Method of producing foamable polystyrene granulate

FIELD: chemistry.

SUBSTANCE: method involves a step for mixing a carbon additive and a foaming agent with molten polystyrene, homogenisation of the mixture, cooling said mixture to extrusion temperature, extrusion and granulation in conditions which prevent foaming. The ratio of the molar quantity of the foaming agent fed to the specific throughput of the apparatus in the mixing zone (Ks) is kept in the range of 0.08-0.23, while maintaining temperature difference at the input and output of the homogenisation step and cooling step in the range of 30-70°C. The carbon additive used is thermally expanded modified graphite in powder form, which contains separate particles with thickness 0.35-5.0 nm and bunches of particles consisting of 10-30 particles (sheets) with average lateral particle (sheet) size of 5-100 mcm, taken in amount of 0.1-0.6% of the total weight of the load.

EFFECT: use of thermally expanded modified graphite in said amount enables to lower thermal conductivity without deterioration of strength characteristics and simultaneous reduction of water absorption of foamed articles which are made from the foamed polystyrene granulate.

2 cl, 1 tbl, 10 ex

 

The invention relates to polymer chemistry, in particular the production capable of polystyrene foam - expanded polystyrene, namely, to obtain granules of polystyrene containing a blowing agent (BA).

Expandable polystyrene (EPS) is widely used in civil and industrial construction for the manufacture of polystyrene foam boards, used for thermal insulation of buildings, for the manufacture of thermal insulation of pipelines and heat runs, etc. In the specified applications from PSV, in addition to a good balance of physical and mechanical properties, a low thermal conductivity. The foam have a low thermal conductivity - 0,039-0,042 W/(m×°K) at 25°C (GOST 15588-86). A further reduction in thermal conductivity of EPS at 15-20% can reduce the specific consumption of the insulation (m31 m2accommodations JV and N 23-02-2003) by 20-25%.

The decrease in thermal conductivity can be achieved by introducing additives that reduce the transmission of infrared radiation through the polystyrene plate, such as carbon black, graphite, titanium dioxide or metal particles, such as aluminum [www.basf.de; www.sunpor.at], especially carbon black and graphite. Effect of reduction in thermal conductivity is achieved with the introduction of 1 to 25 wt.%, better 3 - 8 wt.%, these additives.

However, the introduction of 3-8 wt.% and even the 1 wt.% carbon black or graphite reduces the strength properties obtained from PSV proistemi and increases water absorption, trapping water in the polymer, which may be undesirable for their successful operation, because the captured water increases the conductivity of proistemi, which leads to deterioration of insulating properties of building structures.

A method of obtaining able to foam polystyrene beads by the polymerization of styrene in aqueous suspension in the presence of carbon black or graphite in the form of particles with an average particle size of 0.5 to 200 μm, mainly 2-20 microns, with a bulk weight of 100-500 g/l and a specific surface area of 5-20 m2/g [RU No. 2302432, MCL C08J 9/14, 2005]. In the examples in the polymer injected 2% by weight of polystyrene graphite with an average particle size of 30 μm (examples 1, 2K) and 10 μm (example 3). The obtained granulate captures 1,86% (example 1) and 4.50 wt.% (example 3) water, thereby reducing the amount of added organic VA. Physico-mechanical properties, including values of thermal conductivity and water absorption of proistemi in RU # 2302432 not shown.

Suspension is a method of obtaining PSV has significant drawbacks, such as high operational costs of production, availability of wastewater to be treated, and a wide particle size distribution of the obtained granulate in the finished product. So as to obtain high-quality proistemi required particle PSV certain size with a narrow distribution in granulometrical composition, for suspension PSV required additional surgery sieving into different fractions and utilization of marginal subsistence fractions. Recycling granulate PSV difficult due to the presence of organic VA.

The closest to the essential features of the claimed method is a method of obtaining able to foam polystyrene granulate, including the filing of a blowing agent and additives in a melt of polystyrene in the mixing zone in a static or dynamic mixer, mixing VA and technological additives to the melt at a temperature of not lower than 150°C., cooling the mixture to a temperature of at least 120°C, discharging through the nozzle to the grate with holes whose diameter at the outlet does not exceed 1.5 mm, and granulation facing strands under conditions that prevent foaming of the polymer [US 2005/0156344, MCL VS 44/00, 2005]. Specifies that the size of the granules can be adjusted by additions of plasticizers, the temperature change of the melt or geometric parameters of the granulating device. As a nucleator at the stage of mixing, but before the introduction of the VA, the melt is injected from 0.05 to 1.5 wt.% water.

In the method according to US 2005/0156344 use granulating head with openings not more than 1.5 mm, better 0,2-1,2 mm (1, 9 and 16 of the formula) and get pellets with a diameter of 0.4-1.8 mm (p.22 formula). Granulation is carried out by t is mperature melt polystyrene, mixed with VA, 160-200°C. (examples 1 and 2) and the temperature of the granulating head 180-240°C. (example 2). When the temperature of the melt and head, adding water or plasticizers, when you change the geometry of the holes in the granulating head, you can reduce the diameter of the granules with the same hole diameter. Specifies that obtained by the above method, the granules when the foaming give foam particles with fine cell foam structure, which was identified under the microscope" (examples 7-10), but do not see any apparent density of proistemi obtained from this granulate or their physico-mechanical properties, including thermal conductivity and water absorption.

In US no 2005/0156344 indicates that the particle size of the obtained granulate is "homogeneous" (uniform). Granulometric composition is provided in example 11, which States that "the granules have a narrow size distribution of particles, namely 80% of the granules have a diameter of 0.62 and 0.8 mm, However, is narrow particle size distribution, in which the diameter of at least 90% of the particles lies in the same range (Chemical encyclopedia. M., "Great Russian encyclopedia", 1995, V. 4, s), so the lack of a way for US No. 2005/0156344 is not sufficiently narrow granulometric composition of the product.

The technical result, which is aimed claimed the e invention, is to obtain granules of expandable polystyrene with narrow particle size distribution that gives the processing method of thermoforming penisgay with low conductivity and low water absorption while maintaining a high level of physical and mechanical properties.

This technical result is achieved in that in a method of producing able to foam polystyrene beads, including the stage of filing a blowing agent and additives in the mixing zone, mixing a blowing agent and additives with the molten polystyrene, homogenizing the mixture, cooling it to a temperature of extrusion, extrusion and granulation in conditions preventing foaming, support the molar ratio of the amount of foaming agent to the specific throughput of the equipment in the mixing zone (COP), which represents the ratio of the material flow in kg/hour of stirring speed in revolutions per minute, in the range 0,08-0,23 while maintaining the difference temperatures at the input and output stage homogenization and cooling in the range of 30-70°C, and as technological additives injected modified thermal expanded graphite in the form of a powder comprising individual particles of a thickness of 0.35 to 5.0 nm and packs of particles consisting of 10-30 particles (leaves), with the average lateral size of sheets of 5-100 μm, taken in an amount of 0.1 to 0.6% by weight of the total load.

Under specific bandwidth (CC) equipment in the mixing zone, we mean the ratio of the number passing the material flow (kg/h) to the stirring speed (rpm).

Thermal expanded graphite was obtained by processing natural graphite perchloric acid and rapid heating to a temperature of 600°C, as described in EN No. 2377177, 2009. Expanded graphite is additionally modified ultrasonic treatment (with a frequency of 21 kHz) colloidal suspension in the environment of the oxidant is hydrogen peroxide, as described in [KOMPAN M.E. Ter-Minassian and other technical physics Letters, 2010, T.36, VIP, s-88].

Modified thermal expanded graphite contains 99.9% of carbon and does not contain extraneous inclusions and impurities; has a thickness of individual particles (leaves) of 0.35 to 5.0 nm; powder also includes tutu, consisting of 10-30 separate sheets. The thickness of the packages does not exceed 150 nm. The average lateral size of the particles is 5-100 μm.

In addition to the powder, modified thermal expanded graphite may be in the form of a concentrate based on polystyrene with a dosage of 5-10 wt.%. Production of concentrate were carried out by extrusion of a pre-prepared mixture of polystyrene (90-95 wt.%) with modified thermal expanded graphite (5-10 wt.%) in co-rotating twin screw extruder with a ratio of the length of the screw L to dia is Trou D, equal to 31:1, at a temperature of 180-230°C; the speed of rotation of the augers 300-450 rpm To improve the quality of mixing the obtained concentrate was subjected to repeated extrusion under specified conditions.

Know the use of thermally expanded ("expanded") graphite when receiving PSV suspension polymerization of [RU No. 2223984, MCL C08J 9/20, 200; RU №2253658, MCL C08J 9/20, 2005]. In RU # 2223984 thermal expanded graphite with a density less than 1.5 g/cm3(in examples 1 g/cm3and 0.05 g/cm3and a particle size of 10-20 μm is injected to reduce thermal conductivity of proistemi whose values are not specified in the description as well as water absorption and other physical and mechanical properties. "Expanded graphite is used instead of the usual RU # 2223984 to facilitate the suspension of his situation before polymerization; indicates that more severe nespecheny graphite requires additives polystyrene in the original styrene, the dissolution of which is an additional process stage.

In RU # 2253658 in PSV enter 5-50% "swollen" graphite with an average particle size of 20-100 μm (examples 12-15 wt.%, graphite with a particle size of 45 and 100 μm) to maintain its fire resistance class B1 and B2 according to DIN 4102 without the use of halogenated flame retardants. Other physico-mechanical parameters are missing.

"Expanded graphite used in the above patents, received the processing of graphite with sulfuric acid, followed by heating up to 500-1000°C.

Information available in these patents are not allowed to presuppose that the use of thermally expanded graphite will reduce the conductivity of proistemi without increasing water absorption and deterioration of strength properties.

To obtain PSV used polystyrene with respect srednevozrastnoe molecular mass (Mv) to the coefficient of polydispersity (i.e. the ratio srednevozrastnoe molecular weight (Mw) to srednekamennogo molecular weight (MP)) within (70-115)×103.

As the polystyrene in the present method can be used geopolitical brands starovic® (TU 2214-001-11175949-2003) or other brand of PS (for example, according to GOST 20282-86), molecular weight which is within the specified range of values of the ratio Mv to Mw/Mn. To obtain a PSV can also be used to melt polystyrene with similar molecular characteristics, obtained by continuous polymerization in mass of styrene and last stage of removal of unreacted monomer.

As a blowing agent was used substances selected from the group comprising saturated hydrocarbons, C4-C8such as butane, isobutane, pentane, isopentane, hexane, isohexane and octane, preferably pentane or isopentane, or mixtures thereof.

The processed mixture contained nucleotide sequence that is Thor, which used fine powders of talc, calcium carbonate, kaolin, and mixtures of citric acid and sodium bicarbonate, and azodicarbonamide, azodiisobutyronitrile and other Nucleator in the amount of 0.05-5.0 wt.% mixed with polystyrene or an already prepared by melt polystyrene.

The processed mixture may contain substances that prevent the fire (flame retardants). As a flame retardant commonly used hexabromocyclododecane in the amount of 1-5 wt.%, better to 1.5-2.0 wt.% with a synergistic additive. As a synergistic supplements can be used magnesium-aluminum hydrotalcite, hydroxides of metals, phosphorus compounds, inorganic and organic phosphates, phosphites or phosphonates, or mixtures thereof, and organic compounds with unstable carbon-carbon or oxygen-oxygen bonds.

The processed mixture may contain dyes, for example phthalocyanine, and in particular, the orange dye.

Upon receipt of the granules of expandable polystyrene used as stabilizers thermo - and sweetestrossie. As the stabilizer of thermo - and sweetestrossie used, for example, octadecyl-3-(3,5-ditretbutyl-4-hydroxyphenyl)-propionate or a mixture of Tris-(2,4-ditertbutyl)phosphite with octadecyl-3-3(3,5-ditretbutyl-4-hydroxyphenyl)propionate in the number 0,050,1 wt.% by weight of the boot.

All of these processing AIDS may be directly mixed with polystyrene or melt of polystyrene, obtained from the continuous polymerization of styrene; they can also be introduced in the form of concentrates.

Further, the inventive method is illustrated by examples of specific embodiments, but are not limited to them.

Example 1 (control)

In the mixing zone of node gravimetrically dosage serves 100 mass polystyrene brand starovic 106 In with srednevozrastnoe MM (Mv)equal to 216000, and coefficient of polydispersity (Mw/Mn) of 2.3 (ratio (Mv) to the coefficient of polydispersity is 94×103), there also serves 2,0 mass of hexabromocyclododecane 0,5 mass nucleator - talc.

Educated mixture is fed into the loading zone of the twin-screw extruder with a ratio of the length of the screw L to the diameter D equal to 31:1, where at a temperature of 180-210°C is the melting and mixing in the melt of all components, and then into the mixing zone through the injector served a blowing agent is pentane in the amount of 6.5 wt.% under pressure up to 120 bar. In the mixing zone is a homogeneous mixture of VA and melt polystyrene. The specific throughput of the extruder in the mixing zone (COP) equal to 1.75 kg/h/1/min. While the ratio of the number of pentane (in moles) to the specific throughput of the equipment in the area smashin the I (KS) is equal to 0.18.

Obtained in the mixing zone mass with a temperature of 200°C is fed to the apparatus homogenization and cooling, where the melt is cooled to a temperature of 160°C. the temperature Difference at the inlet and exit stage homogenizing and cooling the mixture is 40°C.

The pulp then passes through a short static mixer to align the concentration and temperature of the flow profile and enters the granulator system of underwater granulation. In cutting the camera underwater pelletizing temperature of water in the range of 40-70°C and a pressure of 8.0-10.0 bar. The mixture of water and granules of expandable polystyrene is served in a centrifugal drier, where the separation of the pellets from the water and drying.

Granules of the finished product covered components that are typically used for surface treatment to improve the workability during processing PSV: complex glycerol esters, antistatic agents or anti-clumping.

For the finished product were used to define the following parameters:

- particle size: average particle diameter, mm mass fraction of granules sifting on a sieve with a mesh size of 1.6 mm and 0.5 mm, %, mass fraction of the main fraction, %, on THE other 2291-008-56925804-2008;

- mass fraction of the pore-forming substance, %, GOST 301-05-202-E,

- mass fraction of residual monomer, wt.%,according to GOST 15820-82.

From the obtained granules of expandable polystyrene (EPS) produced polystyrene plates bespressovyj method, which involves the following stages: preuspeiania PSV water vapor at a temperature 98-104°C, staging (maturation) predsmertnyj pellets, sintering them with the forming block and subsequent cutting on his plate.

For received proistemi - plates - was determined by the following indicators:

density, kg/m3according to the GOST 17177-94;

- compressive strength at 10% linear strain, MPa, according to GOST 17177-94;

ultimate strength in static bending, MPa, according to GOST 17177-94;

- coefficient of thermal conductivity at (25±5)°C W/(m×K), GOST 7076-94;

water absorption for 24 hours, % by volume, according to GOST 17177-94;

- cell size, microns, JV - 30/08;

- self-burning, with, (self-damping).

The values of the properties of the granules EPS and indicators of physico-mechanical properties and thermal conductivity of the obtained polystyrene plates shown in the table.

Examples 2-7, 8 and 9 (control).

Experiments were performed as in example 1, but at the stage of mixing the introduced modified thermal expanded graphite.

Recipe downloads and values of properties peoplet obtained from PSV shown in the table.

Example 10

Experiments were performed as in example 1, but at the stage of mixing the introduced thermal expanded modify the new graphite in the form of a concentrate in polystyrene with a degree of filling 5 wt.%.

Recipe downloads and values of properties penality obtained from PSV shown in the table.

The table shows that the inventive method allows to obtain PSV giving during the processing of a plate with low thermal conductivity, preserving the high strength properties and low water absorption. The increase in the content of the modified thermally expanded graphite in the formulation of loading above 0.6 wt.% (example 8K) did not lead to a further reduction in thermal conductivity, but caused a slight increase in water absorption.

1. The method of obtaining able to foam polystyrene beads, including the stage of filing a blowing agent and additives in the mixing zone, mixing a blowing agent and additives with the molten polystyrene, homogenizing the mixture, cooling it to a temperature of extrusion, extrusion and granulation in conditions preventing foaming, characterized in that the support ratio molar amount foaming agent to a specific bandwidth of the equipment in the mixing zone (COP), which represents the ratio of the material flow in kg/h to the stirring speed in revolutions per minute, in the range 0,08-0,23 while maintaining the difference in pace is the atur on the input and output stage homogenization and cooling in the range of 30-70°C. and as technological additives injected modified thermal expanded graphite in the form of a powder comprising individual particles of a thickness of 0.35 to 5.0 nm and packs of particles consisting of 10-30 particles (leaves), with an average lateral size of sheets of 5-100 μm, taken in an amount of 0.1 to 0.6% by weight of the total load.

2. The method according to claim 1, characterized in that the modified thermal expanded graphite is introduced in the form of a concentrate based on polystyrene with graphite content of 5-10 wt.%.



 

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Polymer composition // 2447091

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Polymer composition // 2447091

FIELD: chemistry.

SUBSTANCE: invention relates to polymer chemistry, specifically to moulding articles made from a polymer composition containing an acrylic copolymer matrix and particles containing an inorganic oxide with weight-average particle size equal to or less than 400 nm. The polymer composition is obtained by polymerising a mixture of methylmethacrylate and one or more copolymerisable lower alkyl(alk)acrylate comonomers in the presence of said particles and a dispersant which contains an ethylenically unsaturated compound containing one ethylenically unsaturated bond. The polymer composition has weight-average molecular weight from 20000 to 250000 Da. Described also is a method of obtaining the polymer composition, a method of obtaining articles from the polymer composition and use of the articles in construction, lighting etc.

EFFECT: polymer composition, obtained in the presence of inorganic oxide particles with size less than 400 nm in the presence of a dispersant which contains an ethylenically unsaturated compound which contains one ethylenically unsaturated double bond, is characterised by higher chemical resistance and improved processability in a melt compared to a polymer composition which does not contain inorganic oxide particles.

40 cl, 4 dwg, 6 tbl, 23 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to antimicrobial agents exhibiting antibacterial activity with respect to test cultures of gram-positive and gram-negative microorganisms which represent copper nanoparticles and copper oxide nanoparticles. The antimicrobial agents according the invention are characterised by specific particle sizes and phase compositions. The nanoparticles have the size of 33.8-103 nm and contain 67-96% of copper and 4-33% of CuO. The copper oxide nanoparticles have the sizes of 77-124 nm and contain 3.3-23% of crystalline copper, 27.1-90% of CuO and 9.05-69.5% of Cu2O.

EFFECT: invention provides preparing the antimicrobial agents which when introduced in the composition of non-woven linen ensure its antibacterial properties, as well as maintain its aesthetic and service characteristics.

2 cl, 8 dwg, 12 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to thermoplastic material and a method of producing said material. The thermoplastic material contains a composition containing a thermoplastic resin, mineral or carbon-containing filler, an optional heat stabiliser and/or UV light stabiliser and/or lubricant and/or rheological property modifier and/or an organic impact-resistance modifier, as well as a comb-shaped polymer containing a polyalkylene oxide group grafted to an unsaturated ethylene monomer. The method involves mixture and subsequent extrusion of said composition components, where the comb-shaped polymer is added to the composition in form of a dry powder obtained at different steps of the process.

EFFECT: obtaining thermoplastic material with high impact resistance and retains satisfactory hardness.

15 cl, 5 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to compositions for foaming foam plastic used in insulation materials at low temperatures. The said composition ontains 1,1,1,3,3-pentafluorobutane (HFC - 365mfc) and 1,1,1,3,3-pentafluoropropane (HFC-245fa) with mass ratio HFC-365mfc/HFC-245fa between 65:35 and 73:27.The invention also relates to a premix for producing foamed polyurethane or modified foamed polyurethane which contains such a foaming composition, at least one polyol and a catalyst for reaction of isocyanates and polyols. The invention also describes a method of producing foamed polyurethane or modified foamed polyurethane using the disclosed foaming composition, as well as heat insulation material which contains foamed polyurethane or modified foamed polyurethane made using the said method. When prepared systems are used completely, the foaming composition does not have an ignition point, which provides safe production of (modified) foamed polyurethane.

EFFECT: foam plastics made from such a foaming composition have coefficient of thermal conductivity which varies insignificantly with temperature, and exhibit better insulation properties in a wide temperature range, especially at low temperatures.

9 cl, 3 ex

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