Process of producing polyurethane integral foams

FIELD: polymer production.

SUBSTANCE: invention relates to production of polyurethane molded products having dense periphery and cellular core using a mixture of foaming agents, particularly containing 50-99% 1,1,1,3,3-pentafluorobutane (HPC 365 mfc) and 1-50% 1,1,1,2,3,3,3-heptafluoropropane (HPC 227 ea). Polyurethane molded products according to invention are characterized by density values varying between 300 and 600 kg/m3 and can be used as wood simulation.

EFFECT: expanded polyurethane foams production possibilities.

3 cl, 2 tbl

 

The invention relates to a method for producing polyurethane molded products having a dense periphery (core layer) with a certain hardness and a cellular core (the so-called integral foam) and to the foams obtained by this method.

The class of materials which has been widely used as a blowing agent in the manufacture of polyurethane integral foams, is a fully halogenated chlorofluorocarbons and, in particular, Trichlorofluoromethane (CFC-11). Concerns about the potential that CFCs cause ozone depletion in the atmosphere, has led to the urgent need for the development of reactive systems, in which harperperennial foaming agents would be replaced with alternative materials, which are acceptable from a security perspective, the environment, and which also provide integral foams having the properties required for many applications in which they are used.

Mentioned alternative foaming agents proposed in the known technical solutions include hydrochlorofluorocarbons and hydrofluorocarbons.

In particular, 1,1-dichloro-1-foraten (HCFC 141b) is used as a blowing agent for polyurethane integral foams, provided the non receipt of foam with reinforced core layer with high surface hardness. However, HCFC 141b still contains chlorine atoms and is therefore dangerous for the environment.

1,1,1,2-Tetrafluoroethane (HFC 134a) used to replace HCFC 141b as a blowing agent in polyurethane integral foam, but results in a product of lower quality due to the lower hardness of the core layer.

German patent 19836662 describes polyurethane integral foams obtained using hydrotherapeutic foaming agents, namely, 1,1,1,3,3-pentafluoropropane (HFC 245fa) and/or 1,1,2,2-Tetrafluoroethane (HFC-134). The hardness of the core layer of foam produced using the aforementioned foaming agents, worse than the foam, foamed using HCFC 141b as a blowing agent.

The purpose of the present invention is to obtain high surface hardness polyurethane integral foams using environmentally friendly foaming agents.

The present invention relates to a method for producing polyurethane molded products having a dense periphery and the honeycomb core, including the stage of interaction of the organic polyisocyanate composition with a polyfunctional, relatively reactive isocyanate composition in the presence of hydrotherapeutic spinymouse the agents, characterized in that a mixture of a blowing agent, which contains or consists of 50-99% by weight of 1,1,1,3,3-pentafluorobutane (HFC 365mfc) and 1-50% by weight, of at least one fluorinated hydrocarbon selected from the group comprising 1,1,1,2-Tetrafluoroethane (HFC 134a), 1,1,1,3,3-pentafluoropropane (HFC 245fa), 1,1,1,3,3,3-hexaferrite and 1,1,1,2,3,3,3,-Heptafluoropropane (HFC 227ea).

When using the aforementioned safe for the environment mixes foaming agents improves the quality of the core layer of the integrated foam in the viewpoint of increasing the strength, hardness and abrasion resistance without compromising other properties of the foam.

Mentioned mixture described in WO 98/27145 for use as foaming agents in the production of foams, in particular rigid insulating polyurethane foams and super-elastic polyurethane foams.

The preferred mixture of foaming agents for use in the present invention contain or consist of 80-99% by weight of 1,1,1,3,3-pentafluorobutane and 1-20% by weight of 1,1,1,2-Tetrafluoroethane, 1,1,1,3,3,3-geksaftorpropena and/or 1,1,1,2,3,3,3-Heptafluoropropane, especially mixtures which contain or consist of 80-99% by weight of HFC-365mfc and 1-20% by weight of HFC134a and/or HFC227ea.

Especially preferred mixtures with HFC 134a contain or consist of 91-95% by weight of HFC-365mfc and 5-9% by weight of HFC 134a; mixtures that SOS is the SNF of these compounds in these quantities have a boiling point of 20° C.

Especially preferred mixtures with HFC 227ea are those which contain or consist of 80-99% by weight of HFC-365mfc and 1-20% by weight of HFC 227ea and especially 85-89% by weight of HFC-365mfc and 11-15% by weight of HFC 227ea; mixtures consisting of these compounds in the above-mentioned quantities, have a boiling point of approximately 23°C.

A mixture of foaming agents of the present invention are used in amounts lying in the range between 2 and 15% by weight based on the weight of reactive to isocyanate composition.

In semi-rigid integral foams content of the mixture of foaming agent is preferably a value between 10 and 15% by weight based on the weight of reactive to isocyanate composition.

In hard integral foam, especially when using it as imitation wood, the content of the mixture of foaming agent is preferably a value between 2 and 10, most preferably between 4 and 8% by weight based on the weight of reactive to isocyanate composition. In addition to improved resistance to scratching and abrasion using foam systems containing a mixture of foaming agents of the present invention also improves the surface quality by reducing the number of surface bubbles that may form. Foamed part, respectively, which is the duty to regulate fewer repairs, to get high vneshnetorgovye quality of the final product with a coating that imitates wood.

Suitable organic polyisocyanates for use in the method of the present invention include any of them, which are known in this field to obtain a polyurethane integral foams, and in particular aromatic polyisocyanates, such as diphenylmethanediisocyanate in the form of its 2,4'-, 2,2'- and 4,4'-isomers and mixtures thereof, mixtures of diphenylmethanediisocyanate (MDI) and oligomers known in this area as "crude" or polymeric MDI (polymethylenepolyphenylisocyanate)having a functionality isocyanate groups is greater than 2, colorvision in the form of its 2,4 - and 2,6-isomers and mixtures thereof, 1,5-naphthalenedisulfonate and 1,4-diisocyanatobutane. Other organic polyisocyanates that may be mentioned include aliphatic diisocyanates, such as isophoronediisocyanate, 1,6-diisocyanatohexane and 4,4'-diisocyanatohexane. Can also be used modified polyisocyanates, for example containing urethane-, urea-, biuret-, allophanate, carbodiimide or uretdione group, or prepolymers with terminal isocyanate groups.

Suitable reactive to isocyanate compounds intended for use in the present invention include any of them, Izv the STN in this field to obtain a polyurethane integral foams. Of particular importance to obtain a semi-rigid polyurethane integral foams are polyols and a mixture of polyols having an average hydroxyl number of from 20 to 200, especially from 20 to 50 mg KOH/g, and a hydroxyl functionality of from 2 to 3. For simple molecular weight polyether polyols is preferably a value in the interval between 2000 and 8000, for complex polyether polyols, preferably between 2000 and 4000. Of particular importance for the production of rigid polyurethane integral foams are polyols, in particular, simple polyether polyols having an average hydroxyl number between 300 and 1850, preferably between 350 and 650 mg KOH/g and a functionality of hydroxyl groups of from 2 to 6, preferably from 3 to 4. Can be used mixtures of different polyols; ratio of mixing depends on the intended use of the integral foam and the desired hardness of the surface of the core layer.

Suitable polyols have been fully described in the known technical solutions and products include interaction alkalisation, such as ethylene oxide and/or propylene oxide, with initiators containing from 2 to 8 active hydrogen atoms per molecule. Suitable initiators include: polyols, for example ethylene glycol, propylene glycol, glycerin, trimethylolpropane, triethanolamine, pentaerythritol, sorbitol and with whom the Crozet; polyamine, such as Ethylenediamine, tolylenediamine (TDA), diaminodiphenylmethane (DADPM) and polymethylenepolyphenylisocyanate; and aminoalcohols, for example ethanolamine and diethanolamine; and mixtures of such initiators. Other suitable polymeric polyols include polyesters obtained by the condensation of appropriate quantities of glycols and polyols of higher functionality with dvuhosnovnyj and poliennali carboxylic acids such as adipic acid, glutaric acid and phthalic acid. Suitable are polymeric polyols, including simple polythioether with terminal hydroxyl groups, polyamides, polyetherimide, polycarbonates, Polyacetals, polyolefins and polysiloxanes. The number of interact polyisocyanate compositions and polyfunctional, relatively reactive isocyanate compositions will depend on the nature of the obtained polyurethane integral foam and are easily identified by experts in the field.

Usually water or other form of carbon dioxide compounds are used together with a mixture of physical foaming agents of the present invention. When the joint chemical blowing agent use water, typical amounts are in the range from 0.2 to 5%, preferably from 0.5 to 3% by weight in the calculation of the and relatively reactive isocyanate compounds.

In addition to the polyisocyanate and polyfunctional reactive relative to the isocyanate compositions and foaming agents forming the foam reaction mixture will typically contain one or more other auxiliary compounds or additives, traditional formulations for the manufacture of polyurethane integral foams. Such optional additives include cross-linkage agents such as low molecular weight polyols such as ethylene glycol, 1,4-butanediol, glycerin, trimethylolpropane and triethanolamine, urethane catalysts, for example tin compounds such as octoate tin or dilaurate dibutylamine, or tertiary amines, such as 1,4-diaza-(2,2,2)-bicicletta, bis-(2-dimethylaminoethoxy) simple ether, dimethylcyclohexylamine or triethylenediamine, surfactants, flame retardants, for example halogenated alkylphosphate, such as Tris-chloropropionate, and fillers such as carbon black.

In the process of obtaining integral foams according to the invention can be used known methods, along with traditional methods of mixing. In this regard, given the reference to European patent 364854.

The density of integral foams of the present invention typically comprise a value in the range from 300 to 600, predpochtitel what about - from 400 to 500 kg/m3.

The resulting surface hardness shore D to rigid integral foams with a density of about 500 kg/m3lies in the interval from 65 to 70. For semi-rigid integral foams surface hardness shore a is a value between 75 and 80 and is achieved at a density of about 350 kg/m3.

Integral foams of the present invention can be used in all areas that use integral foams according to known solutions, such as upholstery, shoes, imitation wood and covers for steering control.

Various aspects of the present invention are explained, but not limited to the scope of the claims, the following examples, using the following ingredients.

Polyol a, which is a simple polyetherpolyols with IT a number of 28 mg KOH/g and a functionality of 3.

Polyol, which is a simple polyetherpolyols with IT a number of 35 mg KOH/g and a functionality of 3.

Polyol C, which is a simple polyetherpolyols with IT a number 380 mg KOH/g and a functionality of 4.

Polyol D, which is a simple polyetherpolyols with IT-the number 420 mg KOH/g and a functionality of 4.

Polyol E, which is a simple polyetherpolyols with IT-800 mg KOH/g and a functionality of 4.

Polyol F, which is on emery polyol.

Polyol G, which represents polypropylenglycol with 1000 Mw.

Polyol H, which is a coloring agent.

Polyol I, which represents the agent of the opening of the cell.

Polyol J, which is glycerin.

Additive A, which is Meg.

Additive, which is diethylene glycol.

Supplement, which is UV-absorber.

Catalyst a, which represents dimethylcyclohexylamine.

The catalyst, which represents dimethylbenzylamine.

Catalyst C, which represents the amine catalyst.

Catalyst D, which represents the amine catalyst.

Catalyst E, which represents the amine catalyst.

Surfactant And which is surface-active substance.

Silicone And that is a silicone surfactant.

Silicone, which is a silicone surfactant.

The stabilizer of a, which is the stabilizer.

Solkane 365/227: a mixture of 93 wt.% HFC 365mfc and 7 wt.% HFC 227ea, commercially available from the company Solvay.

Isocyanate a, which is a variant of the MDI.

Isocyanate, which is a prepolymer MDI.

Isocyanate, which is a variant of the MDI.

Isocyanate D, which is a polymeric MDI.

EXAMPLE 1

P is Logistica integral foams obtained using the ingredients and their quantities, listed below in table 1.

Determine the performance of the following properties of foam: the hardness of the core layer according to DIN 53505, elongation according to DIN 53571, ultimate tensile strength according to DIN 53571, and the residual elongation compression - DIN 53572. Results are also presented in table 1.

The use of a blowing agent according to the invention (foam No. 4) is compared with the known foaming agents, namely, HCFC 141b (foam No. 1), water (foam No. 2) and HFC 134a (foam No. 3).

Using a mixture of foaming agents according to the invention, namely, Solkane 365/227, leads to the hardness of the core layer, which is better than that achieved when using HCFC 141b, while the use of water or HFC 134a leads to reduced hardness of the core layer.

Table 1
UnitFoam No. 1Foam No. 2Foam No. 3Foam No. 4
Polyol Andparts by weight76,3490,23580
Additive Andparts by weight5,737,878,5507
Additivem is SC 2,862,9
Catalystparts by weight0,760,480,990,8
HCFC 141bparts by weight14,31
Waterparts by weight0,72
Polyol Inparts by weight56,7
Polyol Fparts by weight19,3
Catalyst Eparts by weight0,48
Polyol Jparts by weight0,48
Silicone Andparts by weight0,58
Siliconeparts by weight1,29
Polyol Hparts by weightof 5.82
Polyol Iparts by weight2,92
Supplementparts by weight0,225
HFC 134aparts by weight2,50
Solkane 365/227parts by weight12,2
Isocyanate Andparts by weight43
Isocyanate Inparts by weight106
Isocyanate Withparts by weight4845
Start timesec22111620
The gelation timesec45303557
The end of the rise timesec55415862
Density at the free risekg/m36819619083
The molded density kg/m3345365350345
Hardnessshore73556077
Elongation%95100
Tensile strength tensilekPa16701850
The residual elongation compression%1212

EXAMPLE 2

Rigid integral foams for use as imitation wood is obtained using the ingredients and quantities listed below in table 2.

Measure the performance properties of foam: H.D.T (Heat Distortion Temperature is the temperature began to thermal deformation) - according to ISO 75, the modulus of elasticity in bending according to ISO 178, Flexural strength according to ISO 178, impact strength Charpy - ISO 179 and surface hardness according to ISO 868. The results are presented in table 2.

The use of a blowing agent according to the invention (foam No. 8) is compared with the known foaming agents, namely, HCFC 141b (foam No. 5), water is (foam No. 6) and HFC 134a (foam No. 7).

Using a mixture of foaming agents according to the invention, namely Solkane 365/227, results in surface hardness, which is better than obtained when using HCFC 141b (without adversely affecting other properties of the foam), whereas the use of water or HFC 134a reduce the hardness of the core layer.

Table 2
UnitFoam No. 5Foam No. 6Foam No. 7Foam No. 8
Polyol Withparts by weight61,98of 57.572,361,98
Polyol Dparts by weight26,4730,001626,47
Surface-active substance Andparts by weight22
Waterparts by weight0,510,600,600,51
The catalyst Andparts by weight3,201,900,703,20
Stabilizer Andparts by weight0,20
HCFC 141B parts by weight3,74
Silicone Andparts by weight1,91,821,84
Polyol Eparts by weight22,40
Polyol Gparts by weight52
The catalyst Inparts by weight1,21
Catalyst Dparts by weight0,80
HCF 134aparts by weight2,2
Solkane 365/227parts by weight4,00
Isocyanate Dparts by weight102108110102
Start timesec23242822
The gelation timesec75859072
The tack-free timesec100 11012095
Density at the free risekg/m3861259384
The molded densitykg/m3500500500500
H.D.T.°64505964
The modulus of elasticity in bendingMPa780757670785
Flexural strengthMPa25,720,922,225,5
Impact strength CharpyKJ/cm2101310,229,8
Surface hardnessshore D65586268

1. A method of obtaining a polyurethane molded products having a dense periphery and the honeycomb core, including the stage of interaction of the organic polyisocyanate composition with a polyfunctional, relatively reactive isocyanate composition in the presence of hydrotherapeutic foaming agents, characterized in that a mixture of wspania the General agents, which contains 50-99% by weight of 1,1,1,3,3-pentafluorobutane (HFC 365mfc) and 1-50% by weight 1,1,1,2,3,3,3-Heptafluoropropane (HFC 227ea).

2. The method according to claim 1, wherein the mixture of foaming agent contains 80-99% by weight of 1,1,1,3,3-pentafluorobutane and 1-20% by weight 1,1,1,2,3,3,3-Heptafluoropropane.

3. The method according to claim 2, in which the mixture of foaming agent contains 85-89% by weight of 1,1,1,3,3-pentafluorobutane and 11-15% by weight 1,1,1,2,3,3,3-Heptafluoropropane.

4. The method according to claim 2, in which the mixture of foaming agent contains 91-95% by weight of 1,1,1,3,3-pentafluorobutane and 5-9% by weight 1,1,1,2,3,3,3-Heptafluoropropane.

5. The method according to any of the preceding paragraphs, in which this mixture foaming agents are used in a quantity lying in the range between 2 and 15% by weight, based on polyfunctional, relatively reactive isocyanate composition.

6. Polyurethane molded articles obtained by the method defined in any one of claims 1 to 5.

7. Polyurethane molded product according to claim 6, having a density of between 300 and 600 kg/m3.

8. Polyurethane molded product according to claim 7, having a density of between 400 and 500 kg/m3.

9. The use of polyurethane moulded products defined according to any one of p-8, as imitation wood.



 

Same patents:

FIELD: polymer production.

SUBSTANCE: invention relates to foamed polyurethane molded products with thickened edge zone with simplified density and clearly expressed more soft cellular core. Soft to semi-rigid polyurethane integral foamed plastics are prepared by interaction of (i) organic and/or modified organic polyisocyanates or their polymeric precursors with (ii) at least one polyol component with hydroxyl number 20 to 200 and functionality 2 to 6, if necessary in combination with (iii) at least one polyol component with hydroxyl number 201 to 899 and functionality 2 to 3, and also (iv) at least one component functioning as chain extension and having hydroxyl number or amine number 600 to 1850 and functionality 2 to 4 in amount 3 to 20% based on the summary weight of (ii) and (iii), and, if necessary, (v) known additives, activators, and/or stabilizers in presence of 0.05-0.6% water (based on summary weight of (ii) and (iii)) and mixtures of pore agents containing 1,1,1,3,3-pentafluorobutane and at least one other fluoroalkane in amount 0.2-10% of the summary weight of components (ii)-(v). Thus obtained foamed plastics with integral structure are characterized by Shore hardness of edge zone 30 to 90, rigidity in compression deformation 30 and 350 kPa, and apparent density 150 to 900 kg/m3.

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FIELD: polymer production.

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7 cl, 1 tbl, 9 ex

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16 cl, 4 tbl, 4 ex

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16 cl, 4 tbl, 4 ex

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7 cl, 1 tbl, 9 ex

FIELD: organic chemistry, foaming agents.

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4 cl, 4 tbl

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6 cl, 6 tbl

FIELD: polymer production.

SUBSTANCE: invention relates to production of polyurethane molded products having dense periphery and cellular core using a mixture of foaming agents, particularly containing 50-99% 1,1,1,3,3-pentafluorobutane (HPC 365 mfc) and 1-50% 1,1,1,2,3,3,3-heptafluoropropane (HPC 227 ea). Polyurethane molded products according to invention are characterized by density values varying between 300 and 600 kg/m3 and can be used as wood simulation.

EFFECT: expanded polyurethane foams production possibilities.

3 cl, 2 tbl

FIELD: polymer production.

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EFFECT: improved inflammation temperature of mixtures intended for preparing high-quality foamed plastics.

6 cl, 2 ex

FIELD: polymer production.

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EFFECT: achieved lack of foam in effluent after washing of polymer being foamed.

8 cl, 1 tbl, 4 ex

FIELD: chemical industry; methods of production of the foaming styrene polymeric compounds containing the particles of carbon.

SUBSTANCE: the invention is pertaining to the present in the form of the granules of the foaming styrene polymeric compounds containing the carbon particles and having the low contents of pentane. The invention presents the description of the method of production of the foaming styrene polymeric compound, in which styrene is polymerized in the water suspension at presence from 0.1 up to 25 mass % of the graphite or smut particles and from 2.5 up to 5.5 mass % of pentane, all in terms of the monomers. After the water flushing, the produced mass is subjected to drying during less than 1 second by the air stream with the temperature from 50 up to 100°С. The invention also describes the granules of the styrene foaming polymeric compound with the bulked weight above 600 g/l. The granules contain from 0.1 up to 25 mass % of the particles of the graphite or the smut, and also the volatile foaming agent representing the mixture composed of from 2.2 up to 5.0 mass % of pentane and from 1 up to 10 mass % of the water, all in terms of the granules of the styrene foaming polymeric compound. The technical result of the invention is production of the granules of the styrene foaming polymeric compound with the high contents of the internal water at the low contents of pentane which possess the high capability to the foaming.

EFFECT: the invention ensures production of the styrene foaming polymeric compound granules with the high contents of the internal water and the low contents of pentane, which have the high capability to the foaming.

9 cl, 3 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: present invention pertains to the method of obtaining hard polyurethane or polyisocyanurate foams which can be used for making refrigerating machines. The method involves reaction of: (a) organic diisocyanate and/or polyisocyanate with (b) activated aromatic amine polyol, with ratio of equivalents of groups (a) to groups with active hydrogen (b) ranging from 0.9 to 3.0, in the presence of, (c) more carbon dioxide and water, and (d) C3-C5 fluorocarbon. The invention aims at designing a method of producing hard urethane foams, with good physical properties, including a low k-factor, using environmentally acceptable foaming agents. This given task is solved by that, HFC (hydrofluorocarbon) is used as the foaming agent, combined with water and supplementary carbon dioxide.

EFFECT: reduced minimum filling density and filling percentage, required for frost resistant foam plastics at -30°C, as well as the k-factor of the obtained foam plastic.

12 cl, 1 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: there is disclosed application of the composition containing at least one fluorohydrocarbon foaming agent and non-halogenated polar organic oxygen-containing compound of boiling temperature at atmospheric pressure within 30°C to 150°C for making polystyrene foam by plastic foam equipment designed so that to be applied with a foaming agent containing at least one chlorfluorohydrocarbon. Besides there is disclosed method for making foam polymers, implying application of said composition. There is also disclosed polystyrene foam composition containing at least one fluorohydrocarbon foaming agent and non-halogenated polar organic oxygen-containing compound of boiling temperature at atmospheric pressure within 30°C to 150°C, where content of non-halogenated polar organic compound is within 10 to 15 wt %.

EFFECT: simplified production process of high-quality product.

13 cl, 3 ex

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