - 35oC.

2. The method according to p. 1, in which water is added at a content of 25 to 40 wt.% material within the processing time from 15 min to 2 h

3. The method according to p. 2, in which water is added at a content of 25 - 30 wt.% material within a processing time of 1 - 1.5 hours

4. The method according to any of paragraphs.1 to 3, in which the original material has an average diameter of 100 to 200 μm, coefficient of variation (CV) size part, at least 48% and

 

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