Polyetherpolyol production method

FIELD: polymer production.

SUBSTANCE: invention, in particular, relates to improved method for producing polyetherpolyols using double metal cyanide catalysts. Method is accomplished via polyaddition of alkylene oxides to initial compounds having molecular mass between 18 and 2000 and 1 to 8 hydroxyl groups containing active hydrogen atoms, reaction being effected in presence of double metal cyanide catalysts. During the polyaddition reaction, reaction mixture is at least once passed through jet disperser, in which power density is at least 105-106 J/m3 and residence time of reaction mixture per pass is at least 10-5 sec.

EFFECT: enhanced process efficiency and expanded synthetic possibilities.

1 dwg, 3 ex

 

Description

The invention relates to a process for the production of polyether polyols, in particular to a method for production of polyether polyols using double metallocyanide catalysts.

Getting polyether polyols industry carried out mainly by polyprionidae of alkalisation to polyfunctional original compounds, such as alcohols, acids or amines by basic catalysis (e.g., KOH) (see, for example, Gum, Riese & Ulrich (Hrsg.): "Reaction Polymers", Hanser Verlag, München, 1992, S.75-96). After polyaddition basic catalyst must be removed from polyetherpolyols very expensive way, for example by neutralization, distillation and filtration. In addition, the lack of received basic catalysis of polyether polyols is that with increasing chain length continuously increases the content of monofunctional polyethers with terminal double bonds (so-called Manolov) and reduced functionality.

The resulting polyether polyols can be used to obtain polyurethanes (for example, elastomers, foams, coatings), in particular for producing elastic polyurethane foam. Flexible polyurethane foams have little resistance when compressed, have open-cellular structure, are breathable and able to arr is a valid deformation. There are block foam and forming foams (see, for example, Kunststoffhandbuch, Bd. 7, 3. Edition, Hanser Verlag, München, 1993, S.193-252). The foams produced in mass, produce a continuous or periodic manner in the form of a semi-finished product and then make a billet on the appropriate use of dimensions and contours (e.g., upholstered furniture, mattresses). Molding the foam, in contrast, receive periodic manner, wherein the foam is obtained directly in the desired form (by filling foam of the appropriate form).

Double metallocyanide (DMC) catalysts for production of polyether polyols known for a long time (see, for example, U.S. patent US-A 3404109, US-A 3829505, US-A 3941849 and US-A 5158922). The use of such DMC-catalysts for production of polyether polyols and contributes to reduction of the proportion of monofunctional polyethers (Manolov), compared with the conventional receipt of polyether polyols using basic catalysts. Improved DMC-catalysts are described, for example, in European patent applications EP-A 700949, EP-A 761708, international patent applications WO 97/40086, WO 98/16310, German patent applications DE-A 19745120, DE-A 19757574 or DE-A 198102269, in addition, have an extremely high activity and allow you to get the polyether polyols with very low concentration of catalyst (25 ppm or men who e), so that separation of the catalyst from the polyol is no longer required.

Obtained through DMC-catalysis the polyether polyols upon receipt of polyurethane foams, in particular flexible polyurethane foams, can lead to technical problems, for example, to the destabilization of foam (enhanced susceptibility to subsidence foam) or to an excessively large acestei. So DMC-catalyzed the polyether polyols are not in all cases without the consent of the composition may be replaced by the corresponding base catalyzed polyols in obtaining flexible foams.

The closest analogue of the invention is a method of producing polyether polyols by polyaddition of alkalisation to the original compounds containing active hydrogen atoms, in the presence of double metallocyanide catalysts, in which the reaction mixture is passed through a mixer, such as a rotor-stator (see US 5689012 And, 18.11.1997).

The task of the invention is to improve the characteristics of the foam produced in the presence of double metallocyanide catalysts of polyether polyols in the production of polyurethane foams.

The problem is solved by the proposed method of producing polyether polyols by polyaddition of alkalisation to the original compounds with a molecular weight of from 18 to 2000 and from 1 to 8 hydroxyl groups, the content is relevant active hydrogen atoms, in the presence of double metallocyanide catalysts, in which during the polyaddition reaction, the reaction mixture at least once passed through the jet disperser, the energy density which is at least 105J/m3while the residence time of the reaction mixture in the jet disperser in a single pass is at least 10-6seconds.

DMC-catalysts suitable for the proposed according to the invention method, in principle, known. Preferably use DMC-catalysts known from Japanese patent application JP-A 4145123, European patent applications EP-A 654302, EP-A 700949, EP-A 743093, EP-A 761708, international patent applications WO 97/40086, WO 98/16310, WO 99/19062, WO 99/19063, WO 99/33562, German patent applications DE-A 19834572, 19834573, 19842382, 19842383, 19905611, 19906985, 19913260, 19920937 or 19924672. Typical examples are described in European patent application EP-A 700949 highly DMC-catalysts, which along with the double metallocyanide connection (for example, hexacyanocobaltate (III), zinc) and organic complex ligand (e.g. tert-botulinum) additionally contain polyetherpolyols with an average molecular weight of more than 500 g/mol.

As examples of starting compounds with a molecular weight of from 18 to 2000, preferably 62-1000, and with 1-8, preferably 2-6, hydroxyl gr is pami, containing active hydrogen atoms include, for example: butanol, ethylene glycol, diethylene glycol, triethylene glycol, 1,2-propylene glycol, 1,4-butanediol, 1,6-hexanediol, bisphenol a, trimethylolpropane, glycerin, pentaerythritol, sorbitol, sucrose, degraded starch, water, or so-called pre-elongated starter, which is obtained from the above compounds by alkoxysilane.

As alkalisation use preferably ethylene oxide, propylene oxide, butylenes, and mixtures thereof. Synthesis of polyester chains is carried out only with one Monomeric epoxide or statistically or in blocks with 2 or 3 different Monomeric epoxides. For more details on this process are described in "Ullmanns Encyclopädie der industriellen Chemie", Band A21, 1992, str f.

In principle, polyprionidae can be performed in any way alkoxysilane known for DMC-catalysis.

You can use a regular periodic fashion. This DMC catalyst and the original connection is placed in the reactor of periodic action, then the reactor is heated to the desired temperature and to activate the catalyst add enough accelerated. Once the catalyst is activated, as evidenced by a pressure drop in the reactor, continuously add the rest of alkalinized to achievements is of the desired molecular weight of polyetherpolyols.

You can also use the continuous method by which pre-activated mixture of DMC-catalyst and the parent compound are continuously fed to the reactor with continuous action, for example, a continuous reactor with a stirrer (CSTR) or a tubular reactor. Accelerated dosed into the reactor, and the resulting product is continuously displayed.

However, preferably DMC-catalyzed, polyprionidae spend way by which the original connection is continuously fed during the polyaddition. This DMC-catalyzed, polyprionidae may occur during the continuous dosage of starting compound of the periodic method, as described in the international patent application WO 97/29146, or continuous manner, as described in the international patent application WO 98/03571.

DMC-catalyzed, polyprionidae can occur at pressures of from 0.0001 to 20 bar, preferably from 0.5 to 10 bar, particularly preferably from 1 to 6 bar. The reaction temperature is 20-200°C, preferably 60-180°S, especially preferably 80-160°C.

Concentration DMC-catalyst is usually 0,0005-1 wt.%, preferably 0.001 to 0.1 wt.%, particularly preferably 0.001 to 0.01 wt.%, in calculating the number of polyetherpolyols.

Suitable for use in the proposed method, inkjet dispersion is ATOR schematically represented in the attached drawing. Instead of a jet disperser can be used for any other mixer that works on the same principle.

Adherence to the stated minimum values of energy density and residence time of the reaction mixture in the jet disperser in a single pass is essential from the point of view of achieving the above technical result.

When this energy density Ev is determined by the pressure difference at the nozzle (pressure homogenization) ΔpN:

Ev[j/m3]=ΔpH.

According to the invention using the energy density of at least 1×105J/m3preferably, at least 3×105J/m3and particularly preferably at least 5×105J/m3. The residence time of the product in the jet disperser should be at least 1×10-6second, as a rule, from 1×10-5up to 1 second. Typically, the polyol is passed several times through the jet disperser.

Jet disperser should be included in the process of mixing in such a way as to be directly involved in the process of alkoxysilane. With this aim the jet disperser, for example, can be included in the circulation process of pumping in the reactor. Polyetherpolyols passes through the jet disperser together with not yet Rea is of the starter, alkalization and catalyst. The introduction of the reactants and catalyst can be managed independently from the jet disperser elsewhere in the reactor. For implementing the method of the present invention the jet disperser is included in the circulation process of pumping. Thus the energy density required to achieve the desired effect, does not depend on the pressure in the reactor. Decisive is only the energy density in the jet disperser, which is proportional to the pressure loss before the jet disperser.

According to another form of the method of the present invention the jet disperser used for mixing the flow of the educt with the contents of the reactor. Thus educti, for example: 1. the initial mixture containing either a single component or a mixture of suitable compounds containing active hydrogen atoms, 2. accelerated or a mixture of alkalisation, and, optionally, 3. the catalyst suspension, the conditions in which they do not react, homogenize any suitable way, and then stirred in the jet disperser with polyetherpolyols containing active DMC catalyst. Suitable in this case means that we obtain a homogeneous catalyst dispersion.

In another embodiment, educti in any sequence, if possible, che is ez short periods of time, mixed with polyetherpolyols containing the active DMC catalyst. For carrying out this process it is preferable to use multiple series-connected jet dispersers. The sequence of the added reagents in this case to solve the problem is not so significant. It is preferable to first add accelerated or a mixture of alkalisation, and then the initial mixture containing either a single component or a mixture of suitable compounds containing active hydrogen atoms, as so due to the very high local concentrations of low molecular weight starting compounds prevented the possible deactivation of the active catalyst. The addition of the catalyst is undesirable.

Processing of polyether polyols in the jet disperser is conducted usually at temperatures of from 20 to 200°C, preferably 60-180°S, especially preferably 80-160°C.

In the method proposed according to the invention, polyetherpolyols fully or partially get through catalyzed double metallocyanide catalyst polyaddition of alkalisation to the original compounds containing active hydrogen atoms.

In normal periodic process is preferably, for example, be used as starting compounds for DMC-catalysis oligomeric PR is relied alkoxysilane with an average molecular weight from 200 to 2000 g/mol). This is possible through alkoxysilane source of low-molecular compounds, such as 1,2-propylene glycol or glycine, using the normal basic catalysis (e.g., KOH) or acid catalysis.

Also the so-called "EO-SAR" (ethylenoxide end block), which is produced, for example, the interaction of poly(oxypropylene)polyols or poly(oxopropyl/oksietilenom)polyols with ethylene oxide in order to convert the greater part of the secondary hydroxy groups of polyetherpolyols in primary hydroxy-group, which is preferably carried out using basic catalysis (e.g., KOH).

Getting the polyether polyols of the proposed method is preferably carried out so that at least 20 wt.%, preferably, at least 40 wt.% (respectively in terms of the number of accelerated used to obtain polyetherpolyols) used accelerated entered into DMC-catalyzed interaction.

The polyether polyols obtained by the process according to the invention have significantly improved properties foaming upon receipt of soft polyurethane foam.

Examples

Getting polyether polyols

Polyol A (control example)

Polyol a is nominally trifunctional polyetherpolyols with molecular weight of 3000 g/mol, which received preframe the receiving of glycerine with propylene oxide by means of catalysis CON (0,41 wt.%, in the calculation of the number of ready polyetherpolyols) at a temperature of 107°and the subsequent separation of the catalyst by neutralization with sulfuric acid, dehydration and filtering.

Polyol In (reference example)

Polyol b is nominally trifunctional polyetherpolyols with molecular weight of 3000 g/mol, obtained by transformation of glycerine with propylene oxide in continuous dosing source through DMC-catalysis (30 parts per million, based on the number of ready polyetherpolyols, catalyst-based hexacyanocobaltate zinc and DMC, tert-butanol as ligands and received by DMC-catalyzed poly(oxypropylene)diol with an average molecular weight of 4000 g/mol, described in European patent application EP-A 700949, example 1) at a temperature of 130°C.

Polyol With

The polyol is a nominally trifunctionally polyetherpolyols with molecular weight of 3000 g/mol, obtained by reacting glycerol with propylene oxide by DMC-catalysis at a temperature of 130°and a continuous feeding of the parent compound (30 parts per million, calculated on the number of ready polyetherpolyols, linkexecute-DMC-catalyst containing as a ligand tert-butanol, and obtained by DMC-catalyzed poly(oxypropylene)diol with an average forefront of the lar mass of 4000 g/mol, described in European patent application EP-A 700949, example 1). During interaction polyetherpolyols using a membrane piston pump was pumped through the jet disperser (one hole with a diameter of 0.43 mm) in mass flow 16 l/h. The pressure loss in the jet disperser was 10 bar, which corresponds to the energy density 1×106J/m3. The residence time of the reaction mixture in the jet disperser is 4×10-5seconds.

Getting soft polyurethane foam

For a series of comparative studies using the following materials:

Polyol A (control example)
Polyol In (reference example)
Polyol With
TDI:the mixture of isomers 2,4-toluylene diisocyanate and 2,6-toluylene diisocyanate with the ratio of 80:20, commercially available under the name Desmodur®T80 (Bayer AG, D-51368 Leverkusen)
Catalyst 1:bis(dimethylamino)ethyl ester
Silicone stabilizer 1:Tegostab®BF 2370 (Th. Goldschmidt AG, D-45127 Essen)
Catalyst 2:the catalyst on the basis of octoate tin, commercially available under the name of Desmorapid®SO (Rheinchemie Reina Gb, D-68219 Mannheim)

To obtain soft polyurethane foam using the following formula:

The original substanceQuantity (g)
Polyol a, b or C100,0
Water6,0
Silicone stabilizer 10,6
Catalyst 10,1
Catalyst 20,15
TDI73,4

The way to obtain

All the ingredients, except TDI, initially within 20 seconds, stirred with a high speed stirrer. Then added to the mixture of TDI and the composition is homogenized by stirring for 5 seconds. Expanded onto the composition is placed in an open lined paper form with a footprint of 27×13 cm, and after foaming is kept in a heated up to 100°a drying Cabinet for 30 minutes. After cooling, the foam is cut in the middle and subjected to visual analysis.

Example No.PolyolAnalysis of foam
1 (control)Andthin and proper cellular structure, cracks and subsidence no
2 (control)Inrough the I, irregular cellular structure, partially falls
3thin and proper cellular structure, cracks and subsidence no

Thanks proposed according to the invention the processing DMC-catalyzed polyol using a jet disperser receive the product (polyol C)compared with the untreated product (polyol) without problems processed until soft polyurethane foam.

The method of producing polyether polyols by polyaddition of alkalisation to the original compounds with a molecular weight of from 18-2000 and 1-8 hydroxyl groups containing active hydrogen atoms, in the presence of double metallocyanide catalysts, in which during the polyaddition reaction, the reaction mixture at least once passed through the jet disperser, the energy density which is at least 105-106J/m3while the residence time of the reaction mixture in the jet disperser in a single pass is at least 10-6seconds.



 

Same patents:

FIELD: industrial organic synthesis.

SUBSTANCE: production of polyetherpolyols using double metal cyanide catalysts is accomplished via polyaddition of alkylene oxides to starting compounds with molecular mass from 18 to 2000 and 1-8 hydroxyl groups in presence of above catalysts. During polyaddition reaction, reaction mixture is at least once passed through jet disperser, wherein power density is at least 5x105 J/m3 and residence time of reaction mixture in jet disperser is at least 10-6 sec per pass.

EFFECT: expanded assortment of polyetherpolyols allowing production of polyurethane foams characterized by fine cellular structure and lack of pulling-down in the course of formation.

1 dwg, 12 ex

FIELD: physicochemical analytical methods.

SUBSTANCE: invention relates to filling materials for reversed-phase liquid chromatography and provides powdered hydrophobic polymer prepared by reaction of powdered cross-linked (meth)acrylate polymer having hydroxyl group with cross-linking epoxy compound followed by hydrolysis of oxyrane cycles and reaction of thus obtained hydroxyl group-containing compound with epoxy compound containing 6 to 40 carbon atoms. Resulting filling material is characterized by high acid/alkali resistance and capability of retaining column efficiency when making use of different solvents.

EFFECT: enabled chromatogram with sharp picks for polycyclic aromatic compounds.

10 cl, 1 tbl, 4 ex

FIELD: polymerization processes and catalysts.

SUBSTANCE: alkylene oxide polymerization is conducted in presence of catalyst based on bimetallic cyanide complex and initiator containing hydroxyl group. Al last part of the catalyst is preliminarily subjected to treatment by ultrasonic and/or electromagnetic emission. Invention discloses both polymerization catalyst treatment method and catalyst itself.

EFFECT: enabled production of polyether-polyols with low unsaturation level and increased activity of catalyst.

10 cl, 3 ex

FIELD: organic chemistry, polymers.

SUBSTANCE: invention relates to catalysts for polymerization of cyclic esters of formula , wherein M represents tin or germanium atom L and L are independently group of formula -E14(R14)(R'14)(R''14), E15(R15)(R'15) or E16(R16); E14 represents element of 14 group; E15 represents element of 15 group; and E14 represents element of 16 group; R14, R'14, R''14, R15, R'15, and R16 are independently hydrogen atom; alkyl, cycloalkyl or aryl optionally substituted with halogen atom, alkyl cycloalkyl, aryl, nitro or cyano; rest of formula -E'14RR'R''; -E'14 represents element of 14 group; R, R', R'' are independently hydrogen atom; alkyl, cycloalkyl or aryl optionally substituted with halogen atom, alkyl cycloalkyl, aryl, nitro or cyano. Also invention relates to method for production of block- or random copolymers of cyclic esters and copolymers.

EFFECT: improved catalysts for production of heterocyclic compound copolymers.

9 cl, 6 ex

FIELD: continuous production of polyoxyalkylene polyether product.

SUBSTANCE: proposed method includes introduction of first portion of mixture of double metallocyanide catalyst with initial starter into continuous-action reactor for initiating polyoxyalkynylation of initial starter after introduction of alkylene oxide. Proposed method includes: (a) continuous introduction of one or more alkylene oxides into said reactor; (a')continuous introduction of mixture of double metallocyanide catalyst with starter into inlet hole of said reactor for maintenance of catalytic activity at required level; (a")continuous introduction of one or several additional starters in addition to starter introduced into said inlet hole of reactor together with catalyst; these additional starters may be identical to said starter or may differ from it and may contain additional double metallocyanide catalyst; (b) polyoxyalkynylation of combined starters of continuous action of stages (a), (a') and (a") for obtaining polyoxyalkylene polyether product having required average molecular mass; and (c) continuous removal of said polyoxyalkylene polyether product from reactor. Proposed method makes it possible to obtain polyoxyalkylene polyether product of low degree of nonsaturation and narrow polydispersity practically containing no fractions of high molecular mass.

EFFECT: enhanced efficiency.

29 cl, 6 dwg, 7 ex

FIELD: industrial organic synthesis.

SUBSTANCE: polyetherpolyols are synthesized via reaction of diols or polyols with ethylene oxide, propylene oxide, butylene oxide, or mixtures thereof in presence of suspended multimetallic cyanide complex catalyst in reactor provided with stirrer, wherein reaction mixture is recycled with the aid of pump through externally located heat-exchanger.

EFFECT: increased productivity based on unit volume in unit at high quality of product.

9 cl, 4 ex

FIELD: chemistry of polymers, chemical technology.

SUBSTANCE: invention relates to a method for preparing a water-soluble copolymer. Method involves interaction of epichlorohydrin excess with primary or secondary amine or with a mixture of primary or secondary amine and ammonia and the following addition of tertiary aliphatic amine as inhibitor of gel formation. Epichlorohydrin is dosed to primary or secondary amine aqueous solution or a mixture of primary or secondary amine with ammonia at temperature 25-40°C. Then the reaction mixture is heated to 90°C followed by dosing the additional amount of epichlorohydrin wherein the total mole ratio of epichlorohydrin to primary or secondary amine or to a mixture of primary or secondary amine with ammonia = (1.03-1.10):1, respectively. Inhibitor of gel formation is added in the amount 0.2-0.5 mole per 1 mole of epichlorohydrin excess. Invention provides preparing copolymer with structure that provides avoiding formation of gel.

EFFECT: improved preparing method.

2 cl, 1 tbl, 23 ex

Polyether-polyols // 2263684

FIELD: polymer production.

SUBSTANCE: invention relates to a method of producing polyether-polyols via catalytic addition of at least two alkylene oxides to H-functional initiators, during which operation at least one oxyalkylene unit is incorporated as a result of joint dosage of at least two alkylene oxides. Catalyst utilized is at least one metal cyanide-based compound. When performing joint dosage ratios of alkylene oxides to each other is varied.

EFFECT: enabled production of polyether-polyols without clouding and having processing-appropriate viscosity.

8 cl, 12 ex

FIELD: industrial organic synthesis.

SUBSTANCE: process of producing polyether-polyols containing at most 15 ppm sodium or potassium comprises following steps: (a)interaction of initiator having at least to active hydrogen atoms with at least one alkylene oxide in presence of catalyst containing alkali metal hydroxide to form polyether-polyol reaction product; (b) neutralization of polyether-polyol reaction product obtained in step (a) by bringing it into contact with acid having pKa below 5 and water, said acid and said water being introduced in such an amounts that finally content of water is 1 wt % or of the total weight of polyether-polyol present, while molar ratio of acid to alkali metal hydroxide ranges from 0.3:1 to 1.0:1; optionally (c) reduction of content of water in reaction mixture to 0.5 wt % or less of the total weight of polyether-polyol; and (d) removal of salt crystals from polyether-polyol and recovery of neutralized polyether-polyol containing not more than 15 ppm sodium and/or potassium. In the course of neutralization, magnesium silicate or aluminum silicate is added in amount below 0.05 wt parts per 100 wt parts of polyether-polyol and also hydrated inorganic acid metal salt in amount 0.01% of the weight of polyether-polyol.

EFFECT: minimized consumption of heat during neutralization step and reduced neutralization time.

7 cl, 6 ex

FIELD: polymer production.

SUBSTANCE: polyol polyethers are prepared by cycle-cleaving polymerization of ethylene oxide and at least one alkylene oxide having at least three carbon atoms in molecule and attachable to H-functional initiator in presence of catalyst. H-functional initiator binds up to 40% (based on the weight of final polyol polyether) of ethylene oxide or mixture thereof with aforesaid alkylene oxide with at least 98 wt % ethylene oxide in presence of catalyst, which is at least one basic compound. To thus obtained polyol polyether, at least one alkylene oxide as defined above or mixture of ethylene oxide with the latter containing up to 20 wt % ethylene oxide is chemically added using as catalyst at least one metal cyanide-based compound.

EFFECT: enabled preparation of polyol polyethers with high level of ethylene oxide and low hydroxyl number.

3 cl, 3 tbl, 6 ex

FIELD: polymer production.

SUBSTANCE: polyoxyalkylene-polyols are obtained via direct polyoxyalkylenation of acid-sensitive low-molecular initiator with molecular weight below 400 Da in presence of double complex metal cyanide catalyst. Process comprises: (i) creation of appropriate conditions in reactor of polyoxyalkylenation in presence of double complex metal cyanide catalyst; (ii) continuously feeding into reactor alkylene oxide and above-mentioned initiator; and (iii) discharging polyether product. Loss of catalyst activity is reduced by performing at least one of the following operations: acidification of acid-sensitive low-molecular initiator before feeding it into reactor; and treatment of the same with effective amount of a substance other than acid, which reacts with base or absorbs base, before feeding it into reactor.

EFFECT: prevented catalyst from loosing its activity and essentially decreased high-molecular fraction and polydispersity of polyoxyalkylene-polyols.

21 cl, 2 dwg, 2 tbl, 3 ex

FIELD: polymerization catalysts.

SUBSTANCE: invention provides double metal cyanide catalysts for production of polyetherpolyols via polyaddition of alkylene oxides to starting compounds containing active hydrogen atoms, which catalysts contain double metal cyanide compounds, organic complex ligands, and α,β-unsaturated carboxylic acid esters other than above-mentioned ligands.

EFFECT: considerably increased catalytic activity.

6 cl, 16 ex

FIELD: polymerization catalysts.

SUBSTANCE: catalyst is composed of double metal cyanide compound, organic ligand, and two complexing components other than precedent organic ligand and selected from group including: polyethers and polyesters, glycidyl ethers, esters from carboxylic acids and polyatomic alcohols, bile acids, bile acid salts, bile acid esters, bile acid amides, and phosphorus compounds, provided that selected complexing components belong to different classes.

EFFECT: substantially increased catalytic activity.

5 cl, 1 tbl, 16 ex

FIELD: polymer production.

SUBSTANCE: polyol polyethers are prepared by cycle-cleaving polymerization of ethylene oxide and at least one alkylene oxide having at least three carbon atoms in molecule and attachable to H-functional initiator in presence of catalyst. H-functional initiator binds up to 40% (based on the weight of final polyol polyether) of ethylene oxide or mixture thereof with aforesaid alkylene oxide with at least 98 wt % ethylene oxide in presence of catalyst, which is at least one basic compound. To thus obtained polyol polyether, at least one alkylene oxide as defined above or mixture of ethylene oxide with the latter containing up to 20 wt % ethylene oxide is chemically added using as catalyst at least one metal cyanide-based compound.

EFFECT: enabled preparation of polyol polyethers with high level of ethylene oxide and low hydroxyl number.

3 cl, 3 tbl, 6 ex

FIELD: industrial organic synthesis.

SUBSTANCE: process of producing polyether-polyols containing at most 15 ppm sodium or potassium comprises following steps: (a)interaction of initiator having at least to active hydrogen atoms with at least one alkylene oxide in presence of catalyst containing alkali metal hydroxide to form polyether-polyol reaction product; (b) neutralization of polyether-polyol reaction product obtained in step (a) by bringing it into contact with acid having pKa below 5 and water, said acid and said water being introduced in such an amounts that finally content of water is 1 wt % or of the total weight of polyether-polyol present, while molar ratio of acid to alkali metal hydroxide ranges from 0.3:1 to 1.0:1; optionally (c) reduction of content of water in reaction mixture to 0.5 wt % or less of the total weight of polyether-polyol; and (d) removal of salt crystals from polyether-polyol and recovery of neutralized polyether-polyol containing not more than 15 ppm sodium and/or potassium. In the course of neutralization, magnesium silicate or aluminum silicate is added in amount below 0.05 wt parts per 100 wt parts of polyether-polyol and also hydrated inorganic acid metal salt in amount 0.01% of the weight of polyether-polyol.

EFFECT: minimized consumption of heat during neutralization step and reduced neutralization time.

7 cl, 6 ex

Polyether-polyols // 2263684

FIELD: polymer production.

SUBSTANCE: invention relates to a method of producing polyether-polyols via catalytic addition of at least two alkylene oxides to H-functional initiators, during which operation at least one oxyalkylene unit is incorporated as a result of joint dosage of at least two alkylene oxides. Catalyst utilized is at least one metal cyanide-based compound. When performing joint dosage ratios of alkylene oxides to each other is varied.

EFFECT: enabled production of polyether-polyols without clouding and having processing-appropriate viscosity.

8 cl, 12 ex

FIELD: chemistry of polymers, chemical technology.

SUBSTANCE: invention relates to a method for preparing a water-soluble copolymer. Method involves interaction of epichlorohydrin excess with primary or secondary amine or with a mixture of primary or secondary amine and ammonia and the following addition of tertiary aliphatic amine as inhibitor of gel formation. Epichlorohydrin is dosed to primary or secondary amine aqueous solution or a mixture of primary or secondary amine with ammonia at temperature 25-40°C. Then the reaction mixture is heated to 90°C followed by dosing the additional amount of epichlorohydrin wherein the total mole ratio of epichlorohydrin to primary or secondary amine or to a mixture of primary or secondary amine with ammonia = (1.03-1.10):1, respectively. Inhibitor of gel formation is added in the amount 0.2-0.5 mole per 1 mole of epichlorohydrin excess. Invention provides preparing copolymer with structure that provides avoiding formation of gel.

EFFECT: improved preparing method.

2 cl, 1 tbl, 23 ex

FIELD: industrial organic synthesis.

SUBSTANCE: polyetherpolyols are synthesized via reaction of diols or polyols with ethylene oxide, propylene oxide, butylene oxide, or mixtures thereof in presence of suspended multimetallic cyanide complex catalyst in reactor provided with stirrer, wherein reaction mixture is recycled with the aid of pump through externally located heat-exchanger.

EFFECT: increased productivity based on unit volume in unit at high quality of product.

9 cl, 4 ex

FIELD: continuous production of polyoxyalkylene polyether product.

SUBSTANCE: proposed method includes introduction of first portion of mixture of double metallocyanide catalyst with initial starter into continuous-action reactor for initiating polyoxyalkynylation of initial starter after introduction of alkylene oxide. Proposed method includes: (a) continuous introduction of one or more alkylene oxides into said reactor; (a')continuous introduction of mixture of double metallocyanide catalyst with starter into inlet hole of said reactor for maintenance of catalytic activity at required level; (a")continuous introduction of one or several additional starters in addition to starter introduced into said inlet hole of reactor together with catalyst; these additional starters may be identical to said starter or may differ from it and may contain additional double metallocyanide catalyst; (b) polyoxyalkynylation of combined starters of continuous action of stages (a), (a') and (a") for obtaining polyoxyalkylene polyether product having required average molecular mass; and (c) continuous removal of said polyoxyalkylene polyether product from reactor. Proposed method makes it possible to obtain polyoxyalkylene polyether product of low degree of nonsaturation and narrow polydispersity practically containing no fractions of high molecular mass.

EFFECT: enhanced efficiency.

29 cl, 6 dwg, 7 ex

FIELD: organic chemistry, polymers.

SUBSTANCE: invention relates to catalysts for polymerization of cyclic esters of formula , wherein M represents tin or germanium atom L and L are independently group of formula -E14(R14)(R'14)(R''14), E15(R15)(R'15) or E16(R16); E14 represents element of 14 group; E15 represents element of 15 group; and E14 represents element of 16 group; R14, R'14, R''14, R15, R'15, and R16 are independently hydrogen atom; alkyl, cycloalkyl or aryl optionally substituted with halogen atom, alkyl cycloalkyl, aryl, nitro or cyano; rest of formula -E'14RR'R''; -E'14 represents element of 14 group; R, R', R'' are independently hydrogen atom; alkyl, cycloalkyl or aryl optionally substituted with halogen atom, alkyl cycloalkyl, aryl, nitro or cyano. Also invention relates to method for production of block- or random copolymers of cyclic esters and copolymers.

EFFECT: improved catalysts for production of heterocyclic compound copolymers.

9 cl, 6 ex

Up!