Method of obtaining loose powder, containing one or several glycin-n,n-diacetic acid derivatives, and application of loose powder for obtaining pressed agglomerates

FIELD: chemistry.

SUBSTANCE: invention relates to a method of obtaining loose powder, containing one or several glycin-N,N-diacetic acid derivatives of general formula VOOC - CHR - N(CH2COOM)2 (I), from a water solution as an initial material, containing one or several glycin-N,N-diacetic acid derivatives, which is dried by a method of spray drying with the air supply. The method is characterised by the following: the water solution contains one or several glycin-N,N-diacetic acid derivatives in a quantity of ≥84 wt % counted per the total weight of the dry substance. Spray drying is carried out in a drying apparatus, into which the water solution and air are supplied in a continuous-flow mode with the difference of temperatures between the water solution and air in the range from 70 to 350°C. The water solution is dispersed in the drying apparatus with the formation of tiniest liquid drops by its supply onto one or several discs, rotating at a linear rate of ≥100 m/s, or by the creation in it of absolute pressure ≥20 bar by a pump and its supply under the said pressure into the drying apparatus through one or several nozzles. In formula (I) R stands for an alkyl group with the number of carbon atoms from one to twelve and M stands for an alkali metal. The invention also deals with the application of the claimed loose powder for the production of pressed agglomerates, which can be used in solid or liquid cleaning means.

EFFECT: claimed method makes it possible to obtain the powder, possessing good bulk weight, flowability and storage stability.

13 cl, 3 ex

 

The invention relates to a method for producing a free flowing powder containing one or more derivatives of glycine-N,N-luxusni acid, and to the use of loose powder to obtain the pressed agglomerates, as well as the application of pressed agglomerates in solid or liquid detergents, in particular when getting tablets for dishwashing machines.

To obtain a detergent, in particular detergents for textiles, or cleaning agents, in particular detergents for dishwashing machines, can be selected solid or liquid compositions.

Detergents or cleaning agents contain, as a rule, the complexing agents ions iododecane and heavy metals. As such most commonly used derivatives of glycine-N,N-luxusni acid.

Used in the form of loose powders that are formed by synthetic aqueous solutions by the method of spray drying. Such bulk powders should have a higher bulk mass, often in the range from about 0.3 to 0.7 kg/l, and they must have residual moisture in a relatively narrow range of concentrations from about 4 to 8% water in order to be stable during storage, and to ensure that they can be used in subsequent manufacturing operations, representing the pererabotka in extruded agglomerates. Bulk powders with a higher water content too quickly turn into lumps, while free-flowing powders with a lower water content are difficult processing.

In addition, bulk powders should have good flowability.

It is known that bulk powders are formed in the form of particles of various shapes, in particular they can be in the form of hollow spheres, which, depending on wall thickness, can be crushed, they can also be in the form of solid balls or needles.

Hollow beads as solid balls are especially good flowability and the desired high bulk weight in the range from approximately 0.5 to 0.7 kg/l, in particular even when they are in the form of fragmented hollow balls and is ideal for obtaining compact products. Needles, of course, also suitable for obtaining compact products, but they have poor flowability and too low a bulk density ranging from about 0.2 to 0.5 kg/l Solid balls have a high bulk weight and good flowability, but they are not suitable for derivation of these compact products.

Consisting of complexing agents, in particular derived from glycine-N,N-luxusni acid in the form of individual compounds or a mixture of glycols in an amount of from 2 to 10%, bulk powders are pressed between two rolls or die-stamping pre is yourself then they are crushed and fractionary order to obtain the pressed agglomerates.

Extruded agglomerates normally have to have a certain particle size, in particular in the range from about 0.3 to 1.6 mm, which corresponds to an average particle size in the range from approximately 0.6 to 0.7 mm, and we need to ensure that all substances used in the following technological operations, representing pressed into tablets for dishwashing machines have a similar size. This is necessary for uniform mixing of all of the substances and, in particular, to prevent their separation when getting tablets for dishwashing machines.

The present invention was to develop a method, in accordance with which it is possible on an industrial scale to obtain free-flowing powders that match the above requirements.

The solution presents a way to obtain a free flowing powder containing one or more derivatives of glycine-N,N-luxusni acid of General formula (I)

MOOC-CHR-N(CH2COOM)2(I ),

where

R means an alkyl group with the number of carbon atoms ranging from one to twelve and

M means an alkali metal,

from the aqueous solution as a source material containing one or more derivatives of glycine-N,N-luxusni acid, which is dried by the method of spray drying with an air supply, the method differs in that the aqueous solution contains one or more derivatives of glycine-N,N-luxusni acid in quantities of ≥84 wt.% based on the total weight of dry matter, and the fact that the spray drying is carried out in a drying apparatus, in which an aqueous solution and the air fed into the once-through mode with the temperature difference between the aqueous solution and the air in the range from 70 to 350°C, while the aqueous solution is dispersed in the drying apparatus with the formation of tiny liquid droplets by filing one or more disks rotating at a linear speed ≥100 m/s, or by creating it with a pump absolute pressure ≥20 bar and feed it when the pressure in the drying apparatus through one or more nozzles.

It was found that this method can be obtained free-flowing powders containing one or more derivatives of glycine-N,N-luxusni acids, which are not only very good properties, toadies to loose weight, flowability and stability during storage, but in addition to excellent ability to undergo compaction with the formation of the pressed agglomerates with the desired high strength and, consequently, with a low degree of abrasion.

Unexpectedly it was found that the strength of pressed agglomerates dramatically improved in the case where for getting them, use appropriate present invention is free-flowing powders, which are formed from aqueous solutions containing one or more derivatives of glycine-N,N-luxusni acid in pure form, i.e. with a low content generated during their synthesis side component, obtained from aqueous solutions, which contain one or more derivatives of glycine-N,N-luxusni acid in quantities of ≥84 wt.% based on the total weight of dry matter.

For this purpose, in particular, suitable derivatives of glycine-N,N-luxusni acid obtained according to the patent application Germany No. And 4319935 as a result of interaction of the corresponding 2-alkyl - or 2-alkenylphenol or 2-alkyl - or 2-alkenylsilanes or double glycinol formula

or double glycinamido formula

by reaction with formaldehyde and hydrogen cyanide is m or with alkali metal cyanide, or by the reaction iminodiacetic acid or iminodiacetonitrile with relevant monolithically or dialdehyde formula OHC-And-SNO and with cyanide or alkali metal cyanide and subsequent hydrolysis of the available nitrile groups to carboxyl groups.

In addition, corresponding to the invention of a method implemented in a drying apparatus, which in the preferred case, operate so as to achieve a free-flowing powder with a high content of hollow spheres and/or fragmented hollow balls.

This is achieved by rapid drying when entering the drying aqueous solution and used for this purpose, hot air install a large temperature difference, providing a rapid entrainment of the solvent, and due to the fact that drying is carried out in a drying apparatus, including devices that crush coming on spray drying an aqueous solution into very fine droplets with the size of the droplets in the range from 20 to 100 microns.

Required for this temperature for evaporation is achieved by the fact that an aqueous solution and used for drying the air supplied to the drying apparatus with a temperature difference ranging from about 70 to 350°C, in the preferred case in the range from about 150 to 250°C.

In particular, the aqueous solution has a temperature of from about 20 to 10°C, and used for drying the air supplied to the drying apparatus at a temperature ranging from about 150 to 250°C.

In the preferred case of using an aqueous solution that contains one or more derivatives of glycine-N,N-luxusni acid with a total concentration of from 20 to 60% based on the entire weight of the aqueous solution.

When the desired atomization of an aqueous solution can be achieved due to the fact that it is served on one of a rapidly rotating disk or several rapidly rotating disks with a linear speed ≥100 m/C. These conditions are achieved in the dryer with the so-called disk dispersers, which operate at a corresponding speed of rotation of the disk.

You can also get a very fine spray of an aqueous solution due to the fact that its absolute pressure is brought by a pump to ≥20 bar and at this pressure serves it in a single nozzle or multiple nozzles located in the drying apparatus. In the preferred case, this can be used diaphragm pump.

Preferably also, when the absolute pressure in an aqueous solution adjusted to ≥30 bar.

Under high pressure aqueous solution can be fed in the nozzle, the number of which varies from one to thirty, in particular the number of nozzles can be from one on the twenty, in this case, preferably, when each nozzle has a hole in the range from 1 to 4 mm.

Spraying under high pressure aqueous solution occurs in dryers with nozzles, which are known to the expert, for example, Masters Spray Drying Handbook.

When implementing the invention method are free-flowing powder containing one or more derivatives of glycine-N,N-luxusni acid of General formula (I)

,

where

R means an alkyl group with the number of carbon atoms ranging from one to twelve and

M stands for alkali metal.

In the compounds of General formula (I) M means an alkali metal, in the preferred case of sodium or potassium, in a particularly preferred case of sodium.

The remainder R is alkyl group with the number of carbon atoms ranging from one to twelve, in the preferred case, with the number of carbon atoms of from one to six, in a particularly preferred means metal or ethyl residue. In a particularly preferred as component(a) use a salt of an alkali metal and metallireducens acid. In the most preferred case, use chinatravel salt metallireducens acid.

One or more derivatives of glycine-N,N-luxusni acid is used in the form of an aqueous solution, in the preferred case, the AE its concentration is from 20 to 60 wt.% based on the total weight of the solution.

In the preferred case, receive a free flowing powder containing hollow spheres and/or fragmented hollow balls in the amount of ≥60%, while the content carry out the following method: a sample of loose powder is dispersed in silicone oil, get the image in transmitted light when increasing from approximately 56-fold to 300-fold and count the particles constituting the hollow balls and/or crushed hollow balls, as well as the total number of particles in the image in transmitted light, then calculate the percentage of particles that are hollow balls and/or crushed hollow balls in relation to the total number of all particles.

In the preferred case, the relevant invention method are free-flowing powder with a content of hollow balls and splintered hollow balls in the amount of ≥80%.

The object of the present invention is also obtained by application of one of the above ways of loose powder to obtain the pressed agglomerates by pressing loose powder, if necessary together with other components, in particular polyethylene glycols, in the preferred case in the amount of 2 to 10 wt.%, and/or other additives, thus compressing is performed by passing through two rolls or stanova is eaten with subsequent grinding and fractionation. Obtained in this way pressed agglomerates have a high strength and, accordingly, a low degree of abrasion.

Strength determines the following method.

By pressing at the pressure of 200 MPa receive compressed samples for testing in the form of cylinders with a diameter of 12 mm and a height of 4 mm and determine the strength at break in the machine for testing tablets WHT II® company Pharmatest/Hainburg. On the basis of data on fracture toughness (R), height (H) and diameter (D) of the pressed samples in the following formula, calculate the strength (TS) (tensile strength):

TS=VK/(D)

When using the received corresponding to the invention by way of bulk powders strength characteristics are achieved ≥1.45 MPa.

These data, in strength, with a slight abrasion to the magnitude of the order of <5%. Abrasion define the following way: the sample is crushed and fractionated material, in particular, of the extruded sample with a particle size of from 0.3 to 1.6 mm for two minutes is subjected to preliminary screening for a 500 µm sieve and weigh the residue on the sieve, then the test within 10 minutes to stand on a vibrating sieve with an amplitude of 2 mm and determine the quantity passed through the sieve material. This material is considered as abrasi the hydrated wear.

The object of the present invention is also the use of pressed agglomerates of dry powders, obtained by implementing the invention method, in solid or liquid detergents or cleaners, in particular, to obtain tablets for dishwashing machines.

More in detail the invention is illustrated in the following examples.

The method of obtaining 1 (example comparison)

As the initial solution using an aqueous solution trinational salt methylglycine-N,N-luxusni acid with a concentration of 39.4 wt.% and, respectively, with the content trinational salt methylglycine-N,N-luxusni acid of 81.5 wt.% based on the total weight of solids in the original aqueous solution. From this solution in the industrial tower nozzles receive a free flowing powder with a residual water content of 6.5 wt.% with the content of the hollow balls of about 15%. Then this powder is pressed with the addition of 7 wt.% poly (ethylene glycol).

Get the pressed agglomerate (compacted material) with strength (TS), defined above by way of 0.77 MPa.

The method of obtaining 2 (in accordance with the invention)

As the initial solution using an aqueous solution trinational salt methylglycine-N,N-luxusni acid with a concentration of 39.8 wt.% and, respectively, with the content of trinacria the Oh salt methylglycine-N,N-luxusni acid is 84.8 wt.% based on the total weight of dry matter.

From this solution in the industrial tower with plates, rotating at 12900 rpm and get loose powder with a residual water content of 6.0% and a content of hollow balls of about 85%. Then, as shown in example 1, the powder is pressed with the addition of polyethylene glycol.

Get the pressed agglomerate (compacted material) with strength (TS) of 1.99 MPa.

The method of obtaining 3 (in accordance with the invention)

As the initial solution using an aqueous solution trinational salt methylglycine-N,N-luxusni acid with a concentration of 39.9 wt.% and, respectively, with the content trinational salt methylglycine-N,N-luxusni acid 87.1 wt.% based on the total weight of dry matter.

From this solution in the industrial tower nozzles receive a free flowing powder with a residual water content of 0.5% and with a content of hollow balls of about 10%.

Get the pressed agglomerate (compacted material) with the strength of 1.9 MPa.

The above examples clearly show the improvement in the strength of the pressed agglomerates, which are obtained from aqueous solutions containing chinatravel salt methylglycine-N,N-luxusni acid of high purity component ≥84% wt.% based on the total weight of dry matter.

1. The way to obtain a free flowing powder containing one or more ol svodnik glycine-N,N-luxusni acid of General formula (I)
,
where
R means an alkyl group with the number of carbon atoms ranging from one to twelve and
M means an alkali metal,
from the aqueous solution as a source material containing one or more derivatives of glycine-N,N-luxusni acid, which is dried by spray drying method air,
characterized in that
the aqueous solution contains one or more derivatives of glycine-N,N-luxusni acid in quantities of ≥84 wt.% based on the total weight of dry matter, and the fact that
spray drying is carried out in a drying apparatus, in which an aqueous solution and the air fed into the once-through mode with the temperature difference between the aqueous solution and the air in the range from 70 to 350°C., and the fact that
the aqueous solution is dispersed in the drying apparatus with the formation of tiny droplets of liquid by filing one or more disks rotating at a linear speed ≥100 m/s, or by creating it with a pump absolute pressure ≥20 bar and feed it when the pressure in the drying apparatus through one or more nozzles.

2. The method according to p. 1, characterized in that as a derivative of glycine-N,N-luxusni acids use the same salt or more salts methylpyridoxine acid with alkali metals.

3. The method according to p. 1 or 2, characterized in that h is of the drying apparatus is a disk dryer.

4. The method according to p. 1 or 2, characterized in that the dryer is a drying machine with nozzles.

5. The method according to p. 1 or 2, characterized in that the aqueous solution contains one or more derivatives of glycine-N,N-luxusni acid in a total concentration of from 20 to 60 wt.% based on the total weight of the aqueous solution.

6. The method according to p. 1 or 2, characterized in that an aqueous solution of one or more derivatives of glycine-N,N-luxusni acid served with a temperature of from about 20 to 120°C and the air supplied to a temperature of from about 150 to 250°C.

7. The method according to p. 1 or 2, characterized in that the pump is a diaphragm pump.

8. The method according to p. 1 or 2, characterized in that in an aqueous solution using a pump to create absolute pressure ≥30 bar.

9. The method according to p. 1 or 2, characterized in that get loose powder with a content of hollow balls or fragmented hollow balls ≥60%, while the content carry out the following method: a sample of loose powder is dispersed in silicone oil, get the image in transmitted light when increasing from approximately 56-fold to 300-fold and count the particles constituting the hollow beads or crushed hollow balls, as well as the total number of particles in the image in transmitted light, and calculate the percentage content of the particles, which are hollow beads or crushed hollow balls, in relation to the total number of particles.

10. The method according to p. 1 or 2, characterized in that get loose powder with a content of hollow balls or fragmented hollow balls ≥60%, while the content carry out the following method: a sample of loose powder is dispersed in silicone oil, get the image in transmitted light when increasing from approximately 56-fold to 300-fold and count the particles constituting the hollow balls and crushed hollow balls, as well as the total number of particles in the image in transmitted light, and calculate the percentage of particles that are hollow balls and crushed hollow balls, in relation to the total number of particles.

11. The application obtained by the method according to one of paragraphs.1-9 loose powder to obtain the pressed agglomerates with addition or without addition of polyethylene glycol.

12. The use of pressed agglomerates according to p. 11 for use in solid or liquid detergents.

13. Application under item 12 to obtain tablets for dishwashing machines.



 

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19 cl, 2 tbl, 11 ex

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