Method of production of granulated synthetic zeolite-containing component of synthetic detergents

FIELD: technological processes; chemistry.

SUBSTANCE: fine-grained zeolite of A-LSX type with crystal size of 0.9-3.0 micrometer is mixed with carboxymethyl cellulose (CMC), taken in the amount of 3-15 wt % in conversion to dry zeolite. Mixture is extruded. Granules are dried at 130-180°C, crushed and fractionated for production of end product with particle size of 0.2-2.5 micrometer. Fraction of particle with size below 0.2 mm are returned to mixing with CMC.

EFFECT: increase of cation-exchange efficiency.

1 tbl, 7 ex

 

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 production of CMC are synthetic zeolites, which are used as ion exchangers, replacing, partially or completely, the phosphate in the composition of synthetic detergents.

Zeolites, both natural and artificial, are porous crystalline aluminosilicates structure formed from a three-dimensional framework of tetrahedra TO4where T may be a silicon or aluminum. The presence of aluminum in tetrahedral coordination in the crystal lattice determines the excess negative charge is balanced by ions of the alkali metal (Na, K, Rb, Li, or Cs), ions of alkaline earth metal (Mg or CA) or ammonium ions.

Know the use of zeolite As an additive in detergent systems, improving their cleansing action (U.S. Patent N 4649036). Zeolite is used to remove from the wash water of polyvalent metal ions, in particular calcium ions, to the greatest extent determine the hardness of water. However, the zeolite type And does not appreciably reduces the stiffness caused by the presence of the magnesium ion, because it has insufficient pore size relative to the radius e of the CSOs ion in aqueous solution at the initial temperature of the contact during washing with tap water.

At room temperature prior to entry into force of the washing solution, containing, for example, surfactants, bleaching agents, carbonates, etc., the kinetics of magnesium ions is very slow. Therefore, the ability of the zeolite type And remove magnesium ions is insufficient in practice so that the necessary adjuvants.

To improve the action of the scrubbing system and to eliminate the formation of residual coating on the fabric, it is necessary, in fact, completely removed from the scrubbing system calcium ions and magnesium, and as quick as you can. If you do not remove these ions, soluble salts of calcium and magnesium present in the water will increase (due to the presence of other components of the detergent composition is sodium carbonate) to precipitate formation of mixed carbonates of calcium and magnesium and carbohydrates.

In addition, the formation of poorly soluble salts of these ions, especially in detergent compositions containing anionic surfactants, reduces active the specified number of components required for the washing. Added to this is the fact that these salts are deposited in the tissues and this leads to the possible damage to their fibers.

Other known zeolite with washing ability is described, for example, in German patent DD 43221 zeolite type X, which which has pore openings, large enough to provide a high rate of ion exchange, in particular of magnesium ions. However, the ratio Si/Al, which is in contrast to this ratio in the zeolite type And always significantly greater than 1, reduce the overall ion exchange capacity. In addition, the zeolite of type a are available for ion exchange all centers (uniform porous with an average pore diameter of 4,2 Å). In the lattice of the zeolite type X has a cavity, less is available for ion exchange (non-uniform porous system: cavity with pores with an average diameter of 7.4 Å and a cavity with pores with an average diameter of 2.2 Å).

This situation has led to the creation of a zeolite with a ratio Si/Al in the range between 0.9 and 1.1, such as this relation in type zeolite A. Zeolite identified as type zeolite LSX (Low Silica X - low-silicon-type zeolite X), which has the advantages of ion exchange capacity, which is close to the capacity of the zeolite type And because of the relationship of Si/Al. At the same time, the rate of ion exchange, due to its structure, typical of zeolite type x-type Zeolite LSX described, for example, in the United Kingdom patent GB 1580928.

However, the known methods of obtaining type zeolite LSX extremely expensive for economically feasible and commercially viable industrial production. Its reception requires excessively long production time is, in particular, the time of aging, comprising from 15 to 100 hours at temperatures below 50°C. in Addition, the need for synthesis in high regard K2O/(K2O+Na2O) from 0.10 to 0.40 introduces an additional negative point, which is that in the presence of potassium in the final zeolite latter requires cleaning to achieve the desired ion-exchange capacity and exchange rate and characteristics necessary for a product suitable for use in detergents.

Was developed (Patent RU №2148014) simpler and less expensive way to get a new microporous crystalline material, hereinafter referred to as a-type zeolite A-LSX. This zeolite is structure representing the advantages of zeolites of type a, and zeolite type X. in Addition, the zeolite is particularly suitable for use in detergents because it provides high power and speed of removal present in water ions of calcium and magnesium at normal temperature washing.

It should be noted that the zeolite A-LSX provides ion-exchange capacity and rate of exchange of calcium and magnesium are much greater than those obtained when simple physical mixing of the zeolite types a and X. in Addition, the zeolite A-LSX percentage of zeolite LSX is 20-30 wt.%, that is sufficient to achieve the desired goals from the point of view of the exchange capacity and speed of exchange of ions of calcium and magnesium. However, if necessary, the percentage of type zeolite LSX can reach 90 wt.%.

The lack of type zeolite A-LSX is the fact that the zeolite has an average particle diameter from 0.9 to 10 μm, including extreme values, preferably from 1.5 μm to 5 μm, including extreme values. Introduction zeolites in the composition of the CMC is associated with certain difficulties, because zeolites are dusty powder with a particle size of 1.5 to 5.0 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 CMC with 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 receptor detergents.

There is a method of producing granulated engineering CMC components with high bulk weight, containing 15-20 wt.% ethoxylated with ethylene oxide alcohols With12-C24or other nonionic oxyalkylated surfactant, 5 wt.% anionic surfactants, 40-80 wt.% inorganic fillers (tripolitsa the sodium, zeolite type a, sodium metasilicate, soda ash, sodium sulfate), 0.5 to 10 wt.% politologist, polycarboxylic acids, toluensulfonate sodium CMC, optical Brightener and 10-20 wt.% adsorption or crystallization water (application Germany No. 3434864, M CL 01D 11/02, 1986).

The disadvantages of this method is:

1. The content of environmentally harmful compounds of phosphorus, which, falling into natural water bodies, causing their poisoning (eutrophication).

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:

- 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 wt.% zeolite, 5-30 wt.% soda (sodium carbonate), 5-15 wt.% sodium silicate and 25-60 wt.% water;

- 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 surfactant (Patent When And No. 4406808, CL 252-91, 1983).

This method has the following disadvantages.

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 blending.

2. Using, as raw materials for the preparation of granules, coarse zeolite type X, which obviously has 30-40 wt.% lower KOS in Cao than the zeolite of type a, and a lower KOS on MgO, due to the presence of particles of zeolite up to 15 microns.

3. The use of zeolites (raw materials) with a particle size of 15 μm, because the smaller the size, the higher KOS zeolite as Cao and MgO, and therefore, it is desirable to use 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 No. 2016846, SW 33/34, 1994), which provides for mixing of solutions of silicate and sodium aluminate with a molar ratio of SiO2/A2O3equal to 2.0 to 2.5; crystallization of the formed silicoaluminate in type zeolite And at a temperature of 60-100°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 aOH, 5-30 g/l SiO2in 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 wt.% zeolite type a, 25-30 wt.% soda, 2-8 wt.% sodium silicate, 2-5 wt.% sodium hydroxide and 2-15 wt.% water. The product has a KOS on Cao 190-200 mg/g and fractional composition of 80-200 μm.

One of the disadvantages of this method is the possibility of obtaining zeolite component CMC only in the form of microspherical granules (60-200 microns), making them impossible to use in the production of CMC dry mixture. Other low KOS on MgO, since the zeolite type a (NaA) has a high ion-exchange properties when exchanging cations of Na+CA2+and low - in the exchange of Na+Mg2+.

A method of obtaining granulated synthetic zeolite used in the compositions of the CMC (A.C. USSR №1159885, SW 33/28, 1985). The method involves spraying a gas injector of a liquid medium to powdered zeolite with his stirring apparatus with vibracijam 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). what are square granulated zeolite with a binder with a particle size of 0.2-2.5 mm

The known method has the following disadvantages.

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 less than 15 wt.% water (humidity), as a way not provided for drying the granules at a temperature above 100°C. As a result, the finished product crumpled and loses flowability during storage and transportation, which makes it impossible for its use in the production of CMC dry mixture and significantly complicates its use in the production of CMC tower" way (through repulpable and subsequent spray drying).

The well-known "Method of obtaining a granulated synthetic zeolite" (AS the USSR №1156726, 01J 2/20, 2/28; SV 33/28, 1985).

According to this method, the zeolite with a humidity of 20-40 wt.% 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 80°and the number of pseudo is to achieve 0,8-1,2. Get granular zeolite with a binder with a residual moisture content of 5 wt.% and mechanical strength 7-10 kgs/cm2(0.07 to 0.1 kgf/mm2).

This method has the following disadvantages.

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, it is not possible to talk about a granulated product of a complex compound consisting of zeolite and CMC (SAS), necessary for the production of CMC ratio. In recipes CMC zeolite is 10-15 wt.%, and desirable CMC content of about 1 wt.%. If you enter the granular zeolite obtained according to the method, the composition of the CMC in the amount of 10-15 wt.%, the content of CMC will be only 0.05÷0,5-0,075÷0.75 in. 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 tie the irradiation is provided by using only powdered CMC, what complicates the process of mixing with the zeolite and leads to heterogeneous granules and, consequently, may result, with such a small amount of the binder is 0.5 to 5.0 wt.%, to 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.

6. The use of zeolite type a, as the use of coarse zeolite type X, yields a granular component CMC having a low KOS on MgO.

The closest in technical essence and the achieved result of the present invention is a method of obtaining a granulated synthetic zeolite component CMC" (Patent RU №2230778, C11D 3/02, SW 39/22, 2004), which is chosen for the prototype.

According to the method, the fine zeolite type X (predominant crystal size 1-3 μm) is mixed with carboxymethylcellulose (CMC), taken in an amount of 5-10 wt.%, considering the dry zeolite. Moreover, CMC is used in the form of a dry powder or in aqueous solution. The mixture ekstragiruyut. Cutting granules are dried in a belt dryer at a temperature of 130-180°C. Then the granules are crushed and the resulting powder is classified to produce a marketable fraction with a size of 0.2-2.5 mm smaller fraction produced during crushing, again upravlyaut mixing with a binder.

The known method has drawbacks.

1. Low cation exchange capacity (KOS) CMC component to the cations CA2+(X Cao).

2. Not a high cation exchange capacity (KOS) CMC component to the cations of Mg2+(X MgO). Not quite the optimal composition of the CMC component that would meet the requirements of modern compositions CMC.

The task of the invention is to develop a method of producing granulated synthetic zeolite component CMC with improved quality in the high part of KOS on Cao and MgO, balanced with a complex structure (zeolite + surfactant), i.e. the component of the CMC, which can be used in the production of modern detergents by dry blending of raw materials.

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 0.9-3.0 mm) of the zeolite, namely type A-LSX, carboxymethylcellulose, taken in an amount of 3-15 wt.%, considering the dry zeolite. Moreover, CMC is used in the form of a dry powder or in aqueous solution, as in the prototype.

Analysis of the known methods of production of synthetic zeolite and granulated zeolite component CMC showed chipolata fine zeolite type X, the mixture of zeolite with CMC, extruding the mixture with obtaining graft granules and subsequent drying is known. Also known is a method of obtaining and use of CMC powder type zeolite A-LSX. However, only the fact of mixing fine (primary crystal size of 0.9-3.0 mm) of the zeolite, namely type A-LSX, CMC, taken in an amount of 3-15 wt.%, considering the dry zeolite, allows after drying at a temperature of 130-180°to 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 the formulations of modern detergents and high KOS on MgO and Cao.

Previously known process steps: the use of a binder in the form of an aqueous solution of CMC, extruding the mixture, crushing and subsequent classification of the granules produce the desired particle size (0.2 to 2.5 mm), necessary to ensure the possibility of using CMC component in the process of production of detergents by dry blending the 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 conclusion is highlighted in the following.

Mix superfine (mainly the size of the crystals of 0.9-3.0 mm) type zeolite A-LSX (humidity 20-40 wt.%) with CMC, taken in the form of a dry powder (particle size ≤1.5 mm) or aqueous solution, in the amount of 3-15 wt.% by weight of dry zeolite. 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 130-180°in vapor environment. Get a mechanically stable of 0.4-1.0 kg/mm2(40-100 kg/cm2) granules containing 85-97/15-3 wt.% type zeolite A-LSX and CMC, in terms of dry matter, respectively. Granules are crushed to obtain fractions of 0.2-2.5 mm and classified by screening. The fraction less than 0.2 mm again sent for mixing with a binder. Commodity granular synthetic zeolite component CMC has a high KOS on MgO and Cao, flowability, not pilot is not destroyed during transportation and storage and is used in the production of CMC by dry blending.

Example

100 g of fine zeolite A-LSX with moisture content of 20 wt.% mixed with 8.9 g of CMC (added in the form of a solution). The mixing is carried out until a smooth paste. Pasta ekstragiruyut through the die plate screw granulator. The resulting cuttings dried at 130°in vapor environment. On ucaut mechanically strong 0.8 kg/mm 2(80 kg/cm2) pellets containing 90 wt.% type zeolite A-LSX and 10 wt.% CMC, in terms of dry substance. Granules are crushed to obtain fractions of 0.2-2.5 mm and classified by screening. The fraction less than 0.2 mm re-directed to mixing with the binder.

The resulting sample is analyzed.

Calcium ion exchange carried out using a device with an electrode for a specific ion in the standard system. Measure the metabolic ability of the sample to the calcium ion. For this purpose, 1 liter of an aqueous solution containing calcium chloride in the amount of 3,135 mmol of calcium, and 20 cm3buffer solution with a pH of 10.2 mixed and incubated at a constant temperature of 22°C. After immersion pre-stabilized and calibrated specifically for the calcium electrode impose a sample of zeolite corresponding to 1 g of anhydrous product. After 15 minutes, measure the amount of calcium ions in solution.

Magnesium ion exchange carried out on the same device, a modified application of the electrode, specifically designed for magnesium ions. For this purpose, 1 liter of an aqueous solution containing magnesium chloride in the amount of 3,135 mmol magnesium, and 20 cm3buffer solution with a pH of 10.2 mixed and incubated at a constant temperature of 22°C. After immersion pre-stabilized and kalibrovochnye on the magnesium electrode impose a sample of zeolite, corresponding to 1 g of anhydrous product. After 15 minutes, measure the amount of magnesium ions in solution.

Component properties CMC and other data examples are presented in the table.

Use in the preparation of CMC component of the proposed method of zeolite A-LSX with a crystal size greater than 3.0 μm leads to deterioration of the cation exchange capacity (KOS) on Cao and MgO commercial product (example 6 comparative).

The composition and properties of the granular synthetic zeolite component CMC
ExamplesThe composition of the CMC component, zeolite/CMC, wt.%KOS on MgO, mg/gX CaO, mg/gStrength, kg/mm2Return fraction <0.2 mm, wt.%
The placeholderX/CMC = 90-95/10-570-7375-800,6-0,815-30
1A-LSX/CMC = 90/101361720,815
2A-LSX/CMC = 85/151151541,010
3A-LSX/CMC = 97/31502000,435
4A-LSX/CMC = 99/1 (comparative)155 2100,245
5A-LSX/CMC = 80/20 (comparative)1021361,27
6A-LSX/CMC = 90/10 zeolite size of 5.0 μm (comparative)1301620,815

A method of obtaining a granulated synthetic zeolite CMC component comprising a mixture of zeolite and binder - carboxymethyl cellulose (CMC), extruding the mixture, drying the granules at a temperature of 130-180°With their fragmentation fractionation to produce commodity chips with a size of 0.2 to 2.5 mm and the return fraction crumb less than 0.2 mm in a mixture with a binder, characterized in that the mixture serves fine a-type zeolite A-LSX with a crystal size of 0.9 to 3.0 μm and CMC use in the amount of 3-15 wt.% in terms of dry zeolite.



 

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FIELD: technological processes; chemistry.

SUBSTANCE: fine-grained zeolite of A-LSX type with crystal size of 0.9-3.0 micrometer is mixed with carboxymethyl cellulose (CMC), taken in the amount of 3-15 wt % in conversion to dry zeolite. Mixture is extruded. Granules are dried at 130-180°C, crushed and fractionated for production of end product with particle size of 0.2-2.5 micrometer. Fraction of particle with size below 0.2 mm are returned to mixing with CMC.

EFFECT: increase of cation-exchange efficiency.

1 tbl, 7 ex

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SUBSTANCE: fine-grained zeolite of LSX type with crystal size of 1-3.0 micrometer is mixed with carboxymethyl cellulose (CMC), taken in the amount of 3-15 wt % in conversion to dry zeolite. Mixture is extruded. Granules are dried at 130-180°C, crushed and fractionated for production of end product with particle size of 0.2-2.5 micrometer. Fraction of particle with size below 0.2 mm are returned to mixing with CMC.

EFFECT: increase of cation-exchange efficiency in CaO and MgO.

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