Method of making chromate anticorrosive pigment

FIELD: chemistry.

SUBSTANCE: described is a method of making chromate anticorrosive pigment involving suspension of spent chrome-aluminium catalyst in aqueous solution of calcium nitrate and barium nitrate, taken in amount of 10-30% and 5-25% of the mass of catalyst respectively, in mass ratio of catalyst to the said nitrates equal to 65-70:30-35 respectively, dehydration of the obtained mixture with subsequent calcination at 800-900°C for 3-6 hours and grinding. The obtained pigment has anticorrosive effectiveness which surpasses that of the closest analogue by 6-40% and has lower cost.

EFFECT: use of pigment in ground coating improves anticorrosive properties of the coating and increases environmental friendliness.

1 cl, 1 tbl, 15 ex

 

The invention relates to the field of protecting metals from corrosion coating, specifically to a method for producing chromate anticorrosive pigment-based waste homalomena catalyst.

It is known that the main protective function in the system of coatings on metals perform primers, anti-corrosive action of which is largely determined by the type of pigment and its quantitative content in the primer. The most effective are anti-corrosive pigments and inhibitors present in the primer composition can suppress corrosion processes even in violation of the integrity of the protective coating. The most widely used anti-corrosion pigments are finely dispersed substances containing chromium in the higher oxidation state (Cr (VI).

The problems resulting from technological progress in various fields of industry, is the depletion of the natural resource base. Alternative sources of raw materials are industrial waste, containing valuable components.

In particular, a method of obtaining from galvanostatic ferrites of calcium related to the anti-corrosion pigments that protect the metal by means of giving an alkaline reaction corrosive environment, see Makarov V.I., Ladygina O.V., Indacin E.A. fer the of ITA calcium on the basis of galvanic sludge - new effective anti-corrosion pigments // Paint-and-lacquer materials. - 1999. No. 5 - p.3-4.

A method of refining in anticorrosive pigment zinc-iron-phosphate waste process phosphating of steel, see Smirnov S.A. and other anti-Corrosive primer based on zincphosphate sludge // Sbtes. Dokl. nauch.-technology. the meeting. "Application of anti-corrosion coatings in the urban economy, Moscow, 5-6 June, 1989. M.: 1989. p.15.

A method of obtaining corrosion of iron oxide pigment from raw materials containing iron oxide, including leaching of the raw material, drying and grinding, in which the feedstock used used iron oxide catalyst, the waste in the production of isoprene, butadiene, styrene or methylvinylpyridine by dehydrogenation of the corresponding olefinic or alkylaromatic hydrocarbons, see inventor's certificate SU # 1557990, MPK SS 1/24, 1997

Raw material for producing chromate anticorrosive pigment is used chronologicaly the catalyst, resulting in many chemical and oil refineries. The catalyst is dispersed composition comprising the oxide of Cr (III) and minor amounts of oxide CR (VI). The oxide of CR (VI) is highly soluble in water, resulting in an attempt to directly use the specified environment is Yes as anticorrosive pigment has not led to a positive result, as water-soluble compounds reduce the insulating properties of pigmented coatings and quickly washed away by contact with an aqueous medium, see Auvin. Anticorrosive properties of pigment synthesized based on waste homalomena catalyst, and designing primers based on it. The dissertation on competition of a scientific degree of candidate of technical Sciences. - Kazan state technological University, 2002

A method of obtaining chromate anticorrosive pigment, including the suspension in the water is pre-crushed in a ball mill waste homalomena catalyst and calcium oxide (1-25% by weight of catalyst) at a ratio of T:W=1:1, the dehydration of the mixture, calcining it at 750°C with subsequent grinding of the obtained product in a vibratory mill, see Groceryman, Lgeria, Nmilenov and other "anti-Corrosion pigments from waste production and operation homalomena catalyst // Paint-and-lacquer materials and their application. 1998, No. 6, p.8-10. The source of this information is decorative and molar-technical properties of the pigment (color, opacity, content of water-soluble substances) without anti-corrosion characteristics.

Reproduction of the above-described method of producing pig is enta based on waste homalomena catalyst confirmed the characteristics of the pigment, however, corrosion tests showed the absence of the anti-corrosion properties, see Appswell, Sunstein, Ehanyrov, Auvin. Inhibiting pigment-based waste chromium catalyst // Paint-and-lacquer materials and their application. 2005, №7-8, p.54-58.

The closest to the technical nature of the claimed invention is a method for chromate anticorrosive pigment, including the suspension in water of the oxides of calcium and barium spent homalomena catalyst, dehydrating the resulting mixture and calcining at 915°C for 3.5 hours and the grinding of the pigment, see Appswell, Sunstein, Ehanyrov, Auvin. Inhibiting pigment-based waste chromium catalyst // Paint-and-lacquer materials and their application. 2005, №7-8, p.54-58.

The disadvantage is obtained chromate pigment is not sufficiently high corrosion performance.

The task of the invention is to improve the anticorrosion efficiency of chromate pigment derived from spent chromium catalyst.

The technical problem is solved by a method of obtaining chromate anticorrosive pigment, including suspension exhaust homalomena catalyst with compounds of calcium and barium, obezvozhivani the resulting mixture and calcining and grinding, in which the suspension is conducted in aqueous solution of calcium nitrate and barium nitrate, taken in quantity, respectively 10-30% 5-25% of the weight of waste homalomena catalyst when the mass ratio of waste homalomena catalyst and these nitrates equal to 65-70:30-35, respectively, and the calcination is conducted at temperatures of 800-900°C for 3-6 hours.

Technical solution allows to improve corrosion performance of pigment compared to the prototype by 10-40%.

Example 1 specific performance.

Chromate anticorrosive pigment was prepared as follows: first dissolved in 100 cm3water and 30 g of calcium nitrate and 5 g of barium nitrate, respectively 30 wt.% and 5 wt.%, then lead the suspension obtained in the solution of 65 g - 65 wt.% spent homalomena catalyst. After dehydration of the mixture, the product is calcined at a temperature of 820°C for 4 hours, and then pulverized.

Examples 2-15 similar to example 1. The performance conditions and the corrosion rate of efficiency shown in the table.

The resulting pigments are finely dispersed powders yellow-green color, differing in intensity and hue.

For evidence of corrosion properties of the synthesized pigments were investigated interaction Avodah extracts. As a control sample used tetrachromat zinc (GOST 16763-79)related to the most widely used in practice chromium anticorrosive pigments. Aqueous extract of pigments prepared in accordance with known methods, see the book Iagellonicae, Day, Iautomate. Laboratory pigments and pigmented paints, varnishes and lacquers. L.: Chemistry, 1990, s.

In chemical beaker with a capacity of 150-300 cm3placed 15 g of the pigment, poured cylinder 50 cm3distilled water, heated to boiling and boiled for 30 minutes, the Suspension is cooled, the filtrate is poured into the cylinder and bring the volume to 50 cm3distilled water, then mixed with an equal volume of a 6%aqueous solution of sodium chloride. The resulting aqueous extract is used for testing the next day after cooking.

Aqueous extract of lead pigments in contact with the steel 08 KP and can stand up to the establishment of a constant value of the electrochemical potential of the steel. If the steady-state electrochemical potential of the steel ranges of values that is appropriate to its passive state, in aqueous extract or solution of the inhibitor continuously dispense a 5%aqueous solution of sodium chloride. In the dispensing process control the electrochemical potential of the steel. When up is achieving critical concentration of sodium chloride there is a sharp decrease of the electrochemical potential of the steel in the area of active dissolution. The value of the critical concentration of sodium chloride CNaClCRan indicator of the anticorrosion efficiency of aqueous extracts of the studied pigments. The increase of this indicator corresponds to strengthen their pestiviruses actions, see Stepin S.N., Wahin AV, Pelts AV, Ziganshina MR research Method of anticorrosive properties of pigments and pigmented coatings // Paint-and-lacquer materials and their application. 2000, No. 1, s-27.

Table
# ExampleThe content of nitrates to mass homalomena catalyst, wt.%Mode on ignitionCNaClCR, mmol/DM3
Ca(NO3)2·4H2OBa(NO3)2Temperature,
°C
Time, h
123456
1305820 4338
23058604335
33059005343
420158003337
520158204372
620158503362
720109004392
815208205421
9 15208504418
1015208506420
1115208305426
1210258405390
1310258206378
1410258505392
1510258502371
The placeholderChromate anticorrosive pigment 9153,5305
Control sampleTetrachromat zinc312

Thus, the claimed method allows to obtain a chromate anticorrosive pigment, beyond the prototype anticorrosion efficiency by 10-40%, and also widely used tetrachromat zinc on 7-37%. The use of the obtained pigment claimed method comprising primers increases anticorrosive properties.

Recycling of spent chromium catalyst, polluting, aggressive, and sometimes toxic substances, can improve the environment and reduce the cost of anticorrosive pigment.

The method of obtaining the chromate anticorrosive pigment, including suspension exhaust homalomena catalyst with compounds of calcium and barium, dehydration resulting mixture and calcining and grinding, characterized in that the suspension is conducted in aqueous solution of calcium nitrate and barium nitrate, taken in quantity, respectively 10-30% 5-25% of the weight of waste homalomena catalyst when the mass ratio of waste homalomena katal the congestion and these nitrates, equal to 65-70:30-35, respectively, and the calcination is conducted at temperatures of 800-900°C for 3-6 hours



 

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