Polyester polyols from terephthalic acid and oligoalkylene oxides

FIELD: chemistry.

SUBSTANCE: invention relates to a polyester polyol, a method for production thereof and to use thereof to produce rigid foam materials from polyurethanes/polyisocyanurates. The polyester polyol with concentration of ether groups between 9.0 mol/kg polyester polyol and 16 mol/kg polyester polyol is obtained from a mixture containing: A) terephthalic acid (A), B) oligoethylene glycol of formula H-(OCH₂CH₂)_n-OH with an average number of oxyethylene groups n between 3.0 and 9.0, and C) at least one aliphatic dicarboxylic acid selected from a group consisting of succinic acid, glutaric acid, adipic acid, sebacic acid, suberic acid, azelaic acid, decane dicarboxylic acid, dodecane dicarboxylic acid and omega-hydroxycaproic acid.

EFFECT: obtaining polyester polyol which is easy to process when producing rigid foam materials from polyurethanes/polyisocyanurates and simultaneously improves fire-resistance.

13 cl, 2 tbl, 9 ex

This invention relates to a complex of polyether polyols from terephthalic acid and oligonucelotides, method of production thereof and their use for the production of rigid foams made of polyurethane (PUR)/polyisocyanurate (PIR).

Rigid foams of PUR/PIR at the present time in most cases is obtained on the basis of complex polyether polyols, as they have a positive effect on the resistance and thermal conductivity of rigid foams made of PUR/PIR. Upon receipt complex polyether polyols as starting substances are used, primarily, succinic acid, glutaric acid, adipic acid, phthalic acid / anhydride, terephthalic acid and isophthalic acid. In addition to the complex of polyether polyols and sometimes even added a simple polyether polyols, in order to improve characteristics of solubility of pentane in comparison with complex polyether polyols or reduce the fragility containing isocyanurate rigid foams made of PUR/PIR.

In this regard, U.S. patent US 4,039,487 describes complex polyether polyols which can be obtained from glycols with equivalent masses of from 75 to 225 g/mol and aromatic polycarboxylic acids. Partial sharing of aliphatic polycarboxylic acids are not taken into account.

Similarly, s is opaski the patent application EP-A 1834974 limited to, aromatic polycarboxylic acids, and, besides, in U.S. patent US 5,003,027 limited to the processing of complex polyether polyols in the process of reaction injection molding (RIM - Reaction Injection Molding).

In the international application WO-A 99/54380 to produce complex polyether polyols although it is also proposed the use of aliphatic dicarboxylic acids, however, as the source of the aromatic dicarboxylic acid is always used polyethyleneterephtalate (PET). The principal disadvantage of such a method which is based on materials from recycled materials, however, is the potential presence of pollutants debris that should be removed partially costly methods.

U.S. patent US 4,469,824 also based on recycled PET, and as one of the additional components of the reaction offered adipic acid.

However, the use of aromatic acids, in particular, the use of terephthalic acid in obtaining complex polyether polyols may lead to the fact that at room temperature they exist in solid form, and thus their processing in technological processes is difficult.

However, in the prior art did not offer specific guidance for action, with which it would be possible to obtain complex polyetherpolyols, which satisfies all important parameters the frames for processing in the field of rigid foams made of PUR/PIR.

In addition, many traditional rigid foams of PUR/PIR-based complex polyether polyols do not have sufficient fire resistance, since they usually only satisfy the fire resistance class of the OT according to DIN 4102-1.

Therefore, the objective of the invention was to provide a complex polyether polyols and their use in rigid foams made of PUR/PIR lead to improved fire resistance, in particular, lead to the rigid foams of PUR/PIR, which according to DIN 4102-1 meet the fire resistance class B2 and/or tested according to the method of SBI (test with thermal influence of one source of combustion according to DIN EN 13823).

Another objective of this invention to provide a complex poly-epically that can easily be recycled in industrial processes when receiving a rigid foams made of PUR/PIR and to lead to improved fire resistance.

This task according to the invention is solved by providing complex polyetherpolyols, which is obtained from a mixture containing:

(A) terephthalic acid, optionally in the form of a complex Olkiluoto ether with the number of carbon atoms in the alkyl from 1 to 4

(B) oligoethyleneglycols formula H(och₂CH₂)_n-HE srednegalechny number oxyethylene g is UPP n in the interval between the 3.0 and 9.0, and

(C) at least one aliphatic dicarboxylic acid selected from the group consisting of succinic acid, glutaric acid, adipic acid, sabatinovka acid, cork acid, azelaic acid, decanedicarboxylic acid, dodecadienol acid and omega-hydroxypropranolol acid, characterized in that the complex polyetherpolyols has a concentration of ether groups in the range of between 9.0 mol/kg of complex polyetherpolyols and 16 mol/kg of complex polyetherpolyols.

Complex alkilany ester of terephthalic acid with the number of carbon atoms in the alkyl from 1 to 4 preferably is an ester selected from the group consisting of a complex of dimethyl ester of terephthalic acid, diethyl ether complex of terephthalic acid, a complex of di-n-butyl ester of terephthalic acid and a complex of Diisobutyl ester of terephthalic acid. According to this invention the compound of General formula H-(och₂CH₂)_n-IT contains at values

n = 1 oxyethylene group and does not contain ether groups;

n = 2 two oxyethylene group and one ether group;

n = 3 three oxyethylene groups and two ether groups;

n = 4 four oxyethylene group and three ether groups;

n = 5 oxyethylene groups the four ether groups;

n = 6 six oxyethylene groups and five simple ester groups;

n = 7 oxyethylene groups and six simple ester groups;

n = 8 eight oxyethylene groups and seven simple ester groups and

n = 9 nine oxyethylene groups and eight simple ester groups.

Component (B) preferably is a mixture of different oligomeric etilenglikola, and the value n denotes the average number oxyethylene groups in the component (B). Particularly preferably, the component (b) contains oligomers with n = 2 is less than 8 wt. -%, most preferably less than 3 % of the mass. Therefore, for values of n can also be not integer values, such as, for example, 3,1, 3,2 or 3,24.

Preferably oligotrophic (C) have srednekislye molecular weight in the range from 145 to 450 g/mol, particularly preferably in the range from 150 to 250 g/mol.

Preferably the obtained complex polyetherpolyols is the number of ether groups in the range between 9.1 mol/kg of complex polyetherpolyols and 13 mol/kg of complex polyetherpolyols.

The mixture contains at least one aliphatic dicarboxylic acid (S)selected from the group consisting of succinic acid, glutaric acid, adipic acid, sabatinovka acid, cork acid, azelaic acid, decanedicarboxylic acid, dodekanisa the oil acids and omega-hydroxypropranolol acid. Especially preferably the mixture contains at least one aliphatic dicarboxylic acid (S)selected from the group consisting of succinic acid, glutaric acid and adipic acid.

Preferably component (A) is present in an amount of from 10 to 40 wt. -%, particularly preferably in quantities of from 15 to 35 wt. -%, in terms of the total amount of the mixture to produce complex polyetherpolyols according to the invention.

Preferably component (C) is present in an amount of from 60 to 90 wt. -%, particularly preferably in an amount of from 55 to 85 wt. -%, in terms of the total amount of the mixture to produce complex polyetherpolyols according to the invention.

Preferably component (C) is present in an amount of from 0 to 20 wt. -%, particularly preferably in amounts of from 2 to 20 wt. -%, most preferably in an amount of from 3 to 15 wt. -%, and highly preferably in an amount of 5 to 14 wt. -%, in terms of the total amount of the mixture to produce complex polyetherpolyols according to the invention.

Unexpectedly, it was found that the combined use of component (C) with the same in the rest of the recipe is unchanged and the hydroxyl number of complex polyetherpolyols favorably contributes to the reduced viscosity of this complex polyetherpolyols.

Preferably e is from complex polyetherpolyols has a hydroxyl number in the range between 100 mg KOH/g and 400 mg KOH/g, particularly preferably in the range between 110 mg KOH/g and 220 mg KOH/g, most preferably in the range between 150 mg KOH/g and 200 mg KOH/g

HE is a number determined by the fact that the first sample of complex polyetherpolyols injected into the reaction of terminal hydroxyl groups with a certain excess anhydride, e.g. acetic anhydride, the excess anhydride hydrolyzing and determine the content of free carboxyl groups using direct titration with a strong base, e.g. sodium hydroxide. The difference carboxyl groups introduced in the form of anhydride, and experimentally found carboxyl groups is a measure of the number of hydroxyl groups in the sample. If this value is adjusted by the number of carboxyl groups contained in the original sample due to incomplete esterification, i.e., acid number, it turns out HE is number. The results of titrations, in most cases carried out using sodium hydroxide, are translated into an equivalent amount of potassium hydroxide so that the acid and hydroxyl numbers have a dimension in g KOH/kg between a hydroxyl number (#IT) and srednekamennogo molecular weight (M) there is the following mathematical relationship: M=(56100*F)/HE#. While F denotes srednekamennogo functionality can with good approximation be obtained from the formulation. The method of determining IT-as described, for example, in the publication Houben Weyl, Methods der Organischen Chemie, Band XTV/2 Makro-molekulare Stoffe, page 17, Georg Thieme Veriag; Stuttgart 1963.

Molecular weight complex of polyether polyols according to the invention are preferably in the range from 280 to 1120 Yes, especially preferably from 510 to 1020 Yes, extremely preferably from 560 to 750 Yes.

Preferably complex polyetherpolyols according to the invention has an acid number in the range from 0.1 mg KOH/g to 4 mg KOH/g, particularly preferably in the range from 0.2 mg KOH/g to 2.8 mg KOH/g

The method of determining the acid number is described, for example, in the publication Houben Weyl, Methods der Organischen Chemie, Band XIV/2 Makromoleku-lare Stoffe, page 17, and further, Georg Thieme Verlag; Stuttgart 1963.

Preferably complex polyetherpolyols according to the invention at 25°C. has a viscosity, measured according to DIN 53019, in the interval between 800 MPa·s and 4500 MPa·s, particularly preferably in the range between 1000 MPa·s and 3000 MPa·S.

Preferably oligoethyleneglycols () has srednekamennogo number oxyethylene groups n in the area between 3.1 and 9, particularly preferably between 3.5 and 8.

Preferably complex polyetherpolyols has a melting point in the range between -40°C and 25°C, particularly preferably in the range between -20°C and 23°C.

Preferably complex polyetherpolyols according to the invention poluchaetsya mixture, containing terephthalic acid (a) and oligoethyleneglycols (C) of the formula H(och₂CH₂)_n-HE srednegalechny number oxyethylene groups n in the range from 3.0 to 9.0, and at least one aliphatic dicarboxylic acid (S)selected from the group consisting of succinic acid, glutaric acid and adipic acid.

Another object of this invention is a method of obtaining complex polyetherpolyols according to the invention, with the components (a) and (b) preferably in the presence of a catalyst selected from the group consisting of salts of tin(II) and tetraalkoxysilane titanium, interact at a temperature between 160°C and 240°C and a pressure of between 1 and 1013 mbar in the time interval between 7 and 100 hours.

To obtain complex polyether polyols according to the invention can be applied to all known specialist catalysts. Preferably used chloride tin(P) and tetraalkoxysilane titanium. Particularly preferred application of the dihydrate of tin dichloride in an amount of from 20 to 200 ppm, most preferably from 45 to 80 ppm, in terms of all the components used.

The interaction of components to produce complex polyetherpolyols according to the invention preferably is carried out in the mass of the substance.

Another object of this invention is the SPO is about receiving foam from PUR or respectively of PUR/PIR, includes the following stages:

a) dealing at least one compound polyetherpolyols according to the invention with

b) at least one component containing polyisocyanates,

c) at least one foaming agent,

d) at least one or more catalysts,

e) optionally, at least one fire-retardant agent and/or other auxiliary substances or additives

f) optionally at least one compound containing at least two groups reactive toward isocyanates.

As components containing polyisocyanates, consider the conventional aliphatic, cycloaliphatic and, above all, aromatic di - and/or polyisocyanates. Preferably apply toluenediisocyanate (TDI), diphenylmethanediisocyanate (DHS) and, in particular, mixtures of diphenylmethanediisocyanate and polyvinylpolypyrrolidone (polymeric MDI). These isocyanates can also be modified, for example, by including uretdione, urethane, which, carbodiimide, allophanate and, above all, urethane groups. For the production of rigid polyurethane foam is used, in particular, polymeric MDI. The formation of isocyanurates in the prior art is carried out almost exclusively in the process is eacli pricing and leads to flame-proof foams made of PUR/PIR, which are preferably used in technical hard foams, for example, in the construction as insulation boards, sandwich elements and vans to trucks.

As compounds containing at least two groups reactive towards isocyanates, i.e. at least two hydrogen atoms, reactive towards isocyanate group, in General, can be used compounds which outlines the next.

As compounds containing at least two groups reactive towards isocyanates, considering, in particular, those which contain in the molecule two or more reactive groups selected from Oh groups, SH groups, NH groups, NH2 groups and CH-acidic groups, such as, for example, β-dittography. For the production of rigid polyurethane foams, preferably obtained by the method according to the invention, are used, in particular, compounds having from 2 to 8 Oh-groups. Preferably used simple polyether polyols and/or complex polyether polyols. Hydroxyl number of simple polyether polyols and/or complex polyether polyols upon receipt of the hard polyurethane foam is preferably from 25 to 850 mg KOH/g, particularly preferably from 25 to 450 mg KOH/g, molecular weight pre is respectfully represent more than 400 g/mol. Preferably component (f) contains a simple polyether polyols, which are obtained by known methods, for example by anionic polymerization with hydroxides of alkali metals such as sodium hydroxide or potassium hydroxide, or alkali metal alcoholate such as sodium methylate, utility sodium or potassium or isopropyl potassium as catalysts and with addition of at least one type of initiator molecules, which contains related from 2 to 8, preferably from 2 to 6 active hydrogen atoms, or by cationic polymerization with Lewis acids, such as, among others, pentachloride antimony, apirat of boron fluoride or kaolin as catalysts, from one or more alkalisation with the number of carbon atoms in Allenova residue from 2 to 4. In addition, the simple polyetherpolyols can be carried out with the aid of catalysis double metallocyanide catalysts, and in this case it is also possible continuous process.

Suitable acceleratedly are, for example, tetrahydrofuran, 1,3-propylene oxide, 1,2 - or 2,3-builtoutside, stimulated and preferably ethylene oxide and 1,2-propylene oxide. Alkalinity can be used individually, alternately one after another or as mixtures. As molecules initiators consider, for example, Glazer is h, trimethylolpropane, pentaerythritol, sucrose, sorbitol, methylamine, ethylamine, Isopropylamine, butylamine, benzylamine, aniline, toluidine, Tolu-Oldeman, naphtylamine, Ethylenediamine, Diethylenetriamine, 4,4'-methylenedianiline, 1,3-propandiamine, 1,6-hexanediamine, ethanolamine, diethanolamine, triethanolamine, and other two - or polyhydric alcohols, which on its part can also be a simple oligoarticular or mono - or polybasic amines.

In addition, the component (f) may optionally contain complex polyether polyols, chain-extending agents and/or crosslinking agents. As the chain-extending agents and/or cross-linking agents consider, in particular, di - or trifunctional amines and alcohols, first of all, diols and/or trioli with molecular mass of less than 400 g/mol, preferably from 60 to 300. Preferable as compound (f) use simple polyether polyols and/or complex polyether polyols with a hydroxyl number greater than 160, particularly preferably greater than 200 mg KOH/g and particularly preferably a functionality of between 2.9 and 8. Especially preferable as compound (f), reactive towards isocyanates, use simple polyether polyols have an equivalent weight, that is, the molecular weight divided by the functionality of less than 400 g/mol, preferably m is it 200 g/mol. Typically, the compound (f) is present in liquid form.

As the foaming component (C) preferably used are hydrocarbons. These compounds can be used in a mixture with water and/or other physical foaming agents. Below them understand the connections that are dissolved or emulsified in the source materials for the production of polyurethane, and when the conditions of formation of the polyurethane evaporate. This involves, for example, hydrocarbons, halogenated hydrocarbons and other compounds, such as, for example, perforated alkanes, such as perference, perchloromethane, as well as ethers, esters, ketones and/or acetals.

Foaming component (C) preferably used in quantities of from 2 to 45 wt. -%, preferably from 4 to 30 wt. -%, particularly preferably from 5 to 20 wt. -%, in terms of the total weight of components (b) to (f). In a preferred embodiment, the mixture of foaming agent (C) contains hydrocarbons, in particular n-pentane and/or cyclopentane, and water. Particularly preferred hydrocarbons are n-pentane, cyclopentane, isopentane and/or a mixture of isomers. First of all, as a blowing agent (C) apply to the cyclopentane and/or n-pentane.

As catalysts (d) to obtain a foamed polyurethane or according to the state of polyisocyanurate according to the invention are conventional and well-known catalysts for the formation of polyurethanes or polyisocyanurates, for example, organic tin compounds such as tin diacetate, diktat tin, dibutyl-modelart and/or strongly basic amines, such as 2,2,2-diazabicyclo, triethylamine or preferably triethylenediamine, N,N-dimethylcyclohexylamine or simple bis(N,N-dimethylaminoethyl) ether, as well as for catalysis PIR reactions potassium acetate, octoate potassium and aliphatic Quaternary ammonium salt.

These catalysts are preferably used in quantities of from 0.05 to 3 wt. -%, preferably from 0.06 to 2 % wt., in terms of the total weight of all components.

The interaction of the above components is carried out optionally in the presence of additional substances (e), such as, for example, fire tools, fillers, regulators steam formation, foam stabilizers, surfactants and/or stabilizers against the effects of oxidative, thermal or microbial degradation or aging, preferably fire-proof means and/or foam stabilizers. The foam stabilizers denote substances which contribute to the formation of a uniform porous structure during the formation of foam. As examples: siliconsamurai foam stabilizers, such as mixed polymerizate siloxanes and oxyalkylene and other organopolysiloxane, except that what about that products alkoxysilane fatty alcohols, oxaspiro, fatty amines, ALKYLPHENOLS, dialkylphenols, alkylation, alkylresorcinol, naphthol, alternately, naphtylamine, aniline, alkylsilane, toluidine, bisphenol a, alkylated bisphenol a, polyvinyl alcohols, and, in addition, also the products alkoxysilane the condensation products of formaldehyde and alkyl phenols, formaldehyde and dialkylphenols, formaldehyde and alkylation, formaldehyde and alkylresorcinol, formaldehyde and aniline, formaldehyde and toluidine, formaldehyde and naphthol, formaldehyde and alternately, as well as formaldehyde and bisphenol A. as alkoxygroup reagents can be used, for example, ethylene oxide, propylene oxide, poly-THF, and their heavier homologues.

As a fire-retardant means, as a rule, can be applied fireproofing means known from the prior art. Suitable fire retardant means are, for example, brominated ethers (for example, Ixol® B251), brominated alcohols, such as dibromoneopentyl alcohol, tribromoneopentyl alcohol and RNT-4-diol, as well as chlorinated phosphates, such as, for example, Tris(2-chloroethyl)phosphate, Tris(2-chloroisopropyl)phosphate (TSRR), Tris(1,3-dichloroisopropyl)phosphate, Tris(2,3-dibromopropyl)phosphate and tetrakis(2-chloroethyl)ethylendiamin. Besides the already cited Utah halogen-substituted phosphates, to impart fire resistance of solid foams obtained from PUR or respectively of PUR/PIR according to the invention, can also be used inorganic flame retardant tools, such as red phosphorus, compositions containing red phosphorus, hydrate, aluminum oxide, antimony trioxide, ammonium polyphosphate and calcium sulfate or derivatives of cyanuric acid, such as, for example, melamine, or mixtures of at least two flame retardant means, such as, for example, ammonium polyphosphates and melamine and also, if necessary, starch. As other liquid flame retardant that do not contain Halogens, can be used diethylaminophenol (DEEP), triethyl phosphate (Teff), dimethylpropylene (DMPF), diphenylmethylphosphine (DPK) and others. In the framework of this invention, these fire retardant means preferably used in amounts of from 0 to 30 wt. -%, particularly preferably from 2 to 25 wt. -%, in particular, from 2.5 to 3.5 wt. -%, in terms of the total weight of components (b) to (e).

More detailed guidance in relation to the above and other starting substances can be extracted from the literature, for example, Kunststoffhandbuch, Band VII, Polyurethane, Carl Hanser Verlag Munchen, Wien, 1., 2. und 3. Edition 1966,1983 and 1993.

For the production of rigid polyurethane foams, the polyisocyanates (b) and components (a)and optionally (f), are introduced into the reaction in such number is two, that the isocyanate index of the foam is from 90 to 600, preferably from 150 to 500, particularly preferably from 180 to 450.

Rigid polyurethane foams can be obtained in batch or continuous modes using known methods. The specialist is known, among other things, receipt of foam in blocks (in continuous and batch modes), use in one-component systems (periodic mode) and in insulating the forming foam (periodic mode). The invention described here applies to all methods, but preferably by a continuous process dvuhnitochnogo the conveyor, and as the covering layers can be applied to flexible and/or rigid materials.

Rigid polyurethane foams according to the invention preferably have isolation cells, more than 90 %, particularly preferably more than 95 %.

Preferably the foams according to the invention of PUR or respectively of PUR/PIR have a density of 28 g/cm³up to 300 g/cm³especially preferably from 30 g/cm³to 50 g/cm³.

The use of rigid polyurethane foams according to the invention is carried out, in particular, for thermal insulation, for example, cooling devices, tanks or facilities, for example, in the form of insulated pipes, sandwich elements, insulating panels or is placitella.

As polyurethanes in the framework of this patent application also understand polymeric adducts of isocyanates, which, in addition to urethane groups contain other groups which they form, for example, by the reaction of isocyanate groups with themselves, for example, which group or which arise by the reaction of isocyanate groups with groups other than hydroxyl groups, and these groups most likely to be present in the polymer together with the urethane groups.

Another object of this invention is the use of complex polyether polyols, which are obtained as described above, to obtain a polyurethane. Polyurethane is a multi-purpose construction material, which finds application in many areas. Due to the large variety of raw materials that can be used, can be derived products with different properties, for example, rigid foams for insulation, blocks of soft foam for mattresses, molded soft foam for car seats and cushions on the seats, sound-absorbing foams for insulation, thermoplastic foams, foams for shoes or fine foams and dense system for molding and thermoplastic polyurethanes.

Next out is retina explained in detail by means of examples.

Examples

A list of the starting compounds used in Examples

A) obtaining a complex polyetherpolyols

Example 1 (according to the invention):

In a 4-liter flask with 4 neck equipped with a mantle, mechanical stirrer, internal thermometer, a column Packed with bodies with a height of 40 cm, the column head downward fridge for intensive cooling and membrane vacuum pump, in a nitrogen atmosphere at 100°C was placed 2280 g to (11.4 mol) of PEG 200. Within about 5 minutes was added under stirring 732 g (to 4.41 mol) of terephthalic acid and to this was added 83 mg of the dihydrate of tin dichloride. Within 2 hours they were heated to 230 °C, and water was distilled, and the turbidity of the reaction mixture disappeared. Then added 314 g (2.34 mol) technology. glutaric acid and was heated for an additional 90 minutes at 230°C. then was added 83 mg of the dihydrate of tin dichloride and created a vacuum for reaching the end of 30 mbar.

Under these conditions, continued additional condensing another 5.5 hours. Cooled and identified the following characteristics:

Analysis of complex polyester:

V = the Example for comparison. Example 3 (V) does not correspond to the invention, because the receipt was not applied component (S) (here examples: technology. glutaric acid). Example 4 (V) does not correspond to the invention, because the share of simple ester groups from oligoarticular is less than 9 mol/kg of ester and because the proportion of components that are not components (A), (B) or (C)is more than 10 wt. -%, in the specific case of use 14,1 % of the mass. of ethylene glycol. The same is true for sample 5 (V)6 (V) and 7 (V). In addition, table 1 shows that complex polyether polyols and 4 (V)5 (V)6 (V) and 7 (V), is not relevant to the invention, have the disadvantage that at room temperature are in the solid state, while complex polyether polyols 1, 2, 3, and 8 according to the invention are liquid, so that is good. Although 9(V) and satisfies this criterion, however, does not contain t is refshalevej acid, what other issues is the lack of fire resistance.

Source materials for rigid foams made of PUR/PIR:

a) a Complex polyester of examples 1, 2, 3, 8, 9 (V)

Additives to the foam consisting of b.) d.):

b) a Crosslinking agent of the company Evonik

C) Tegostab stabilizer firm Evonik

d) DMCHA, N,N-dimethylcyclohexylamine company Rheinchemie

e) TCPP, Tris(1-chloro-2-propyl)phosphate Lanxess

f) n-Pentane firm Kraemer & Martin

g) demineralized Water

h) Activator: Desmorapid VP.PU 1792 Bayer MaterialScience

i.)Desmodur VP.PU 44V40L - polyisocyanate from Bayer Material-Science

The index denotes the molar ratio of all isocyanate groups and all hydrogen atoms reactive in the reaction tchugaev-Servicenow.

In laboratory scale all original substance compositions for solid foam, except for the polyisocyanate component, otesyvajutsja in a paper Cup, thermostatics to a temperature of 23°C, mixed with a laboratory mixer firms Rap-draulik (for example, type LM-34 company Pendraulik) and, if necessary, supplemented by volatile blowing agent (pentane). Then under stirring to paleologou mixture was added polyisocyanate component (also temperature-controlled to 23°C), this song was intensively mixed, and poured the reaction mixture into the lined paper wooden forms. During the foaming process were defined setting time and end time sticking. After 24 hours from the blank of foam were cut samples for testing cubic shape with long faces 9 see

Was determined by the following characteristics:

Table 2 shows that all the foams according to the invention achieve fire class B2, while the foam 16 (V) in this case, expectations, though equipped with the same amount of flame retardant means TSRR.

1. Complex polyetherpolyols with a concentration of ether groups in the range of between 9.0 mol/kg of complex polyetherpolyols and 16 mol/kg of complex polyetherpolyols, which is obtained from a mixture containing:
(A) terephthalic acid (A),
(B) oligoethyleneglycols formula H-(OCH₂CH₂)_n-OH with srednegalechny number oxyethylene groups n in the interval between the 3.0 and 9.0 and
(C) at least one aliphatic dicarboxylic acid selected from the group consisting of succinic acid, glutaric acid, adipic acid, sabatinovka acid, cork acid, azelaic acid, decanedicarboxylic acid, d is decanedicarboxylic acid and omega-hydroxypropranolol acid.

2. Complex polyetherpolyols according to claim 1, characterized in that the component (A) is present in an amount of from 10 to 40% of the mass. in terms of the total amount of the mixture.

3. Complex polyetherpolyols according to claim 1, characterized in that the component (B) is present in an amount of from 60 to 90% of the mass. in terms of the total amount of the mixture.

4. Complex polyetherpolyols according to claim 1, characterized in that the component (C) is present in an amount of from 2 to 20% of the mass. in terms of the total amount of the mixture.

5. Complex polyetherpolyols according to claim 1, characterized in that this complex polyetherpolyols has a hydroxyl number in the range between 100 mg KOH/g and 400 mg KOH/g

6. Complex polyetherpolyols according to claim 1, characterized in that this complex polyetherpolyols at 25°C has a viscosity, measured according to DIN 53019, in the interval between 800 MPa·s and 4500 MPa·S.

7. Complex polyetherpolyols according to claim 1, characterized in that oligoethyleneglycols () has srednekamennogo number oxyethylene groups n in the area between 3.1 and 9.

8. Complex polyetherpolyols on one or more of claims 1 to 7, characterized in that this complex polyetherpolyols has a melting point in the range between -40°C and 25°C.

9. The method of obtaining complex polyetherpolyols on one or more of claims 1 to 8, characterized in that components (A), (B) and (C) in the presence of a catalyst selected from the group consisting of salts of tin (II and titinterracial, interact at a temperature between 160°C and 240°C and a pressure of between 1 and 1013 mbar in the time interval between 7 and 100 hours.

10. The use of complex polyetherpolyols on one or more of claims 1 to 8 to obtain a foam of polyurethane (PUR) or, respectively, of polyurethanes/polyisocyanurate (PUR/PIR).

11. The method of producing foam from PUR or respectively of PUR/PIR, comprising the following stages:
a) dealing at least one compound polyetherpolyols on one or more of claims 1 to 8
b) at least one component containing polyisocyanates,
c) at least one foaming agent,
d) at least one or more catalysts,
e) optionally, at least one fire-retardant agent and/or other auxiliary substances and additives,
f) optionally at least one compound containing at least two groups reactive toward isocyanates.

12. The foam of PUR or respectively of PUR/PIR obtained by the method according to item 11.

13. The use of foam from PUR or respectively of PUR/PIR method according to claim 11 for producing insulated pipes, sandwich elements, insulating panels or cooling devices.