Aqueous composition comprising chemical microgel bound with aqueous polymer

FIELD: chemical compositions, polymers.

SUBSTANCE: invention relates to aqueous compositions comprising particles of chemically cross-linked water-soluble or water-dispersed chemical microgel. Invention proposes an aqueous composition comprising particles of chemically cross-linked water-soluble or water-dispersed chemical microgel bound with at least one bridge water-soluble or water-dispersed polymer wherein its chemical composition differs from chemical composition of indicated particles. The amount of chemical microgel particles is from 0.05 to 40% dry mass of the composition mass, and the amount of bridge polymer provides exceeding the viscosity value of the composition by at least three times or preferably it exceeds or equal to 10-fold viscosity value of chemical microgel particles an aqueous solution, and exceeds viscosity value of the bridge polymer an aqueous solution under the same conditions. Also, invention proposes a method for preparing of the claimed an aqueous composition. Proposed composition can be used in the field for mining petroleum and gas deposits, and in manufacturing detergents and cosmetics also. Invention provides enhancing stability of the composition.

EFFECT: improved and valuable properties of composition.

25 cl, 2 tbl, 2 ex

 

Description

The object of the present invention are aqueous compositions containing particles of chemical microgel associated with at least one bridging polymer, and, more specifically, in the form of viscous fluid substances or gel.

It also relates to a method for obtaining such aqueous compositions, as well as to their use and to products containing these compositions.

Known mainly two types of gels, chemical gels and physical gels.

One of the main advantages of chemical gels is that they have relatively high moduli of elasticity and well withstand fluctuations in temperature. In addition, they may have low sensitivity to the introduction of conventional additives such as bases, acids, surfactants, etc. However, these systems are not reversible in the event of exposure to effort shift, which greatly limits their use. Indeed, typically, the gels used in the conditions of the shear stress, and the user is interested in the fact that after removal of the shear stress was restored to the initial viscosity of the gel. However, chemical gels do not have such properties.

The specified property of reversibility, at least partly, present in the physical gels. In fact, they possess the try property to recover after shifting the viscosity, which fluid had before the influence of shearing forces. In addition, quite often, these gels have rheological profile-thinning type (when the viscosity of the gel decreases with increasing shearing forces). The problem is that the change of the rheological properties of such gels is uncontrolled, when they are subjected to changes in external temperature and, possibly, changes in the chemical composition (by introducing additives), etc. in addition, these gels are essentially viscoelastic fluid substances which possess the property of gel within a short period, and viscous properties remain for a long period.

One of the objectives of the present invention is to develop a gel that would have the properties of stability inherent not only to the gels chemical type, but also the physical type.

These and other problems are solved in the framework of the present invention, the object of which is an aqueous composition comprising particles of chemical water-soluble or water-dispersible microgel associated with at least one water-soluble or water-dispersible bridging polymer, the chemical nature of which differs from the chemical nature of these microgel particles; and the particles of the chemical microgel is from 0.05 up to 40% (based on dry weight by weight of the composition, and the number of bridging polymer is such that the viscosity of the composition is at least three times, preferably ten times greater than or equal to ten times the viscosity of the aqueous solution of the particles of the chemical microgel and exceeds the viscosity of an aqueous solution bridging polymer under the same conditions.

The object of the present invention is the first method of obtaining the specified composition, according to which:

a) get in the aqueous phase chemical gel by polymerization of one or more selected monomers and cross-linking agent or by chemical cross-linking of the polymer after polymerization,

b) grind the obtained gel to obtain particles of chemical microgel,

C) in the aqueous phase is introduced into the contact of these particles chemical microgel at least one bridging polymer.

The invention relates also to the second method of obtaining the composition, whereby perform the following steps:

a) receive particles of chemical microgel by the polymerization of one or more selected monomers and cross-linking agent in microreactors and/or when mixing and/or in the presence of at least one agent-limiting circuit, or by chemical cross-linking of the polymer in paleolibertarians period in microreactors and/or during the mixing process

b) in the aqueous phase centuries is out at the contact of these particles chemical microgel at least one bridging polymer.

The composition according to the invention allows to obtain a gel, which is at least partially or completely reversible gel. The rheological profile of the water composition is mainly thinning profile type. Thus, when the composition is subjected to shear and the viscosity decreases when the stop shift state again the viscosity increase and even return to its original value. If the flow profile has a thickening nature, then when you stop shift reversibility is that there is a reduction of viscosity and even restores the initial value of viscosity. In addition, the composition according to the invention forms a gel, which better retains its rheological properties in harsh temperature conditions, for example, when working in the mode of shear stress, while regular physical gels them lose.

It should also be noted that depending on the nature of the microgel particles and bridging polymer rheological behavior of the composition can be adjusted depending on pH (gels, initiated pH-gels sensitive to pH) and this is a definite advantage.

Other characteristics and advantages of the present invention become apparent upon further reading of the description and example.

It should noted the ü, that the aqueous composition according to the invention can be in the form of a gel. More specifically, the gel is called composition, the elastic modulus (G') is greater than or equal to the loss (G") in the frequency interval from 1 to 10 Hz and geometry type cone-plane; and the units measure linear viscoelastic at 25°using rheometer Rheometrics or Carrimed.

In addition, unless otherwise indicated, the viscosity was measured by a viscometer of type Carrimed with the geometry of the cone-plane, and the measurement was carried out at 25°and the gradient shift with 1-1.

In the description text of the specified conditions of temperature and pH value of the composition refers to the composition as such prior to its application, regardless of whether it contains only the copolymer and the substance having the charge or it entered other miscellaneous components required to obtain the finished composition (product).

In addition, it should be clarified that the term "polymer" means homopolymers and copolymers.

Bridging polymer is referred to as water-soluble or water-dispersible, if not observed phenomena of macroscopic phase separation in an hour after the start of curing of the polymer in solution or in dispersion in an aqueous phase at the same concentration and temperature, as for the compositions according to the invention.

In addition, motorstore is passed or water-dispersible particles of a chemical called microgel particles chemically cross-linked polymer and swelling under the action of an aqueous solution.

As mentioned above, one of the first components of the aqueous composition according to the invention are water-soluble or water-dispersible particles of chemical microgel.

More specifically, the number of particles chemical microgel is from 0.05 to 10% dry matter by weight of the composition, preferably from 0.1 to 5% dry matter by weight of the composition.

In accordance with the preferred method of carrying out the invention srednesemennyh the particle size of the chemical microgel is from 0.3 μm to 10 mm, preferably from 1 to 1000 microns and more preferably from 1 to 100 microns.

Srednesemennyh size determined by optical microscopy.

Additionally, the particles of the chemical microgel consist of at least one water-soluble or water-dispersible chemically cross-linked polymer.

The specified polymer can be obtained directly in crosslinked form, for example, by introducing into one or more of the monomers constituting the polymer, at least one cross-linking agent, which in most cases is a multifunctional monomer.

The specified polymer can also be obtained at the stage of chemical crosslinking in paleolibertarians period, i.e. by merging stage after polymerization of one or more monomers included in the composition of this polymer.

In a preferred embodiment, the OS is the hope of the invention the polymer, from which to obtain particles of chemical microgel, is such that the number of water-soluble units of the specified polymer is at least 50% of the number of units of the polymer, preferably at least 80 wt.% from the polymer.

Under hydrophilic link imply a monomer selected from those monomers which, after homopolymerization with a degree of polymerization of from 40 to 100 form a polymer soluble in the conditions of temperature and pH of the composition. More specifically, the temperature is from 15 to 35°C.

Polymers, which form particles of chemical microgel, get at least a hydrophilic non-ionic, ionic or potentially an ionisable (in particular, depending on pH) monomers.

More specifically, the nonionic hydrophilic monomers selected from ethylene oxide; amides of mono - and polycarboxylic acids, linear, branched, cyclic or aromatic, containing at least one ethylene linkage or derivatives such as (meth)acrylamide, N-methylol(meth)acrylamide; some esters, derivatives of (meth)acrylic acid, such as 2-hydroxyethyl(meth)acrylate; vinyl esters, forming a polyvinyl alcohol blocks after hydrolysis, such as vinyl acetate, vinyl Versatate® (vinylation), finalproject, N-Vigipirate individually or in a mixture.

<> As ionic or potentially an ionisable hydrophilic monomers can mainly be explained by anionic or potentially anionic monomers containing at least one carboxylic, sulfonic, sulfuric, phosphonic, phosphoric, sulfonterol group, their respective salts or corresponding precursors.

In particular, the polymers can be obtained from at least one monomer chosen from:

mono - and polycarboxylic linear, branched, cyclic or aromatic acids, N-substituted derivatives of these acids, monoamino polycarboxylic acids containing at least one ethylene linkage;

linear, branched, cyclic or aromatic vinylcarbazole acids;

- amino acids containing one or more ethylene ties, individually or in mixtures, sulfonic or phosphonic derivatives, macromonomers derived from such monomers, salts or precursors of these monomers. It should be recalled that the term macromonomer means a macromolecule that contains one or more polymerizing groups.

As examples of suitable monomers specifically include:

acrylic acid, methacrylic acid, fumaric acid, taconova acid, citraconate acid, maleic acid, olein is a new acid, linoleic acid, linolenic acid, acrylamidoglycolate acid, 2-propene-1-sulfonic acid, metalinsulator acid, styrelseledamot acid, α-acrylamidophenylboronic acid, 2-sulfoaildenafil, sulfopropyl acid, bis-sulfopropyl acid, bis-alphapapillomavirus acid, sulfatereducing acid, monophosphoryl ether hydroxyethylmethacrylate acid, and alkali metal salts, e.g. sodium, potassium or ammonium salt;

- N-methacryloylamido, N-acryloyldimethyl;

individually or in mixtures, as well as macromonomer derivatives of these monomers, salts or precursors of such monomers.

It should be noted, without leaving the scope of the present invention that it is possible to use monomers which are precursors of the above-described monomers. This means that these monomers contain links, which, after their incorporation into the polymer can be converted, in particular, by chemical treatment such as hydrolysis, in the above matter.

In accordance with a second embodiment of the hydrophilic ionic or potentially ionic monomers selected from cationic or potentially cationic monomers.

As such monomers can be used, not limited to:

- aminoalkyl the(meth)acrylate, aminoalkyl(meth)acrylamide;

the monomers containing at least one secondary, tertiary or Quaternary amino group or a heterocyclic group containing a nitrogen atom, vinylamine, ethylenimine;

ammonium salts diallyldimethyl;

individually or in mixtures, as well as macromonomers derived from such monomers, salts of these monomers.

These monomers may contain a counter-ion selected from halogen atoms, e.g. chlorine, sulfates, hydrosulfate, alkyl sulphates, phosphates, citrates, formats, acetates.

As examples of cationic monomers that can be part of the cationic block copolymer, can be called:

- dimethylaminoethyl(meth)acrylate, dimethylaminopropyl(meth)acrylate, ditretbutilfenol(meth)acrylate, dimethylaminomethyl(meth)acrylamide, dimethylaminopropyl(meth)acrylamide;

- ethylenimine, vinylamine, 2-vinylpyridine, 4-vinylpyridine;

- chloride trimethylaminoethyl(meth)acrylate, methyl sulfate of trimethylammoniumchloride, chloride benzyldimethylammonium(meth)acrylate, chloride 4-benzylbenzimidazole ethyl acrylate, chloride trimethylaminoethyl(meth)acrylamide, chloride trimethylammoniumphenyl;

- chloride ammonitellidae;

individually or in mixtures, as well as macromonomer derived from these monomers.

No output is beyond the scope of the invention, you can use one or more amphoteric monomers, which, depending on the pH make an overall positive, negative or zero charge. You can also use one or more monomers zwitterionic type, which have a zero charge, regardless of pH.

In addition, polymers that form particles of chemical microgel, if desired, can be derived from hydrophobic monomers.

More specifically, the hydrophobic monomers are selected from:

of propylene oxide, butylene oxide;

- esters of mono - or polycarboxylic acids, linear, branched, cyclic or aromatic, containing at least one ethylene linkage,

- αβ-Ethylenediamine NITRILES, vinyl ethers, vinyl esters, vinylaromatic monomers, vinyl halides or vinylidene;

- hydrocarbon monomers, linear, branched, aromatic or non-aromatic, containing at least one ethylene linkage,

individually or in mixtures, as well as macromonomers derived from these monomers.

As specific examples of the hydrophobic monomers used to obtain polymers can be called:

the propylene oxide, butylene oxide;

- esters of (meth)acrylic acid and an alcohol containing from 1 to 12 carbon atoms, for example, met the l(meth)acrylate, ethyl(meth)acrylate, propyl(meth)acrylate, n-butyl(meth)acrylate, tert-butyl(meth)acrylate, isobutyl(meth)acrylate, 2-ethyl hexyl acrylate;

- vinyl acetate, vinyl Versatate®finalproject, vinyl chloride, vinylidenechloride, simple metilidinovy ether, simple ethylenically ether;

- vinyl NITRILES, including, in particular, those containing from 3 to 12 carbon atoms, for example, Acrylonitrile and Methacrylonitrile;

- styrene α-methylsterol, vinyltoluene, butadiene, chloroprene;

individually or in mixtures, as well as macromonomer derived from these monomers.

Polymers, which form particles of chemical microgel may be homopolymers or copolymers.

In addition, their structure can be of any type. For example, the copolymers can have a statistical or block structure. In addition, regardless of whether they contain or do not contain different monomers, the polymers can be linear, branched, may have a comb-shaped or star-shaped structure. The person skilled in the art can easily choose the type of monomers of the above, as well as their corresponding number in order to obtain a complete chemical water-soluble or water-dispersed microgel.

Following are descriptions of obtaining particles of chemical microgel.

According to the first the method of the invention, the particles of the chemical microgel obtained by carrying out the following stages:

a) get in the aqueous phase chemical gel by polymerization of one or more selected monomers and cross-linking agent or by chemical cross-linking of the polymer after polymerization,

b) the obtained gel is crushed to obtain particles of chemical microgel.

It should be clarified that the polymers that form the particles of the chemical microgel, mainly produced by radical polymerization, however, you can successfully use other types of polymerization, for example, anionic or cationic polymerization.

Can also be used depending on the monomers, polymerization by migrating groups or polymerization by opening of a cycle (for example, in the case of the polymerization of cyclic N-carboxyanhydride).

Preferably, the polymers are obtained by carrying out at least one stage of radical polymerization to obtain a living polymer.

As examples of the polymerization method, called controlled polymerization or polymerization with obtaining living polymers can in particular be mentioned:

the methods described in applications WO 98/58974, WO 00/75207 and WO 01/42312 that use a radical polymerization agent control type xanatos,

- the way of radical polymerization, controlled with the help of agents of type complex ditiberio is, as described in the application WO 98/01478,

the method described in the application WO 98/03894, in which the polymerization is carried out in the presence of precursors of nitroxides,

- the way of radical polymerization, controlled with the help of agents of type dithiocarbamato described in the application WO 99/31144,

- how radical polymerization controlled by agents of type dithiocarbonates described in the application WO 02/26836,

- how radical polymerization controlled by agents of type complex dithiophosphoric esters described in the application WO 02/10223,

the method described in the application WO 96/30421 in which carry out radical polymerization by transferring atoms (ATRP),

- how radical polymerization controlled by agents, chain transfer, which is described Otu et al., in Makromol. Chem. Rapid. Commun., 3, 127 (1982),

- how radical polymerization controlled by degenerative transfer of iodine, which is described Tatemoto et al., in Jap. 50, 127, 991 (1975), Daikin Kogyo Co Ltd Japan and Matyjaszewski et al., in Macromolecules, 28, 2093 (1995),

- the way of radical polymerization, controlled derivatives tetraphenylmethane unveiled D.Braun et al., in Macromol, Symp. 111, 63 (1996), or

- how radical polymerization controlled by complexes of organocobalt described Wayland et al., in J. Am. Chem. Soc. 116, 7973 (1994).

If the polymers, which form particles of chemical microgel, have a modular structure, the polymerization reaction for them is Holocene prefer to spend in the presence of at least one agent control, in particular, compounds of the type xanatos, dithiocarbamates, complex ditiberio.

If the polymers do not have a modular structure, acceptable conventional radical polymerization (i.e., no agent control).

In accordance with the first variant of this method of implementation, the polymer that forms the particles of chemical microgel, obtained by polymerization in the aqueous phase of one or more selected monomers, and at least one cross-linking agent. In this case, the polymerization and the stitching takes place simultaneously.

As monomers used monomers listed above in the description of polymers.

Used crosslinking monomers contain at least two functions, which are reactive in the selected method of polymerization. In the case of radical polymerization using at least one monomer containing at least two ethylene communication, but not more than 10 ethylene linkages, which are known as reactive in radical polymerization.

Preferably, such monomers contain two ethylene communication. You can, for example, to specify derivatives: acrylic, methacrylic, acrylamide, methacrylamide, vinyl ester, simple vinyl ether, diene, styrene, alpha-methylstyrene and allyl.

The monomers belonging to these with whom mastam, are vanillacream, anhydride methacrylic acid, alismataceae, dimethacrylate of ethylene glycol, phenylenediacrylate, diethylene glycol dimethacrylate, triethylene glycol dimethacrylate, dimethacrylate of tetraethyleneglycol, dimethacrylate of polyethylene glycol 200 dimethacrylate of polyethylene glycol 400, 1,3-butanediol dimethacrylate, 1,4-butanediol dimethacrylate, 1,6-dimethacrylate of hexanediol, 1,12-dimethacrylate dodecanediol, 1,3-glycerol dimethacrylate, dimethacrylate of diurethane, trimethacrylate of trimethylolpropane. Family of multifunctional acrylates include, for example, vinylacetat, diacrylate bisphenol a epoxy, diacrylate dipropyleneglycol, diacrylate tripropyleneglycol, diacrylate of polyethylene glycol 600, diacrylate of ethylene glycol, diacrylate diethylene glycol, diacrylate triethylene glycol, diacrylate tetraethyleneglycol, the ethoxylated diacrylate neopentyl glycol, diacrylate butanediol, diacrylate of hexandiol, aliphatic diacrylate urethane, triacrylate of trimethylolpropane, ethoxylated triacrylate of trimethylolpropane, propoxycarbonyl triacrylate of trimethylolpropane, propoxycarbonyl triacrylate glycerol, aliphatic triacrylate urethane, tetraacrylate of trimethylolpropane, pentacarinat of dipentaerythritol. From vinyl ethers may be mentioned, in particular, vinylketones, simple divinely the ether of diethylene glycol, simple divinely ether of butanediol-1,4, simple divinely ether of triethylene glycol. As allyl derivatives can, in particular, to call diallylphthalate, chloride of diallyldimethylammonium, diallylmalonate, nutritionrelated, diallylphthalate, diallylmalonate, diallylamine, N,N'-diallylammonium, N,N'-diallyl-2,2,2-triptorelin, allyl ether dialysateusual acid, 1,3-dellicarpini, triallylamine, triallylamine, treelistener, triallylamine, triallyl-1,3,5-triazine-2,4,6(1H,3H,5H)Trion. Of the derivatives of acrylamide, in particular, can be called N,N'-methylenebisacrylamide, N,N'-methylenebismethacrylamide, glocalisation, diarylethylene acid. As the styrene derivatives include, for example, divinylbenzene and 1,3-diisopropenylbenzene. From diene monomers can, in particular, to call butadiene, chloroprene and isoprene.

Of cross-linkable monomers, preferred are N,N'- methylenebisacrylamide, divinylbenzene and diacrylate of ethylene glycol.

In addition, a specialist can easily determine the amount of cross-linking agent depending on the desired degree of crosslinking and taking into account the fact that particles of chemical microgel were water-soluble or water-dispersible, in the sense as described above, to obtain the microgel high quality.

Reactualization carried out in the presence of at least one source of free radicals. Such a radical polymerization initiator can be chosen from classical initiators usually used in radical polymerization, namely:

- hydrogen peroxides, such as tertiary hydroperoxide, butyl, cumene hydroperoxide, trebucheeeeeet, trebucheeeeeet, trebucheeeeeet, trebucheeeeeet, trebotivishta, peroxide of lauroyl, Tretiakova, trebucheeeeeet, peroxide of Dicumyl, benzoyl peroxide, potassium persulfate, ammonium persulfate,

- azo compounds such as 2,2'-azobis(isobutyronitrile), 2,2'-azobis(2-butanetriol), 4,4'-azobis(4-valeric acid), 1,1'-azobis(cyclohexanecarbonitrile), 2-(trebuchet)-2-cyanopropyl, 2,2'-azobis[2-methyl-N-(1,1 bis(hydroxymethyl)-2-hydroxyethyl]propionamide, 2,2'-azobis(2-methyl-N-hydroxyethyl)propionamide, 2,2'-azobis(N,N'-dimethylaminopyridine)dichloride, 2,2'-azobis(2-amidinopropane)dichloride, 2,2'-azobis(N,N'-dimethylaminobutyric), 2,2'-azobis(2-methyl-N-[1,1-bis(hydroxymethyl)-2-hydroxyethyl]propionamide), 2,2'-azobis(2-methyl-N-[1,1-bis(hydroxymethyl)ethyl]propionamide), 2,2'-azobis[2-methyl-N-(2-hydroxyethyl]propionamide), 2,2'azobis(isobutyramide)dihydrate,

- redox systems containing such combinations as mixtures of hydrogen peroxide and similar compounds with one or more salts is elesa, salts containing trivalent titanium, etc. and reducing sugars; persulfates, perborate or perchlorate of alkali metals or ammonium, in combination with the alkali metal bisulfate and reducing sugars; persulfates of alkali metal in combination with arylphosphine acid and reducing sugars.

Usually the amount of the initiator such that the quantity of the formed radicals was not more than 50 mol.%, preferably not more than 20 mol.% in relation to the amount of polymer or agent of control.

The temperature may vary from room temperature to 150°depending on the nature of the monomers used.

Mainly the polymerization is carried out in aqueous solution.

In accordance with a second embodiment of the first method embodiment of the invention, the polymer that forms the particles of chemical microgel is obtained by polymerization in the aqueous phase of one or more monomers selected from the subsequent stage of the knitting of the specified polymer (composition after polymerization).

At this stage you can use cross-linking agents mentioned above.

Conditions for the exercise of knitting the same reaction conditions, polymerization, except that it does not enter the agent's control.

So, the stitching is carried out in the presence of at least one initiator, the rich the content is that the formed radicals are not more than 50 mol.%, preferably not more than 20 mol.% in relation to the number of polymer.

It should be clarified that depending on the nature of the monomers forming the polymer, cross-linking may be carried out by reacting the functional groups of the polymer between them. For example, it may be the esterification reaction or transesterification.

In this case, the polymer can enter the catalysts inherent in these reactions, such as acids and bases.

In accordance with another variant of the cross-linking of polymers can be performed by the multifunction depolymerizing compounds containing at least one chemical group, opposite to the group or groups contained in the stitched polymer. For example, you can use dologite connection for cross-linking of the polymer containing at least one block of poly(2-dimethylaminoethylacrylate) or glutaraldehyde for cross-linking of the polymer type, polyvinyl alcohol, etc.

The polymer is recovered from the reaction mixture in the traditional way, for example by precipitation in herstorical.

Once the polymer, crosslinked chemically derived, it is crushed.

This operation is carried out in the traditional way. For this you can use a regular grinder, and ultrasound.

Usually is on such an operation is carried out, when the polymer is in the form of a dispersion in herstorical. This operation is carried out for a time sufficient to obtain srednekamennogo particle size of from 0.3 μm to 10 mm, preferably from 1 to 1000 μm, and more preferably from 1 to 100 microns.

In accordance with the second method of implementation of the particles of the chemical microgel obtained by polymerization of one or more selected monomers and cross-linking agent in microreactors and/or mixing and/or in the presence of at least one of the limiter circuit, or by chemical crosslinking after polymerization in micro-reactors and/or in the conditions of mixing of a polymer obtained by polymerization of one or more monomers selected.

It should be clarified that the polymer that forms the particles of chemical microgel can be obtained by polymerization in microreactors and/or in the conditions of mixing.

All of the above regarding the nature of the monomers, cross-linking agents, the presence or absence of agent control, remains in force in relation to the second method of implementation; the difference lies essentially in how to carry out the polymerization reaction and possibly joining.

As for the limiter circuit, it may be selected from transfer agents radicals, for example, compounds like thiols (see Sherrington, Poymer, 41 (2000)), or of the agents control type nitroxide (see D. H. Solomon and coll. Macromol. Rapid Commun. 18, 755 (1997) and Polymer 42, 5987 (2001)). The use of these agents prevents the formation of macroglia.

The purpose of the second method of implementation is the possibility of obtaining particles of chemical microgel without the implementation stage grinding of the polymer. To achieve this goal the polymerisation process is carried out either in microreactors, or in conditions of mixing, or in the presence of the limiter circuit, or a combination of these options.

More specifically, the microreactors are droplets of the emulsion, which in this case is the inverse emulsion (water in oil).

The implementation of the emulsion polymerization is not for professionals any difficulties.

More specifically, the organic phase comprises an organic solvent that is not miscible with water and inert under the reaction conditions. As examples of the solvent can be called hexane, heptane, isoparaffin fraction, etc.

In addition, the organic phase of the emulsion further comprises at least one surface-active substance.

Preferably, the surfactant is chosen from those which are soluble, at least partially in the organic phase of the emulsion.

Mainly surfactants that can be used in the EBM method implementation more specifically, selected from non-ionic surfactants with low products HLB (hydrophilic-lipophilic balance) (in particular, less than or equal to 8).

Acceptable are alkoxysilane fatty alcohols, alkoxysilane triglycerides, alkoxysilane fatty acids may alkoxysilane esters sorbitan, alkoxysilane fatty amines; number alkoxysilane links (ethoxylated, oxypropylene, oxybutylene) is that the products HLB value less than or equal to 8. It should be noted that the polymerization reaction can also be carried out using amphiphilic polymer to stabilize the inverse emulsion, alone or in mixture with one or more of the above surfactants.

As examples of such polymers can, in particular, to call triple polyhydroxystearic-glycol-polyhydroxystearic polymers (for example, products group Arlacel ICI).

In accordance with the preferred method of implementation of the inverse emulsion contains an amphiphilic polymer or a mixture of several of such polymers.

The total amount of surfactants and/or amphiphilic polymer is preferably from 2 to 10 wt.% from the oil phase.

If the polymerization is carried out in conditions of mixing, topramezone should be sufficient to shift the reaction mixture thus to obtain the length of the polymer.

It should be noted that the possible combination of these two methods.

Finally, you can stage crushing of the particles obtained in the above stage, without leaving the scope of the invention.

The second component of the mixture according to the invention is bridging polymer. It is water-soluble or water-dispersible polymer having a chemical nature different from the chemical nature of the particles of the microgel, which are described above.

It should be clarified that bridge the polymer has the chemical composition (nature)that is different from the composition of the microgel particles, since the General structure of the polymers differ by the nature of the repeating units, or the corresponding proportions of the recurring units.

In addition, bridging polymer and particles of chemical microgel is associated at least partially reverse way. Indeed, the composition comprising bridging polymer and particles of the microgel has such rheological characteristics that the difference between the initial viscosity and viscosity after processing by applying shear forces for 5 minutes at a speed of 100-1measured after curing of the composition within 24 hours, or below 50%, preferably lower than or equals to 20% of the initial viscosity.

As was the decree is but higher the number of bridging polymer is such that the viscosity of the composition is at least three times greater than the viscosity of an aqueous solution of the particles of the chemical microgel and exceeds the viscosity of an aqueous solution bridging polymer under the same conditions (concentration, temperature). Preferably, the viscosity of the composition is at least 10 times higher than the viscosity of an aqueous solution of the particles of the chemical microgel and exceeds the viscosity of an aqueous solution bridging polymer under the same conditions.

Bridging polymer, more specifically, consists of at least one polymer, molecular weight mass is between 103to 5,107g/mol, more specifically, from 104up to 107g/mol, preferably from 5,105to 5,106g/mol. These molar weight weight determined according to the method of MALLS(multi-angle light scattering) in combination with gel permeation chromatography.

In accordance with a preferred characteristic of the invention used bridge the polymer has a linear structure, possibly containing grafted side chains grafted molecules).

In accordance with the first variant of the invention bridging polymer is produced at least from hydrophilic monomers, non-ionic, ionic or potentially an ionisable and possibly from hydrophobic monomers.

As hydrophilic and hydrophobic monomers, by mentioning is mentioned above, you can refer to the lists, which list such monomers described above in connection with the description of the polymers, which are particles of a chemical gel.

You can call different methods of polymer synthesis, meaning that bridge polymers are not crosslinked compounds. Therefore, a crosslinking agent, preferably, do not enter during or after receipt of these polymers.

Bridging polymer is selected depending on the nature of cross-linked polymer, which gives the fraction of a chemical microgel, and so was the interaction between the two compounds, i.e. bridge between the polymer and the particles of the chemical microgel.

For example, if you want to obtain particles of the chemical microgel and bridging polymer, United through interaction with the electrostatic nature of this polymer is chosen such that the total charge of the particle chemical microgel was opposite to the General charge bridging polymer. More specifically, if the particles of the chemical microgel containing anionic units, bridging polymer is chosen so that some of its recurring units had the cationic or potentially cationic charges (e.g., pH, when using the composition).

Preferably, the bridging polymer has a degree of Polym the polarization of the charged monomers from 5 to 10.

Preferably, in the case of this kind of interaction is at least 50 %, preferably at least 80% of the number of monomers forming the polymer chain bridging polymer and particles of chemical microgel, have no ionic charge.

In accordance with another characteristic of the particle chemical microgel bridge and the polymer are linked through interactions hydrophobic-hydrophobic communication. In this case, particles of the chemical microgel and bridge the polymer contains units that are able to associate in aqueous phase through such links.

As an example, interactions of this type can be called the Association of microgel particles containing a long alkyl chain (for example, C8-C22and above)associated with the bridging polymer type alkylacrylate containing, for example, from 8 to 22 or more carbon atoms.

In accordance with the second characteristic of the particles of the chemical microgel bridge and the polymer are linked through interactions hydrogen bonds. In this embodiment, particles of the chemical microgel and bridge the polymer contains units that are able to associate in aqueous phase by means of such relations (e.g., carboxyl links and/or amide and links of simple ether and/or alcohol and/or amine).

In this case, the bridging polymer and particles of chemical micro is the appropriate fields contain groups for example, carboxylic acid, alcohol, simple ester, amide.

In accordance with a second embodiment of the invention, the bridging polymer contains at least one polymer selected from chemically modified or unmodified biopolymers.

In accordance with this option, the biopolymers are selected from polysaccharides such as galactomannan, glucomannan, succinogenes, xanthan gum, cellulose, alginates, gelatin, whether or not chemically modified.

The choice of biopolymer (non-ionic, hydrophobic, anionic, cationic) depends on the chemical nature of the particles of the microgel, and implement it in such a way that the interaction between particles and bridging polymer were of the type listed above, namely, electrostatic interaction, hydrophobic-hydrophobic, type hydrogen bonds.

The composition according to the invention can be obtained by carrying out the following stages:

a) receiving in the aqueous phase chemical gel by polymerization of one or more selected monomers and cross-linking agent or by chemical cross-linking of the polymer after polymerization,

b) grinding the obtained gel to obtain particles of chemical microgel,

in an introduction to a contact in the aqueous phase of these particles chemical microgel and at least one is about bridging polymer.

According to other variant composition was prepared by carrying out the following stages:

a) obtaining particles of chemical microgel by the polymerization of one or more desired monomers and cross-linking agent in microreactors and/or mixing and/or in the presence of at least one of the limiter circuit, or by chemical cross-linking of the polymer after polymerization carried out in microreactors and/or in the conditions of mixing,

b) introducing into contact with the aqueous phase of these particles chemical microgel and at least one bridging polymer.

In each of these two options the first two stages have already been described in detail in the description of the polymers, which are particles of chemical microgel.

With regard to the latter stage, it is carried out by simple mixing of bridging polymer and particles of chemical microgel.

The invention relates also to the use of the composition described above, in the development of oil and gas fields, in the field of detergents, cosmetics, metal processing (transformation and deformation), as a rheological agent or an agent capable of stabilizing the viscosity.

Finally, the last object of the invention is the products that contain the specified composition; the products are designed for so the x areas as the development of oil and gas fields, detergents, cosmetics.

Below, specific examples are not restrictive.

Example 1

Synthesis of microgel PAA/RNEA

Stage 1: synthesis of block copolymer PAA-b-RNEA (polyacrylic acid-b-polyhydroxyethylmethacrylate)5000-b-30000

The synthesis of the first block

In a three-neck flask equipped with a fridge, a magnetic stirrer and a heating bath, put on 30 mg of acrylic acid (AA), 1,255 gAbout-ethyl-S-(1-methoxycarbonyl)Etiler)xanthate (CH3SNCO2CH3)S(C=S)OEt, 0,147 g AIBN and 125 ml of acetone. The medium is heated to 70°C for 20 hours. The solvent is evaporated in vacuum and the polymer was dried in vacuum until a constant mass.

Srednekamennogo molar mass (Mn) measured steric exclusion chromatography (SEC)using a calibration with linear standards PAA.

Mn=4300 g/mol.

Synthesis of disloca

In a three-neck flask equipped with a fridge, a magnetic stirrer and a heating bath, placed 10 mg polyacrylic acid (PAA) with xanthan end group, as described above, 74 g of distilled water and 148 g of acetone.

The medium is heated to 70°C for 30 minutes

At 70°With injected continuously 69,8 g hydroxyethylacrylate (NEA) for 2 h 45 min and immediately (in "shot") 0,076 g azoisobutyronitrile (AIBN). Through DV is the hour, and then after four hours from the beginning of introduction of the monomer introduced two portions of AIBN in 0,076 g each. Heated and stirred for 16 hours.

The final dry extract was 26.4 wt.%.

Stage 2: cross-linked block copolymer

The above copolymer solution was incubated for 30 days at 40°in the drying chamber. Using light scattering, and then conventional microscopy keep in time with the formation of microgels.

Preparation of a gel

Receive an aqueous solution containing 3.2 wt.% obtained microgel with a pH equal to 7 (installed using water molar sodium hydroxide solution).

Get a water solution containing 0,82% cationic polymer, Glokill PQ (manufactured by Rhodia Chimie). Bring the solution pH to 7 using sodium hydroxide solution.

Then get water mixture by mixing equal amounts of a and B.

Also received a mixture of A' and B' by the corresponding dual cultivation of solutions a and b water (with a constant pH 7)

MixtureViscosity*(PA·)
A'<0,1
In'<0,1
C10

*viscosity was measured using a viscometer of type Carrimed, with the geometry of the cone-plane; the measurements were carried out at 25°when the gradient of the engines with 1 -1.

Example 2:

Synthesis of microgel PAA/Pam

Stage 1: synthesis of block copolymer PAA-b-PAm (polyacrylic acid-b-polyacrylamide)5000-b-60000

The synthesis of the first block

In a three-neck flask equipped with a fridge, a magnetic stirrer and a heating bath, a place of 7.7 g of acrylic acid (AA), 0.32 g of O-ethyl-S-(1-methoxycarbonyl)Etiler)xanthate (CH3SNCO2CH3)S(C=S)OEt and 0.22 g of 4,4'-azobis(4-cyanovalerianic acid), 2.5 g of isopropanol and 16.7 g of water. The medium is heated to 70°C for 6 hours.

Take a sample and measure it srednekamennogo molar mass (Mn) steric exclusion chromatography (SEC)using a calibration with linear standards PAA.

Mn=4500 g/mol.

Synthesis of disloca

The polymer from stage 1, the temperature of which support equal to 70°add 92,3 g of acrylamide, 0.21 g of 4,4'-azobis(4-cyanovalerianic acid) and 215,8 g of water. Wednesday heated for 6 hours.

Take a sample and measure it srednekamennogo molar mass (Mn) Mn=49000.

Stage 2: synthesis of microgel-based PAA and Pam.

10 g of two-block copolymer with stage 1 diluted with water to a concentration of 12%. 1.18 g of N,N'-methylenebisacrylamide and 20 g of 4,4'-azobis(4-cyanovalerianic acid) is introduced into the solution dibaca. The mixture is then heated to 70°C for 5 hours.

Obtained in this way, the product forms a transparent p is the target in the water. It could not be filtered using a filter for GPC hole size 0.45 µm, which proves the formation of microgel.

Preparation of a gel

Receive an aqueous solution containing 6 wt.% obtained microgel with pH 7 (adjusted with aqueous molar solution of sodium hydroxide).

Get a water solution containing 1.6% of the cationic polymer, Glokill PQ (manufactured by Rhodia Chimie). the pH of the solution In the set is equal to 7 using sodium hydroxide solution.

Then get water mixture by mixing equal amounts of a and B.

Also received a mixture of A' and B' by the corresponding dual cultivation of solutions a and b water (with a constant pH 7)

MixtureViscosity*(PA·)
A'<3
In'<3
C>10

*viscosity was measured using a viscometer of type Carrimed, with the geometry of the cone-plane; the measurements were carried out at 25°when the gradient shift with 1-1.

Note. The term "bridging polymer" means the polymer, which connects at least two particles of the chemical microgel with the formation of a "bridge" between the two particles.

1. Aqueous composition containing particles of a chemically cross-linked in rastvorimogo or water-dispersible chemical microgel, associated with at least one bridging water-soluble or water-dispersible polymer, the chemical composition different from the chemical composition of these particles, and the number of particles chemical microgel is from 0.05 to 40% dry matter by weight of the composition, and the number of bridging polymer is such that the viscosity of the composition is at least greater than three times, preferably greater than or equal to ten times the viscosity of the aqueous solution of the particles of the chemical microgel and exceeds the viscosity of an aqueous solution bridging polymer under the same conditions.

2. The aqueous composition according to claim 1, characterized in that the number of particles chemical microgel is from 0.05 to 10% dry matter by weight of the composition, preferably from 0.1 to 5% dry matter by weight of the composition.

3. The aqueous composition according to claim 1, characterized in that the number of bridging polymer is such that the mixture of particles of chemical microgel and bridging polymer is a water-soluble or water-dispersible.

4. The composition according to claim 1, characterized in that the number of water-soluble units of the specified polymer is at least 50% of the number of units of the polymer, preferably at least 80 wt.% from the polymer.

5. The composition according to claim 1, characterized in that srednesemennyh the particle size of the chemical microgel extending t is from 0.3 μm to 10 mm, preferably from 1 μm to 1000 μm, more preferably from 1 μm to 100 μm.

6. The composition according to claim 1, characterized in that the bridging polymer consists of at least one polymer, theoretical weight molar mass is from 103up to 5·107g/mol, more specifically from 104up to 107g/mol, preferably from 5·105up to 5·106g/mol.

7. The composition according to claim 1, characterized in that the polymers, which are particles of chemical microgel, and bridging polymer is produced at least from hydrophilic monomers, non-ionic, ionic or potentially an ionisable and possibly hydrophobic.

8. The composition according to claim 1, wherein the non-ionic hydrophilic monomers may be selected from ethylene oxide; amides of mono - and polycarboxylic acids, linear, branched, cyclic or aromatic, containing at least one ethylene linkage, or derivatives thereof, such as (meth)acrylamide, N-methylol(meth)acrylamide; some esters, derivatives of (meth)acrylic acid, for example, 2-hydroxyethyl(meth)acrylate; vinyl esters, allowing to obtain blocks of polyvinyl alcohol after hydrolysis, for example, vinyl acetate, vinyl Versatate®, finalproject, N-vinylpyrrolidone, separately or in a mixture.

9. The composition according to claim 1, characterized in that Jonny is or potentially ionic hydrophilic monomers are selected from anionic or potentially anionic monomers, containing at least one carboxylic, sulfonic, sulfuric, phosphonic, phosphoric, sulfonterol group, the corresponding salts or their respective predecessors.

10. The composition according to claim 1, characterized in that the anionic or potentially anionic monomers selected from mono - and polycarboxylic acids, linear, branched, cyclic or aromatic, N-substituted derivatives of such acids, monoamino polycarboxylic acids containing at least one ethylene linkage; vinylcarbazole acids, linear, branched, cyclic or aromatic; amino acids containing one or more ethylene ties; individually or in a mixture, sulfonic or phosphonic derivatives, macromonomers derived from such monomers, salts or precursors of such monomers.

11. The composition according to claim 1, characterized in that the hydrophilic ionic or potentially ionic monomers selected from the following cationic or potentially cationic monomers: aminoalkyl(meth)acrylate, aminoalkyl(meth)acrylamide; monomers containing at least one secondary, tertiary or Quaternary amino group or a heterocyclic group containing a nitrogen atom, vinylamine, ethylenimine; ammonium salts diallyldimethyl; separately or in mixtures, as well as macromonomers derived so the x monomers, salts of these monomers.

12. The composition according to claim 1, characterized in that the hydrophilic ionic or potentially ionic monomers contain one or more amphoteric and/or zwitterionic monomers.

13. The composition according to claim 1, characterized in that the polymers, which are polymer particles and bridging the connection, receive at least from a hydrophobic monomer selected from propylene oxide, butylene oxide; esters of mono - or polycarboxylic acids, linear, branched, cyclic or aromatic, containing at least one ethylene linkage, αβ-Ethylenediamine NITRILES, vinyl ethers, vinyl esters; vinyl aromatic monomers, vinyl halides or vinylidene; hydrocarbon monomers, linear, branched, aromatic or non-aromatic, containing least one ethylene linkage, separately or in mixtures, as well as macromonomers derived from these monomers.

14. The composition according to claim 1, characterized in that the bridging polymer contains at least one polymer selected from biopolymers, chemically modified or unmodified.

15. The composition according to claim 1, wherein the biopolymers are selected from polysaccharides such as galactomannan, glucomannan, succinogenes, xanthan gum, cellulose, and igenity, gelatin, chemically modified or unmodified.

16. The composition according to claim 1, characterized in that the particles of the chemical microgel and bridge the polymer bound by electrostatic interactions, and the total charge of the particle chemical microgel total opposite charge bridging polymer.

17. The composition according to claim 1, characterized in that the particles of the chemical microgel and bridge the polymer bound by hydrophobic interactions hydrophobic type, and particle chemical microgel and bridge the polymer contains units that are able to associate in aqueous phase with the help of these links.

18. The composition according to claim 1, characterized in that the particles of the chemical microgel bridge and the polymer are linked by interactions, hydrogen bonds, and particle chemical microgel and bridge the polymer contains units that are able to associate in aqueous phase with the help of these links.

19. A method of obtaining a composition described in any one of claims 1 to 18, characterized in that carry out the following stages:

a) get in the aqueous phase chemical gel by polymerization of one or more selected monomers and cross-linking agent or by chemical cross-linking of the polymer after polymerization,

b) grind the obtained gel to obtain particles of chemical microgel,

C) in water f the se enter into contact with these particles the chemical microgel at least one bridging polymer.

20. A method of obtaining a composition described in any one of claims 1 to 18, characterized in that carry out the following stages:

a) receive particles of chemical microgel by the polymerization of one or more selected monomers and cross-linking agent in microreactors and/or mixing and/or in the presence of at least one of the limiter circuit or by chemical crosslinking in microreactors and/or mixing after polymerization of the polymer,

b) in the aqueous phase is introduced into the contact of these particles chemical microgel at least one bridging polymer.

21. The use of a composition described in any one of claims 1 to 18 or obtained by the method according to one of claim 19 or 20, in the development of oil or gas fields.

22. The use of a composition described in any one of claims 1 to 18 or obtained by the method according to one of claim 19 or 20, in the field of detergents.

23. The use of a composition described in any one of claims 1 to 18 or obtained by the method according to one of claim 19 or 20, in cosmetics.

24. The use of a composition described in any one of claims 1 to 18 or obtained by the method according to one of claim 19 or 20, in the field of metal.

25. Products containing composition described in any one of claims 1 to 18 or obtained by the method according to one of claim 19 or 20, intended for use in the development of the oil is, or gas fields, the field of detergents, cosmetics.



 

Same patents:

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SUBSTANCE: method of preparing controlled-size microgels, which can be used in oil and gas wells to prevent water inflow, consists in introducing polymer and suitable crosslinking agent into porous and permeable medium. Passage and passage velocity of polymer and crosslinking agent are controlled such as to provide crosslinking of polymer to form microgel aggregates in porous and permeable medium and to control sizes of aggregates leaving this medium. Removed solution contains microgel aggregates essentially equal in size.

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3 cl, 1 tbl, 8 ex

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Water dispersion // 2183646
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FIELD: polymer production.

SUBSTANCE: invention provides composition for preparation of gradient hydrogel polymer material based on copolymers of acrylamide and N,N'-methylene-bis-acrylamide representing following system: (i) mixture of dilute solution containing 2-3% acrylamide, 0.1-0.2% N,N'-methylene-bis-acrylamide, 0.01% ammonium persulfate, and, as viscosity regulator, 0.5-2.0% glycerol or 1:1 mixture of glycerol and polyvinyl alcohol, each taken in amount 3.5-8.0%, in bidistilled water and (ii) and concentrated solution containing 6-45% acrylamide, 0.6-1.0% N,N'-methylene-bis-acrylamide, and 0.04% ammonium persulfate in bidistilled water, said dilute solution constituting 75-80% and said concentrated solution 20-25% of the total weight of the system. Components are distributed in gradient manner in final system. Invention also discloses a method of preparing gradient hydrogel polymer material based on above-indicated copolymers and indicated gradient hydrogel polymer material. Value and direction of gradient of modulus of elasticity of hydrogel polymer materials is controlled by concentration of viscosity regulator.

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3 cl, 1 tbl, 8 ex

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SUBSTANCE: invention relates to a method for applying onto wood substrate coating with increased resistance to effects of chemical products. Method comprises following stages: (i) addition, to aqueous polyatomic alcohol suspension, of composition based on isocyanate(s) and anionic surfactant having hydrophilic portion containing anionic group and lipophilic portion containing hydrocarbon radical, isocyanate(s)-based composition containing no more than 30% surfactant bound to isocyanate group, to form aqueous emulsion of isocyanate(s) and surfactant; (ii) applying resulting mixture onto wood surface of substrate; and (iii) aging to complete reaction of isocyanate(s) with polyatomic alcohol required to form polyurethane coating.

EFFECT: increased strength of coating (at a level of 90 units) and acquired resistance to a variety of chemical, cosmetic, and woof products according to corresponding standard.

18 cl, 4 dwg, 5 ex

FIELD: chemical compositions, polymers.

SUBSTANCE: invention relates to aqueous compositions comprising particles of chemically cross-linked water-soluble or water-dispersed chemical microgel. Invention proposes an aqueous composition comprising particles of chemically cross-linked water-soluble or water-dispersed chemical microgel bound with at least one bridge water-soluble or water-dispersed polymer wherein its chemical composition differs from chemical composition of indicated particles. The amount of chemical microgel particles is from 0.05 to 40% dry mass of the composition mass, and the amount of bridge polymer provides exceeding the viscosity value of the composition by at least three times or preferably it exceeds or equal to 10-fold viscosity value of chemical microgel particles an aqueous solution, and exceeds viscosity value of the bridge polymer an aqueous solution under the same conditions. Also, invention proposes a method for preparing of the claimed an aqueous composition. Proposed composition can be used in the field for mining petroleum and gas deposits, and in manufacturing detergents and cosmetics also. Invention provides enhancing stability of the composition.

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25 cl, 2 tbl, 2 ex

FIELD: polymer materials.

SUBSTANCE: invention, in particular, relates to hydrophobically modified water-soluble polymers or complexes of the latter with surfactants and discloses a method for selectively inhibiting gelation of hydrophobically associating gel-forming liquid containing hydrophobically associating water-soluble polymers or complexes of the latter with surfactants. Advantage of invention resides in that, when thus inhibited liquid contacts with a hydrocarbon medium, inhibitory effect is preserved and gelation does not occur and, when liquid contacts with an aqueous medium, inhibitory effect is cancelled and gelation takes place. Inhibitor is selected such that it is well soluble in aqueous media but insoluble in hydrocarbon media, for example ethanol or methanol. Hydrophobically associating substance in associating gel-forming liquid is, in particular, hydrophobically modified water-soluble polymer based on polyacrylamide containing 84.4 or 88.8 mol % acrylamide units, 1.5 mol % n-dodecylacrylamide units, and 14.1 or 9.7 mol % sodium acrylate units. Surfactant used in polymer complexes is, in particular, cetylpyridinium chloride. Invention further discloses associating gel-forming liquid containing 1 to 10% by weight of hydrophobically associating substances and also composition for treating oil well, which comprises associating liquid. Disclosed is also a method for selectively blocking water entry into producing oil well from underground water-bearing formations. Invention can thus be used in oil production to control water inflows in oil-production well allowing restriction of water entry into well without unfavorably affecting oil production process.

EFFECT: facilitated gelation control in polymer-containing liquids.

4 cl, 2 dwg, 1 tbl

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