Method of producing siccative for paint materials

FIELD: chemistry.

SUBSTANCE: invention relates to production of siccatives which enable to dry paint materials based on alkyd, uralkyd and oily film-formers. The method of producing a siccative involves reaction of 2-ethylhexanoic acid with zinc oxide, cobalt hydroxide and manganese dioxide (pyrolusite) with successive feeding of components: zinc oxide at 90-100°C, cobalt hydroxide at 110-120°C, manganese dioxide (pyrolusite) at 120-130°C with simultaneous addition of ethylene glycol, followed by addition of a solvent: white alcohol and/or nefras C4, and/or rocket engine fuel TS-1 or mixtures thereof.

EFFECT: broader capabilities of using the siccative, low power consumption, high hardness of the film of the paint material.

2 tbl

 

The invention relates to the production of drying, ensuring the drying of paints and varnishes based on alkyd, Uralkalij and oil film-forming.

The driers are catalysts for liquid-phase free-radical polymerization by oxygen residues of unsaturated fatty acids in paint and varnish materials. As driers are commonly used soluble in oils and organic solvents connection of some transition and non-transition metals (Co, Mn, Pb, Zn, Zr, and others) - mainly salts of monocarboxylic acids (Soaps). The most common soap 2-ethylhexanol and 2-italytravel, naphthenic acids.

In paints driers are usually administered in the form of two or three-component mixtures containing Sol transition (Co, Mn and others) and intransitive (Pb, Ca and others) metal. The amount of added metal is determined by its activity, and the selection of combinations of metals is their synergistic effects. The most common Co-Pb, Mn-Pb, Pb-Mn-Co, Co-Mn-Zn, etc.

In industry driers receive two ways. The most common deposition method, based on exchange reactions occurring in aqueous solution between the metal salt and alkaline soap of the appropriate acid (e.g., patent of Russia №2182916, 2131446, 2261882, 2266939, MCL C09F 9/00). The General disadvantage of this method is the fast availability of large amounts of sewage, containing alkaline impurities and heavy metals, the multistage and the complexity of the process, loss of solvent.

Another method of production is a fusion of the oxides, hydroxides or salts (carbonates, acetates) metal with acids at 320-360°C. (Chemical encyclopedia, vol-4, Moscow, Great Russian encyclopedia, 1995, s-670)

A method of obtaining the desiccant interaction oxides (hydroxides) of metals of variable valency with carboxylic acid dissolved in mineral spirit. (patent GB891858, 21.03.1962).

From the patent GB891858, is known for use as compounds siccatives metal oxides (hydroxides) cobalt, manganese, zinc and others, and as organic carboxylic acids using 2-ethylhexanol acid.

The proposed method for the desiccant is fundamentally different from the well-known the United Kingdom patent GB 891858:

a way of getting mixed 3 metal drying agent, and not odnomernogo;

- known project proposes the dissolution of the carboxylic acids in mineral spirit to the stage of interaction of the acid with oxides (hydroxides) metals, water distillation and unreacted low molecular weight acids, administered at the initial stage of the process, which increases the production losses, impact on the environment, increases the cost of the production process.

From the local method of getting drier by fusing at a temperature of 240-260°C pre-dehydrated sunflower oil with a mixture of pyrolusite, oxide of cobalt and titanium dioxide (Ed. St. USSR 632713, MCL C09F 9/00, publ. 1977). The disadvantage of this method is the high temperature process, resulting in the burning of organic products. Desiccant obtained in this way is characterized by a low metal content and high color.

A method of obtaining a fused lead-manganese drier by dehydration of vegetable oil and fusing it with further heating with lead oxide and manganese dioxide at a temperature of 190-200°C (patent of Russia №2141499 C1, MCL C09F 9/00, publ. 1999) Disadvantages: high temperature fusing, additional stages of the process: hydrolysis of the oil with water and dehydration.

Closest to the claimed method is a method of getting drier by fusing lead litharge and pyrolusite with fatty acid component, which is used as the high-boiling fraction of α-branched monocarboxylic acids having an acid number 119-175 mg KOH/g, the process is carried out at 170-200°C (ABT. St. USSR №1261275, MCL C09F 9/00, publ. 1984)

A significant disadvantage of this process is the high chromaticity of the obtained product (600 mg J2/100 g in a mixture with linseed oil), which leads to the impossibility of its use in paints bright and white tones, and low concentration of metals dissolve in the e of the desiccant. The scarcity and variability of the composition of monocarboxylic acids, which is waste, it is not possible to obtain a stable composition and properties of the driers. High temperature process requires high energy consumption in the production of drying.

The prototype of the claimed method is a method of obtaining light desiccant interaction zinc oxide or lead with 2 ethylhexanoic acid with two heated to 105°C for the first and up to 120°C at the second stage in the presence of a reaction accelerator, which is used as the unsaturated low molecular weight cooligomers, and further dilution in an organic solvent, in which a mixture of white spirit with 25-75% of the mass. distillation of unreacted hydrocarbon polymerization of liquid pyrolysis products. Synthesis of drying is conducted at a molar ratio of the initial reagents: zinc oxide or lead: 2-ethylhexanoate acid = 1,0:1,7-2,5 (patent of Russia №2281308 C2 (1), MCL C09F 9/00).

A significant disadvantage of this method is its applicability to get only odnomernogo drying agent, i.e. desiccant containing one metal (zinc or lead). In the paint industry are, as a rule, mixed driers, ensuring the required degree of drying film coatings for the production of which require the tsya several odnomernykh driers mixed in the required proportions. As a result, there is a need to install additional equipment and personnel. Complicated technological preparation of mixed driers, increase energy costs and production costs. In addition, the known method is two-stage, more complex, requires the introduction of an accelerator of the reaction. Received desiccant has a high viscosity (up to 196-200), which complicates its use at low temperatures, especially in winter.

The task facing the creators of the invention is the expansion of technological capabilities (i.e. the scope of the desiccant), the possibility of its application for Uralkalij paint materials, improved stability and catalytic activity of the desiccant, reducing energy consumption for the process by sequential loading into the reactor, the source of raw materials and the introduction of ethylene glycol.

The problem is solved by using as a fatty acid component 2-ethylhexanoic acid with an acid number 365-390 mg KOH/g, as metal-containing compounds of zinc oxide, cobalt hydroxide and manganese dioxide. The proposed combination of the components and the method of obtaining enable the process of obtaining a mixed 3-component of the second desiccant in a single reactor in a sequential loading of components. Upon receipt of this desiccant in the industry required 4 stage: 3 stage receiving one-component drying stage and mixing them in a certain ratio. In this case, required or reactors of different size due to significant differences dosing odnomernykh driers or at full load reactor wastage of raw materials, the increase in stocks odnomernykh driers, large power consumption, which greatly reduces production efficiency.

The tests have shown high efficiency and stability of mixed cobalt-manganese-zinc desiccant when used for drying is not only alkyd enamels and oil paints at a concentration of 1.5-2.5% wt. in relation to the film, but also a new class Uralkalij paint materials at a concentration of 1.5-2.5% wt. in relation to the film-forming.

The essence of the invention is that the method of obtaining a drying agent for paints and varnishes by fusing zinc oxide, cobalt hydroxide and manganese dioxide with a fatty acid component as a fatty acid component used 2-ethylhexanoyl acid with an acid number 365-390 mg KOH/g with a progressive download component: zinc oxide at 90-100°C, cobalt hydroxide at 110-120°C, manganese dioxide p and 120-130°C with simultaneous introduction to reduce the reaction temperature of the glycol in the amount of 3-5% wt. with respect to manganese dioxide (pyrolusite).

The main functions used siccative metals:

Zinc is used as an auxiliary drier. Slows down the initial rate of drying of the surface, but accelerates bulk drying. Increases the hardness of the film coatings. Improves wetting and dispersing pigments. Used as antiseptic additives. Improves spill coatings. Protects the film from wrinkling.

Recommended amount: 0,10-0,20% metal dry substance.

Cobalt is one of the most active metals to accelerate the surface of the drying film. Sub pellicle layer remains fluid, which causes puckering of thick films, independently almost not used, but only in a mixture with other metals. The desiccant has a blue-violet shade, less effect on the color change of the film in the wet state and aging utverzhdenii of the paint film in comparison with other driers. The most widely used desiccant that requires smaller dosage and thus provides the most rapid effect of coating formation.

Recommended amount: 0,05-0,10% metal dry residue.

Manganese is one of the most active siccative metal, accelerating the drying of the film, both at the surface and in volume. The main disadvantage is due to the color of the t is to a as a light brown divalent manganese goes mainly in dark brown trivalent manganese. Requires exact matching of concentration, overdose of desiccant may lead to a reduction in the rate of drying.

It is recommended to use in combination with cobalt, lead.

Recommended amount: 0,06-0,12% metal dry substance.

The proposed method for spot 3 metal cobalt-manganese-zinc desiccant with the content of the active metals: cobalt, 0.5 to 1.0 wt.%, manganese 1.0 to 2.0 wt.%, zinc 2.0 to 4.0% by weight. allows you to get efficient, cost-effective desiccant, combining the advantages of its constituent odnomernykh driers (synergistic effect).

The method is as follows:

In a reactor equipped with a stirrer and reflux condenser, download 2-ethylhexanoyl acid, with constant stirring download zinc oxide, gradually increase the temperature to 90-100°C and stirred until complete dissolution. Download hydroxide cobalt, increase the temperature to 110-120°C, stirred until complete dissolution.

Download manganese dioxide (pyrolusite), ethylene glycol, raise the temperature of the reaction mass up to 120-130°C and stirred for 4-5 hours at this temperature until complete dissolution of the components (the control is carried out visually on the transparency of the sample on a glass plate). The optimum temperature range of the heat detected by experiment.

The molar ratio of the starting components: cobalt hydroxide: of manganese dioxide: zinc oxide: 2-ethylhexanoate acid 0,067-0,074:0,144-0,159:0,243-0,268:1,0 respectively.

The concentrated cobalt-manganese-zinc desiccant analyze for metals, cooled, diluted with organic solvents (white spirit (GOST 3134-78), and/or nefras-4 (TU 0251-003-78158825-2008) and/or jet fuel TS-1 (GOST 10227-86) or their mixture) 53,0-77,0% wt. to obtain the commodity form of desiccant. As the fatty acid component used 2-ethylhexanoyl acid (TU 2431-0353505711-01), as the zinc component is zinc oxide (GOST 10262-73), as cobaltstream component hydroxide cobalt II (TU 2611-001-469133-78-2002), as the mn containing component is manganese dioxide (pyrolusite) (TU 6-10-1806-86).

The activity received drying agent was tested on the drying time of paint coatings to grade 3 at 20°C according to the method set forth in GOST 19007-73, standard varnish PF-060 (TU 2311-007-98438521-2008) and WRF-1105 (TU 2310-003-98438521-2008), the hardness of the film according to GOST 5233-89.

Recipes and technological modes of obtaining driers are presented in table 1, properties driers obtained by the proposed method in comparison with the properties of the desiccant obtained by the method described in the prototype presented in table 2. The results shown in tables 1, 2 allow to draw a conclusion about the achievement of the goal.

The technical result from application of the proposed method is to obtain in a single reactor at a progressive download source components and certain temperature conditions in the presence of reducing the temperature of the process additives, ethylene glycol mixed ternary cobalt-manganese-zinc desiccant with a certain ratio of the active metal. This will allow to extend the possibilities of application of desiccant to reduce the energy consumption for its production and cost, to increase the hardness of the film of paint material.

The effectiveness of the obtained driers confirmed by the results of the laboratory tests OOO PKF "Laura" (Shebekino) on the drying time of alkyd (PF-060) and walking (WRF-1105) varnishes (table 2). A test report is attached.

The problem to which the invention is directed resolved.

2. The number of cooligomers from initial reagents, % wt.
Table 1.
A method of obtaining a drying agent for paints
Recipes and technological modes of obtaining dryers
Index Desiccant
the prototype of the " sample No. 3
New dryers
Sample 1Sample 2Sample 3Sample 4Sample 5
1. The molar ratio of reagents:
Hydroxide cobalt:: 2-ethylhexanoate acid-0,067:1,00,071:1,00,074:1,00,071:1,00,071:1,0
Manganese dioxide:: 2-ethylhexanoate acid-0,144:1,00,152:1,0strength of 0.159:1,00,152:1,00,152:1,0
Zinc oxide:: 2-ethylhexanoate acid1:2,50,243:1,00,256:1,00,268:1,00,256:1,00,256:1,0
2,0-----
3. The number of ethylene glycol from loading manganese dioxide, % wt.-5,05,05,03,04,0
4. Downloads (g/%)
2-ethylhexanoate acid617/53,1318,2927,3936,5327,3927,39
Zinc oxide100/8,612,493,744,993,743,74
unsaturated niskama the molecular cooligomers 14,3/1,23-----
a mixture of white spirit and distillation430/37,03-----
The cobalt hydroxide-0,791,181,581,181,18
Diocese manganese-1,582,373,162,372,37
Ethylene glycol-0,080,120,16 0,070,09
The solvent (TS-1)-76,7765,2053,5865,2553,61
ONLY1161,3/a 100.0100,0100,0100,0100,0100,0
5. Stage process: (1st level)
Temperature, °C105909090100100
Time, h0,90,50,50,50,50,5
6. Stage process: (2-I the stupa is ü)
Temperature, °C120110110110120120
Time, h1,80,50,50,50,50,5
7. Stage process: (3rd level)
Temperature, °C-120120120130130
Time, h-5,04,54,04,04,0

the figure 2.
A method of obtaining a drying agent for paints
The properties of the desiccant
IndexDesiccant on the prototype of the " sample No. 3New dryers
Sample 1Sample 2Sample 3Sample 4Sample 5
1. Mass fraction, %
Cobalt-0,50,751,00,750,75
Manganese-1,01,52,01,51,5
Zinc162,03,04,03,03,0
2. The density PR is 20°C kg/m 31047895895897895895
3. Viscosity by viscometer B3-246 at a temperature (20,0±0,5)°C, with160 (B3-4)1011111111
4. Color by iodometric scale, mg of iodine/100 cm3151010101010
(when diluted 1:10 GOST 1003-73)
5. The storage stabilityStable over the years (at ambient temperature)Stable over the years (at ambient temperature)
7. Activity in the varnish PF-060 (1.5% drying), drying time to degree 3 at 20°C, hNo data22-2320-21 18-1920-2120-21
8. Activity in the lacquer WRF-1105 (1.5% drying), drying time to degree 3 at 20°C, hNo data6-76-75-65-65-6

A method of obtaining a drying agent for paints and varnishes by reacting 2-ethylhexanoic acid with zinc oxide, a hydroxide of cobalt and manganese dioxide for a progressive download component: zinc oxide at 90-100°C, cobalt hydroxide at 110-120°C, manganese dioxide at 120-130°C with simultaneous introduction to reduce the reaction temperature of the glycol in the amount of 3-5 wt.% with respect to manganese dioxide and a molar ratio of initial components: cobalt hydroxide:of manganese dioxide:zinc oxide:2-ethylhexanoate acid 0,067-0,074:0,144-0,159:0,243-0,268:1,0 with the subsequent introduction of solvent: white spirit, and/or nefras C4, and/or jet fuel TS-1 or mixtures thereof in the amount of 53,0-of 77.0 wt.%, providing the content of the active metals in the mixed cobalt-manganese-zinc desiccant: cobalt, 0.5 to 1.0 wt.%, manganese 1.0 to 2.0 wt.%, zinc 2.0 to 4.0 wt.%.



 

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FIELD: chemistry.

SUBSTANCE: invention relates to production of siccatives which enable to dry paint materials based on alkyd, uralkyd and oily film-formers. The method of producing a siccative involves reaction of 2-ethylhexanoic acid with lead oxide, cobalt hydroxide and manganese dioxide (pyrolusite) with successive feeding of components: lead oxide at 90-100°C, cobalt hydroxide at 110-120°C, manganese dioxide (pyrolusite) at 120-130°C with simultaneous addition of ethylene glycol, followed by addition of a solvent: white alcohol and/or nefras C4, and/or rocket engine fuel TS-1 or mixtures thereof.

EFFECT: broader processing capabilities, low power consumption.

2 tbl

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SUBSTANCE: siccative is obtained by fusing 2-ethylhexanoic acid with a mixture of lead oxide (yellow lead) and cobalt hydroxide. Fusion is carried out while feeding said components simultaneously at temperature 110-120°C and molar ratio of cobalt hydroxide, lead oxide and 2-ethylhexanoic acid of 1.0:2.8-10.4:7.4-17.8, respectively. Further, a solvent white alcohol and/or nefras C4 and/or jet engine fuel TS-1 or mixture thereof is then added in amount of 50-58 wt %.

EFFECT: ensuring drying of paint materials based on alkyde, uralkyde and oily film-forming materials.

3 tbl

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2 tbl

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Liquid hardening // 2447114

FIELD: chemistry.

SUBSTANCE: invention relates to curing agents for air-drying alkyd-based resins, coating compositions, such as paint, varnish, wood stain, inks and linoleum floor coverings. Described is a curable liquid medium containing a) from 1 to 90 wt % of an alkyd-based resin and b) from 0.0001 to 0.1 wt % of a siccative in form of an iron or manganese complex with a tetradentate, pentadentate or hexadentate nitrogen donor ligand.

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6 cl, 3 tbl, 3 ex

FIELD: polymer materials and corrosion protection.

SUBSTANCE: invention relates to cold-drying anticorrosive coating compositions, which can be used in petroleum, gas, power, chemical, and other industries for protection surfaces of iron articles and structures. Composition of invention is based on binder, namely alkyd-styrene resin or poor alkyd resin in amount 11.0-44.0%. Composition further comprises 0.3-5.0% tannin or tannin derivatives as anticorrosive additive, 3.0-24.0% pigments, 5.0-22.-% fillers, and balancing amount of organic solvent.

EFFECT: enhanced protective properties.

4 cl, 2 tbl, 5 ex

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