The method of obtaining covered with a protective shell particles peroxisome

 

(57) Abstract:

The invention is intended for the chemical industry and can be used to obtain detergents. Crystallized supersaturated solution peroxysalts. The obtained particles cause the protective shell of the alkali metal salt of an inorganic acid, such as HCl, H2SO4H2CO3H2B4O7H2SiO4. The application of lead in the VAT for subsequent crystallization, equipped with a stirrer, which he placed above the salt. The temperature is kept lower than the crystallization temperature and mixing conditions govern. After coating, the particles are separated by centrifugation and dried. As agent for the application shell, you can use the agent vysalivaniya present in the mother solution accompanying the suspension peroxysalts. 9 C.p. f-crystals, 4 PL.

The invention relates to a method of producing solid, covered with a protective shell particles peroxisome (salts nakilat), which are used in various types of industry as carriers of active oxygen in the solid state and, in particular, in the production of detergents.

From the La coating on the solid particles peroxysalts, and subsequent drying are covered with a protective sheath product (European patent A 1-459625).

There is also known a method which consists in mixing in the mixer pre-dried peroxocarbonate with an aqueous solution of the agent, servant to obtain a protective shell (Borat), and drying the resulting mixture (European patent 0487256).

These known methods, however, have the disadvantage that require complex installations, including unit for applying a protective shell, which in addition to the mixer or evaporator, contains its own units for drying, independent units for drying is not covered with a protective shell particles of protocole.

The method according to the invention allows to obtain economically stable particles peroxisome and narrow particle size distribution by means of a continuous method that did not require complex industrial installations, including several blocks for drying.

The invention relates to a continuous method for producing a protective sheath of solid particles of at least one peroxysalts, of at least one alkali metal by covering the particles peroxysalts, of the composition used to produce a protective sheath according to which the; is at the final stage the obtained crystal particles is subjected to the operation of centrifugation and drying; and between the stage of crystallization and phase centrifugation include stage, which is transferred into a tank with an agitator, called Chan for crystallization, the suspension of particles peroxysalts, of the stage of crystallization; in the above VAT for subsequent crystallization of introducing at least one employee to obtain a protective sheath agent and perform the above crystallization agent on the surface of the particles peroxysalts, in controlled conditions of temperature and agitation.

Under proxool understand any inorganic compound that is solid under normal conditions of temperature and pressure, which, when dissolved in water releases hydrogen peroxide and a salt of an inorganic acid. Examples of peroxisome corresponding method according to the invention are peroxoborate, PEROXYDICARBONATE phosphates and peroxidation carbonates.

The method according to the invention is intended in particular to get covered with a protective film of solid particles peroxoborates or peroxiderythromycin carbonates of alkali metals. He D. is natov alkali metals.

The method is applicable to obtain a protective shell particles peroxisome any alkali metal. It is well suitable for receiving a protective shell particles peroxisome sodium and potassium, gives excellent results in the case of obtaining covered with a protective shell particles peroxisome sodium.

The method according to the invention are particularly suitable for obtaining covered with a protective sheath peroxidation sodium carbonate formula 2Na2CO33H2O2usually called peroxycarbonates sodium.

The method is also applicable to obtain a mixture covered with a protective sheath few peroxisome, for example a mixture covered with a protective sheath peroxoborate and peroxidation carbonate of alkali metals. It can also be used to obtain a mixture covered with a protective sheath peroxisome various alkali metals, such as, for example, covered with a protective shell particles peroxisome sodium and potassium.

Under which serves to produce a protective shell composition, see composition suitable for coating a protective shell particles peroxisome, i.e., to cover their most uniform with Aut in several stages. The first stage is prepared particles peroxisome by continuous crystallization water supersaturated solution of the above peroxysalts. This stage of crystallization can be performed in the molds of various types. Usually well suited molds are traditionally used in the chemical and pharmaceutical industries. Examples of such molds are given in the work of H. Perry and D. Green W. "Perry's Chimical Enginner''s Handbook" 6th edition, MGraw-Hill, new York, 1984, S. 19-24, 19-40.

It is also possible alternatively to use molds-classifiers, i.e., molds, which also implements the classification of the resulting particles, to make a more narrow particle size distribution.

According to the invention particles peroxisome at the final stage is subjected to the centrifugation operation to press to remove most part of the mother solutions of the crystallization process. This operation is carried out in industrial centrifuges are commonly used in the chemical and pharmaceutical industries.

Centrifuged particles are then dried in the respective device. Can be used any type of industrial dryer, PI is a, they contain. Suitable driers are usually satisfactory drying with a stream of hot air. Give a good dryer fluidized bed of particles in a stream of hot air.

According to the invention the stage of applying a protective coating on the particles peroxisome include between stages of crystallization and centrifugation.

According to the invention a coating of protective shell particles peroxisome implement by moving coming out of the mold suspension of particles in a tank with stirrer, in which additional crystallization, called "subsequent crystallization", which is used to produce a protective shell composition around the particles peroxisome.

Under the VAT with stirrer see Chan, equipped with a stirrer capable of homogenizing the aqueous suspension of particles of peroxisome.

Can be used with any types of mixers provided that they do not create too much shear stress, which can lead to the fragmentation of particles peroxisome. In practice, satisfactory results provide a rotary stirrer, of which well suitable rotary blade mixer, acting in concert with the Central axis, results in the VAT for subsequent crystallization of introducing at least one agent, used to produce a protective shell. The above agent can be introduced either in the form of an aqueous concentrated solution or in the form of solid particles.

Under the concentrated solution see the solution, slightly supersaturated in the conditions of temperature and pressure prevailing in the tank for subsequent crystallization.

According to the invention can be used used to produce a protective sheath agents of different types. You can also use a mixture of several different agents, servants to produce a protective shell.

Preferably, as used to produce a protective shell agent you can use a salt of at least one inorganic acid alkali metal.

Preferably, choose from the strong acids inorganic acids. Excellent results give hydrochloric and sulphuric acids, in particular in relation to the salts sodium chloride and sodium sulfate.

Other interest, inorganic acids are carbonic acid, tetraborate acid and silicic acid, in particular in respect of such salts as sodium carbonate, borax and sodium silicate.

Employees for gaining the AI. Alternatively, it is also possible to enter into a VAT for subsequent crystallization in the form of a mixture with a suspension of particles of peroxisome. Under this option, agents, servants to produce a protective shell that can occur from the camera for crystallization. Other interest option is to use as an employee to obtain a protective shell agent, agent vysalivaniya, which may be present in the mother solution of the crystallization slurry particles peroxisome entered in the VAT for subsequent crystallization. Royal solutions of crystallization process usually contain such an agent vysalivaniya, when crystallization is performed in the deposition method using the additive total ion (method of vysalivaniya or "salting out").

Temperature and pressure stage of crystallization must be suitable for the aqueous solution was slightly supersaturated with respect to the employee to obtain a protective sheath agent.

For reasons of convenience typically operate at atmospheric pressure.

The preferred embodiment of the method according to the invention consists in loading tank to follow Christ is to saturation at a temperature of 1-2oC higher than that prevailing in the tank for subsequent crystallization and removal of continuously heat from the tank to the subsequent crystallization to make a supersaturated solution at a controlled temperature above Chan.

According to the first variant of the invention the temperature of the VAT for subsequent crystallization choose identical, which prevails in located above the mould.

According to the second variant of the invention the temperature of the VAT for subsequent crystallization set at a value lower than located above the mould.

Preferably, the temperature of the VAT for subsequent crystallization set when the value is lower by at least 5oC the one that prevails in the mould. Particularly preferably, the temperature of the VAT for subsequent crystallization set when the value is lower by at least 10oC temperature in the mould.

VAT for subsequent crystallization according to the method of the invention typically includes a device capable of staying cool in a VAT of aqueous solution. Suitable any known device for heat transfer in chemical reactors. You can, for example, the I liquid, the role of heat from the tank. Alternatively, you can also equip Chan double wall, in which circulates the coolant.

As the coolant, you can use liquid coolants used in refrigeration industry, or chilled brine. Good results were obtained when using chilled brine NaCl.

When they are introduced separately into a VAT for subsequent crystallization, is used to produce a protective sheath agent, if necessary, the above-Chan can be cooled to a temperature below that of Chan for crystallization in order to find the optimum deposition conditions used to obtain the containment of the agent around the particles peroxisome.

When the nature of the employee to obtain a protective sheath agent allows, it is sometimes possible, however, to work in a VAT for subsequent crystallization at the same temperature as the mold.

Instead, when as an employee to obtain a protective sheath agent use the agent vysalivaniya present in the mother solution, accompanying particles peroxysalts, it is usually recommended to operate at temperatues to produce a protective shell, around particles peroxysalts.

The following examples are given to illustrate the invention is in no way limiting its scope.

In all these examples, mention the value of stability peroxysalts in a detergent base. Its measurement consists in mixing in the dry state 10 wt.% tested peroxysalts, with 90 wt.% the base detergent powder of the following composition:

anionic detergents, g/kg - 199

carbonate, g/kg - 97,3

soluble compounds, g/kg < 0,03

soluble compounds of Si, g Si/kg - 10

soluble compounds S, g S/kg - 55

soluble compounds P, g P/kg 2,8

non-ionic detergents, g/kg - 22

nonanoyloxybenzenesulfonate, g/kg - 13

sulfate, g SO4kg - 143

The resulting mixture has a titer against active oxygen, which is close to 1.5% (determined by iodometry).

Several samples of each test mixture is placed in a Cup of paperboard, laminated with wax, with a capacity of approximately 120 ml Cup is then filled about half with 50 g of the mixture. Each Cup is then tightly closed and store in an environment controlled at the 32oC, and where prevailing relative humidity of 80%.

the HN stability correspond to the residual active oxygen, expressed in mol.%, in relation to the original content at the beginning of storage.

Example IR (not according to invention)

Get peroxidation sodium carbonate (LTU or peroxocarbonate" sodium, 2Na2CO33H2O2in the crystallizer - classifier from a solution of hydrogen peroxide containing crystallization accelerators, and a solution of sodium carbonate containing stabilizers and agents vysalivaniya, the following operating conditions (see tab. 1).

PKN obtained at the outlet of the crystallizer-classifier, and then centrifuged in an industrial centrifuge company KRAUSS-MAFFEI type Hz25 with the volume of the drum 2,5 DM3. Centrifugation PKN carried out in semi-continuous mode as follows:

- introduction 1-1,5 l of suspension PKN (250-450 g solids) and uterine fluids in a rotating drum (2000 rpm);

- centrifugation with a speed of 2000 rpm for 80-90 seconds;

- decrease the speed of rotation of the drum up to 400 revolutions/min;

- removal layer with a knife and unloading centrifuged PKN with a moisture content of 8-12 wt.%;

- increased speed of rotation of the drum to 2000 rpm;

- a new filling cycle, centrifugation, Eskom the fluidized bed volume of 1.4 DM3(diameter of 1.5 DM), in a stream of hot air with the performance of 30-40 m3/h at 110-120oC. the temperature of the fluidized bed 65-70oC and the average residence time of POC is 10-20 minutes. The resulting product has the following characteristics (see tab. 2).

The dissolution rate is determined in the following method.

In the amount of demineralized water to 1000 ml, supported at the temperature of 15 1oC, in a glass with a capacity of 2 l, immerse the mixer in stainless steel with two vertical blades with a length of 42 mm and a height of 11 mm, arranged at a right angle, and rotate it with controlled velocity 35010 rpm. Then enter 20,01 g covered with a protective film sample PKN in a glass and immediately put in motion chronometer. Then mark the conductivity of the solution all the time for 5 minutes, and conductivity after 15 minutes of mixing. In addition, draw a calibration curve depending on the conductivity measured after 15 minutes mixing time in the following amounts covered with a protective sheath PKN: 1,0; 1,5; 2,0 and 2,5. Dealing conductivity of the sample, measured after 2 minutes on a standard curve, make a conclusion about the weight compared to the weight of dissolved PKN-to-weight ratio of all of the used sample and expressed in %.

Examples 2-4 (according to the invention).

In the process of obtaining peroxocarbonate sodium as described in example IR, enter the stage of crystallization between the stage of crystallization and phase centrifugation. Conditions this stage crystallization are given in table. 3.

The results of the research covered with a protective film products are shown in table. 4.

1. Continuous method of producing solid, covered with a protective shell particles, at least one peroxysalts, of at least one alkali metal by covering the particles peroxysalts, of using used to produce a protective shell composition, according to which the first stage is continuously crystallized saturated solution peroxysalts, of any known method, followed by a stage of applying a protective shell, in which the VAT with stirrer, called Chan for crystallization, transfer suspension of particles peroxysalts, obtained at the stage of crystallization, in the above-Chan enter at least one is used to produce a protective sheath agent and perform the above crystallization agent on the surface of the particles peroxysalts, in a controlled temperature environment is ing and drying.

2. The method according to p. 1, characterized in that the temperature in the VAT for subsequent crystallization is lower than the temperature during crystallization.

3. The method according to p. 2, characterized in that the temperature in the VAT for subsequent crystallization below, at least 5oWith the temperature during crystallization.

4. The method according to any of paragraphs.1 to 3, characterized in that is used to produce a protective shell agent is chosen among the salts, at least one inorganic acid alkali metal.

5. The method according to p. 4, wherein the inorganic acid is a strong acid.

6. The method according to p. 5, wherein the strong acid is hydrochloric acid or sulfuric acid.

7. The method according to p. 4, wherein the inorganic acid is carbonic acid.

8. The method according to p. 4, wherein the inorganic acid is tetraborate acid.

9. The method according to p. 4, wherein the inorganic acid is silicic acid.

10. The method according to p. 3, characterized in that serving to produce a protective shell agent is the agent vysalivaniya present in the mother solution, accompanied

 

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23 cl, 4 dwg, 4 tbl

FIELD: chemistry.

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EFFECT: creation of sodium percarbonate particles possessing increased long storage stability.

14 cl, 2 ex, 4 dwg

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