A method of obtaining a granulated synthetic zeolite component sms

 

The invention relates to a process for producing granulated zeolite components of synthetic detergents (CMC) and may find application in the production of CMC in the chemical industry. A method of obtaining a granulated synthetic zeolite CMC component includes a mixture of fine zeolite type And size of the crystals of 1-3 μm and a humidity of 20-40% with a binder - carboxymethyl cellulose, which is used in the form of a dry powder or an aqueous solution in the amount of 5-10 wt.% in terms of dry zeolite, extruding the mixture, drying the obtained granules on a belt drier at 130-180oWith the fragmentation of the granules to obtain the fractional composition crumbs 0,2-2,5 mm and their classification, and the fraction of crumb size less than 0.2 mm again sent for mixing with a binder. The technical result increased the mechanical strength of the granules, their high cation-exchange capacity of the Cao, the flowability and nebelnest. table 1.

The invention relates to a process for producing granulated zeolite components of synthetic detergents (CMC) and may find application in the production of CMC in the chemical industry.

Wide application in the product or phosphate in the composition of synthetic detergents.

However, the introduction of zeolite in the composition of the CMC is associated with certain difficulties, because zeolites are dusty powder with a particle size of 2 to 8 μm, which complicates the technology, poor working conditions and reduces quality of the final product. According to GOST 25644-83 standard in the manufacture of synthetic detergents are granules with a size in the range of 0.2-2.5 mm

The use of powdered zeolite, thus, eliminates the possibility of preparation of CMC by dry mixing the raw material components in the formulation of detergents.

There is a method of producing granulated engineering CMC components with high bulk weight, containing 15-20% ethoxylated with ethylene oxide alcohols With12-C24or other nonionic oxyalkylated surfactant, 5% anionic surfactants, 40-80% of inorganic fillers (sodium tripolyphosphate, zeolite type a, sodium metasilicate, soda ash, sodium sulfate), 0.5 to 10% of palifosfamide, polycarboxylic acids, toluensulfonate sodium CMC, optical Brightener and 10-20% adsorption or crystallization environment (application Germany 3434854, M CL C 11 D 11/02, 1986).

The disadvantages of this method are: 1. Content ecology).

2. Use in the composition of many kinds of raw materials, which significantly complicates the process of pelletized product.

A known method of obtaining a granulated zeolite component of the CMC-containing carbonates and zeolites, which provides for: - the preparation of zeolites of types a or X in the form of powders by hydrothermal crystallization of mixtures of silicate and sodium aluminate, separating the mother liquor, washing and drying of the zeolite (average particle size of the zeolite is less than 15 microns); - preparation of a suspension consisting of 20-60% zeolite, 5-30% soda (sodium carbonate), 5-15% of sodium silicate and 25-60% water, and lowering the viscosity of the mixture; - spray drying the mixture with the formation of spherical granules with a moisture content 2-16 wt. % and cation exchange capacity (KOS) by Cao 170-190 mg/g product; mixing the obtained granules with nonionic surfactants (U.S. Patent 4406808, CL 252-91, 1983).

This method has drawbacks: 1. The possibility of obtaining a granulated zeolite for the CMC method spray drying aqueous slurry of raw materials only in the form of microspherical beads of a size 60-200 μm, which makes it impossible to use such a product in the preparation of CMC by dry the em 20-30% lower KOS on Cao, what type zeolite A.

3. The use of zeolites (raw material) with an average particle size less than 15 μm, because , the smaller the size, the KOS zeolite above, and preferably the use of powdered zeolite with a crystal size of not more than 4 μm.

A known method of obtaining a granulated zeolite filler for synthetic detergents (RF patent 2016846, 01 33/34, 1994, BI 14), which provides for mixing of solutions of silicate and sodium aluminate with a molar ratio of SIO, SIS2/Al2About3equal to 2.0 to 2.5; crystallization of the formed silicofluorides in type zeolite And at a temperature of 60-100oWith for 0.4 to 6.0 h and spray drying the suspension of the zeolite in the mother solution with a concentration of: 100-250 g/l zeolite, 55-110 g/l NaOH, 5-30 g/l SIO, SIS2in the flue gas stream containing CO2. Thus there is a complete or partial neutralization of sodium hydroxide, leading to the formation of granulated zeolite filler for CMC containing: 50-60% of zeolite type a, 25-30% ash, 2% and 8% of sodium silicate, 2-5% sodium hydroxide and 2-15% of water. The product has a KOS on Cao 190-200 mg/g and fractional composition of 80-200 μm.

The disadvantages of this method include the possibility of obtaining tseolitsoderzhashchikh CMC dry mixture.

A method of obtaining granulated synthetic zeolite used in the compositions of the CMC (A. C. the USSR 1159885, 01 33/28, 1985, BI 21). The method involves spraying a liquid medium to powdered zeolite with stirring by means of a pneumatic nozzle in the apparatus librarypage layer. As a liquid environment using aqueous suspension of zeolite with a binder at a ratio of solid and liquid phases, is equal to (0.2 to 1.0):1. As a binder used aqueous solutions of surface-active substances (surfactants). Get granular zeolite with a binder with a particle size of 0.2-2.5 mm

The known method has drawbacks: 1. The complexity and multi-stage methods of obtaining granules associated with the preparation and use only water suspensions of zeolite and surfactant as a binder.

2. High energy consumption, since the deposition occurs when the ratio (0.2 to 1.0):1 between the solid and liquid phases.

3. The inability to obtain granules containing not more than 15% of water (humidity), because the method is not provided for drying the granules at a temperature above 100oC. As a result, the finished product crumpled and loses flowability during storage and transportation, which makes it impossible to use OBM (via repulpable and subsequent spray drying).

The closest in technical essence and the achieved result of the present invention is a method of obtaining a granulated synthetic zeolite" (SU 1156726 And 23.05.1985), which is chosen for the prototype.

According to this method, the zeolite with a humidity of 20-40% is mixed with a binder - powder-like carboxymethyl cellulose (CMC), taken in an amount of 0.5-5.0 wt.% calculated on the dry zeolite and having a particle size of not more than 1.5 mm Mixture ekstragiruyut through the grate screw granulator, and the resulting granules with a diameter of 4.5 mm and a length of 6-9 mm dried in the fluidized bed apparatus at 80oAnd the number of pseudoseizure of 0.8-1.2. Get granular zeolite with a binder with residual moisture of 5% and mechanical strength 7-10 kgs/cm2(0.07 to 0.1 kgf/mm2).

This method has drawbacks: 1. The use of a binder in the amount of 0.5-5.0 wt.% calculated on the dry zeolite does not provide granules of zeolite with a binder necessary mechanical strength. Granules collapse to a fraction of less than 0.2 mm during storage and transportation.

2. The use of a binder in the amount of 0.5-5 wt.% calculated on the dry zeolite is not possible to speak about its granular product, as integrated connection, enabling the 10-15 wt. % and the desired content of the CMC of about 1 wt.%. With the introduction of granulated zeolite obtained by a known method, if the composition of the CMC 10-15 wt.% zeolite, the content of the CMC just(0,05-0,5)-(0,075-0,75). Thus, it is necessary to enter CMC in the form of separate types of raw materials directly in the CMC.

3. Granules of zeolite with a binder diameter of 4.5 mm and a length of 6-9 mm cannot be used to obtain the CMC, dry mix, as well as dust (fraction <0,2 mm), formed during storage and transportation. As already noted, the desired particle size of the granular zeolite of 0.2-2.5 mm

4. As a binder is provided for use only powdered CMC, which complicates the process of mixing with the zeolite and leads to heterogeneous granules and, consequently, may result in such a small amount of the binder is 0.5 to 5.0% by mechanical destruction.

5. Drying in the fluidized bed apparatus extruded granules leads to the formation of microcracks on the granules and decrease of their mechanical strength.

The aim of the invention is to develop a method of producing granulated synthetic zeolite component CMC with improved quality in parts of the particle size distribution (linzirowanii complex structure (zeolite+CMC), i.e., this component of the CMC, which can be used in the manufacture of detergents by dry blending of raw materials.

This objective is achieved in that the fine zeolite type a (primary crystal size of 1-3 microns) is mixed with carboxymethylcellulose, taken in the form of a dry powder with a particle size of <1.5 mm, or an aqueous solution in the amount of 5-10 wt.%, in terms of dry zeolite. The mixture ekstragiruyut, granules with a diameter of 4 mm and a length of 5-8 mm and dried in a belt dryer, crushed to obtain fractions of 0.2-2.5 mm and classified. After classification faction crumb size less than 0.2 mm again sent for mixing with a binder.

Comparative analysis of the proposed method with the prototype allows to conclude that the claimed method differs from the known mixture of superfine (primary crystal size of 1-3 μm) of the zeolite, namely type a, carboxymethyl cellulose, taken in an amount of 5-10 wt.%, considering the dry zeolite. Moreover, CMC is used either in the form of a dry powder (as in the prototype), or in aqueous solution. The difference is also in the drying of extruded pellets, which is carried in a belt dryer at a temperature of 130-180

These techniques allow to conclude that the proposed solution meets the criterion of "Novelty".

Analysis of the known methods of obtaining synthetic granular zeolites and zeolite-containing fillers CMC showed that the mixture of zeolite with CMC, extruding the mixture with obtaining graft granules and subsequent drying is known. However, only the fact of mixing fine (predominant crystal size 1-3 μm) of the zeolite, namely type a, with CMC, taken in an amount of 5-10 wt.%, considering the dry zeolite, allows after drying in a belt dryer at a temperature of 130-180oTo obtain a mechanically stable pellets of the synthetic component of the CMC. Moreover, such a component of the CMC, which has a balanced (optimal) chemical (ratio of zeolite/SAS) composition for use in detergent formulations.

The use of a binder in the form of an aqueous solution of CMC can provide a high degree of homogeneity in the extrudable mixture and, as a consequence, high strength pellets. Only new operations crushing and subsequent classification of the granules results of particle size (0.2 to 2.5 mm) n the house dry mixed ingredients. The use of particles less than 0.2 mm, formed by crushing, again when receiving component CMC helped to create a closed, waste-free, environmentally safe production.

The essence of the invention consists in the following.

Mix superfine (mainly the size of the crystals of 1-3 microns) zeolite type a (humidity 20-40%) with CMC, taken in the form of a dry powder (particle size1.5 mm) or aqueous solution, in the amount of 5-10% of the total weight of dry zeolite with CMC. The mixing is carried out until a homogeneous paste. Pasta ekstragiruyut through the die plate screw granulator. The obtained extrudates - cuttings with a diameter of 4 mm and a length of 5-8 mm and dried in a belt dryer at a temperature of 130-180oWith vapor in the environment. Get mechanically strong 0,6-0,8 kg/mm2(60-80 kg/cm2) granules containing 90-95/10-5 wt. % zeolite type a and CMC, in terms of dry matter, respectively. Granules are crushed to obtain fractions of 0.2-2.5 mm and classified by screening. Fraction less than 0.2 mm again sent for mixing with a binder. Commodity granular synthetic zeolite component CMC has a high x Cao 170-200 mg/g), high flowability, not pilot, n is the reamers shown in the table.

The lower input of the binder is less than 5 wt.% causes deterioration of the durability of the pellets, increasing the number of particles less than 0.2 mm after crushing and deterioration of conditions of storage, transportation, and enter into the composition of the CMC.

The increase in the input of the binder in excess of 10 wt.% reduces KOS by Cao and gives the granules suboptimal structure (zeolite/CMC).

The use of any other type zeolite instead of zeolite type a, even with high dispersion (primary crystal size of 1-3 µm) decreases by at least 15-20% of KOS for Cao prepared product.

Temperature 130-180oWith drying in a steam-air mixture in the belt dryer is governed by the conditions of the real dryers, need to give granules moisture content of 5-10% and prevent burning CMC in the drying process.

Claims

A method of obtaining a granulated synthetic zeolite component of synthetic detergents (CMC) comprising a mixture of zeolite with a humidity of 20-40% with a binder - carboxymethyl cellulose (CMC), extruding and drying the mixture of granules, characterized in that the mixture serves fine zeolite type And size of the crystals of 1-3 μm, and carboxymethylcellulose ispolzuya belt dryer at 130-180oC, crushed to obtain the fractional composition crumbs of 0.2-2.5 mm, classify, then crumb granular zeolite component CMC of less than 0.2 mm is recycled for mixing with a binder.

 

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