Powder dodge and composition based polyolefin resin

 

The invention relates to powder clarifier number sorbitol-xylitol-acetaline connections for clarification of a semicrystalline polyolefin resins and compositions based on it. The composition is obtained by mixing Dodge the specified number with the polyolefin resin by heating the mixture from a temperature above the melting temperature of the resin and up to at least 170oAnd stirring the mixture until complete dissolution of the resin. The proposed clarifier eliminates the haze of polyolefins during their processing. 3 S. and 17 C.p. f-crystals, 3 tab., 10 Il.

This invention relates to the field of processing of polyolefins and applies powder clarifier used in this area. According to the invention as used Dodge powder acetals xylitol or sorbitol. The invention also relates to compositions based on polyolefin resin obtained by adding a specified clarifier.

The use of bleaching substances for reduction of turbidity particles of crystalline polyolefins are well known. Representatives of acetals of sorbitol and xylitol, which were used as brightening substances listed in the following U.S. patents: - Hamada and others, the patent is tetali sorbitol, having at least one chlorine or bromine - Deputy - Kobayashi and others, U.S. patent 4532280 Di (methyl - or tilsammen benzyliden)-sorbite - Williams and others, U.S. patent 4845137
Derivatives dibenzylidene-sorbitol having at least one substituted group containing sulfur
Kobayashi and others, U.S. patent 4954291
A mixture of diacetate sorbitol and xylitol obtained from a mixture of dimethyl - or trimethylsilanol benzaldehyde and unsubstituted benzaldehyde
- Rekers., U.S. patent 5.049.605
Bis-(3,4-dialkylanilines)-sorbite, including deputies, forming a carbocyclic ring.

Additionally, the basic structure of bleaching chemicals used in the polypropylene described in the publication of the patent description Japan 85157213/26 (Mitsubishi Petroch K. K.) and 88130662/19 (Sumitomo Chem. Ind. K. K.).

Production brightening substances known from the above references from Murai, and other U.S. patent 3721682 and patent description GB 2115405 A New Japan Chemical Comp.

I think that Dodge should melt and recrystallization, forming a very thin mesh on the inside of the polyolefin. This crystalline grid provides the formation of active centers, which reduces the size of the spherulite formed in the polymer during cooling. Small spherulites scatter VI is arachnet.

Transparent polypropylene obtained by mixing clarifier with the main polyolefins, during which introduce other additives, such as antioxidants, acid acceptors and grease, and then ekstragiruyut mixture at a temperature of about the melting point of bleaching substances.

A more popular method of obtaining a transparent polyolefin includes pre-mixing of all or some of the additives with part of the main polymer with obtaining powder masterbatches. Uterine mixture is metered into the extruder with the addition of the basic polymer, which eliminates the need for large mixers. When the extrusion is usually formed small granules.

Alternative itself uterine mixture can be extruded and granulated. These concentrates pellets can be mixed with the polyolefin, which ekstragiruyut without additives to obtain a product having the desired concentration of bleaching substances, usually from 0.01 to 2 or 3 wt.%.

There are a number of difficulties associated with the use of sorbitol or xylitol-acetaline brightening agents in polyolefins. One of the big problems is the formation of "white spots" or bubbles in the production process of the resin. Small bubbles formed at injecti is.

One approach found by experiment, is the introduction of small amounts of polar fatty additives such as glycerylmonostearate or fatty amides, the content of the sorbitol acetal transparent polyolefin. These additives reduce the number of bubbles observed in the produced batches, but do not resolve the problem. In addition, polar fatty additives leads to plaque on the surface or slowly migrate on the surface of the receiving parties and form a "wax" growths that are not removed.

The second approach used to solve bubbles containing sorbitol and xylitol acetal transparent polygeline is melting the polymer at the temperature for 3 to 10oFrom above the melting point of bleaching substances. Although this solution is workable, it has several significant negative aspects. Sorbitol-acetaline clarifiers are usually the melting point by 50 to 100oWith higher than polyolefins, in which they are inserted. Processing of the polyolefin at a temperature above the melting temperature of the clarifier may cause discoloration and the formation of odors in plastic. It is also difficult to control the temperature in a large production extruder, so usually at the beginning of the process is whether sublimation at a temperature of about the melting point. Treatment above the melting point of the clarifier may cause a weakening of the flow of extrusion, which may be undesirable.

The third approach used to remove bubbles or "fish eyes" in the containing sorbitol acetals transparent polyolefins, was described in U.S. patent 4954291 Kobayashi and others (especially columns 1, 2, 3, 4). This method involves the use of a mixture of diacetate sorbitol formed from a mixture of benzaldehyde and di - or trimethylamine benzaldehyde. The composition has a relatively low melting point, however, can be processed at a temperature above its melting point to avoid bubbles. However, the composition has a relatively poor degree of lightening compared to diacetylene sorbitol derived from alkyl substituted benzaldehydes.

The invention largely solves the problem of "white spots" or bubbles in a transparent polyolefin. The exact mechanism of bubble formation and the role of polar fatty additives that they play to remove bubbles, not fully understood.

In addition to diazelam sorbitol and xylitol with some success as substances forming the centers of crystallization of the polyolefin, were used salts of aromatic carboxylic acids, such as sodium benzoate is described in the polymer with the formation of active centers, sodium benzoate with a melting point above 300oWith not melted during processing and will decompose before melting. Further, it was found that sodium benzoate is not soluble and is not mixed with polyolefins. Therefore, the use of sodium benzoate as a nucleating agent depends on its dispersion in the polymer melt, which should be as large as possible: in the area from 1 to 10 microns. "Plastic Additives Handbook", Gachter et al., editor, Hanser Publishers, Munich, Germany, p.p.671-683 (1985) and Btnsbergen; "Heterogeneous Nucleation in the Crystallization of Polyolefins (1)" Polymer 11, p.p. 253-267 (1970).

Obviously, the crystallization effect of diacetals sorbitol or xylitol appears, mainly, regardless of their physical characteristics to their processing, they need to be dispersed and recrystallized in the polyolefin.

The present invention relates to the clarifiers sorbitol-xylitol-acetylenic compounds, which can be introduced into the polyolefin resin with the product without the "white spots" or bubbles, without the use of excessive temperature processing, which can cause discoloration and appearance odor.

The invention is illustrated in the drawings:
Fig. 1 is a micrograph agglomerated dibenzylideneacetone brightening prophetic is 3 - micrograph agglomerated di-(parameterbindings)-Sarbinowo brightening substances.

Fig. 4 is a micrograph agglomerated di-(paratellurite)-Sarbinowo brightening substances.

Fig. 5 is a micrograph agglomerated brightening substances mixed aldehyde-sorbitol obtained from benzaldehyde and di - or trimethylpropane benzaldehyde.

Fig. 6 is a micrograph agglomerated bis-(3,4-di-methylbenzylidene)-Sarbinowo brightening substances.

Fig. 7 is a micrograph agglomerated bis-(5',6',7',8'-tetrahydro-2-naphthalide)-Sarbinowo brightening substances.

Fig. 8 is a micrograph of ultrathin dibenzylideneacetone brightening substances, which is the product of the sputtering shown in Fig. 1.

Fig. 9 is a micrograph of ultrathin bis-(3,4-dimethylbenzylidene)-Sarbinowo brightening substances, which is the product of the sputtering shown in Fig. 6.

Fig. 10 is a micrograph of ultrathin bis-(5',6',7',8'-tetrahydro-2-naftalin)-Sarbinowo brightening substances, which is the product of the sputtering shown in Fig. 7.

All micrograph made with magnification of 1000 times.

Aswell the de p=0 or 1;
m and n are independently 0-3;
R is in each case independently selected from C1-8-alkyl, C1--alkoxy, hydroxy, halogen, C1-6-alkylthio, C1-6-alkylsulfate and 4 - or 5-membered accelgroup, forming a carbocyclic ring with adjacent carbon atoms of the unsaturated original ring.

Especially interesting brightening substances, where p=1 and the value of R is selected from C1-4-alkyl, chlorine, bromine, thioether and 4-membered alkyl group forming a carbocyclic ring with adjacent carbon atoms of an unsaturated source ring. The specific examples of brighteners according to the invention include:
dibenzylidene-sorbitol,
di(para-methylbenzylidene)sorbitol,
di(ortho-methylbenzylidene)sorbitol,
di(para-ethylbenzamide)sorbitol,
bis(3,4-dimethylbenzylidene)sorbitol,
bis(5',6',7',8'-tetrahydro-2-naftalin)sorbitol,
bis(trimethylaniline)xylitol and
bis(methylbenzylidene)sorbitol.

In the scope of the present invention also includes compounds obtained by mixing aldehydes, including substituted and unsubstituted benzaldehyde, such as the condensation product of sorbitol and a mixture of p-methylbenzaldehyde and o-methylbenzaldehyde, and the condensation product of sorbitol and a mixture of benzaldehyde and 2,4-dimethy is.

Diacetate used in the present invention, can be obtained by various known methods.

In General, these processes involve the reaction of 1 mole of D-sorbitol or D-xylitol with 2 moles of aldehyde in the presence of an acid catalyst. The temperature of the reaction will greatly depend on characteristics such as the melting point of the aldehyde or aldehydes used for the reaction.

Examples of suitable reaction media are cyclohexane, or a combination of cyclohexane and methanol. Water produced during the condensation is removed by distilleria. Usually mixed reaction occurs several hours after which the reaction mixture is cooled, neutralized, filtered, washed, e.g. with water or alcohol, and then dried.

The above link provides additional details of the synthesis brightening substances. Of course, if desired, a mixture of benzaldehyde and/or substituted benzaldehydes can be introduced into the reaction mixture.

Diacetate sorbitol and xylitol obtained by the above methods, may contain impurities are by-products of monoacetal and triacetate. To remove these impurities with the introduction of diacetone the polyolefin resin is not always necessary, but can akasol to be performed, for example, removing impurities triacetate extraction with an appropriate non-polar solvent prior to filtration. When the removal of impurities, the product can be purified so that the number of diacetyl in the composition will comprise 90% or more.

In industrial production the product is dried using heat or heat and vacuum. The product is ground using a mechanical grinding equipment with subsequent grinding in a finger or rod mill. The milled product is usually diffuse through the sieve equipment, removing a large fraction. The size of the sieve is typically 40-80 mesh for maximum particle size of between 176 and 420 microns. This definition of particle size is not very precise operation. Therefore, to determine the maximum particle size usually use the size that have 97% of particles from the total number of particles or d97. Sieves finer 80 mesh is not used, as they tend to stick together or be blocked very quickly. The ratio of rooms sit in sacks and the particle sizes of the following:
US standard ASTME 11-61
the sieve 40 mesh = 420 µm
US standard ASTME 11-61
sieve 80 mesh = 176 μm
Advances in the solution to the above problem of the "white spots" or bubble shows rbit/, obtained from Milliken Chemical, Spartanburg, South Carolina, USA, with d97250 μm and the average particle size of 84 μm, was dispersible in mineral oil and placed on a hot object table of the microscope. The sample was heated from room temperature at a rate of 10oWith in a minute. Observed the formation of bubbles on a separate particles at 223oWith up to melting particles at 228oC.

Dibenzylidene-sorbitol example 1 was investigated by scanning electron microscope with magnification of 1000 times. In Fig. 1 micrograph of the product indicates that the individual particles are agglomerated in a very small fibers or "primary particles". The surface of the agglomerates seems to be sintered or melted. I believe that these sintered particles catch the gas or volatile liquids that are released when the particle becomes soft before melting. If this process occurs during the manufacturing operations, there are white spots or bubbles. Moreover, suppose that trapped gases inside the sintered particles cause their isolation and therefore interfere with efficient heat transfer, which is required during melting and dissolution of the clarifier in the polymer melt.

Surprisingly, analysis of other promiseto all these substances are agglomerated in a very small fibers or "primary particles", the surface which seems to be sintered.

Table. 1 shows the number of the figure, a brightening agent, trade name and manufacturer of industrial products.

It was proposed to grind the sample brightening substances described in example 1 (dibenzylidene-sorbitol from Milliken Chemical, to determine the surface of the sintered particles.

Example 2
Dibenzylidene-sorbitol example 1, with d97250 μm and the average particle size of 84 μm was placed in pseudovariety layer created by the counterflow jet apparatus - model number AFG 100, manufactured by Micron Powder System. The apparatus was equipped with a deflection control type classifier. The sample was intensively sprayed and dispersed to obtain particles, characterized by d97less than 8 μm, and an average diameter of particles less than 4 microns, measured by laser light scattering. These measurements were confirmed by microscopy analysis. Fig. 8 is a micrograph of the crushed product with magnification of 1000 times. By reducing the size of the volumetric packing density of the powder sample also decreased with value (0.475) to 0,142 g/cm3.

Example 3
A small amount of ultrathin dibenzylidene-sorbitol brightening substances, which Prem the stage of the microscope. Ultrafine particles of dibenzylidene-sorbitol "disappeared" at 170oWith no air bubbles. In significant contrast to the agglomerated sintered material which must be heated to 223-228oWith before he gives off gas and then melted.

The term "dissolved" is used here to describe the phenomenon of diffusion of bleaching substances in the molten polymer at temperatures even below the melting point of bleaching substances. Given the viscosity of the polymer melt, it is not necessary to homogenize the distribution of brightening substances in the resin. However, the observed recrystallization brightening substances from the polymer melt after its dissolution.

In addition to reducing the size of the particles brightening substances in example 2, the substances listed in table. 1, were dispersed and scattered.

According to the results of the analysis of these crushed materials can be made the following conclusions.

Diacetate sorbitol or xylitol can be characterized as "filiform, crystalline primary particles having a length of 5-10 μm and a diameter of 0.3 to 0.7 μm. It was found that these primary particles and small agglomerates of these particles, consisting of several and is in a transparent polymer and insulation brightening substances during the process.

It was found necessary to apply the present invention are brightening substances in the form of a powder having an average particle size less than 15 microns. Preferably, the bleaching substance had particles, characterized by d97less than 20 microns, and an average particle size of less than 10 μm, most preferably d97less than 10 microns and the average particle size of less than 6 microns.

Besides reducing the particle size of counterflow jet fluidized bed, there are other methods that can be used in the production of sorbitol - acetaline clarifiers with chopped green particles.

Spray drying in a fluidized bed is one of the possible methods. In normal commercial production using digital shredding, followed by air classification. The most complete review of shredding technology can be found in the following articles: Kukla "Understand Your Size-Reduction Options", Chemical Engineering Process, pp. 23-35 (May, 1991); and Hixon, "Select An Effective Size-Reduction System", Chemical Engineering Process, pp. 36-44 (May, 1991).

After the jet spray may experience mechanical education or static adhesion of fiber-like particles forming the "balls" or other vague Association. However, these assets the existing technologies for brightening substances.

The distribution of particles brightening substances described here, the size was measured using the technique of laser light scattering.

The sample powder was first dispersible in water using surfactants as wetting. The turbid mixture is constantly stirred and circulated through the cell. The laser beam passes through the cell, causing scattering of light associated with the distribution of particle sizes. The scattered light is collected in the photodiode and is converted into a histogram or distribution of particle sizes. Fiber material, which is mechanically stuck, usually razobratsya and easily dispersed by this method.

In General, the results of laser light scattering are in good agreement with the results obtained by microscopic analysis. The presence of vague associations and geometric effects may cause an error in the microscopic analysis, therefore, believe that laser methods are more accurate. The polyolefin resin may include aliphatic polyolefins and copolymers obtained from at least one aliphatic olefin and one or more ethylene unsaturated co monomer. Basically comonomers, if present, are small to the improvement of the transparency of the polyolefin or be due to other properties of the polymer. Samples include acrylic acid, methacrylic acid, their esters, vinyl acetate, etc.

Samples of the polyolefin resin, the transparency of which can be greatly improved by the present invention are polymers and copolymers of aliphatic monoolefins containing from 2 to 6 carbon atoms, having an average molecular weight of from 10000 to 2000000, mostly from 30000 to 300000, such as polyethylene, linear low density polyethylene, polypropylene, semi-crystalline ethylene/propylene copolymer (statistical or block), poly(1-butene) and polymethylpentene.

The polyolefin resin of the present invention can be described as semi-crystalline, linear, regular polymers, which can optionally contain side chains that found in conventional low density polyethylene. Other polymers which can be used fine particles of bleaching substances of the present invention are polyethylene terephthalate, polyethylene terephthalate modified with glycol, polybutylene terephthalate, and polyamides.

Other additives can also be used in the compositions of the present invention, if only they will not degrade the properties. They are even beneficial Preeti and include plasticizers, lubrication, catalytic converters; antioxidants, light stabilizers, dyes, and other substances that form the centers of crystallization, etc. Some of these additives can contribute to the further improvement of useful properties, including improved aesthetic properties, ease of production and increasing its stability.

The amount of brightening substances that are added to the polyolefins may vary within wide limits depending on whether or not the composition is used as a concentrate. For use in castings take from 0.01 to 3 weight. part brightening substances on 100 weight. resin parts, preferably 0.05 to 2 weight. part of the clarifier 100 weight. resin parts. When quantity is less than 0, 01 weight. part of the characteristics of the transparent resin can be good enough, if more than 3 weight. parts there has been a slight improvement in the transparency of the resin.

It is possible to use concentrates 100 weight. parts brightening substances on 100 weight. parts of the polyolefin resin.

In industry usually used concentrates containing less than 33 weight. part brightening substances, most preferably less than 15 weight. parts brightening substances on 100 weight. resin parts.

The way igen to the industrial mixture of bleaching substances and polyolefins. The term "mixture" is commonly used to describe the process of dispersion of the clarifier in the resin when the resin is in the molten state, for example, heated to the melting point. Often the main resin that looks like a sponge, mixed with other additives, including brightening substances, and extruded. The resin usually squeeze out a second time at the end of the process of obtaining final particles, for example, by injection casting, vdavleniem casting-blown, injection casting, blowing, extrusion casting blowing, casting under pressure, rotational casting, profile extrusion, extrusion of sheets, thermal molding, film extrusion and film extrusion with orientation.

Regardless of how many times a mixture of resin and clarifier were extrudible or mixed in some other way in the molten state, it is important that the Dodge was distributed in the melt resin. In many cases, the dissolution will be accompanied by melting of the clarifier, distributed in the melt resin. However, the advantage of this method is that the clarifier can be dissolved in the melt of the resin, even without reaching the melting point of the clarifier.

In promyshlennosti change depending on the particles of the polyolefin. Typically, linear low-density polyethylene ekstragiruyut between 130 and 170oWith, polypropylene ekstragiruyut between 210 and 240oC. the above temperatures are likely to melt or the temperature of the raw material, i.e., the temperature of the polymer, than the temperature of the barrel of the extruder. It should be noted that when using a pre-prepared brightening substances, the process temperature raise 3-6oC above the melting temperature of bleaching substances.

Unlike industrial products, which are not subjected to preliminary grinding, bleaching substances of the present invention are dissolved in the polyolefin resin at temperatures below 170oC. Therefore, brighteners in the present invention may connect with the resin at temperatures below the melting point of bleaching substance, which is a great advantage in comparison with earlier methods.

The following comparative examples illustrate the unexpected improvement that are possible in the claimed invention.

Example 4
Each of brightening substances described in table. 1, was mixed with sadamakai and polymer based on polypropylene RCP 4 MFR in a paddle mixer in the following sootnoshenie the RCP 4 MFR
0,25 weight. parts of the clarifier 100 weight. parts of the polyolefin resin.

The mixture was extrudible through odnogolosy single screw extruder, with a ratio length/diameter of 32: 1, equipped with a mixing tip Maddux, at different temperatures to determine the minimum temperature required to avoid the formation of bubbles.

The initial temperature was 200oAnd it was increased by 5oIn each subsequent period of time interacting particles, if detected the formation of bubbles.

For the analysis of bubbles formed granules were investigated injection casting of these plates 2"3"0,05" if 210oWith a 40-ton injection-casting machine. Plates were analyzed visually for the presence of bubbles. The experiment was repeated after the jet spray of each of the above brightening substances in ultra-thin powder before mixing them with sadamakai and resin.

The results are presented in table. 2.

Industrial materials had dimensions d97from 180 to 420 microns and the average particle size of from 28 to 120 μm. In all cases, the melting point of brightening substances should be raised on 3-7oWith extrude the teli had d97from 4 to 20 μm and the average particle size of 2 to 9 μm. In each case ultra brightening substance could be connected with polypropylene at a minimum temperature of 200oWith in a single screw extruder.

Micrograph of ultrathin particles dibenzylidene-sorbitol, bis(3,4-dimethylbenzylidene) sorbitol and bis-(5',6',7',8'-Tetra-hydro-2-naphthalide)-sorbitol (see above footnote 1,6 and 7) shown in Fig. 8, 9 and 10, respectively.

Only a few primary particles ultra brightening substances with a reduced size of the agglomerated particles. This ultra brightening substance has the ability to mix at lower temperatures, they need less heat when loading, the reaction goes faster, which is important for the extrusion.

A method of producing compositions based on the polyolefin resin of the present invention has the advantage that it does not require the use of fatty acids and helps to avoid related problems in a transparent resin.

A significant advantage of the process at a lower temperature is no discoloration of resins, sublimation and removal of coatings and in the absence of deviations from the set value

The present invention is most favorable for diacetate sorbitol and xylitol obtained with substituted benzaldehyde, which have a relatively high melting point, i.e., melting point 250oC and above, and therefore very difficult to use in polyolefins. These brightening agents may be incorporated at temperatures above 170oWith, mainly 180-230oC.

There is, of course, many other additives and modifiers that are covered by the scope of the present invention and indicated in the claims.

The applicant has been tested at a pilot plant to confirm theory that commercially available dibenzylidene-sorbitol of Milled (MILLAD) 3905 from Milliken chemical under the compounding below the melting temperature of the clarifier can give the bubbles in the finished product; and that the same dibenzylidene being milled in a jet mill before compounding below its melting point, will dissolve in the resin and will not give bubbles in the finished products.

Experiment
The additive was mixed on a bench setup with agitator belt screw blade at a nominal 12 MFR Amoco RCP. Each composition was compoundable in the melt on loterie 20 mesh (850 microns) to ensure minimal filtering. The melting temperature in the extruder was maintained at 213-215oC.

The composition was evaluated on the quality of the dispersion, turbidity and color to send in Shelby plastics (Ohio) for injection molding.

Tests on the injection molding was performed on 9 July 1992 in Shelby plastics. The test used the 450-ton van Dorn.

Double chamber shape provided 10 "servin Saver" container with cap. In the test used, the temperature of the raw material 222oC.

In table.3 shows the composition of the tested compositions.

From the experiment we can draw the following conclusions.

1. Composition containing commercial Milled (Millad) 3905 with d97=250 units, gives the bubbles at the edges of parts molded by injection molding.

2. Compositions containing primary particles of Millad 3905 with d97=12 units, do not give bubbles at the edges of parts molded by injection molding.

3. Glycerol monostearate and oleamide have little effect, but the data of the applicant in this work are not final.

4. Agglomerates of Millad 3905 give gas bubbles during melting. These gas bubbles get into the details, molded by injection molding, because machines for casting under pressure intended for Polyethene

1. Powder Dodge, representing a compound of General formula

where p= 0 or 1;
m and n are independently equal to 0 to 3;
the value of R in each case independently selected from the group of C1-8alkyl, C1-4alkoxy, hydroxy, halogen; C1-6alkylthio; C1-6alkylsulfate and 4 - or 5-membered accelgroup, which forms a carbocyclic ring with adjacent carbon atoms of unsaturated original ring
moreover, the average particle size of the powder clarifier less than 15 microns.

2. Powder clarifier under item 1, characterized in that it has an average particle size less than 10 microns.

3. Powder clarifier under item 2, wherein p is 1 and R is selected from the group: C1-4alkyl, chlorine, bromine, C1-6alkylthio and 4-membered accelgroup, forming a carbocyclic ring with adjacent carbon atoms of the unsaturated original ring.

4. Powder clarifier under item 1, characterized in that it has an average particle size less than 6 microns.

5. Powder clarifier under item 4, wherein p is 1 or R is selected from the group: C1-4alkyl, chlorine, bromine, C1-6alkylthio and 4-membered accelgroup, forming a carbocyclic ring with adjacent atoms, the melting point 250oC or higher.

7. Powder clarifier under item 1, characterized in that it has a melting point 250oC or higher.

8. Composition based polyolefin resin obtained by mixing 100 weight. including polyolefin resin selected from semi-crystalline copolymers With2-6aliphatic monoolefins, from 0.01 to 100 weight. including clarifier selected from the compounds of General formula

where p is 0 or 1;
m and n are independently 0-3;
the value of R in each case independently selected from the group of C1-8alkyl, C1-4alkoxy, hydroxy, halogen; C1-6alkylthio; C1-6alkylsulfate and 4 - or 5-membered accelgroup, which forms a carbocyclic ring with adjacent carbon atoms of unsaturated original ring
the clarifier is in powder form, characterized by an average particle size less than 15 microns, heating the mixture from a temperature above the melting temperature of the resin and up to at least 170oWith; and stirring the mixture, when the resin is in the molten state, until complete dissolution of the clarifier in the resin.

9. The composition according to p. 8, characterized in that the mixture comprises from 0.01 to 15 weight. including clarifier 100 weight. including polyolefin resin.

10. HDMI is 10, characterized in that R= 1 and R is selected from the group: C1-4alkyl, chlorine, bromine, C1-6alkylthio and 4-membered accelgroup, forming a carbocyclic ring with adjacent carbon atoms of an unsaturated source ring.

12. The composition according to p. 9, characterized in that the clarifier has an average particle size less than 6 microns.

13. The composition according to p. 12, wherein p= 1, and R is selected from the group of C1-4alkyl, chlorine, bromine, C1-6alkylthio and 4-membered accelgroup, forming a carbocyclic ring with adjacent carbon atoms of an unsaturated source ring.

14. The composition according to p. 13, characterized in that the mixture is heated to a temperature of at least 180oC.

15. The composition according to p. 8, characterized in that the mixture comprises about 0.1-3 weight. including clarifier 100 weight. including polyolefin resin.

16. The composition according to p. 15, characterized in that the clarifier has an average particle size less than 10 microns.

17. The composition according to p. 16, characterized in that R= 1 and R is selected from the group: C1-4alkyl, chlorine, bromine, C1-6alkylthio and 4-membered accelgroup, forming a carbocyclic ring with adjacent carbon atoms of an unsaturated source ring.

18. Composition based polyolefin resin obtained by mixing 100 ve is s, from 0.01 to 100 weight. including clarifier selected from compounds of the formula

where p is 0 or 1;
m and n are independently 0-3;
R in each case independently selected from the group of C1-4alkyl, chlorine, bromine, C1-6alkylthio and 4-membered accelgroup, forming a carbocyclic ring with adjacent carbon atoms of unsaturated original ring
the clarifier is in powder form, characterized by an average particle size of less than 10 microns, heating the mixture from a temperature above the melting temperature of the resin to at least 170oWith and below the melting point of the clarifier, stirring the mixture while it is in molten state, until complete dissolution of the clarifier in the resin.

19. The composition according to p. 18, characterized in that R= 1 and R is selected from the group: C1-4alkyl, chlorine, bromine, C1-6alkylthio and 4-membered accelgroup, forming a carbocyclic ring with adjacent carbon atoms, unsaturated original ring.

20. The composition according to p. 19, characterized in that it is obtained by heating the mixture to a temperature of 180-230oC.

 

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Epoxy composition // 2160291
The invention relates to compositions of polymer compositions based on epoxy Dianova resins and their hardeners which can be used as a binder for the production of GRP materials, in particular of shell structures

The invention relates to a method of obtaining modified in the 16,17-position epothilones, according to which the protected position of 3.7 or unprotected epothilone a or b a) hydronaut double bond in position 16,17 or) double bond in position 16,17 spend epoxidation and, if necessary, the obtained epoxide reduced to the alcohol in position 16, to a method for epothilone-N-oxides, in which the protected position of 3.7 or unprotected epothilone And or transferred to N-oxide, the N-oxide optionally subjecting the reaction of Qatar; the method of obtaining modified in the C-19 position epothilones by metallizirovanaya in position C-19 secured or unsecured epothilone a or b, as well as to modified epothilones General formula I
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