The way to prevent agglomeration hygroscopic and sublimirovannogo powder nitrogen-containing compounds

 

(57) Abstract:

The essence of the invention: preventing agglomeration hygroscopic and sublimirovannogo powder nitrogen-containing compounds selected from the group of triethylenediamine, inorganic salt, such as ammonium sulfate, ammonium chloride, addition of poly (oksietilenom)diglycolic acid f-crystals , where n is an integer with an average mol. m 400 - 4000 in the amount of 0.1 - 2 wt.h. on 100 wt.h. powder in the environment of the solvent, followed by drying. table 1.

The invention relates to a method of preventing agglomeration of powders, glued to stick together. In particular, it relates to a method for preventing agglomeration of powders based on the use of poly (oksietilenom) diglycolic acid as antiglomerular.

Powdery amine such as piperazine or triethylenediamine (TED), is a compound, which usually has the cohesion and adhesion and, thus, easily glomeridae. In addition to these specific powdered compounds are usually easy aglomerados highly hygroscopic powders or easily sublimating the powders due to the absorption of small amounts of water or due to the increased temperature. Patocka it extremely difficult. As measures to prevent agglomeration of such agglomerated powders generally used to remove impurities, contained in the powder, and increasing the particle size of the powder, and a method of adding antiglomerular to the powder or storage method of this powder in a closed container. However, among agglomerated powders there is one that sticks together even when stored in a closed container, such as a piperazine, or highly sublimating substances such as TED, who has a tendency to easily glomerulopathy during storage. Therefore, there is no acceptable method of preventing agglomeration of such powders. Next to these powders is characterized by a very high sintering ability and is usually difficult to prevent agglomeration by increasing the particle size. Effective method of preventing agglomeration of such highly agglomerated powders is the introduction of an appropriate antiglomerular.

When choosing such antiglomerular you must choose a agent who are able to exert effective action when using it in perhaps fewer, and which produces no odor or staining powder when adding it. Chrome is the purpose of the latter, and not roads. As traditional antiagglomerants known powdered silicon dioxide (Japanese unexamined patent publication N 203039 1982 (and glycols) Japanese examined patent publication N 46758, 1988). However, powdered silicon dioxide is effective only as an agent, temporarily reducing the contact of the crystals with each other, and it antiglomerular action is not so large and long. On the other hand, liquid antigamente, such as glycols, you can just mix it with powdered TED. However, the result is a dampening powder TED and during prolonged storage, the liquid flows to the bottom of the tank, causing uneven distribution by volume capacity and reduce antiglomerular steps.

At the same time, in Japanese examined patent publications N 62241, 1988 and N 3142, 1989 indicated that adding polymer TED as an additive at the stage of deposition, it is possible to simplify the implementation process and to facilitate thereby the control process and that the polymer TED characterized by high antiglomerular effect, therefore, the desired effect can be achieved by adding very small amounts of polymer. However, it is usual to have the cohesion, and adhesion. To reduce these parameters are usually used operations such as granulation or classification. However, in the case of agglomerated powders, such as vysokouglerodistoy powders, such as TED, due to changes in external temperature processes of sublimation and condensation, which leads to the formation of strong colophony connections between particles (crystals) powder. Thus, for TED tends to be full agglomeration in the vessel, and such material is difficult to grind.

Usually TED obtain or synthesize, for example, from N-AMINOETHYLPIPERAZINE or acetylpiperidine. TED obtained in this way is a yellowish crystals. As a by-product it contains alkylpiperazine or so on This side product in some degree has antiglomerular action. However, in recent years there has been a need in crystals TED high purity and, as a consequence, it now produces crystals of TED having a purity not less than 99.9% as a result of improved treatment methods. Accordingly dramatically increased the sintering ability of TED and difficulties associated with its production process and stored the operating ability which prevent agglomeration can be effectively accomplished by adding nebolshogo number antigamente, soluble in various solvents, which are inexpensive and do not deteriorate the physical properties of the powder, in comparison with traditional methods.

As a result of extensive research conducted with regard to these requirements, the possibility of effective regulation of the process of agglomeration of the powder by using as antiglomerular poly (oksietilenom) diglycolic acid, and on the basis of the establishment of this fact came to the development of the present invention.

Thus, the invention provides a method for preventing agglomeration aglomeracionnoe powders, which provides for the introduction of a powder of poly (oksietilenom) diglycolic acid as antiglomerular.

Hereinafter the invention will be discussed in detail with reference to preferred variants of its implementation.

In the invention agglomerated powder means highly hygroscopic and/or sublimating powder selected from the group of TED, inorganic salt, e.g. ammonium sulfate, ammonium chloride.

Suppose that the mechanism to prevent agglomeration in the invention is as follows. Poly(oksietilenom) digitalia acid has a high solubility in various solvents. The solution of such poly(oksietilenom) diglycolic acid in water or any organic solvent is mixed with the powder, then dried and receive a film of poly(oksietilenom)diglycolic acid on the surface of the powder and thus microcapsular crystals, thereby preventing any possible contact kristalloobrazuyushchikh components with the external atmosphere or the contact of the crystals with each other, resulting in the absorption of moisture, sub is glomerulone action.

Poly(oksietilenom) digitalia acid of the invention is a compound of the following formula 1.

HOOCCH2----/OCH2CH2/---- OCH2COOH, where n is an integer not less than 1.

Poly(oksietilenom) digitalia acid appears to be under the trademark "REO acid" company "Kawaken Fine Chemicals K. K.". This poly(oksietilenom)digitalia acid supplied to the market three types #400, # 1000 and #4000, depending on the average molecular weight.

In the invention, no particular limitation on the average molecular weight of poly(oksietilenom)diglycolic acid. Acid with low molecular weight is a high-viscosity liquid, and high molecular weight product is a solid. Therefore, for the introduction of poly(oksietilenom)diglycolic acid necessary solvent. However, preferred is poly(oksietilenom)digitalia acid having a high molecular weight, which becomes solid at the stage of drying after the introduction, or in the state of the target product.

According to the invention, the amount of poly(oksietilenom)diglycolic acid, is introduced into the powder, typically 0.1-2%, preferably 0.5 to 1%. Further, in the invention are not things with which after receiving the powder this powder and a solution of poly(oksietilenom)diglycolic acid in water or an organic solvent are thoroughly mixed using a mixing device, such as a ribbon mixer or a Y-shaped mixer. However, when using such mixing equipment, the process is complicated and the cost increases. Therefore, if a solution of poly(oksietilenom)diglycolic acid in water or an organic solvent spray or otherwise enter on the stage of udaleniya fluid immediately after deposition, i.e., a brick of crystalline TED in a centrifuge and then dried, it can be effectively and evenly to cover the surface of the crystals TED without the use of mixing equipment. In another embodiment, it can be added at the stage of deposition, as described in Japanese examined patent publication N 62241, 1988.

In appearance poly(oksietilenom)diglycolamine acids are substances from colorless transparent liquid white paraminophenol solids and are chemically resistant. Therefore, they do not have negative effects on the physical properties of the powder and have a high solubility in various solvents and, thus, possess excellent properties as additives or agents for coating.

The invention provides meet the modern requirement of the method is howling acids are added to the powder with the purpose of coating on the surface of the powder and give high antiglomerular properties due to the suppression of absorption of moisture and sublimation powder and prevent contact of the powder particles to each other.

P R I m e R 1. In 5-quart mixer flow type introduced and mixed with 1 kg of powder TED and 10 g of poly(oksietilenom)diglycolic acid #4000/REO acid production Kawaken Fine Chemical K. K. as antiglomerular dissolved in 50 ml of methanol. The mixture was dried in a vacuum mixer and got a sample.

The degree of agglomeration and evaluation standards were measured as follows. Namely, the obtained sample was Packed in a container of size 5x5 cm and a height of 2 cm and put plastic plate 5x5 see Above put the weights weighing 300 g and the container was stored in a desiccator with a relative humidity of not more than 1%. During storage, the pressure on the crystals was 12 g/cm2. After storage in a desiccator for one month weights and capacity have learned from him and the pressure was moved to the Central part of the crystal unit with a plastic bottom plate, by using a Durometer type Kiya, which reads the pressure value at fracture. Thus obtained value was classified according to the following three groups, which are used as indexes for evaluating the degree of agglomeration:

Group A. the crystal unit, which can easily be destroyed if aglomeracji.

Group C. the Crystal unit with the bursting pressure of not more than 10.0 kg/cm2that can't be destroyed easy blow which has significant agglomeration throughout the volume.

Group C. the Crystalline block, which requires a much stronger blow to destruction with the bursting pressure of not less than 10.0 kg/cm2and running a full agglomeration.

The obtained results are included in group A. So installed that antiglomerular takes excellent antiglomerular properties. In addition, the powder was in the dry state and when it is dissolved in such a solvent as dipropyleneglycol, insoluble fraction was not found.

P R I m e R 1 (comparative). The degree of agglomeration was measured in the same manner as in example 1, using TED, not containing antiglomerular. The obtained results are included in the group, and found that agglomeration has increased significantly.

P R I m m e R 2 (comparative). 1 kg of TED and 2 g of silica gel (manufactured by "Nippan Silica Gel Kogyo K. K.", bulk density 40 g/l, the average particle size of 2 mm thoroughly mixed in a Y-shaped mixer and the resulting mixture was used as a sample. In other words, the process is glomeruli.

P R I m e R 3 (comparative).

The process was carried out as in example 1, except that instead of poly(oksietilenom)diglycolic acid as antiglomerular used a polyethylene glycol #200 (manufactured by "Kanto Kagaka"). Measured the degree of agglomeration of the product and found that the resulting value it is included in group C. in Addition, the powder was wet.

P R I m e R 4 (comparative). 3000 ml of methanolic solution [containing 50 wt. including TED and 50 wt. hours of methanol was placed in a flask having an internal volume of 5000 ml, and was added 0.15 g of polymer TED (copolymer of ethylene and piperazine), synthesized according to Japanese unexamined patent publication N 62241) 1988. From the mixture was removed with methanol by using an evaporator, resulting in a 1 in 100 ml of methanol was distilled. The remaining liquid was left to stand at room temperature, and then cooled to 20aboutC. Precipitated precipitated crystals TED was filtered under vacuum on filter paper N 5S, and then dried under vacuum resulting in a received 450 g of crystals of TED. The polymer TED contained in the crystals TED, was 0.05 g (III HR per million). As for this sample, the degree awesome protivokorrozionnoe action but when dissolved in solution dipropyleneglycol observed turbidity.

P R I m e R 5. The process was performed as in example 1, except that as antiglomerular instead of poly(oxyethylenenitrilo acid #4000 used poly(oksietilenom)diglycolic acid #1000. As a result, the degree of agglomeration is included in group A.

P R I m e R 6. The process was performed as in example 1, except that as antiglomerular instead of poly(oksietilenom)diglycolic acid #4000 used poly(oksietilenom)diglycolic acid #400.

P R I m e R 7. The process was performed as in example 1, except that as antiglomerular instead of powder TED used the ammonium chloride. Assessed the degree of agglomeration of the product. It was established that the degree of agglomeration is included in group A.

P R I m e R 8 (comparative). The process was performed as in example 7, except that poly(oksietilenom)diglycolic acid was added. In the result, it was found that the amount of ammonium chloride significantly agglomerated, and the degree of agglomeration is included in group C.

P R I m e R 9. The process is carried out that is that ammonium. Assessed the degree of agglomeration of the product. It was established that the degree of agglomeration is included in group A.

P R I m e R 10 (comparative). The process was performed as in example 8, except that poly(oksietilenom)diglycolic acid was added. In the result, it was found that the amount of ammonium sulfate significantly agglomerated, and the degree of agglomeration is included in group C.

P R I m e R 11. The method was conducted in the same manner as in example 1, except that poly(oksietilenom)digitalia acid was used at 2 o'clock by weight for 100 hours by mass of powder of TED. As a result, the degree of agglomeration is included in group A.

P R I m e R 12. The method was conducted in the same manner as in example 1, except that poly(oksietilenom)digitalia acid was used in an amount of 0.1 PM mass for 100 hours by mass of powder of TED. As a result, the degree of agglomeration is included in group A.

The results of examples 140 shown in the table.

The WAY to PREVENT AGGLOMERATION HYGROSCOPIC AND SUBLIMIROVANNOGO POWDER NITROGEN-containing COMPOUNDS selected from the group of triethylenediamine, inorganic salt, such as ammonium sulfate, ammonium chloride, povysheniya stability of the powder, as polymer additives using poly(oksietilenom)diglycolic acid of General formula

HOOCCH2OCH2CH OCH2COOH ,,

where n is an integer,

with an average mol. m 400 - 4000, and poly(oksietilenom)diglycolic acid is administered in an amount of 0.1 - 2.0 wt. hours at 100 wt. including powder.

 

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