A method of obtaining a composite pigment

 

(57) Abstract:

Use: for coloring plastics, plastic materials, synthetic fibres, and in the manufacture of paints and varnishes. The essence of the invention: a method of obtaining a composite pigment includes processing inorganic carrier hydroxide of alkaline metal, then the organosilicon amine and then adding to the reaction mixture of hydrochloric acid to the equimolar ratio with the specified amine. Next on the processed media to instill sulfoacetate in the form of sodium salt in the reaction mixture is injected calcium chloride, allocate the obtained pigment and dried. Components taken in the following ratio, wt.h.: inorganic carrier 100; the alkali metal hydroxide of 0.2 - 0.5; organosilicon amine 0,3 - 3,0; direct or acid dye 5 - 25; calcium chloride is 0.1 - 0.5. 1 C. and 8 C.p. f-crystals, 1 table.

The invention relates to a process for the synthesis of composite pigments in which the organic dye is chemically bound with an inorganic carrier. Composite pigments suitable for the manufacture of paints, coloring of plastics, plastic materials and synthetic fibres.

Iswm aminopropyltriethoxysilane with subsequent inoculation acidic organic dye [1].

The disadvantages of this method are the use of the acid form of sulfonates having low solubility in water and low concentration of dye grafted to the surface, which causes the transparency of the coating and loss of use of colored material as a pigment.

In the prior art there is also known a method of producing pigment by grafting organic dye with reactive groups at the silicon atom to the inorganic carrier [2].

The disadvantage of this method is the necessity of using organic solvents, special synthesis of dyes with reactive groups.

As the closest analogue to the proposed invention, the selected method of obtaining a composite organic-inorganic pigment, including interaction organosilicon amine with oxides of titanium, aluminum, silicon or mixtures of these oxides and the subsequent inoculation of organic dye containing specially introduced reactive groups are epoxy, isocyanate, chlorosulfonic, and so on, the selection of the obtained pigment from the reaction mixture and drying [3].

The disadvantage of this is TEZ dyes with reactive groups.

Task to be solved by the present invention is directed, is the production of composite pigments having improved complex characteristics color density, hydrophobicity and oil absorption, as well as the expansion of the range of cheap inorganic carriers through the use of siliceous waste mining of coal and fly ash of thermal power plants.

A new method for producing a composite organic-inorganic pigments includes a step of activating the surface of the inorganic carrier hydroxide of an alkali metal. Activated inorganic carrier is treated with the organosilicon amine and then adding to the reaction mixture of hydrochloric acid to the equimolar ratio with the organosilicon amine. Then carry out the inoculation of sodium salts sulfoacetate with subsequent introduction into the reaction mixture of calcium chloride. Source components to obtain a composite pigment taken in the following ratio, wt.h.:

Inorganic media - 100

The hydroxide of an alkali metal - 0,2-0,5

Organosilicon amine - 0,3-3,0

Sodium salt of sulfatases - 5-25

Calcium chloride - 0,1-0,5

As kremsier ,

where

R= C2H5, R1= (CH)2)3, R2= R3= H (I), R=C2H5, R1=(CH2)3, R2=R3=CH2CH (OH)CH2OOCC(CH3)=CH2(II), R=C2H5, R1=(CH2)3, R2=H, R3= CH2CH(OH)CH2OOCC(CH3)= CH2(III), R= C2H5, R1= CH2, R2= H, R3=(CH2)6NH2(IV), R= CH3; R1=(CH2)3, R2=R3=H (V), R=CH3; R1=(CH2)3, R2=H, R3=(CH2)2NH2(VI).

All used organosilicon amines are commercially available products:

I - am-9 - aminopropyltriethoxysilane, THE 6-02-724-77

II - Recondensed - 3-N,N-[bis(2-hydroxy-3-methacryloxypropyl) amino] propyltriethoxysilane, THE 6-02-1-036-91.

III - Cocondensate - 3-N-[(2-hydroxy-3-methacryloxypropyl) amino]propyltriethoxysilane, THE 6-02-1-802-94.

IV - AGM-3 - [(6-aminohexyl)aminomethyl]triethoxysilane, THE 6-02-586-86.

V - A-1100 - 3-aminopropyltrimethoxysilane, the product of the company Union Carbide.

VI - Z-6020 - [3-(2-amino-ethyl)aminopropyl]trimethoxysilane, product of Dow Corning.

We used azo-, diazo-, triphenylmethane is The 6-36-0204187-412-90, acid bright red G GOST 16164-79, acid scarlet OST 6-14-37-80, direct yellow To GOST 14178-78, direct bright orange GOST 26023-83, straight black 2C GOST 21810-76, direct ruby lightfastness MU GOST 23378-78.

As the inorganic carrier used titanium dioxide, aluminum hydroxide, calcium carbonate, precipitated or pyrogenic silicon dioxide (white carbon black, silica, Aerosil), various silicates (talc, kaolin, powdered quartz). Also can be used as the inorganic carrier siliceous waste mining of brown coal (rock) with the content of SiO260-64 wt. %, Al2O326-30 wt. %, impurities else, THE 113-03-0020951070-93, and fly ash of thermal power plants.

Example 1. Mix 5 kg white black with 125 ml of 20% NaOH solution for 15 min, incubated 40 min, add 50 ml of aminopropyltriethoxysilane (AGM-9), stirred for 15 min, incubated for 40 minutes add 22 ml of concentrated HCl (equimolar ratio with AGM-9), mix, make a solution of the dye acid yellow lightfastness (750 g in 150 ml water), stirred for 1 h, add 25 g of CaCl2, stirred for 15 min, separated pigment by filtration, dried at 110-120oC for 1.5 h, the Output of the pigment 92%. With the g, abrasive capacity of 4.1% in the Same way were getting pigments in examples 2-47, the results of which are shown in the table.

The resulting pigments are loose not agglomerated powders, insoluble in water, intensely colored, not migratory in the painted material. Characteristics of the pigments listed in the table.

Testing of pigments was carried out according to GOST 11279-83. The organic dyes. Test methods for pigments and varnishes.

Abrasive capacity was determined by the weight loss of the friction plates with a suspension of the pigment. In relative units abrasive capacity of the media was:

Fly ash from thermal power 100

Powdered quartz - 19

Talc - 15

Chalk - 2,3

Abrasive capacity of the obtained pigments listed in the table.

From the table it follows that the proposed method allows to obtain organic-inorganic pigments with a high content of grafted dye (from 1 to 25%) and improved characteristics in coverage and hydrophobicity. The new method makes possible shot dye in an inert medium (as, for example, in the case of titanium dioxide) and pozvolyayuthee their abrasive capacity up to 10 times (breed), that reduces wear and clogging of the pigment particles from natira. The use of calcium chloride upon receipt of the pigments in 1.5-2 times better ukryvistosti

1. A method of obtaining a composite pigment interaction inorganic carrier with silicone Amin, further grafting of the organic dye, the selection of the target product and drying, characterized in that the interaction is subjected to an inorganic carrier, pretreated with alkali metal hydroxide, one or more organosilicon amines of the formula

(RO)3SiR1NR2R3,

where R = CH3C2H5;

R1= (CH2)3CH2;

R2= H, CH2CH(OH)CH2OOCC(CH3)=CH2;

R3= H, CH2CH(OH)CH2OOCC(CH3) = CH2, (CH2)6NH2, (CH2)2NH2,

with the subsequent addition of hydrochloric acid to the equimolar ratio with silicone Amin, inoculation organic dye, which is used as direct or acid dyes, and the introduction of the reaction mixture of calcium chloride for subsequent mixing ratio, mA is in 0,3 - 3,0

Direct or acid dye - 5 - 25

Calcium chloride - 0,1 - 0,5

2. The method according to p. 1, characterized in that the inorganic carrier used substance selected from the group comprising titanium dioxide, aluminum hydroxide, calcium carbonate.

3. The method according to p. 1, characterized in that the inorganic carrier used precipitated or pyrogenic silicon dioxide selected from the group comprising white carbon black, Aerosil, and silica gel.

4. The method according to p. 1, characterized in that the inorganic carrier used aluminosilicate.

5. The method according to p. 4, characterized in that the aluminosilicate used substance selected from the group comprising talc, kaolin, powdered quartz.

6. The method according to p. 4, characterized in that the aluminosilicate use the breed, which is the waste mining coal with a content of SiO260 - 64 wt.%, Al2O326 - 30 wt.%, impurity - rest.

7. The method according to p. 4, characterized in that the aluminosilicate use fly ash of thermal power plants with the content of SiO260 - 64 wt.%; Al2O326 - 30 wt.%, impurity - rest.

8. The method according to any of paragraphs.1 - 7 different the group, including aminopropyltriethoxysilane, 3-N,N-[bis(2-hydroxy-3 - methacryloxypropyl)amino] propyltriethoxysilane, 3-N-[(2-hydroxy-3-methacryloxypropyl) amino] propyltriethoxysilane, [(6-aminohexyl)aminomethyl] triethoxysilane, 3-aminopropyltrimethoxysilane, [3-(2-amino-ethyl)aminopropyl] trimethoxysilane.

9. The method according to any of paragraphs.1 to 8, characterized in that as a direct or acid dye used azo-, triphenylmethane and antrahinonovye sulfoacetate.

 

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15 cl, 3 dwg, 5 tbl

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20 cl, 14 dwg, 7 tbl, 15 ex

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7 cl, 10 dwg, 13 ex

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