Fluorescent concentrate for coloring polyethylene and method thereof

 

(57) Abstract:

The inventive development of the final form of coloring substances, in particular the composition migrationology.com dye concentrate and the means of obtaining it used for fluorescent staining of polyethylene in mass. The concentrate contains a high-pressure polyethylene 53,37 - 58,37% , liquid paraffin for the production of protein-vitamin concentrate 4,73 - 10,24% , daylight fluorescent pigment based melamineformaldehyde or melamineformaldehyde polymer and fluorescent component 34,58 - 36,45% , formaldehyde scavenger (ammonium salt) 0,69 - 2,28% . A method of obtaining a concentrate is that in the mixer load granulated polyethylene and daylight fluorescent pigment in the form of pieces of size 2 - 120 mm, stirred at ambient temperature until the pigment particle size 0.5 - 1.0 mm, the mass add liquid paraffin and continue to grind the mixture for 0.5 - 2.0 hours, then connect the heating, add formaldehyde scavenger and continue to grind a lot at 120 - S 1.5 to 2.5 hours 2 C. p. F.-ly, 5 PL.

The invention relates to the ATA, used for fluorescent staining of polyethylene in mass.

The most common and cheapest method of dyeing polyethylene is the so-called method of "dry" painting, which involves dusting granules of the polymer and subsequent homogenizing it into the molten polymer during processing.

However, this method has significant drawbacks. In its application it is impossible to obtain products with high quality paint, it is difficult to achieve different color and exact concentration of the pigment in the polymer remain low and sanitary working conditions due to significant dust workshop, which is due to the shedding of dye from the surface of the granules in the process of dusting and during processing. In addition, the low adhesion of the powdered pigment to the granules of polyethylene is not possible to mechanize the process of dyeing (transfer of powdered pigment polyethylene impossible pneumatic transport due to the shedding of pigment and sticking it on the inside of the pipe wall).

Partially it is possible to improve the adhesion of the dye to the polymer granules, applying wetting agents: vaseline oil is completely not solve the issue of improvement of sanitary and hygienic working conditions, quality of painting, the possibilities of mechanization of the process.

One of the factors that affect the quality of staining, is dispersible dyes and pigments in the district requested the polymer. The most famous way of getting legalisierung forms is the creation of concentrates or masterbatches. The processes of dyeing with the use of such final form of pigments, providing a high degree of dispersion of particles of the dye, gradually begin to replace other types of dyeing processes. As of 1980 , the EEC countries 60% of the colored polyolefin was produced by this method (compared to 50% in 1975 ). In the 80-ies in the United States from the sphere of dyeing of plastics dry pigments almost completely supplanted final forms of the pigments.

Domestic industry does not produce fluorescent concentrates for dyeing of polymers. Abroad fluorescent concentrates produced by the Company "Swada (London), and the form "Hoechst" (oral information of the exhibition "Chemistry-87) and the study obtained from representative samples.

Also known is a method of obtaining concentrates containing fluorescent pigments and synthetic materials such as polyethylene, polypropylene is at a temperature of 150-180about, Shutter speed for 30-60 min and grinding it to powder.

The disadvantage of this method of obtaining a concentrate is a powder discharge form that does not allow you to evenly distribute powder concentrate among the granules of the polymer.

In recent years, the domestic industry produces aluminescent the masterbatch polyethylene (TU 6-05-05-149-81), which includes the following components, wt. % : Polyethylene wax 36,0-47,1

The high-pressure polyethylene 24,0-31,4 Dyes of 40.0 to 15.0

Such a masterbatch is produced by mixing all the components in the internal type mixer at a temperature of 180-190aboutC, followed by pouring the mass of baking, cooling and crushing the obtained superconcentrate to particle sizes of 0.3 to 3.0 mm

The masterbatch make it possible to obtain dyeing of polymers of different saturation, reduce dust workshop.

However, polyethylene, painted concentrates on the basis of the specified structure, not always evenly and accurately painted. Good quality paint will get some organic pigments and varnishes, and concentrates nastava should be attributed to the low viscosity of the melt, due to the presence in the structure of the polyethylene wax in a concentration of up to 47% , which has a plasticizing effect on the coated polyethylene, complicates plastic grinding pigments, and also causes the release of superconcentrate in the form of crushed crumbs. The irregular shape of the particles of crushed crumbs complicate the process of mechanical dosing superconcentrate.

On the basis of the indicated composition was obtained fluorescent concentrate containing the following components, percent :

Fluorescent fluorescent

pigment (Suite) on the basis of

melamineformaldehyde-

formaldehyde or

melaniemadisont-

sulfamethazole-

tion (MTSF) polymer and

fluorescent are total 25 titanium Dioxide 10

Polyethylene wax PV-200 39

Polyethylene VD brand 12003-200 26

After synthesis and unloading of the apparatus pigment is a colored pieces of brittle porous mass (size pieces reach 100-120 mm), which must be milled to a size of 5-50 microns, providing a high quality paint polyethylene. The grinding process is time consuming, leads to high pollution workshop, nepozvoliteljno load the mixture of high-pressure polyethylene (low density) brand 12003-200 and polyethylene wax and heated to 200aboutC for 2 h, after which the mixture is stirred for 2 hours Then reduce the temperature to 180aboutWith and into the mixer load the calculated amount of crushed as described above powdered pigments. Dispersion of pigments produced within 3 hours, and every 30 min to change the direction of rotation of the blades of the agitator. Molten concentrate is poured in a thin layer on the pallet, covered triacetate film; after partial solidification of the mass cut with a knife into pieces the size of 2x2 see After complete cooling, the pieces are crushed to crumbs.

The disadvantages of this concentrate are bad colorimetric properties due to the poor distribution Suite in concentrate (point and activate the dye agglomerates in painted concentrate polyethylene), low melt viscosity, which does not allow to obtain a concentrate in the form of granules and produce plastic grinding pigment, the release of formaldehyde into the environment in the process of obtaining a concentrate and in the manufacture of colored products, not enough high brightness colored polyethylene.

The aim of the invention is to improve the uniformity of distribution of the pigment in the hub, the increase is due to the high dispergirovannom dye concentrate), process simplification and improvement of sanitary-hygienic working conditions.

This objective is achieved in that famous composition comprising high-density polyethylene (GOST 16337-77) and a coloring component - Suite-based MTSF-polymer and fluorescent component according to the invention contains liquid paraffin for the production of protein-vitamin concentrates (TU 38.101856-84) and formaldehyde scavenger in the following ratio, wt. % :

The high-pressure polyethylene 58,37-58,37

Paraffin liquid for Pro-

production of protein-Vita - mine concentrates 4,73-10,24

Suite for coloring

polyethylene-based

MTSF-polymer and Lumi - nascentes component 34,58-36,45

The absorber formalde guide 0,69-2,28 as well as the fact that the method of obtaining a concentrate comprising a mixture of initial components and homogenization of the mixture by heating and subsequent unloading of the finished product, according to the invention, the source of the polyethylene used in the form of granules, and sequential function - in the form of pieces size 2-120 mm, the mixing is carried out at ambient temperature until the pigment particle size 0.5-1.0 mm, then the reaction mixture was added liquid paraffin on THE 38.101856-84 and continue ismalic the aldehyde and homogenize the mass at 120-145aboutC for 1.5 to 2.5 hours

As the formaldehyde scavenger can be used ammonium salts: ammonium bicarbonate, ammonium acetate, and other, forming with formaldehyde of low connectivity products.

As the basis in the concentrate used high-pressure polyethylene in the form of granules, which also fulfills the role of a grinding agent, which allowed us to apply the pigment is not in powder form and in the form of pieces, and to renounce the use of milling machines. The use of polyethylene in the amount below the lower limit (experiment 4) leads to the formation of poorly homogenized with polyethylene pigment which forms agglomerates of pigment for coloring polyethylene. The increase in the concentration of polyethylene above the upper limit of (6) leads to the decrease of saturation concentrate.

Liquid paraffin (TU 38.101856-84) is a mixture of n-alkanes with a small (1% ) impurity content isoparaffins, naphthenic and aromatic hydrocarbons. Start boiling point not lower than 200aboutWith, the end boiling point not higher than 320aboutC, flash point not lower than 80aboutC.

Liquid paraffin facilitates the grinding of the pigment in the cold from 0.5-1.0 mm to is Eniseli components of the composition.

For binding of residual formaldehyde is usually used phenols, simple and complex esters, glycols. The best of the investigated substances recognized as malonic ether.

The use of ammonium salts for binding of formaldehyde is unknown and is not obvious, because they do not react with formaldehyde and reacting the product of decomposition of the ammonia as it obrazovaniya.

Fluorescent fluorescent pigments on the basis of MTSF-polymer and fluorescent component intended for coloring polyethylene and have a high migration resistance. They are well crushed and homogenizers with other components of the concentrate, which allows to obtain colored polyethylene with high quality distribution of pigment.

Obtaining fluorescent concentrate is heated in the internal mixer of the type equipped with a Z-shaped blades, auger unloading device for granulating mass.

In the mixer load granulated polyethylene (GOST 16337-77) and daylight fluorescent pigment in the form of pieces for the specified recipe and stirred at room temperature in the mixer for 0.5 to 2.0 hours At this crush is his grinding the pigment to the mixture of liquid paraffin (TU 38.101856-84) and continue grinding by stirring the mixture at room temperature for 0.5 to 2.0 hours to obtain a homogeneous thin suspension. Then connect the heating, add formaldehyde scavenger and homogenize the mass at a temperature of 120-145aboutC (the optimal temperature of 130-135about(C) for 1.5-2.5 h, after which the pulp is cooled, cut into granules. Sometimes to improve the grinding of the pigment in weight add acetone, which is then fully Argonauts when heated mass.

The obtained fluorescent concentrate is a colored granules.

According to the claimed technical solution is made and investigated the composition of the concentrates, containing a Suite of different colours:

Suite orange-red. C. N 649735) (as fluorescent component used a mixture of N-familymed-4-aminonaphthalene acid and rhodamine R j), see table. 2.

Suite lemon yellow for polyethylene (A. C. N 649736, THE 6-09-4926-80) (as fluorescent component used N-familymed-4-aminonaphthalene acid); see table. 3.

Suite yellow 2664 (and. C. N 1484826, THE 6-09-26-652-88) (MTSF-polymer is a polycondensation product of melamine, urea, n-toluensulfonate, formaldehyde and fluorescent component of the N-aminoamide-4-morpholinothio acid); see table. 4.

Suite bright orange for the polyethylene shall Rosolini-3] -N-phenylnaphthalene), see tab. 5.

The quality of the concentrates is determined by the properties of the concentrate and painted them with high-pressure polyethylene, which must meet certain requirements: the color should be uniform without agglomerates dye, Suite and liquid paraffin should not migrate to the surface of the dyed polyethylene, physico-mechanical and colorimetric properties of polyethylene should not deteriorate, the content of formaldehyde released into the working area in the dyeing of polyethylene should be minimal.

The uniformity of dyeing of polyethylene is characterized by the localization of retained pigment in point, and include (agglomerates), larger than 0.2 to 0.5, inclusive, which recorded visually similar to THE 6-05-05-149-81 "Masterbatch pigments (CRU)",

In addition, the degree distribution of the pigment concentrate is determined by the number of transparent inclusions (particles of pigment, not mixed with the other components of the concentrate in the concentrate (table. 2-5).

The definition of migration sustainability carried out also according to THE 6-05-05-149-81.

Determination of tensile strength and relative elongation carried out according to GOST 14236-31.

Colorimetry.

Specific examples of the preparation of the concentrate fluorescent fluorescent pigments based on MTSF-polymer and fluorescent components.

P R I m e R 1. In a mixer with a capacity of 25 liters, equipped with a Z-shaped mixer, auger for unloading concentrate, heater, load 7 kg (53,37 wt. % ) of granulated polyethylene brand 103030-020 and 4.52 kg (34,58 wt. % ) daylight fluorescent pigment in the form of pieces of porous size 2-120 mm and stirred at room temperature for 1.5 h, then add 1,22 kg (10,24 wt. % ) liquid paraffin THAT 38.101856-84 and continue stirring at room temperature for 2 h Connect the heating, add 0,19 kg (about 1.35 wt. % ) of ammonium bicarbonate and continue heating at 145aboutAnd the mass is mixed for 1.5 hours Then the pulp through a die, cooled, cut into granules.

P R I m e R 1A (table. 4).

Carried out analogously to example 1, but the pieces of porous Suite size 2-120 mm was stirred at room temperature for a period of 0.25 h

P R I m e R 1B (table. 4).

Carried out analogously to example 1, but after adding ammonium bicarbonate continue heating and stirring for 1.0 hours

P R I m m e R 2.

P R I m e R 2A (PL. 2).

Carried out analogously to example 2, but the temperature of mixing of the finished concentrate is 110aboutC.

P R I m e R 3.

In the mixer, similar to that described in example 1 load 7 kg (57,12 wt. % ) of granulated polyethylene brand 108-08 and to 4.46 kg (36,45 wt. % ) daylight fluorescent pigment in the form of pieces of porous size 2-120 mm and stirred at room temperature for 1.5 h, then add 0.7 kg (5,73 wt. % ) liquid paraffin THAT 38.101856-84 and continue stirring at room temperature for 1.0 hours Then connect the heating, add 0.08 kg (0,69 wt. % ) acetic acid ammonium and continue stirring at 135aboutWhen="ptx2">

Carried out analogously to example 3, but the temperature of mixing of the finished concentrate is 155aboutC.

P R I m e R 3b (table. 3).

Carried out analogously to example 3, but the time of grinding the mass to obtain a homogeneous suspension is 0.25 PM

Other examples 4-11 summarized in table. 1-5, which shows the formulations and the results of the studies concentrate and painted them with polyethylene. Examples 12-14 describe the production of concentrate using powdered Suite.

P R I m e R 12. In a mixer with a capacity of 25 liters, equipped with a Z-shaped mixer, auger for unloading concentrate, heater, load 7 kg (53,37 wt. % ) polyethylene VD brand 12003-200, to 4.52 (34,58 wt. % ) Sequential function lemon yellow for polyethylene in powder form (TU 6-09-4926-80) and 1.22 kg (10,24 wt. % ) liquid paraffin THAT 38.101856-84 for the production of PVC and stirred at room temperature for 0.5 hours Then connect the heating, add 0,19 kg (of 1.85 wt. % ) of ammonium bicarbonate, continue heating at a temperature of 120aboutAnd the mass is mixed for 1.5 hours the pulp through a die, cooled, cut into granules.

P R I m e p 13. In the mixer, similar to that described in example 12, the load 7 kg (57,12 wt. % C. N 649735) and 0.7 kg (5,73 wt. % ) liquid paraffin THAT 38.101856-84 for the production of PVC, stirred at room temperature for 1.0 h, connect the heating, add 0.08 kg (0,69 wt. % ) acetic acid ammonium and continue stirring at 135aboutWith over 2,0 including the pulp through a die, cooled, cut into granules.

P R I m e R 14. In the mixer, similar to that described in example 12, the load 7 kg (58,37 wt. % ) polyethylene VD brand 10803-020, 4,15 kg (34,62 wt. % ) Sequential function yellow 2664 in powder form (TU 6-09-26-652-88), 0,56 kg (4,73 wt. % ) liquid paraffin for the production of PVC, stirred at room temperature for 0.5 h, connect the heating, add 0,27 kg (2.26 wt. % ) of ammonium bicarbonate and continue stirring at 145aboutWith over 1,5 hours the pulp through a die, cooled, cut into granules.

P R I m e R 15. In the mixer, similar to that described in example 12, the load 7 kg (58,37 wt. % ) polyethylene VD brand 10803-020, 4,12 kg (34,62 wt. % ) Sequential function bright orange for polyethylene in powder form (TU 6-09-26-569-87), 0,56 kg (4,73 wt. % ) liquid paraffin for BVK, stirred at room temperature for 1.0 h, connect the heating, add 0,27 kg (2.26 wt. % ) of ammonium bicarbonate and continue stirring at The quality of the concentrates is determined by the properties of the concentrates and painted their high-pressure polyethylene (see table. 2-5).

Staining polyethylene concentrate is produced by mixing the concentrate and pellets of polyethylene and subsequent processing into articles by extrusion or injection molding.

In the preparation of the concentrate according to the method prototype on the plate size HH,3 mm has 5-10 inclusions pigment size of 0.5-2.0 mm. Similar plates made of the proposed composition of the inclusions does not have (PL. 2-5).

The quality distribution of pigments in polyethylene, painted the proposed composition, good, agglomerates dyes are absent (PL. 2-5).

Presented in table. 2-5 data migration Suite and liquid paraffin testify about their migration resistance. The lack of migration of liquid paraffin from concentrate is a guarantee of migration sustainability in painted declare concentrate polyethylene.

Physico-mechanical properties of polyethylene films, painted the proposed composition of the concentrate and the concentrate prototype, indicate the absence of the impact of the proposed composition on the tensile strength and elongation of the films (table. 2-5).

Content is considerably reduced formal (0.04 to 0.17 mg/m3), dramatically reduced dust work areas when the grinding of the pigment after its synthesis (eliminated stage grinding of the pigment in the mills of the type "Excelsior"), and at colouring concentrate polyethylene (the polyethylene granules are mixed with pellets of the concentrate without causing dusting). (56) Kamenskaya So Century. and other Staining on polymer materials. L. : Chemistry, 1985, S. 18.

Lambs N. N. Structurally colored polymers and materials based on them. M. , 1987, S. 85.

Symposium on fluorescent pigments, M. , 1987, S. 10, 12.

Patent Germany N 2546118, CL 09 To 11/06, 1971.

Report of ONPO "Plastpolymer", N 2167-34; 01840067821, L. , 1984, S. 50.

1. Fluorescent concentrate for coloring polyethylene, including high density polyethylene and daylight fluorescent pigment based melamineformaldehyde or melamineformaldehyde polymer and a fluorescent component, characterized in that, with the aim of improving the uniformity of distribution of the pigment concentrate, improve color and physico-mechanical characteristics of colored polyethylene, as well as improving sanitary and hygienic working conditions, the concentrate further sosnosky ammonium in the following ratio of components, wt. % :

The high-pressure polyethylene 53,37 - 58,37

Liquid paraffin for the production of protein-vitamin concentrates 4,73 - 10,24

Daylight fluorescent pigment based melamineformaldehyde or melamineformaldehyde polymer and fluorescent component 34,58 - 36,45

Ammonium bicarbonate or ammonium acetate 0,69 - 2,28

2. The method of obtaining fluorescent concentrate for coloring polyethylene by mixing the high-pressure polyethylene with a daylight fluorescent pigment based melamineformaldehyde or melamineformaldehyde polymer and fluorescent component and homogenizing the mixture by heating, characterized in that, to simplify the process and improve sanitary and hygienic working conditions, the polyethylene used in the form of granules, and daylight fluorescent pigment in the form of pieces of size 2 - 12 mm, the mixing is carried out at ambient temperature until the pigment particle size 0.5 - 1.0 mm, followed by introduction of the mixture of liquid paraffin for the production of protein-vitamin concentrate, the crushing weight for 0.5 - 2.0 hours to obtain the GNSO 120 - 145oC for 1.5 to 2.5 hours

 

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FIELD: dyes and pigments.

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EFFECT: improved properties of dyes.

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2 cl, 1 dwg

FIELD: luminescent materials.

SUBSTANCE: invention provides novel electroluminescent material comprised of injecting layer, metal chelate complex-based active luminescent layer, hole-transition layer and hole-injecting layer. Luminescent substance is selected from oxyquinolate metallocomplexes of zinc 8-hydroxy-2-methoxyquinolate and zinc 8-hydroxy-2-methylquinolate. Electroluminescent material shows emission in green spectrum region.

EFFECT: increased heat resistance and widened choice of stable green-emitting materials.

2 cl, 3 ex

FIELD: organic chemistry.

SUBSTANCE: invention relates to new individual compounds of benzoxazine class and to a method for their preparing. Invention describes 2-aroylmethylene-2,4-dihydro-1H-3,1-benzoxazine-4-ones of the formula (I): wherein R means hydrogen atom (H) (a), -CH3 (b), -OCH3 (c), -OC2H5 (d), chlorine atom (Cl) (e) eliciting fluorescent properties and stable in UV-light. Also, invention a method for preparing abovementioned compounds. Proposed compounds elicit fluorescent properties and can be used as the parent substances for synthesis of new heterocyclic systems.

EFFECT: improved preparing method, valuable properties of compounds.

4 cl, 6 ex

FIELD: capillary defectoscopy; compositions of the color penetrants.

SUBSTANCE: the invention is pertaining to the color capillary defectoscopy, in particular, to the compositions of the color penetrants applied to the color control over the items of the high-duty. The penetrant contains the mixture of the following composition: xanthene dyes of the yellow-orange fluoresceine and red-dark blue rhodamine of 3-6 %, the surfactant of 10-40 %, the rest - the dissolvent. The ratio of the mixture of the yellow-orange and the dark blue - red dyes compounds 1:2, as the surfactant use neonol or syntanol. The technical result of the invention is creation of the color penetrant of the lowered volatility, the reduced flammability, the extra-high sensitivity ensuring detection of the minimal flaw with the opening width of 0.5-1 microns and the improved reliability and stability of the monitoring of the items in conditions of repairs and operation.

EFFECT: the invention ensures detection of the minimal flaw with the opening width of about 1 micron, improved reliability and stability of the monitoring of the items in conditions of repairs and operation.

1 tbl

FIELD: polymer materials.

SUBSTANCE: invention provides luminescent material showing semiconductor properties and being product of complex polymerization in glow discharge, which is formed as a supported polymer layer located either between electrodes or on any of electrodes. Starting pyrromethene complex is difluoroborate complex of 1,3,5,7,8-pentamethyl-2,6-diethylpyrromethene (Pyrromethene 567). Method of preparing luminescent semiconductor polymer material comprises glow-discharge polymerization for 2 to 120 min of Pyrromethene 567 vapors at temperature preferably 250-350°C, pressure 10-1 to 10-2 Pa, and discharge power 0.5-3 W. Resulting luminescent polymer is characterized by thickness preferably 0.001-10 μm, conductivity 1·10-10 to 5·10-10 Ohm-1cm-1 (20°C), luminescence emission maximum in the region of 540-585 nm at band halfwidth 55-75 nm. Polymer is obtained with quantum yield 0.6-0.8 and is designed for creation of film light-emitting devices.

EFFECT: improved performance characteristics of material.

13 cl, 3 ex

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